Title of Invention

"A COMPOSITION USEFUL AS AN ACID AND CORROSION RESISTANT COATING AND PROCESS THEREOF"

Abstract This invention relates to a composition useful as an acid and corrosion resistant and process thereof. This invention particularly relates to a composition of coating in which a fraction of machining waste is mixed with the polymeric binder and allied chemicals. This coating can be used to protect concrete, metals etc. from acidic or chemicals vapours/environment against corrosion. This composition utilizes the fine powder obtained from the machining waste of Printed circuit board plant and cashew nut shell liquid. This composition is eco-friendly and helps in utilizing non-degradable industrial waste and can efficiently be used to produce acid and urea resistant coating.
Full Text This invention relates to a composition useful as an acid and corrosion resistant coating and process thereof. This invention particularly relates to a composition of coating in which a fraction of machining waste is mixed with the polymeric binder and allied chemicals. This coating can be used to protect concrete, metals etc. from acidic or chemicals vapours/environment against corrosion.
Manufacturing units of Printed Circuit Board (PCB) generate a huge amount of machining waste which generally contain glass fibers, copper chips, fine powder of silica, epoxy resin and glass fiber. This fine powder creates pollution problem in and around the dumping sides. Through washing and gravity separation, fine powder present in the machining waste could be separated. This powder has potential of being used as filler material for plastics industry. As compared to other filler materials such as calcium carbonate, talk, titanium dioxides etc, this powder has low density due to the presence of around 23% of epoxy resin in it. The reference can be made to technical report on, "Utilization of glass epoxy waste", report No. RRL/PG/GNFC/TR-1, January, 2002 by Regional Research Laboratory, Bhopal.
This fine powder contains cured epoxy resin, glass fibre, fine silica mainly and is unutilized till date except for land filling which is not a solution due to environmental hazards. Secondly, a valuable source is also wasted. There is no literature available about a process or composition related to machining waste of PCB plant for utilization.
The protective coatings available in the market are mainly based on polyurethanes, epoxy, acrylic, alkyds, polyesters etc. These coatings are manufactured for general environmental protection such as water vapours, U V radiation. As far their composition is concerned in addition to base polymeric component, several other ingredients are used with different objectives. Example of these additional chemicals / components are dryer, extender, pigments, flow modifier, wetting agents, catalyst etc. Amongst the various polymeric binders, CNSL (Cashew nut shell liquid) based resins are considered most economical however their application is limited due to their dark brown colour. CNSL based resins are known for their excellent chemical resistance, acid resistance and corrosion resistance properties. Many researchers have developed several surface coatings. Reference can be made to Indian patent 28 (1942) 424, filed by S. Siddiqui and A. A. Khan, Paint Technology 11, (1946) 94 by S. K. Ranganathan & K. G. Tandon, Journal of Scientific and Industrial research 12, B (1953) 411 contributed by H. H. Mathur and J. S. Aggarwal in which the researchers claimed several compositions for various surface coatings by using CSNL. B. B. Choudhary claimed in Indian patent 60, 166 (1957) a corrosion resistant varnish by heating CNSL in presence of Litharge. R. Bhattacharya claimed in Indian patent 66, 370 (1960) that on heating CNSL in Lac at 150°C produces a resinous material which is useful for water proofing. M. T. Harvey
filed several British patents 630220 (1950), 628, 921 (1949) 636, 221(1950) and U S patents 1, 725,793 (1919), 1,939, 301 (1931) 1, 838, 076 (1931), 1,838,077 (1931) claiming several surface coatings by using CNSL. The search results on U S patent also show that no patent has been filed on surface coatings based on CNSL resin onward 1975. There are several patents, which are related to development of friction material by using CNSL.
The true fruit of the cashew tree is the nut, a kidney shaped structure 1-1.5 inch long that is attached to the end of the fleshy receptacle or enlarged peduncle which is generally known as the cashew apple. The pericarp of the nut consists of a coriaceous epicarp, spongy mesocarp and stony endocarp. The kernel covered with testa membrane is contained in a shell 1/8 inch thick. The mesocarp consists of a honey comb network of cells which contain a viscous resinous material called cashenut shell liquid (CNSL) and is a natural protection against insects for the kernel.
Cashew nut shell liquid (CNSL) is traditionally obtained as a by product during the isolation of the kernel.CNSL consists mainly of anacardic acid (90%) and cardol (10%). Commercial CNSL consists of cardanol, cardol, small percentage of anacardic acid and polymerised materials along with trace amounts of gallic acid, glucosides, etc.Accordingly, the present invention provides a composition useful as an acid and
corrosion resistant coating comprising; a polymer material prepared from Cashew
nut shell liquid (CNSL) resin 50 to 95 wt % of total resin, alkyd resin 5 to 50 wt % of total resin and drying oil 02 to 15 wt % of total resin, fine powder of machine waste generated in printed circuit board plant 5 to 55 wt % total resin, thinner 20 to 50 wt % of total resin, mix dryer 2 to 6 wt % of total resin.
Accordingly, the present invention provides also provides a process for preparation of composition useful for making acid and corrosion resistant coating which comprises (i) mixing of cashew nut shell liquid resin 50 to 95 wt % of total resin, alkyd resin 5 to 50 wt % of total resin and drying oil 02 to 15 wt % of total resin, in a mixer for a period in the range of 30 to 120 minutes at a temperature in the range of 150 to 240°C, cooling the mixed material to room temperature , (ii) transferring the matarial obtained in step (i) to a rotary ball mill mixer, adding fine powder of machining waste generated in printed circuit board plant 5 to 55 wt % of total resin, thinner 20 to 50 wt % of total resin and mixing the whole mass for a period in the range of 2 to 24 hours, until a uniform dispersion is obtained , mixing dryer 2 to 6 wt % of total resin for a period in the range of 2 to 10 minutes in the same mixer to obtain coating composition and storing in the air tight containers.
In an embodiment of present invention, the drying oil may be selected from a group consisting of soybean oil, linseed oil, fish oil, rubber seed oil, rung oil, sun flower oil. In another embodiment of the present invention, the fibers and powder can be taken from machining waste of printed circuit board, or other fabrication industries of FRP material. The size of machining waste for this application should be less than 45 micron preferably below 20 microns meter.
In yet another embodiment of present invention, the thinner may be selected from toluene, benzene, methylated spirit, mineral turpentine oil, kerosene or a mixture of any two of the above in the ratio of 1 to 10.
The main object of this invention is to provide a composition useful for making
acid and corrosion resistant coating by using a fraction of machining waste
generated in printed circuit board plant and CNSL resin.
Another object of this invention is to provide a process of making coating material
useful for acid and corrosive environment.
Accordingly, the present invention provides an acid and corrosion resistant
coating composition comprising a polymer matarial [ prepared from CNSL resin
50 to 95 wt % of total resin, alkyd resin 5 to 50 wt % of total resin and drying oil
02 to 15 wt % of total resin ], fine powder of machine waste generated in printed
circuit board plant 5 to 55 wt % total resin.thinner 20 to 50 wt % of total resin,mix
dryer 2 to 6 wt % of total resin.
Accordingly, the present invention provides a process for preparation of
composition useful for making acid and corrosion resistant coating which comprises mixing of cashew nut shell liquid resin 50 to 95 wt % of total resin, alkyd resin 5 to 50 wt % of total resin and drying oil 02 to 15 wt % of total resin, in a mixer for a period in the range of 30 to 120 minutes at a temperature in the range of 150 to 240°C, cooling the mixed material to room temperature , transferring the matarial obtained in step (1) to a rotary ball mill mixer, adding fine powder of machining waste generated in printed circuit board plant 5 to 55 wt % of total resin, thinner 20 to 50 wt % of total resin and mixing the whole mass for a period in the range of 2 to 24 hours, until a uniform dispersion is obtained , then mix dryer 2 to 6 wt % of total resin for a period in the range of 2 to 10 minutes in the same mixer and store in the air tight containers.
In an embodiment of present invention, the drying oil may be selected from a group consisting of soybean oil, linseed oil, fish oil, rubber seed oil, tung oil, sun flower oil.
In another embodiment of the present invention, the fibers and powder can be taken from machining waste of printed circuit board, or other fabrication industries of FRP material. The size of machining waste for this application should be less than 45 micron preferably below 20 microns meter.
In yet another embodiment of present invention, the thinner may be selected from toluene, benzene, methylated spirit, mineral turpentine oil, kerosene or a mixture of any two of the above in the ratio of 1 to 10.
In another embodiment of present invention, the CNSL resin could have
concentration above 40% solid content for this formulation.
In another embodiment the dryer is selected form Cobalt Naphthanate, Lead
Naphthanate and Manganese Naphthanate or a mixture thereof.
The detailed process of making acid and corrosion resistant coating by using a
fraction of machining waste generated in printed circuit board plant is given
below.
A) The mixing of cashew nut shell liquid resin 50 to 95 wt % of total resin alkyd resin 5 to 50 wt % of total resin and drying oil 02 to 15 wt % of total resin, in a mixer for a period in the range of 30 to 120 minutes at a temperature in the range of 150to240°C.
B) The mixed resin ingredients are cooled to room temperature.
C) Then the mix is transferred to a rotary ball mill mixer. The fine powder of machining waste 5 to 55 wt % of resin mix thinner 20 to 50 wt % of total resin mix are mixed.
D) Mixing the whole mass for a period in the range of 2 to 24 hours, until a uniform dispersion is obtained.
E) Then mix the dryer/dryers 2 to 6 wt % of total resin for a period in the range of
2 to 10 minutes in the same mixer.
F) Store the mix in an airtight container.
CNSL resin and alkyd resin were blended at 230°C as mentioned above and no
chemical reaction was occurred as can be referred to A. I. Aligbodion et al in
Indian Journal of chem. Tech., Vol. 4, (2001) Page 378.
Novelty and inventive steps of composition useful for making acid and corrosion
resistant coating resides in the material selection consisting a fraction of
machining waste generated in printed circuit board, CNSL resin, alkyd resin and
drying oil.
The following examples are given by way of illustration and therefore should not
be construed to limit the scope of the present invention.
Example 1
Following ingredients were taken
Ingredients Composition Wt % of resin
1. CNSL resin (70 wt % solid content) 90 g 90.00
2. Alkyd resin (Unsaturated polyester resin) 10 g 10.00
Total resin 100.00
3. Fine powder obtained from the machining 40 g 40.00 waste of PCB plant ( 4. Drying oil (Soybean oil) 12 g 12.00
5. Cobalt Naphthanate (.0005% metal) 1.5 ml 1.50
6. Manganese Naphthanate (.0002% metal) 1.5 ml 1.50
7. Thinner (Turpentine oil) 60 ml 60.00
CNSL resin, alkyd resin, drying oil were weighed accurately and agitated continuously at 220 °C for 50 minutes. Resultant mixture was cooled to room temperature and transferred to ball mill mixer. In ball mill, mixer powder obtained from machining waste was added to this mixture. The thinner was also added at this time and mixing/grinding was continued for 8 hrs. After getting a uniform dispersion 3 wt % of total resin of dryer mixture containing 1.5 wt % of total resin cobalt Naphthanate and 1.5 wt % of total resin manganese Naphthanate were added and mixed in the same ball mill mixer for 5 minutes. The material was taken out from the mixer and stored in airtight bottles.
The prepared paint was coated on mild steel strips by using a brush. After 48 hours, the coating was tested for scratch resistance and passed 1kg load. Acid and urea resistance tests were conducted as per IS 159. One sample was immersed for 24 hours in a solution containing 20g of sulfuric acid per 100ml of water. The coated plate was removed and washed with water and air dried for two hours at room temperature. Another sample was immersed in a solution containing Nitric acid, sulphuric acid and water in volumetric ratio of 1:3:16 respectively. After 24 hours, sample was removed, washed and dried in air. Third sample was immersed in saturated solution of urea was allowed to stand 24 hours at room temperature. Then washed with water and dried in air.
These samples were tasted and compared with commercial samples and found better than epoxy based and acrylic based coatings. No significant change in colour on surface was observed. The gloss was good and colour was brown.
Example -2
Following ingredients were taken
Ingredients composition Wt % of resin
1. CNSL resin ( 70 wt % solid content) 90 g 90.00
2. Alkyd resin (Unsaturated polyester resin) 10 g 10,00
Total resin 100.00
3. Fine powder obtained from the machining 60 g 60.00
waste of PCB plant ( 4. Drying oil (Soybean oil) 12 g 12.00
5. Cobalt Naphthanate (0.0005% metal) 2.0 ml 2.00
6. Manganese Naphthanate (0.0002% metal) 2.0 ml 2.00
7. Thinner (Turpentine oil) 80.0 ml 80.00
CNSL resin, alkyd resin, drying oil were weighed accurately and agitated continuously at 220 °C for 50 minutes. Resultant mixture was cooled to room temperature and transferred to ball mill mixer. In ball mill, mixer powder obtained from machining waste was added to this mixture. The thinner was also added at this time and mixing/grinding was continued for 10 hrs. After getting a uniform dispersion, 4 wt % of total resin dryer mixture containing 2 wt % of total resin cobalt Naphthanate and 2 wt % of total resin of manganese Naphthanate were added and mixed in the same ball mill mixer for 5 minutes. The material was taken out from the mixer and stored in airtight bottles.
The prepared paint was coated on mild steel strips by using a brush. After 48 hours, the coating was tested for scratch resistance and passed 1kg load. Acid and urea resistance tests were conducted as per IS 159. One sample was immersed for 24 hours in a solution containing 20g of sulfuric acid per 100ml of water. The coated plate was removed and washed with water and air dried for two hours at room temperature. Another sample was immersed in a solution containing Nitric acid, sulphuric acid and water in volumetric ratio of 1:3:16 respectively. After 24 hrs, sample was removed, washed and dried in air. Third
sample was immersed in saturated solution of urea was allowed to stand 24 hours at room temperature. Then washed with water and dried in air.
These samples were tasted and compared with commercial samples and found better than epoxy based and acrylic based coatings. No significant change in colour on surface was observed. The glass was good and colour was brown.
Example-3
Following ingredients were taken
Ingredients composition Wt % of resin
1. CNSL resin ( 70 wt. solid content) 80 g 80.00
2. Alkyd resin (Unsaturated polyester resin) 20 g 20.00
Total resin 100.00
3. Fine powder obtained from the machining 20 g 20.00 waste of PCB plant ( 4. Drying oil (Soybean oil) 12 g 12.00
5. Cobalt Naphthanate (0.0005% metal) 1.5 ml 1.50
6. Manganese Naphthanate (0.0002% metal) 1.5 ml 1.50
7. Thinner (Turpentine oil) 60.0 ml 60.00
CNSL resin, alkyd resin, drying oil were weighed accurately and agitated continuously at 240 °C for 30 minutes. Resultant mixture was cooled to room temperature and transferred to ball mill mixer. In ball mill, mixer powder obtained from machining waste was added to this mixture. The thinner was also added at
this time and mixing/grinding was continued for 8 hrs. After getting a uniform dispersion, 3 wt % of total resin dryer mixture containing 1.5 wt % of total resin cobalt Naphthanate and 1.5 wt % of total resin of manganese Naphthanate were added and mixed in the same ball mill mixer for 5 minutes. The material was taken out from the mixer and stored in airtight bottles.
The prepared paint was coated on mild steel strips by using a brush. After 48 hours, the coating was tested for scratch resistance and passed 1kg load. Acid and urea resistance tests were conducted as per IS 159. One sample was immersed for 24 hours in a solution containing 20g of sulfuric acid per 100ml of water. The coated plate was removed and washed with water and air dried for two hours at room temperature. Another sample was immersed in a solution containing Nitric acid, sulphuric acid and water in volumetric ratio of 1:3:16 respectively. After 24 hrs, sample was removed, washed and dried in air. Third sample was immersed in saturated solution of urea was allowed to stand 24 hours at room temperature. Then washed with water and dried in air.
These samples were tasted and compared with commercial samples and found better than epoxy based and acrylic based coatings. No significant change in colour on surface was observed. The glass was good and colour was brown.
The main advantages of the present invention are
i) This composition utilizes the fine powder obtained from the machining
waste of PCB plant, ii) This composition is eco-freindly and helps in utilizing non-degradable
industrial waste, iii) This composition can efficiently be used to produce acid and urea
resistant coating, iv) This composition is economical., v) This coating gives good scratch resistance.





We claim:
1. A composition useful as an acid and corrosion resistant coating comprising; a polymer material prepared from Cashew nut shell liquid (CNSL) resin 50 to 95 wt % of total resin, alkyd resin 5 to 50 wt % of total resin and drying oil 02 to 15 wt % of total resin, fine powder of machine waste generated in printed circuit board plant 5 to 55 wt % total resin, thinner 20 to 50 wt % of total resin, mix dryer 2 to 6 wt % of total resin.
2. A process for preparation of composition as claimed in claim 1, which comprises; (i) mixing of cashew nut shell liquid resin 50 to 95 wt % of total resin, alkyd resin 5 to 50 wt % of total resin and drying oil 02 to 15 wt % of total resin, in a mixer for a period in the range of 30 to 120 minutes at a temperature in the range of 150 to 240°C, cooling the mixed material to room temperature , transferring the material obtained in step (i) to a rotary ball mill mixer, adding fine powder of machining waste generated in printed circuit board plant 5 to 55 wt % of total resin, thinner 20 to 50 wt % of total resin and mixing the whole mass for a period in the range of 2 to 24 hours, until a uniform dispersion is obtained , mixing dryer 2 to 6 wt % of total resin for a period in the range of 2 to 10 minutes in the same mixer to obtain coating composition and storing in the air tight containers.
3. A process as claimed in claim 1, wherein cashew nut shell liquid resin
is selected from 40% concentrations and above.
4. A process as claimed in claim 1, wherein drying oil in selected from a group consisting of soybean oil, linseed oil, fish oil, rubber seed oil, tung oil, sunflower oil.
5. A process as claimed in claim 1, wherein thinner is selected from a group consisting of toluene, benzene, methylated spirit, mineral turpentine oil, kerosene or a mixture of any of two of the above in the ratio of 1:10.
6. A process as claimed in claim 1, wherein the fine powder of machining waste can have
size less than 45 µm preferably below 20 µm.
7. A process as claimed in claim 1, wherein the dryer is selected from Cobalt
Naphthanate, Lead Naphthanate and Manganese Naphthanate or a mixture thereof.
8. A composition useful as an acid and corrosion resistant coating and process thereof substantially as herein described with reference to the examples accompanying this specification.

Documents:

1756-DEL-2004-Abstract-(29-12-2010).pdf

1756-del-2004-abstract.pdf

1756-DEL-2004-Claims-(29-12-2010).pdf

1756-del-2004-claims.pdf

1756-DEL-2004-Correspondence-Others-(29-12-2010).pdf

1756-del-2004-correspondence-others.pdf

1756-DEL-2004-Description (Complete)-(29-12-2010).pdf

1756-del-2004-description (complete).pdf

1756-DEL-2004-Form-1-(29-12-2010).pdf

1756-del-2004-form-1.pdf

1756-del-2004-form-18.pdf

1756-DEL-2004-Form-2-(29-12-2010).pdf

1756-del-2004-form-2.pdf

1756-DEL-2004-Form-3-(29-12-2010).pdf

1756-del-2004-form-3.pdf

1756-del-2004-form-5.pdf


Patent Number 248579
Indian Patent Application Number 1756/DEL/2004
PG Journal Number 30/2011
Publication Date 29-Jul-2011
Grant Date 26-Jul-2011
Date of Filing 17-Sep-2004
Name of Patentee COUNCIL OF SCIENTIFIC AND INDUSTRIAL RESEARCH
Applicant Address RAFI MARG, NEW DELHI-110 001, INDIA.
Inventors:
# Inventor's Name Inventor's Address
1 SYED AZHAR RASHEED HASHMI REGIONAL RESEARCH LABORATORY, HOSHANGABAD ROAD, BHOPAL 462026, INDIA.
2 NAVIN CHAND, REGIONAL RESEARCH LABORATORY, HOSHANGABAD ROAD, BHOPAL 462026, INDIA.
3 AJAY NAIK REGIONAL RESEARCH LABORATORY, HOSHANGABAD ROAD, BHOPAL 462026, INDIA.
4 VINOD KUMAR NEMA GUJARAT NARMADA VALLEY FERTILIZERS COMPANY LIMITED, POST OFFICE NARMADA NAGAR-392015, BHARUCH, INDIA.
PCT International Classification Number C09D 5/08
PCT International Application Number N/A
PCT International Filing date
PCT Conventions:
# PCT Application Number Date of Convention Priority Country
1 NA