Title of Invention

"AN IMPROVED PROCESS FOR REDUCTION OF TOTAL DISSOLVED SOLIDS FROM SPENT WASH OF DISTILLERY"

Abstract This invention related to an improved process for the reduction of total dissolved solids (TDS) from spent wash of distillery. More particularly the invention is related to an improved process for the reduction of total dissolved solids from spent wash of distillery using natural adsorbent. The process does not involve use of expensive chemicals or enzymes thus it is cost effective and does not involve any use of special equipment thus it is easy to handle. The process end products are not hazardous in nature, thus it is an eco-friendly process.
Full Text This invention related to an improved process for the reduction of total dissolved solids (IDS) from spent wash of distillery.
More particularly the invention is related to an improved process for the reduction of total dissolved solids from spent wash of distillery using natural adsorbent. Most of the industrial waste water treatment processes are found to be effective in reducing BOD as well as COD, but not TDS of the effluent. Intern, these processes add total dissolved solids in the effluent. Thus it is observed that industrial processes along with effluent treatment processes generate lot of total dissolved solids which when let out in the natural stream result, in the increase of dissolved solids in the river bed. This ultimately leads to the pollution of the drinking water sources and also soil degradation. The major contaminants due to the industrial wastewater in surface and ground water sources vary with the types of industry. Total Dissolved Solids (TDS) can be defined as, the concentration in milligram of distinct molecular & ionic species together per liter of the effluent. The TDS generating pollutants include the raw materials, process chemicals, process intermediates and by products like :
l.Organics that deplete the oxygen content and impose a great load on the biological units.
2.Inorganics like carbonates, chlorides, sulfates and nitrogenous compounds encourages the growth of undesirable biola in the body of the water. 3.Acid alkali streams that are unsuitable for the growth of aquatic life. 4.Toxic substances like sulfates, cyanides, alcohols etc. which may cause damage to flora and fauna. The methods generally employed to reduce TDS from the effluents are as follows:
Chemical Precipitation, Evaporation, Ion-Exchange, Membrane Filtration involving Dialysis, Microfiltration, Ultrafiltration, Reverse osmosis, Pervaporation and Electrodialysis
The alcohol industry popularly known as distillery, in India is based on molasses as the principal raw material. Molasses contains around 15% of fermentable sugars, out of which 9% is utilized for conversion into alcohol during fermentation. The balance sugar along with organic & inorganic chemicals in the molasses find their way into the effluent popularly known as spent wash which is acidic in nature. Spent wash which is dark in color has high BOD,COD & TDS. The origin of dark color is mainly due to plant pigments, melanoidins, polyphcnolic compounds and caramels which are produced by thermal degradation and condensation reactions of sugar. The main constituents of the TDS of the spent wash are as follows : Reducing sugars - 1.20%, Sulphated ash - 3 to 4%, Dry matter 9 to 11%, Carbonated ash 3 to 3.5%, aluminum and iron oxide 0.05%, magnesium oxide 0.3%, phosphorus pentoxide 0.03%, potassium oxide 1.2%, nitrogen 0.12 to 0.20%, sulphate 0.80%, free sulphur 0.70% and chlorine 0.60%, potassium metabisulphite and potassium sulphite 0.5% and sodium sulphite 0.5%.
In order to conform to environmental quality guidelines a number of primary and secondary treatment systems such as clarifiers, aerated lagoons, trickling filters, biomethanation and other biological systems are installed. All these treatments remove reasonably good amount of COD,BOD but not color toxicity and inorganic impurities. Due to stringent environmental norms such partially treated effluents of distillery are not allowed to be mixed in the natural stream. In the prior art the following methods are used to reduce TDS of effluents Several methods hitherto used are described in brief herein bellow :
Bacterial cultures in treatment of industrial waste containing toxic organic compounds.
Pandya, M. T. (Dep. Microbiol., Jaihind Coll., Mumbai 400 020, India). Proc. -WEFTEC '97, Water Environ. Fed. Annu. Conf. Expo., 70th, Volume 7, 269-279. Water Environment Federation: Alexandria, Va. (English) 1997. CODEN: 66SHAP. DOCUMENT TYPE: Conference CA Section: 60 (Waste Treatment and Disposal) CA 129:320258
Pandya has shown the versatility of metabolic routes offers exciting possibilities for biol. research and biotechnol., both in the exploration of the metabolic/evolutionary potentials in microorganisms and in the development of innovative application in treatment of wastewater contg. toxic org. compds. Strains of Pseudomonas, Nocardia, Micrococcus, Bacillus, and Rliodococcus were isolated from soil and sludge samples by using the enrichment culture cultivation technique. The nutrient balance maintained in effluents were in ratio of 100:10:1 for COD:N:P and at pH 7-8. Mixed cultures of these strains showed >95% redn. in COD of effluents contg. amines and their derivs. The plant-scale trials showed a redn. in COD from 3000 ppm to 100 ppm in 24 h in effluent supplemented with only phosphoric acid and at pH -7-8. In effluents contg caprolactam and spin finish oils, a redn. in COD from 6000 ppm to 200-300 ppm in 72 h was obsd. The treated effluent, after sand and carbon filtration, was reused in cooling towers. Pseudomonas and Nocardia strains showed complete removal from seawater of 1000 ppm phenol and 1% crude oil in 72 h. The degraded oil showed significant changes with regard to phys. and chcm. properties. Mixed culture of Bacillus, Pseudomonas, and Micrococcus showed excellent growth in effluents from bulk drug manuf. under anaerobic and aerobic condition; the COD redns. were 70-78%
at total dissolved solids of 8-10%. Some of these bioaugmented cultures are
successfully used for treatment of effluents in industries.
Recycling of water in bleached kraft pulp mills by using electrodialysis.
Tsai, Shih-Perng; Pfromm, Peter; Henry, Michael P.; Fracaro, Anthony T. (CORPORATE SOURCE Argonne National Laboratory, Argonne, IL 60439, USA). Proc. - TAPPI Int. Environ. Conf, Volume 2, 831-838. TAPPI Press: Atlanta, Ga. (English) 1999. CODEN: 67VSAC. DOCUMENT TYPE: Conference CA SECTION/CROSS-REFERENCE(S) CA Section: 60 (Waste Treatment and Disposal) Section cross-reference(s): 43, 61, CA 131:120127 Tsai et al reported conservation of water in bleached kraft pulp mills by recycling the bleach plant effluent directly without treatment will cause accumulation of inorg. non-process elements (NPEs) and serious operational problems. An electrodialysis process is developed for recycling the acidic bleach plant wastevvater of bleached kraft pulp mills. Electrodialysis functions as a selective kidney to remove inorg. NPEs from bleach plant effluents. Acidic bleach plant effluents from several mills using bleaching sequences based on C102 were characterized. The total dissolved solids were mostly inorg. NPEs. Na was the predominant cation and chloride was present at significant levels in all these effluents. In lab. electrodialysis expts., selective removal of chloride and potentially harmful cations, such as K, Ca, and Mg, were removed efficiently. Rejection of org. compds. was £98%. Electrodialysis was resistant to membrane fouling and scaling, in a 100-h lab. expt. Based on a model mill with 1000 ton/day pulp prodn., the economic anal, suggests that the energy cost of electrodialysis is Total dissolved solids removal from water produced during the in situ recovery of heavy oil and bitumen.
Kok, S.; Zaidi, A.; Solomon, R. (Wastewater Technol. Cent., Environ. Canada, Burlington, ON, Can.). J. Can. Pet. Technol., 28(1), 100-5 (English) 1989. CODEN: JCPMAM. ISSN: 0021-9487. DOCUMENT TYPE: Journal CA Section: 60 (Waste treatment and Disposal) Section cross-reference(s): 51, 61, CA 111:28074
Kok et al reported that total dissolved solids were removed from produced water from recovery of heavy oil and bitumen by steam flooding or steam stimulation by vapor-compression evapn. in a steam-heated evaporator of length 4.6 m, outside diam. 50.8 mm, and wall thickness 6.3 mm at a feed flow rate of 19 L/h with total dissolved solids levels of 12,000-64,000 mg/L and oil and grease concns. of 10-310 mg/L. The produced water recoveries were 67-93%, and the obsd. heat-transfer coeffs. were 3650-4050 W/m2-K. A preliminary est. indicated that the capital cost would be approx. S8.9 million (1986 Canadian dollars) for a plant treating 3800 m3/day of produced water, with estd. annual operating costs of SI.2-1.9 million, depending on the produced water characteristics and the mode of operation of the evaporator.
Separation of hazardous organics by low presure membranes: treatment of soil-wash rinse water leachates.
Bhartacharyya, D.; Kothari, A. (Dep. Chem. Eng., Univ. Kentucky, Lexington, KY, USA). Report, EPA/600/R-92/035; Order No. PB92-153436, 141 pp. Avail. NITS From: Gov. Rep. Announce. Index (U. S.) 1992, 92(11), Abstr. No. 229,173 (English) 1992. DOCUMENT TYPE: Report CA Section: 60 (Waste Treatment and Disposal) Section cross-reference(s): 19, CA 119:145816
Low-pressure, thin-film composite membranes were evaluated to treat soil-wash leachates so that treated water could be recycled back to the soil washing step. Expts. were done with SARM (synthetic Anal. Ref. Matrix) soils. Membrane performance was evaluated with leachates obtained from different wash solns. The effect of fine suspensions in leachates was also studied. A soln.-diffusion model was modified to include an adsorption resistance term in water flux; this term was correlated with bulk concn. using the Freundlich isotherm. The correlation was used to predict water flux drop at different bulk concns. or to predict water flux at different recoveries. Thin-film composite membranes effectively treated leachate from rinse water used to wash contaminated soil. In addn., feed preozonization significantly improved water flux.
Water reuse in the pulp and paper industry: evaluation of four microfiltration applications.
Silva, Claudio M.; Reeve, Douglas W.; Woodhouse, Kim; Husain, Hadi; Behmann, Henry (Department of Chemical Engineering and Applied Chemistry, Pulp and Paper Centre - University of Toronto, Toronto, ON M5S 1A4, Can.). Int. Environ. Conf. Exhib., Volume Bk. 3, 1035-1044. TAPPT Press: Atlanta, Ga. (English) 1998. CODEN: 66BYAP. DOCUMENT TYPE: Conference CA Section: 43 (Cellulose, Lignin, Paper, and Other Wood Products) Section cross-reference(s): 60 CA 129:42457
Silva et al have shown four potential applications for microfiltration membrane processes in the recycling of specific liq. streams in pulp and paper mills. Each type of effluent was tested on a bench scale device: (1) old newsprint (ONP) de-inking effluent contg. flexog. ink; (2) effluent from a paper coating operation; (3) effluent from a bleached chemithermomech. pulp (BCTMP) mill; and (4) effluent from a
board mill using recycled old corrugated container (OCC). The 1st 3 were tested using a submerged microfiltration module, and the last using a submerged microfiltration membrane bio-reactor. The microfiltration of ONP de-inking effluent completely removed flexog. ink. The quality of the permeate was suitable for recycling to the paper mill. It was possible to cone, the effluent from the paper coating operation to a consistency of 16.5%, removing 96% of the original water. The retention of suspended solids by microfiltration led to very good permeate quality. The integration of both the retentate and the permeate into the paper mill process is feasible. Although the microfiltration membrane retains the suspended solids in the BCTMP effluent, the permeate contains high levels of total dissolved solids which are not removed. Further treatment is required in order to allow the integration of this stream into the process. By treating OCC effluent using a membrane bio-reactor (MBR), overall removal of COD and BOD5 of 95% and 99%, resp., was achieved. The quality of the final effluent meets requirements for recycling this stream into the process. Removal of phosphate ion from water.
Hamano, Seiichi; Yamam'shi, Osamu (Sumitomo Chemical Co, Japan). Jpn. Kokai Tokkyo Koho JP 07163975 A2 27 Jun 1995 Heisei, 5 pp. (Japan). CODEN: JKXXAF. CLASS: ICM: C02F001-28. ICS: B01D015-00; C02F001-58. APPLICATION: JP 93-314790 15 Dec 1993. DOCUMENT TYPE: Patent CA Section: 61 (Water) Section cross-reference(s): 60, CA 123:208373 Hamono et al has studied that the process consisted of contacting phosphate-contg. water with acid-coated activated A1203 adsorbents having sp. surface area 3100 m2/g and showing pH 3-6 in water at 80°. Preferably, the acids are HC1, HF,
HN03, H2SO4, and/or AcOH. The process is useful for removal of phosphate
from (waste)water.
Adsorption of disperse dye by various adsorbents.
Lin, Sheng H. (Dep. Chem. Eng., Yuan-Ze Inst. Technol., Taoyuan 32026, Taiwan). J. Chem. Technol. Biotechnol., 58(2), 159-63 (English) 1993. CODEN: JCTBED. ISSN: 0268-2575. DOCUMENT TYPE: Journal CA Section: 60 (Waste Treatment and Disposal) Section cross-reference(s): 41 CA 119:233104 Lin Sheng had conducted a lab. investigations of C.I. Disperse Red 60 adsorption on mol. sieves, activated alumina, granular activated C (GAC), diatomite, and sawdust. The effectiveness of these adsorbents to remove pollution and reduce the color of disperse dye was examd. and compared with that of powd. activated C (PAC). Activated alumina has only 61% COD removal efficiency in comparison with PAC, whereas those of mol. sieves, GAC, and diatomite are much lower. In terms of color removal, activated alumina and mol. sieves are as effective as PAC while GAC, diatomite, and sawdust are much less effective. The monolayer Langmuir isotherm represented well the measured adsorption data; the const, adsorption isotherm parameters were detd. for all adsorbents. The simplified mass transfer model proposed previously was also used to est. mass transfer coeffs. using the initial adsorption data for several adsorbents.
Nutrient and metal content of water, sediment and soils amended with bauxite residue in the catchment of the Peel Inlet and Harvey Estuary, Western Australia.
Summers, R. N.; Pech, J. D. (Agriculture Western Australia, Community Catchment Centre, PO Box 376, Pinjarra, W.A. 6208, Kampala, Australia). Agnc., Ecosyst. Environ., 64(3), 219-232 (English) 1997 Elsevier CODEN: AEENDO.
ISSN: 0167-8809. DOCUMENT TYPE: Journal CA Section: 19 (Fertilizers, Soils, and Plant Nutrition) Section cross-reference(s): 61 CA 127:318482 Summers et al had studied that the Peel Inlet and Harvey Estuary in Western Australia are susceptible to algal blooms fed by phosphorus in run-off. The surrounding catchment is dominated by sandy soils which do not retain phosphorus. Bauxite residue, the alk. byproduct from the extn. of alumina from bauxite with caustic soda, has been applied to the soil to increase the phosphorus retention and improve the soil. This study examines the effectiveness of bauxite residue in retaining phosphorus and also the impact of bauxite residue on other water quality parameters. Water, sediment and soils from sites amended or not amended with bauxite residue were analyzed to establish the effect of bauxite residue and the background levels of heavy metals. Bauxite residue was applied at 20 ton ha-1 to 1600 ha of a 4300 ha catchment and the phosphorus concn. in drainage water dropped by more than 30% in the first year. A 32 ha sandy catchment was treated with 80 ton h-1 bauxite residue and it maintained a 75% lower phosphorus concn. than an adjacent untreated catchment over 4 yr. The phosphorus concn. in the effluent from a domestic sewage treatment plant was reduced by an av. of 88% over two years after infiltration through a sand bed amended with bauxite residue. No difference was detected between the water quality of catchments amended with bauxite residue and comparable catchments, based on concns. of a no. of heavy metals. High levels of heavy metals were found in some areas, unrelated to bauxite residue, mainly in the downstream receiving waters of the catchment. This was probably related to byproducts of combustion and motor vehicle emissions.
Treatment of phosphates in effluent produced by elutriation of activated alumina used for phosphate adsorption for secondary treated wastewater.
Nakamura, Takeshi; Ota, Mitsunobu (Unitika Ltd., Japan). Jpn. Kokai Tokkyo
Koho JP 09085263 A2 31 Mar 1997 Heisei, 4 pp. (Japan). CODEN: JKXXAF.
CLASS: ICM: C02F001-58. APPLICATION: JP 95-250744 28 Sep 1995.
DOCUMENT TYPE: Patent CA Section: 60 (Waste Treatment and Disposal)
Section cross-reference(s): 19 CA 127:23117
Nakamura et al have shown that the title effluents are treated by mixing with
returned wastewater (from dewatering of digestion sludge) for controlling
[NH4+]/[P043-] to be 31, adding Mg compds. for controlling [Mg2+]/[P043-] also
to be 31, adjusting the resultant mixt. at pH 7.5-10, and stirring for recovery and
removal of P043- as NH4MgP04 (MAP) particles. Not less than 80% of P043- in
the effluent is removed and MAP solid particles with good pptg. property and
useful as a fertilizer are produced without requiring addnl. NH4 addn.
Spoiled alumina as an adsorbent.
Bokade, S. S.; Thergaonkar, V. P.; Deshkar, A. M. (Natl. Environ. Eng. Res. Inst.,
Nagpur 440 020, India). Indian J. Environ. Health, 32(4), 383-8 (English) 1990.
CODEN: UEHBP. ISSN: 0367-827X. DOCUMENT TYPE: Journal CA Section:
60 (Waste Treatment and Disposal) Section cross-reference(s): 17, 43 CA
115:141671
Bokade et al have shown that spoiled alumina from the A1(OH)3 manufg. plants
was activated at 400° and used for adsorption treatment of wastewater from paper
mill and dairy plants. Results showed COD and color removals of 84 and 99%,
resp.
Treatment of phosphates in effluent produced by elutriation of activated alumina used for phosphate adsorption for secondary treated wastewater.
Nakamura, Takeshi; Ota, Mitsunobu (Unitika Ltd., Japan). Jpn. Kokai Tokkyo
Koho JP 09085263 A2 31 Mar 1997 Heisei, 4 pp. (Japan). CODEN: JKXXAF.
CLASS: ICM: C02F001-58. APPLICATION: JP 95-250744 28 Sep 1995.
DOCUMENT TYPE: Patent CA Section: 60 (Waste Treatment and Disposal)
Section cross-refercncc(s): 19 CA 127:23117
Nakamura et al have shown that the title effluents are treated by mixing with
returned wastewater (from dewatcring of digestion sludge) for controlling
[NH4+]/[P043-] to be 31, adding Mg compds. for controlling [Mg2+]/[P043-] also
to be 31, adjusting the resultant mixt. at pH 7.5-10, and stirring for recovery and
removal of P043- as NH4MgP04 (MAP) particles. Not less than 80% of P043- in
the effluent is removed and MAP solid particles with good pptg. property and
useful as a fertilizer are produced without requiring addnl. NH4 addn.
Spoiled alumina as an adsorbent.
Bokade, S. S.; Thergaonkar, V. P.; Deshkar, A. M. (Natl. Environ. Eng. Res. Inst,
Nagpur 440 020, India). Indian J. Environ. Health, 32(4), 383-8 (English) 1990.
CODEN: IJEHBP. ISSN: 0367-827X. DOCUMENT TYPE: Journal CA Section:
60 (Waste Treatment and Disposal) Section cross-reference(s): 17, 43 CA
115:141671
Bokade et al have shown that spoiled alumina from the A1(OH)3 manufg. plants
was activated at 400° and used for adsorption treatment of wastewater from paper
mill and dairy plants. Results showed COD and color removals of 84 and 99%,
resp.
Neutralization of wastewaters using solid agents.
Kessel, Bemhard (Fed. Rep. Ger.). Ger. Offen. DE 3838701 Al 9 Aug 1990, 6 pp.
(Germany) CODEN: GWXXBX. CLASS: ICM: C02F001-66. ICS: B01D053-34;
F23J015-00. APPLICATION: DE 88-3838701 15 Nov 1988. DOCUMENT
TYPE: Patent CA Section: 60 (Waste Treatment and Disposal) Section cross-
reference(s): 59 CA 113:197167
Kessel Bernhard had studied the wastewaters, e.g., flue gas condensates, are
neutralized by passage through a granular or powd. neutralizing material which is
loaded in a plastic mesh or similar container. The containers can be replaced easily
when exhausted. Preferably the wastewaters flow into the side of the charge, which
is placed in a close-fitting basin inside a vessel. The treated effluent overflows the
basin into the vessel and exits via an offtake pipe low in the opposite side of the
vessel.
Reuse of alumina after treatment of wastewater containing fluorides.
Hattori, Takeo; Tatsumoto, Hideki (Fac. Eng., Chiba Univ., Chiba 260, Japan).
Chem. Express, 5(7), 509-12 (English) 1990. CODEN: CHEXEU. DOCUMENT
TYPE: Journal CA Section: 60 (Waste Treatment and Disposal) Section cross-
reference(s): 49 CA 113:84222
Takeo et al have shown that the sintering of alumina used for the treatment of F--
contg. wastewater was studied for reuse. This alumina could not be densified
because of swelling. The sintering of mixt. (2/1, 1/1, and 1/2) of this powder and
virgin alumina was densified without any swelling.
Composite inorganic gel-organic polymer adsorbents.
Robinson, Eric (UK). PCT Int. Appl. WO 8908500 Al 21 Sep 1989, 12 pp.
DESIGNATED STATES: W: JP, NO, US; RW: AT, BE, CH, DE, FR, GB, IT,
LU, NL, SE. (World Intellectual Property Organization) CODEN: PIXXD2. CLASS: ICM: B01J020-28. APPLICATION: WO 89-GB245 10 Mar 1989. PRIORITY: GB 88-6605 19 Mar 1988. DOCUMENT TYPE: Patent CA Section: 48 (Unit Operations and Processes) Section cross-reference(s): 38, 60, 61, 66, 67, CA 112:9382
Robinson has reported that, the adsorbents have org. polymer intimately distributed throughout the inorg. gel of Si02 and/or A12O3. The polymer is starch, dextran/ chitosan, CMC, Na CMC, poly(vinyl ale.), etc, The polymer is added to a precursor of the inorg. sol or to the inorg. sol. before gelation, and the gel is aged for 2-48 h. The invention adsorbents are used in liq. effluent treatment, for the removal of heavy metals and other toxic materials, in the treatment of potable water, in sepn. processes and ion exchange, and as biocatalyst and heterogeneous catalyst support.
Purification of a waste stream from a tanning process by adsorption on an adsorbent comprising a mixture of alumina and Y zeolite. Bush, John F.; Fleming, Hubert L. (Aluminum Co. of America, USA). U.S. US 4717483 A 5 Jan 1988, 6 pp. (United States of America) CODEN: USXXAM. CLASS: ICM: C02F001-28. NCL: 210681000. APPLICATION: US 86-877554 23 Jun 1986DOCUMENT TYPE: Patent CA Section: 60 (Waste Treatment and Disposal) CA 108:137369
NH3 and org. impurities are removed from tanning effluents of pH 4-8 by contacting with an adsorbent bed comprising activated A1203 (size 5-10 m) 50-95 and activated Y zeolite (size 300°
for Futagawa, Michio; Matsui, Susumu; Kimoto, Kazuo (Osaka Gas Co., Ltd., Japan). Jpn. Kokai Tokkyo Koho JP 62121697 A2 2 Jun 1987 Showa, 4 pp. (Japan) CODEN: JKXXAF. CLASS: ICM: C02F003-08. APPLICATION: JP 85-259499
19 Nov 1985. DOCUMENT TYPE: Patent CA Section: 60 (Waste Treatment and Disposal) CA 107:120519
Futagawa et al have treated wastewater using microorganism-immobilizing particles in a fluidized bed and then the particles overgrown by immobilized microorganisms are sepd. into microorganisms and particles for their reuse. A portion of the effluent from the sepn. stage in the fluidized bed at the top is mixed with air and sepd. by a static mixer and a liq. cyclone into a gas, microorganisms, and particles. The resulting gas is released from the top of the liq. cyclone, and the sep. microorganisms and particles are recycled and mixed with wastewater at the inlet of the fluidized bed. The use of alk. agents is conserved and the removal of microorganisms is increased from 10% to 30% by this method. Thus, wastewater was treated in a fluidized bed contg. microorganism-immobilizing particles, e.g., activated C, sand, anthracite, plastics, glass, silica gel, or Si02-A1203, at 10,000-15,000 mg/L mixed liquor volatile suspended solids. C02 was released from the top of a cyclone after aeration and the effluent was neutralized with NaOH. The use of NaOH for neutralization was 20% of that by a conventional method without releasing C02 by aeration.
Treatment of organic wastewater.
Takahashi, Hisashi; Futamatsu, Takumi; Miyake, Akihiro (Sumitomo Metal Mining
Co, Ltd, Japan). Jpn. Kokai Tokkyo Koho JP 62042792 A2 24 Feb 1987 Showa,
5 pp. (Japan) CODEN: JKXXAF. CLASS: ICM: C02F001-72. ICS: C02F001-02.
APPLICATION: JP 85-182532 20 Aug 1985. DOCUMENT TYPE: Patent CA
Section: 60 (Waste Treatment and Disposal) Section cross-rcferencc(s): 51 CA
107:102099
Takahashi et al have reported that wastewater contg. org. substances is contacted
with an oxidn. catalyst contg. 31 of Pt, Pd, Ru, Rh, and Ag metals or its oxides at
200-600° under atm. pressure in the presence of an O-contg. gas. The ami. of the
0-contg. gas is preferably greater than or equal to that stoichiometrically required
to oxidize and to decomp. the org. substances. Thus, a coal liquefaction plant
wastewater effluent contg. 20,000 mg/L total org. C (TOC) was injected into a
heated column contg. a PI-A1203 catalyst at 290°, 1866 h-1 liq. space velocity, and
an oxygen equiv. ratio 2.0; the treated wastewater contained 11 mg/L TOC (99.94%
removal).
Advanced treatment of sewage with inorganic adsorbent.
Inoue, Gennosuke; Okabe, Toshiyuki (Zosui Sokushin Cent, Japan). Sangyo to
Kankyo, 13(10), 40-4 (Japanese) 1984. CODEN: SAKADF. ISSN: 0285-5380.
DOCUMENT TYPE: Journal CA Section: 60 (Waste Treatment and Disposal) CA
102:83847
Inoue at al have shown that a Mg compd. and an Al compd. mixt. was calcined at
500-600° to prep. MgOxxA120.nH20, where x = 0-0.25, and MgOxnH20 was
formed on the surface. The resulting adsorbent is regenerated at 550-600° for ~35
min. The adsorbent removes COD, BOD, P043-, Ca hardness, and total silicates at -40, -70, 395.7, -65, and >66.7%, resp. The process may be used for pulp wastewater or molasses prodn. wastewater. Decolorization of reactive dye solutions using complex oxides.
Kaneko, Shoji; Miura, Masataka; Nakamura, Motoshi; Maejima, Yoshio (Dep. Ind.
Chem., Shizuoka Univ., Hamamatsu, Japan). Kankyo Gijutsu, 10(9), 708-9
(Japanese) 1981. CODEN: KAGIDX. DOCUMENT TYPE: Journal CA Section:
60 (Waste Treatment and Disposal) CA 96:11205
Reactive dyes, C.I. Reactive Yellow 2 [50662-99-2] and C.I. Reactive Blue 26
[12225-43-3], were removed with a A1203.MgO adsorbent, and the decolorization
was almost 100% at pH 4-10 in 24 h which was observed by Kaneko et al.
Granular oil adsorbent in waste water.
Sato, Hiroshi; Sugimori, Shuichi; Uchida, Hiroyuki (Mitsubishi Rayon Co., Ltd.,
Japan). Jpn. Kokai Tokkyo Koho JP 54057482 9 May 1979 Showa, 3 pp.
(Japanese). (Japan). CODEN: JKXXAF. CLASS: 1C: B01D015-00; C02C005-02.
APPLICATION: JP 77-124696 18 Oct 1977. DOCUMENT TYPE: Patent CA
Section: 60 (Sewage and Wastes) CA 91:145647
Sato et al have used a tapalgite clay 50-90 and A12O3 gel 10-50% as binder when
mixed, granulated, and heated at 70-250°. Thus, 700 g of clay was kneaded with
20% alumina gel extruded through a 9 mesh metal net, and heated in an air stream
at 200°. Water of 202-3 ppm turbidity contg. turbine oil 20 and nonionic surfactant
1 ppm was passed through the 2 diam. ' 55 cm column (filling d. 0.5) at 4.28 m/h to
decrease to 1-2 ppm turbidity.
Doped alumina for wastewater treatment.
(Kernforschungszentrum Karlsruhe G.m.b.H., Fed. Rep. Ger.). Jpn. Kokai Tokkyo Koho JP 54016388 6 Feb 1979 Showa, 6 pp. (Japanese). (Japan). CODEN: JKXXAF. CLASS: 1C: B01D015-00; C02C005-02. PRIORITY: DE 77-2726192 10 Jun 1977. DOCUMENT TYPE: Patent CA Section: 60 (Sewage and Wastes) Section cross-reference(s): 39 CA 91:62188
A1203 is surface treated with an anion 0.5-10% (optional), then doped with a cation 0.5-10% to prep, an adsorbent for wastcwater treatment. The dopants are 31 alk. earth metal salts, or Fe and/or Cr. The anions arc C1-, N03-, S042-, and phosphates. Thus, a soln. contg. A1(N03)3 and Ca(N03)2 was mixed with a A1(OH)3 soln. to pH 9. The ppts. was aged and sepd., then activated at 500-800° to prep. Ca2+-doped A1203. Wastewater from dyeing contg. 1500 mg C/L was stirred with the 5% Ca-doped A12O3 and the C removal was 100%. Purification of pulp-bleaching waste water with aluminum oxide. Ullrich, H. (Dr. C. Otto und Co., Bochum, Ger.). Prog. Water Technol., 10(5-6), 89-96 (English) 1978. CODEN: PGWTA2. ISSN: 0306-6746. DOCUMENT TYPE: Journal CA Section: 60 (Sewage and Wastes) Section cross-reference(s): 43 CA 90:1093 81
Ullrich has used AI203 to adsorb pulp-bleaching wastewater contaminants such as lignosulfonic acid [8062-15-5], chlorinated lignin, and other lignin compds. Because of stringent regulations at Lake Constance, Germany, a plant was developed for cleaning 240 m3 pulp-bleaching wastewater/h by A1203. The adsorbent, laden with contaminants, is regenerated in a rotary kiln and returned to the adsorption process. The color (lignin components) of the wastewater is reduced from3550tol55mgPt/L
Recycling of waste water from dyehouses after treatment with active alumina.
Hepp, Helmut; Offenbartl, Helmut (Bergheim, Ger.). Melliand Textilber. Int., 59(7), 589-92 (German) 1978. CODEN: MTXIAW. ISSN: 0375-9350. DOCUMENT TYPE: Journal CA Section: 60 (Sewage and Wastes) Section cross-reference(s): 39 CA 89:203537
Helmut & Helmut have showed that wastewater from dyeing polyester and polyamide staple fiber was purified by treatment with Compalex, an activated A1(OH)3 with sp. surface area 200 m2/g and pore vol. 35 cm3/100 g. The influent was acidified with HC1 to pH 2.5 and passed through 3 glass columns contg. A1(OH)3 at 60° to remove 65-80% of the org. matter. Removal of >95% was achieved by passing partially purified wastewater through a column of activated C (0.2 kg/m3 of wastewater).
Purification of pulp bleaching plant effluent with aluminum oxide. Ullrich, Hansjurgen (Dr. C. Otto und Co., Bochum, Ger.). Alkaline Pulping/Second. Fibers Conf., [Pap.], 141-6. TAPPI: Atlanta, Ga. (English) 1977. CODEN: 37HMAR. DOCUMENT TYPE: Conference CA Section: 60 (Sewage and Wastes) Section cross-reference(s): 43 CA 88:176656 Ullrich has observed that the wastes are purified by adsorption and by pptn. on the g-aluminum oxide surfaces; this is achieved by pH control to dissolve the aluminum oxide and then reppt. it. The aluminum oxide is regenerated at ~500° in an oxidizing atm.
In the hitherto known processes main drawbacks are use of bacterial cultures which is time consuming and not easy to operate, processes like electro-dialysis or membrane technology requires lot of energy and hence expensive.

The literature search showed that the Alumina has been used for the treatment of Paper & Pulp effluent, Removal of phosphates from waste water, removal of dyes from dye industry, removal of inorganics from sewage, also organics from waste water and for fluoride removal, but, it has not been used to remove dissolved solids from distillery waste water.
The objective of the present invention is to provide an improved process for the reduction of total dissolved solids from spent wash of distillery.
The process of the present invention reduces TDS at ambient temperature from spent wash from distillery, thus saving energy cost, the operation does not involve any use of mineral acid thus, avoiding any corrosion problems.
The process involves two steps flocculation with mixture of salts of Group III and transition metal along with an oxide of alkaline earth metal followed by the use of alumina as adsorbent.
There is a continued interest on development of new improved process for reduction of TDS produced during the alcohol fermentation. It is well known fact that lignin and TDS in such type of effluents are not easily biodegradable and hence, have disposal problems in the natural environment.
Accordingly the present invention provides an improved process for the reduction of total dissolved solids from spent wash of distillery which comprises mixing spent wash effluent with flocculating agent for a period ranging from 10 -30 minutes, at a temperature in the range of 20 to 30 °C, allowing the effluents to
Accordingly the present invention provides an improved process for the reduction of total dissolved solids from spent wash of distillery which comprises mixing spent wash effluent with flocculating agent such as herein described for a period ranging from 10-30 minutes, at a temperature in the range of 20 to 30°C, allowing the effluents to settle for a period of 3 to 4 hours, separating the supernatant, contacting the said supernatant with a natural adsorbent as herein described and incubating the said mixture for a period of 5 to 30 minutes, at a temperature ranging form 25 to 70°C followed by filtration to obtain the desired IDS reduced effluent.
In an embodiment of the present invention the flocculating agent used is a mixture of sulphate or chloride or nitrate of element selected from Group III elements and transition metals along with an oxide of alkali or alkaline earth metal selected from group I or II elements and also with a small amount of natural earth such as dolomite and bentomite.
In an embodiment of the present invention, wherein the mixture of sulphate of Group III element and transition metal used is preferably a mixture of sulphate of aluminum and iron.
In an another embodiment the oxide of alkali or alkaline earth metal from Group I or II used is sele3cted from the group consisting of oxides of sodium, potassium and magnesium, preferably an oxide of calcium.
In yet another embodiment the natural adsorbent used is selected from the group consisting of alumina, silica gel, carbon, rice husk carbon and brick powder, preferably alumina.
Novelty of the present invention lies is the use of Alumina that has born been used earlier for the reduction of IDS from distillery Spent Wash. The used alumina after activation can be reused as adsorbent, so the process becomes cost effective.
The end products of the process are not hazardous thus process is eco-friendly.
The process of the present invention is described herein bellow with reference to the examples which are illustrative only and should not be construed to the limit of the scope of the present invention in any manner.
Example-1
In the first step of the treatment 400 ml spent wash was diluted with 1600 ml fresh water in a 2 lit beaker to which a flocculent, comprising a mixture of metal salts viz. aluminum sulphate, ferrous sulphate and , dolomite and bentonite (400 mg) in 40 : 5: 5 and calcium oxide (20g) was added, stirred and poured in a two lit. measuring cylinder and incubated for four hours at ambient temperature. The supernate thus obtained was analyzed for its TDS content. The TDS value of the treated sample was found to be 2620 ppm.
Example - 2
The supernate obtained after treating the effluent as mentioned in the Example -1,
(50 ml) was taken in a 100 ml conical flask to which 2.5, 5,7.5,10 and 12.5 gms of
alumina was added and the mixture was incubated for 30min on a mechanical
shaker at 25°C. After incubation the supernatant was decanted and analyzed for its
TDS content. The results were tabulated as follows :
% Pulp Density 5 10 15 20 25
TDS in ppm 1260 980 1060 1080 1200
% Reduction 51.9 62.6 59.5 58.7 54.2
Example - 3
The supernate obtained after treating the effluent as mentioned in the Example -1 , (50 ml) was taken in a 100 ml conical flask to which 5gms of alumina was added and the mixture was incubated for 5, 10, 20,30 and 40 minutes on a mechanical
shaker at 25°C. After incubation the supernate was decanted and analyzed for its
IDS content. The results were tabulated as follows:
Timeinmin. 5 10 20 30 40
TDSinppm 1490 980 1060 1080 1200
% Reduction 43.1 52.6 62.2 62.6 54.9
Example -4
The supemate obtained after treating the effluent as mentioned in the Example -1,
(50 ml) was taken in a 100 ml conical flask to which 5 gms of alumina was added
and the mixture was incubated for30 minutes on a mechanical shaker at 25, 35, 45,
55 and 65°C. After incubation the supernate was decanted and analyzed for its TDS
content. The results were tabulated as follows:
Temperature in0 C 25 35 45 55 65
TDSinppm 980 1230 1030 1210 1180
% Reduction 62.6 53.05 60.1 53.8 54.9
Advantages of the invention are
The present invention involves the treatment of spent wash from distillery to reduce
its TDS content.
The present invention involves reduction of TDS at ambient temperature thus
saving energy cost.
The process does not involve any use of mineral acid, thus avoiding corrosion
problems.
The process does not involve use of expensive chemicals or enzymes thus it is cost
effective.
The process does not involve any use of special equipment thus it is easy to handle.
The process end products are not hazardous in nature, thus it is an eco-friendly
process.



We Claim:
1. An improved process for the reduction of total dissolved solids from spent wash
of distillery which comprises mixing spent wash effluent with flocculating agent
such as herein described for a period ranging from 10-30 minutes, at a
temperature in the range of 20 to 30°C, allowing the effluents to settle for a period
of 3 to 4 hours, separating the supernatant, contacting the said supernatant with a natural adsorbent as herein described and incubating the said mixture for a period of 5 to 30 minutes, at a temperature ranging form 25 to 70°C followed by filtration to obtain the desired IDS reduced effluent.
2. An improved process as claimed intlaim 1, wherein the flocculating agent used is
a mixture of sulphate or chloride or nitrate of element selected from Group III
elements and transition metals along with an oxide of alkali or alkaline earth
metal selected from group I or II elements and also with a small amount of natural
earth such as dolomite and bentomite.
3. An improved process as claimed in claims 1 to 2, wherein the mixture of sulphate
of Group III element and transition metal used is preferably a mixture of sulphate
of aluminum and iron.
4. An improved process as claimed in claims 1-3, wherein the oxide of alkali or
alkaline earth metal from Group I or II used is selected from the group consisting
of oxides of sodium, potassium and magnesium, preferably an oxide of calcium.
5. An improved process as claimed in claims 1-4, wherein the natural adsorbent used
is selected from the group consisting of alumina, silica gel, carbon, rice husk
carbon and brick powder.
6. An improved process for the reduction of total dissolved solids from spent wash
of distillery, substantially described herein before with reference to the examples
accompanying this specification.


Documents:

178-del-2002-abstract.pdf

178-del-2002-claims.pdf

178-del-2002-complete specification (granted).pdf

178-del-2002-correspondence-others.pdf

178-del-2002-correspondence-po.pdf

178-del-2002-description (complete).pdf

178-del-2002-form-1.pdf

178-del-2002-form-18.pdf

178-del-2002-form-2.pdf

178-del-2002-form-3.pdf


Patent Number 242160
Indian Patent Application Number 178/DEL/2002
PG Journal Number 34/2010
Publication Date 20-Aug-2010
Grant Date 17-Aug-2010
Date of Filing 28-Feb-2002
Name of Patentee COUNCIL OF SCIENTIFIC & INDUSTRIAL RESEARCH
Applicant Address RAFI MARG, NEW DELHI-110001, INDIA.
Inventors:
# Inventor's Name Inventor's Address
1 PRAMOD PRABHAKAR MOGHE NATIONAL CHEMICAL LABORATORY, PUNE 411 008, MAHARASHTRA, INDIA.
2 VINITA VINAY PANCHANADIKAR NATIONAL CHEMICAL LABORATORY, PUNE 411 008, MAHARASHTRA, INDIA.
3 ASHWINI VINAYAK POL NATIONAL CHEMICAL LABORATORY, PUNE 411 008, MAHARASHTRA, INDIA.
4 PRAKASH KONDIBA BAHIRAT NATIONAL CHEMICAL LABORATORY, PUNE 411 008, MAHARASHTRA, INDIA.
5 PRIYADARSHINI KUDLU NATIONAL CHEMICAL LABORATORY, PUNE 411 008, MAHARASHTRA, INDIA.
PCT International Classification Number B09B 1/24
PCT International Application Number N/A
PCT International Filing date
PCT Conventions:
# PCT Application Number Date of Convention Priority Country
1 NA