Title of Invention	"A PROCESS FOR THE PREPARATION OF CHEMICAL RESISTANT FLYASH-POLYMER COMPOSITE MATERIAL"
Abstract	A process for the preparation of chemical resistant flyash - polymer composite material The present invention relates to a process for the preparation of chemical resistant flyash - polymer composite material. The fly ash polymer composite material prepared by this method has enhanced chemical resistance. The invention provides a novel way of converting fly ash, a huge waste from thermal power station, into a composite material by utilizing the modulated cross linking reactions of naturally occurring polymers available from agro sources and also of custom made sol-gel polymers originating from phenolic and aminopolymers. The fly ash polymer composite material, a chemically resistant one as shown above, can be made in several moulds such as bricks, panels, tiles etc., thereby providing a methodology for utilization of waste fly ash into useful construction materials with enhanced chemical resistance.

Title of Invention

"A PROCESS FOR THE PREPARATION OF CHEMICAL RESISTANT FLYASH-POLYMER COMPOSITE MATERIAL"

Abstract

A process for the preparation of chemical resistant flyash - polymer composite material The present invention relates to a process for the preparation of chemical resistant flyash - polymer composite material. The fly ash polymer composite material prepared by this method has enhanced chemical resistance. The invention provides a novel way of converting fly ash, a huge waste from thermal power station, into a composite material by utilizing the modulated cross linking reactions of naturally occurring polymers available from agro sources and also of custom made sol-gel polymers originating from phenolic and aminopolymers. The fly ash polymer composite material, a chemically resistant one as shown above, can be made in several moulds such as bricks, panels, tiles etc., thereby providing a methodology for utilization of waste fly ash into useful construction materials with enhanced chemical resistance.

Full Text	The present invention relates to a process for the preparation of chemical resistant flyash - polymer composite material. The present invention particularly relates to improvements in or relating to a process for preparation of fly ash polymer composite material with enhanced chemical resistance. The main usage of the invention is large scale utilization of fly ash which is a waste product coming out of various thermal power stations in our country. In our country, nearly 40 million tones of fly ash are accumulating every year posing a serious environmental problem. Safe and efficient disposal of fly ash is the utmost need of each and every thermal power station. Therefore, this invention will have direct impact and application as an ancillary unit within each and every thermal power station. This invention will also directly lead to a considerable saving in the construction sector because of enhanced durability of building components. It is fairly well known that fly ash is presently utilized in cement industry as partial replacement for ordinary Portland cement. Lime - flyash bricks are also being used in construction industry. Reference may be made to chemistry of cement and concrete, edited by F.M. Lea, Edward Arnold's Publishers Limited, London, 1956, pp 379 where in Lime - Pozzolana concrete has been mentioned. The draw back is that long period of moist curing is essential to the development of higher strength and rapid drying has worst injurious effects. Reference may please be made to H.S. Meissner, American Society for Testing Materials, special Technical Publication No.99 (1950) pp 16 and P.F. Blanks; Proceedings of American Concrete Institute; 46 (1950) 701 wherein Portland Pozzolana Cement has been referred to. The main drawback is reduction in strength. Fly ashes of low carbon content indicate that their substitution for 30% by weight of Portland cement reduces the strength of concrete wet cured at 70°F by about 35-40% at 28 days. For a 40% substitution, the corresponding reduction was 60% at 28 days. The main objective of the present invention is to provide a novel process for the preparation of chemical resistant fly ash based composite using polymer which obviates the drawbacks detailed above. Another object of the present invention is to develop a process wherein fly ash, the waste product of thermal power station is utilized to the maximum extent. Yet another object of the present invention is to develop a process wherein naturally occurring polymers are utilized. Yet another object of the present invention is to develop a process wherein the modulated cross linking of polymers is utilized for the preparation of fly ash polymer composite. Accordingly the present invention provides a process for the preparation of chemical resistant fly-ash - polymer composite material which comprises a) condensing polymer matrix selected from natural origin in natural form or modified/functionaiised resin form or custom made composite of polymer of phenolic and aminopolymers in sol gel form of the kind herein described with aldehyde and optionally with catalyst of the kind as herein described , b) contacting the fly-ash with above said polymer matrix as obtained in step a) in a ratio in the range of 60 to 80% in presence of solvent, optionally adding cross linking agent to obtain mixture, c) incubating the above said mixture for a period ranging in between 2-8 hrs, d) pouring it into mould of any size and subjecting to compression at compression pressure in the range of 2-4 tons for a period of 1-10 minutes, e) curing the above said composite at a temperature ranging from 80-200° C for a period ranging from 1-5 hrs to obtain the desired composite material. In an embodiment of the present invention the polymer matrix of naturally occurring origin used is selected from the group consisting of cashew nut shell liquid (CNSL), CNSL resin and guar-gum . In an another embodiment of the present invention the polymer matrix of naturally occurring resin used is in a prefunctionalized form selected from resin liquid and epoxidation. In an another embodiment of the present invention the custom made polymer used is selected from phenolic, amino and acrylic family. In an another embodiment of the present invention the solvent used is selected from the group consisting of water, xylene, turpentine oil and ethyl methyl ketone. In an another embodiment of the present invention the cross linking agent used is selected from the group consisting of hexamine, rosin, dicycopentamine, epichlorohydrin, substitute amine and functionalised acrylates In an another embodiment of the present invention the sol-gel polymer is custom made by using the catalyst selected from Na2C03, NaOH, K2CO3 and KOH. In an another embodiment of the present invention the condensation of polymer matrix originating from both natural origin and custom made is effected with aldehyde selected from the group consisting of formaldehyde, acetaldehyde, propinaldehyde and butyraldehyde. In an another embodiment of t\e present invention the ratio of fly ash to be compounded with polymer resin of natural origin or custom made is in the range of 60-80% with respect to the chosen macromolecular resin matrix for constituting the composite. In an another embodiment of the present invention the solvent for polymer of natural origin is in the ratio of 3:1 to 5:3 with respect to the basic resin matrix. In an another embodiment of the present invention the ratio of aldehyde to monomer polymer is in range of 1:2 to 1:3. In an another embodiment of the present invention the curing temperature in the sol gel routed composite is preferably ranging from 80-100°C for a period ranging preferably from 1-3 hours for constituting the composite. In an another embodiment of the present invention the titled composite fulfills the requirements of standard specification for chemical masonry units as per the ASTM C279-88 standards. In an another embodiment of the present invention the titled composite shows higher electrical resistance than ordinary country brick after acid treatments. Characteristics of fly ash polymer composite Water absorption characteristics: The fly ash polymer composite block as described shows a water absorption of 3%, when the block is subjected to test as prescribed by ASTM C 279 - 88. Accordinc to the standard specification for chemical resistant masonry units, this water absorption value corresponds to a value specified for Type II chemical resistant brick. Chemical resistant characteristics: The block of fly ash polymer composite prepared as described when subjected to sulphuric acid solubility test as per the specification ASTM C279-88 conforms to the value of only 4 % which is lower than the limit of 8% prescribed in this specification. Electrical resistance Test: The electrical resistance, a measure of chemical resistance of fly ash polymer composite block is determined periodically after immersion in 10% H2SO4 and 10% HCI at regular intervals of time. The values of electrical resistance is compared in Table 1 with country bricks. This table indicates higher chemical resistance as evidenced by higher values of electrical resistance. (Table Removed) The following examples describe the nature of the invention and should not be misconstrued as the only formulation. (Table Removed) A strong and sturdy block of size 220 x 100 x 75 mm is thus obtained. (Table Removed) A strong and sturdy cylinder of size 5 cm dia x 4 cm height is obtained Thus this invention provides a novel way of converting fly ash, a huge waste from thermal power station, into a composite material by utilizing the modulated cross linking reactions of naturally occurring polymers available from agro sources and also of custom made sol-gel polymers originating from phenolic and aminopolymers. The fly ash polymer composite material, a chemically resistant one as shown above, can be made in several moulds such as bricks, panels, tiles etc., thereby providing a methodology for utilization of waste fly ash into useful construction materials with enhanced chemical resistance. We claim: 1. A process for the preparation of chemical resistant fly-ash - polymer composite material which comprises a) condensing polymer matrix selected from natural origin in natural form or modified/functionalised resin form or custom made composite of polymer of phenolic and aminopolymers in sol gel form of the kind herein described with aldehyde and optionally with catalyst of the kind as herein described , b) contacting the fly-ash with above said polymer matrix as obtained in step a) in a ratio in the range of 60 to 80% in presence of solvent, optionally adding cross linking agent to obtain mixture, c) incubating the above said mixture for a period ranging in between 2-8 hrs, d) pouring it into mould of any size and subjecting to compression at compression pressure in the range of 2-4 tons for a period of 1-10 minutes, e) curing the above said composite at a temperature ranging from 80-200° C for a period ranging from 1-5 hrs to obtain the desired composite material. 2. A process as claimed in 1, wherein the polymer matrix of natural origin used is selected from the group consisting of cashew nut shell liquid (CNSL), CNSL resin and guar-gum . 3. A process as claimed in claims 1 and 2, wherein the polymer matrix of natural origin resin in a prefunctionalized form is selected from resin liquid and epoxidation. 4. A process as claimed in claims 1 - 3, wherein the solvent used is selected from the group consisting of water, xylene, turpentine oil and ethyl methyl ketone. 5. A process as claimed in claims 1 - 4, wherein the cross linking agent used is selected from the group consisting of hexamine, rosin, dicycopentamine, epichlorohydrin, substitute amine and functionalised acrylates 6. A process as claimed in claims 1 - 5, wherein the catalyst used is selected from Na2C03, NaOH, K2CO3 and KOH. 7. A process as claimed in claims 1-6, wherein the condensation of polymer matrix originating from both natural origin and custom made is affected with aldehyde selected from the group consisting of formaldehyde, acetaldehyde, propinaidehyde and butyraldehyde. 8. A process as claimed in claims 1-7, wherein the solvent for polymer matrix of natural origin resin form is in the ratio of 3:1 to 5:3. 9. A process as claimed in claims 1-8, wherein the ratio of aldehyde to polymer is in range of 1:2 to 1:3. 10. A process as claimed in claims 1 - 9, wherein the curing temperature in the sol gel routed composite is preferably ranging from 80-100°C for a period ranging preferably from 1-3 hours for constituting the composite. 11. A process for the preparation of chemical resistant fly-ash - polymer composite material substantially as herein described with reference to the examples.

Full Text

The present invention relates to a process for the preparation of chemical resistant flyash - polymer composite material.
The present invention particularly relates to improvements in or relating to a process for preparation of fly ash polymer composite material with enhanced chemical resistance.
The main usage of the invention is large scale utilization of fly ash which is a waste product coming out of various thermal power stations in our country. In our country, nearly 40 million tones of fly ash are accumulating every year posing a serious environmental problem. Safe and efficient disposal of fly ash is the utmost need of each and every thermal power station. Therefore, this invention will have direct impact and application as an ancillary unit within each and every thermal power station. This invention will also directly lead to a considerable saving in the construction sector because of enhanced durability of building components.
It is fairly well known that fly ash is presently utilized in cement industry as partial replacement for ordinary Portland cement. Lime - flyash bricks are also being used in construction industry.
Reference may be made to chemistry of cement and concrete, edited by F.M. Lea, Edward Arnold's Publishers Limited, London, 1956, pp 379 where in Lime - Pozzolana concrete has been mentioned. The draw back is that long

period of moist curing is essential to the development of higher strength and rapid drying has worst injurious effects.
Reference may please be made to H.S. Meissner, American Society for Testing Materials, special Technical Publication No.99 (1950) pp 16 and P.F. Blanks; Proceedings of American Concrete Institute; 46 (1950) 701 wherein Portland Pozzolana Cement has been referred to. The main drawback is reduction in strength. Fly ashes of low carbon content indicate that their substitution for 30% by weight of Portland cement reduces the strength of concrete wet cured at 70°F by about 35-40% at 28 days. For a 40% substitution, the corresponding reduction was 60% at 28 days.
The main objective of the present invention is to provide a novel process for the preparation of chemical resistant fly ash based composite using polymer which obviates the drawbacks detailed above.
Another object of the present invention is to develop a process wherein fly ash, the waste product of thermal power station is utilized to the maximum extent.
Yet another object of the present invention is to develop a process wherein naturally occurring polymers are utilized.
Yet another object of the present invention is to develop a process wherein the modulated cross linking of polymers is utilized for the preparation of fly ash polymer composite.

Accordingly the present invention provides a process for the preparation of chemical resistant fly-ash - polymer composite material which comprises a) condensing polymer matrix selected from natural origin in natural form or modified/functionaiised resin form or custom made composite of polymer of phenolic and aminopolymers in sol gel form of the kind herein described with aldehyde and optionally with catalyst of the kind as herein described , b) contacting the fly-ash with above said polymer matrix as obtained in step a) in a ratio in the range of 60 to 80% in presence of solvent, optionally adding cross linking agent to obtain mixture, c) incubating the above said mixture for a period ranging in between 2-8 hrs, d) pouring it into mould of any size and subjecting to compression at compression pressure in the range of 2-4 tons for a period of 1-10 minutes, e) curing the above said composite at a temperature ranging from 80-200° C for a period ranging from 1-5 hrs to obtain the desired composite material.
In an embodiment of the present invention the polymer matrix of naturally occurring origin used is selected from the group consisting of cashew nut shell liquid (CNSL), CNSL resin and guar-gum .
In an another embodiment of the present invention the polymer matrix of naturally occurring resin used is in a prefunctionalized form selected from resin liquid and epoxidation.
In an another embodiment of the present invention the custom made polymer used is selected from phenolic, amino and acrylic family.
In an another embodiment of the present invention the solvent used is selected from the group consisting of water, xylene, turpentine oil and ethyl methyl ketone.
In an another embodiment of the present invention the cross linking agent used is selected from the group consisting of hexamine, rosin, dicycopentamine, epichlorohydrin, substitute amine and functionalised acrylates
In an another embodiment of the present invention the sol-gel polymer is custom made by using the catalyst selected from Na2C03, NaOH, K2CO3 and KOH.
In an another embodiment of the present invention the condensation of polymer matrix originating from both natural origin and custom made is effected with aldehyde selected from the group consisting of formaldehyde, acetaldehyde, propinaldehyde and butyraldehyde.
In an another embodiment of t\e present invention the ratio of fly ash to be compounded with polymer resin of natural origin or custom made is in the range of 60-80% with respect to the chosen macromolecular resin matrix for constituting the composite.
In an another embodiment of the present invention the solvent for polymer of natural origin is in the ratio of 3:1 to 5:3 with respect to the basic resin matrix.
In an another embodiment of the present invention the ratio of aldehyde to monomer polymer is in range of 1:2 to 1:3.
In an another embodiment of the present invention the curing temperature in the sol gel routed composite is preferably ranging from 80-100°C for a period ranging preferably from 1-3 hours for constituting the composite.
In an another embodiment of the present invention the titled composite fulfills the requirements of standard specification for chemical masonry units as per the ASTM C279-88 standards.
In an another embodiment of the present invention the titled composite shows higher electrical resistance than ordinary country brick after acid treatments.
Characteristics of fly ash polymer composite
Water absorption characteristics:
The fly ash polymer composite block as described shows a water absorption of 3%, when the block is subjected to test as prescribed by ASTM C 279 - 88. Accordinc to the standard specification for chemical resistant masonry units, this water absorption value corresponds to a value specified for Type II chemical resistant brick.
Chemical resistant characteristics:
The block of fly ash polymer composite prepared as described when subjected to sulphuric acid solubility test as per the specification ASTM C279-88 conforms to the value of only 4 % which is lower than the limit of 8% prescribed in this specification.
Electrical resistance Test:
The electrical resistance, a measure of chemical resistance of fly ash polymer composite block is determined periodically after immersion in 10% H2SO4 and 10% HCI at regular intervals of time. The values of electrical resistance is compared in Table 1 with country bricks. This table indicates higher chemical resistance as evidenced by higher values of electrical resistance.
(Table Removed)
The following examples describe the nature of the invention and should not be misconstrued as the only formulation.
(Table Removed)
A strong and sturdy block of size 220 x 100 x 75 mm is thus obtained.

(Table Removed)
A strong and sturdy cylinder of size 5 cm dia x 4 cm height is obtained
Thus this invention provides a novel way of converting fly ash, a huge waste from thermal power station, into a composite material by utilizing the modulated cross linking reactions of naturally occurring polymers available
from agro sources and also of custom made sol-gel polymers originating from phenolic and aminopolymers. The fly ash polymer composite material, a chemically resistant one as shown above, can be made in several moulds such as bricks, panels, tiles etc., thereby providing a methodology for utilization of waste fly ash into useful construction materials with enhanced chemical resistance.

We claim:
1. A process for the preparation of chemical resistant fly-ash - polymer
composite material which comprises a) condensing polymer matrix
selected from natural origin in natural form or modified/functionalised
resin form or custom made composite of polymer of phenolic and
aminopolymers in sol gel form of the kind herein described with
aldehyde and optionally with catalyst of the kind as herein described ,
b) contacting the fly-ash with above said polymer matrix as obtained in
step a) in a ratio in the range of 60 to 80% in presence of solvent,
optionally adding cross linking agent to obtain mixture, c) incubating
the above said mixture for a period ranging in between 2-8 hrs, d)
pouring it into mould of any size and subjecting to compression at
compression pressure in the range of 2-4 tons for a period of 1-10
minutes, e) curing the above said composite at a temperature ranging
from 80-200° C for a period ranging from 1-5 hrs to obtain the desired
composite material.
2. A process as claimed in 1, wherein the polymer matrix of natural
origin used is selected from the group consisting of cashew nut shell
liquid (CNSL), CNSL resin and guar-gum .
3. A process as claimed in claims 1 and 2, wherein the polymer matrix of natural origin resin in a prefunctionalized form is selected from resin liquid and epoxidation.
4. A process as claimed in claims 1 - 3, wherein the solvent used is selected from the group consisting of water, xylene, turpentine oil and ethyl methyl ketone.
5. A process as claimed in claims 1 - 4, wherein the cross linking agent used is selected from the group consisting of hexamine, rosin, dicycopentamine, epichlorohydrin, substitute amine and functionalised acrylates
6. A process as claimed in claims 1 - 5, wherein the catalyst used is selected from Na2C03, NaOH, K2CO3 and KOH.
7. A process as claimed in claims 1-6, wherein the condensation of polymer matrix originating from both natural origin and custom made is affected with aldehyde selected from the group consisting of formaldehyde, acetaldehyde, propinaidehyde and butyraldehyde.
8. A process as claimed in claims 1-7, wherein the solvent for polymer matrix of natural origin resin form is in the ratio of 3:1 to 5:3.
9. A process as claimed in claims 1-8, wherein the ratio of aldehyde to polymer is in range of 1:2 to 1:3.
10. A process as claimed in claims 1 - 9, wherein the curing temperature in the sol gel routed composite is preferably ranging from 80-100°C for a period ranging preferably from 1-3 hours for constituting the composite.
11. A process for the preparation of chemical resistant fly-ash - polymer composite material substantially as herein described with reference to the examples.

Documents:

404-del-2001-abstract.pdf

404-del-2001-claims.pdf

404-del-2001-correspondence-others.pdf

404-del-2001-correspondence-po.pdf

404-del-2001-description (complete).pdf

404-del-2001-form-1.pdf

404-del-2001-form-18.pdf

404-del-2001-form-2.pdf

404-del-2001-form-3.pdf

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Patent Number

242253

Indian Patent Application Number

404/DEL/2001

PG Journal Number

35/2010

Publication Date

27-Aug-2010

Grant Date

19-Aug-2010

Date of Filing

29-Mar-2001

Name of Patentee

COUNCIL OF SCIENTIFIC & INDUSTRIAL RESEARCH

Applicant Address

RAFI MARG, NEW DELHI-110001, INDIA.

Inventors:

#	Inventor's Name	Inventor's Address
1	MEENAKSHI SUNDARAM RAGHVAN	CENTRAL ELECTROCHEMICAL RESEARCH INSTITUTE KARAIKUDI-630006, TAMILNADU INDIA.
2	SESAADRI SRINIVASAN	CENTRAL ELECTROCHEMICAL RESEARCH INSTITUTE KARAIKUDI-630006, TAMILNADU INDIA.
3	KRISHNAN KUMAR	CENTRAL ELECTROCHEMICAL RESEARCH INSTITUTE KARAIKUDI-630006, TAMILNADU INDIA.
4	RATHINAVEL VEDALAKSHMI	CENTRAL ELECTROCHEMICAL RESEARCH INSTITUTE KARAIKUDI-630006, TAMILNADU INDIA.
5	ANDIAPPAN MADHAVAMAYANDI	CENTRAL ELECTROCHEMICAL RESEARCH INSTITUTE KARAIKUDI-630006, TAMILNADU INDIA.
6	SETHURAMAN PITCHEMAN	CENTRAL ELECTROCHEMICAL RESEARCH INSTITUTE KARAIKUDI-630006, TAMILNADU INDIA.
7	NERUR SANKARANARAYANAN RENESWAMY	CENTRAL ELECTROCHEMICAL RESEARCH INSTITUTE KARAIKUDI-630006, TAMILNADU INDIA.

PCT International Classification Number

C08K 3/36

PCT International Application Number

N/A

PCT International Filing date

PCT Conventions:

#	PCT Application Number	Date of Convention	Priority Country
1			NA