Title of Invention

A PROCESS OF PREPARATION OF ARSENIC SELECTIVE MEDIA

Abstract

In the present invention under consideration, provides an efficient method for the preparation of a high performance adsorbent material for arsenic and phosphate ions starting with inexpensive materials to have hydrated ferric oxide as the active substance supported in a large amount on polymeric structure of anion exchange resin which is insoluble in water or elution of iron is zero. The adsorbent material obtained according to the method of the present invention under consideration is useful for the adsorption of the arsenic trivalent and the pentavalent arsenic and the phosphate ions selectively without alternating the water quality parameters from the groundwater.

Full Text

FORM-2 THE PATENTS ACT, 1970 (39 of 1970) AND THE PATENTS RULES, 2003 COMPLETE SPECIFICATION (See Section 10; Rule 13) 1. TITLE OF THE INVENTION; "A Process of Preparation and Synthesis of Arsenic Selective Media." 2. APPLICANT: (a) NAME: ION EXCHAGE (INDIA) LIMITED. (b) NATIONALITY: AN INDIAN COMPANY INCORPORATED UNDER THE COMPANIES ACT, 1956. (c) ADDRESS: TIECICON HOUSE, DR. E. MOSES ROAD, MAHALAXMI, MUMBAI-400 011, MAHARASHTRA, INDIA. The following specification describes the nature of the invention and the manner in which it is to be performed: - A PROCESS OF PREPARATION AND SYNTHESIS OF ARSENIC SELECTIVE MEDIA 3. PREAMBLE TO THE DESCRIPTION Field of Invention The present invention relates to a process of preparation and synthesis of arsenic selective media. Background of the Invention & the Related Art Arsenic contamination is a very serious problem in the underground waters in Eastern parts India (West Bengal) and Myanmar. The normal concentration of arsenic is around 0.1 to 1.5 ppm. The excess intake of arsenic leads to various skin diseases like hyper pigmentation, keratoses melanomas that disfigure the skin like in leprosy also it causes to cardiovascular, renal, hematological, respiratory disorders and cancer and gangrene. The entire population of 5.31 millions of West Bengal is continuously living under the threat of arsenic contamination. Arsenic contamination is also found in the underground waters in some other countries too, like, the central European countries viz. Poland, Belgium & Hungary, the South & Central American countries viz. Argentina, Chile & Mexico, the Asian countries viz. Japan, Vietnam, Taiwan, Thailand & China. Some mining areas of U.S.A. too the underground water is seriously contaminated by arsenic. -2- As per the World Health Organization's (WHO), the current provisional guidelines, the allowable level of arsenic in the drinking water is at 0.01 ppm and as per the previous guidelines the same was at 0.050 ppm. However, the developing countries like India are still finding it quite difficult even to follow the previous guidelines and reduce the arsenic level in the drinking water at 0.05 ppm. Keeping in view the above difficulties & shortcomings in view the invention under consideration. 4. DESCRIPTION OF THE INVENTION The invention under consideration aims to provide an efficient method for the preparation of an adsorbent loaded hydrated ferric oxide in a high loading and with a remarkable resistance against the leaking from the supporting carrier material to ensure a good durability of the adsorbent material with a stable adsorption capacity Thus , the method of the present invention under consideration for the preparation of a high adsorbent ferric oxide loaded polymer structure comprises the following step of: • Bringing a porous carrier material having pores into the contact with the ferric salt. • The ferric salt is impregnate on porous polymer matrix • Drying the porous material to a porous carried material loaded with an iron compound by contacting with ether/alcohol with sufficient time. -3- • Bringing the dried porous material into the contact with an aqueous alkaline solution to hydrolyze the iron compound. • Subjecting the porous material supporting the hydrolyzed ferric compound to a oxidation treatment at 35-50 degree with strong oxidant. • Hydrated ferric oxide thus formed on polymer structure base. THE DETAIL DESCRIPTION OF THE PREFERRED EMBODIMENTS: An iron compound as the starting material of the inventive method is the ammonium ferric sulphate or the ammonium ferric nitrate. These compounds can be either used singly or in the combination of both. The alcoholic solvent used in the process is preferable a lower alcohol like, methyl, ethyl and propyl alcohol. The polymeric material is also not particularly limitative, the porous ion exchange resin based on the crosslinked matrix with various porocities. The various types of anion exchange resin like isoporous, gel and macro porous type I and type II in beads of particle size in range of 50(0.297mm) to 14(1.41mm) US standard. In practicing the method of the present invention under consideration, a porous carrier material is brought into the contact with the ferric salt with an excess amount to impregnate iron compound upto matrix structure. Thus, the carrier material after the drying treatment of alcohol solution, the concentration of an iron -4- compound on the matrix is as high as possible because amount of iron compound supported matrix can be enriched. In the next place, the obtained iron compound impregnated polymer carrier structure compound and freed from the alcoholic solvent into contact with an aqueous solution of alkaline compound such as sodium hydroxide, potassium hydroxide, ammonium hydroxide though not particularly limitative, so that, an iron compound is hydrolyzed and is converted to the hydrated ferric oxide which is insoluble in the water. The concentration of alkaline solution is usually in the range of 8-40% by weight. The hydrolysis reaction proceeds at an increased rate as the concentration of the alkaline compound is increased. It is not always necessary to conduct the hydrolysis at an elevated temperature since the reaction can be proceed at a moderate rate, even at the room temperature. The hydrolysis reaction usually takes 1-2 hours or the duration depends on the concentration of the alkali compound and the reaction temperature. A further step to follow the above described hydrolysis reaction is the removal of an excess alkali compound and the oxidation with an air, oxygen, hydrogen peroxide, etc. It is preferable to have pH 5-8 at 30-40°C for at least 3 hours or preferably 8-20 hours or preferably at the temperature 45-60°C for at least for 15 hours in a corrosion-resistant reactor. As describe above, the present invention under consideration, provides an efficient method for the preparation of a high performance adsorbent material for arsenic and phosphate ions starting with inexpensive materials to have hydrated ferric oxide as the active substance supported in a large amount on polymeric structure of anion exchange resin which is insoluble in water or elution of iron is zero. -5- The adsorbent material obtained according to the method of the present invention under consideration is useful for the adsorption of the arsenic trivalent and the pentavalent arsenic and the phosphate ions selectively without alternating the water quality parameters from the groundwater. In the method of present invention under consideration for the preparation of an adsorbent material is described in more detail by way of the following examples which, however, never limit the scope of the invention in any way Application Example No. 1: 100 gm of ferric salt dissolved in 500 ml of deminerilized water, 150 gm of beads of the crosslinked polystyrene anion exchange isoporous resin (INDION FFIP) stirred for 2 hours for the removal of the excess ferric salt and dried with the methyl alcohol for three hours. Evaporate the alcohol at 35-40°C and deep the resin in 8-10% alkali solution for3-4 hours till pH gets alkaline. Removes the excess alkali and treat the beads with the potassium permanganate. The adjusted final pH 7-8. The media has tested for Arsenic Adsorption capacity (ADC). The ADC is 0.7 gm/liter. Application Example No.2: 200 gm of ferric salt dissolved in 500 ml of demineralized water, 200 gm of beads of the crosslinked anion type II(NIP) resin stirred for 2 hours for the removal of the excess ferric salt and dried with the ethyl alcohol for 8-12 hours. Evaporate the alcohol at 35-40°C and deep the resin in 8-10% alkali solution for 3-4 hours till pH gets alkaline. Removes the excess alkali and treat the beads with the potassium permanganate. The adjusted the final pH 10. The media has tested for Arsenic Adsorption Capacity (ADC). The ADC was 0.4 gm/liter. -6- Application Example No. 3: 175 gm of ferric salt dissolved in 500 ml of demineralized water, 300 gm of beads of the crosslinked matrix anion resin (INDION FFIP) stirred for 2 hours and the estimated percent (%) acidity and the chloride of the elute water. Remove the excess of the ferric salt and dry the same with an ethyl alcohol for 8-12 hours. Evaporate the alcohol at 35-40°C and deep the resin in 8-10% alkali solution for 3-4 hours till pH gets alkaline. Removes the excess alkali and observed arsenic affinity of the media. The media has tested for Arsenic Adsorption Capacity (ADC). The ADC was 1.399 gm/liter. Application Example No.4 175 gm of ferric salt dissolved in 500 ml of demineralized water, 300 gm of beads of the crosslinked anion type-1 macroporous resin (INDION 810) stirred for 2 hours and the estimated percent (%) acidity and the chloride of the elute water. Remove the excess of the ferric salt and dry the same with an ethyl alcohol for 8-12 hours. Evaporate the alcohol at 35-40°C and deep the resin in 8-10% alkali solution for 3-4 hours till pH gets alkaline. Removes the excess alkali and is fethet treated with the hydrogen peroxide and adjusted the final pH of resirv was 5-6. The media has tested for Arsenic Adsorption Capacity (ADC). The ADC was 1.654gm/liter. Application Example No.5: A 200 gm bead of the weak base anion resin (INDION 850) in the hydroxide form is treated with the ferrous salt and the salt of sodium and potassium (8-10%) for three hours. Remove the excess salt and further treatment was given with 8-10% -7- potassium permanganate for 8-10 hours. Maintained the final pH 5-6 of finished resin and estimated Arsenic Adsorption Capacity (ADC). The ADC was 0.205 gm/liter. 5. We claim: 1. A process of preparation and synthesis of arsenic selective media. 2. A process of preparation and synthesis of arsenic selective media as claimed in claim 1, using an iron compound as the starting material being the ammonium ferric sulphate or the ammonium ferric nitrate being either used singly or in the combination of both. 3. A process of preparation and synthesis of arsenic selective media as claimed in claims 1 & 2, using the alcoholic solvent preferably being a lower alcohol like, methyl, ethyl and propyl alcohol. 4. A process of preparation and synthesis of arsenic selective media as claimed in claims 1, 2 & 3, using the polymeric material not being particularly limitative, the porous ion exchange resin based on the crosslinked matrix with various porocities being used. 5. A process of preparation and synthesis of arsenic selective media as claimed in claims 1, 2, 3 & 4, using various types of anion exchange resin like isoporous, gel and macro porous type I and type II in beads of particle size in range of 50(0.297mm) to 14(1.41mm) US standard. 6. A process of preparation and synthesis of arsenic selective media as claimed in claims 1, 2, 3, 4 & 5, under which bringing a porous carrier material having pores into the contact with the ferric salt & the ferric salt being impregnate on porous polymer matrix & further drying the porous material to a porous carried material loaded with an iron compound by contacting with ether/alcohol with sufficient time, then, bringing the dried -9- porous material into the contact with an aqueous alkaline solution to hydrolyze the iron compound, further, subjecting the porous material supporting the hydrolyzed ferric compound to a oxidation treatment at 35-50 degree with strong oxidant and hydrated ferric oxide thus formed on polymer structure base. -10- 7. A process of preparation and synthesis of arsenic selective media as claimed in claims 1, 2, 3, 4, 5 & 6 providing an efficient method for the preparation of a high performance adsorbent material for arsenic and phosphate ions starting with inexpensive materials to have hydrated ferric oxide as the active substance supported in a large amount on polymeric structure of anion exchange resin which being insoluble in water or elution of iron is zero. 8. A process of preparation and synthesis of arsenic selective media as claimed in claims 1, 2, 3, 4, 5, 6 & 7, under which the adsorbent material being obtained according to the method of the present invention under consideration being useful for the adsorption of the arsenic trivalent and the pentavalent arsenic and the phosphate ions selectively without alternating the water quality parameters from the groundwater.

Documents:

1227-MUM-2009-ABSTRACT(29-10-2012).pdf

1227-mum-2009-abstract.doc

1227-mum-2009-abstract.pdf

1227-MUM-2009-CLAIMS(AMENDED)-(29-10-2012).pdf

1227-mum-2009-claims.doc

1227-mum-2009-claims.pdf

1227-MUM-2009-CORRESPONDENCE(IPO)-(30-9-2009).pdf

1227-mum-2009-description(complete).doc

1227-mum-2009-description(complete).pdf

1227-mum-2009-form 1.pdf

1227-MUM-2009-FORM 13(19-6-2013).pdf

1227-MUM-2009-FORM 18(19-5-2010).pdf

1227-mum-2009-form 2(title page).pdf

1227-mum-2009-form 2.doc

1227-mum-2009-form 2.pdf

1227-mum-2009-form 3.pdf

1227-MUM-2009-REPLY TO EXAMINATION REPORT(29-10-2012).pdf

1227-MUM-2009-SPECIFICATION(AMENDED)-(29-10-2012).pdf