Indian Patents. 232875:A PROCESS FOR THE PRODUCTION OF CONDENSATE OF TOLUENE-NAPHTHALENE SULPHONATES, AN ADDITIVE FOR COAL WATER SLURRY

Title of Invention	A PROCESS FOR THE PRODUCTION OF CONDENSATE OF TOLUENE-NAPHTHALENE SULPHONATES, AN ADDITIVE FOR COAL WATER SLURRY
Abstract	Methanol is reacted in presence of catalyst system comprising of an iron containing compound and a tin containing compound with or without an organic compound containing C, N, O, P, S, diamine, diketone, and or diphosphines as a ligand to produce acetic acid or methyl acetate. The reaction is effected in a solvent containing nitro or nitrile group.

Full Text	The present invention relates to a process for the production of condensate of toluene -naphthalene sulphonates, an additive for coal -water slurry. The main usage of the invention is in the preparation of high concentration coal-water slurry fuel achieving desirable flow property and stability. Reference may be made to patent No.JP 1062392 dated 08.03.1989, wherein additives for coal water slurry (CWS) containing compounds prepared by sulphonating (alkyl) naphthalene, anthracene and biphenyl and condensing with formaldehyde & fatty acids, have been described. Reference may also be made to Japanese Patent Nos.JP1062391 dt. 08.03.1989, JP 1054097 dt.01.03.1989, JP 1182392 dt.20.07.1989 and JP 63156891 dt.29.06.1988, wherein additives for coal water slurry - containing formaldehyde condensates of naphthalene/(alkyl) naphthalene sulphonic acids, fatty acids and polyethylene polyamine fatty acid amide compounds or compounds obtained from ethylene oxide and alkyl phenol/ polyhydric alcohols etc, have been described. The drawbacks of the above processes are that reactions have to be carried out in several stages with various types of specific compounds and the final additive package requires extensive pretreatment and selective purification methods, thus making the process tedious and uneconomical. Besides, the performance of the additive packages was not upto the desired level. Owing to these disadvantages of naphthalene based additives, the Japanese developed an efficient additive, namely sodium polystyrene sulphonate (PSS) which is used for commercial production of coal-water slurry (Ref. H.Arai and T.Ukigaki, Proc.16 Int. Tech. Conference of Coal Utilisation and Fuel System, Florida(1991) 423-433 ). PSS being the proprietary additive package of a Japanese company, its preparation method are fully guarded and the additive is highly expensive. Reference may also be made to work of J.L. Morrison, B.G. miller and A.W. Scaroni, proc. 18 Int. Tech. Conf. Coal Utilisation and Fuel Systems, April 26-29(1993) 361-368, Florida, U.S.A., wherein an ammonium based sulphonated naphthalene condensate has been used as the dispersant for coal-water slurry fuels. However, the slurry formulation with this dispersant requires a pH modifier & a stabliser. The main object of the present invention is to provide a process for the production of condensate of toluene-naphthalene sulphonates, an additive for Coal-water slurry, which obviates the drawbacks as detailed above. Another object of the present invention is to remove the tedious pretreatment and purification steps involved in itherto known processes for the preparation of sulphonated naphthalene/alkyl naphthalene based additives. Still another object of the present invention is to develop a new additive most suited to low-rank Indian coals for production of Coal water-slurry fuels having desired viscosity and stability. Yet another object of the present invention is to develop a low-cost, environmentally safe additive package based on coal carbonization products. Accordingly the present invention provides, a process for the production of condensate of toluene-naphthalene sulphonates, an additive for coal-water slurry, which comprises sulphonation of toluene at a temperature in the range of 90°-130°C, for a time period in the range of 2-8 hrs and naphthalene at a temperature in the range of 130°-165°C, for a time period in the range of 2-8 hrs, then condensing together toluene sulphonic acid and naphthalene sulphonic acid with formaldehyde at a temperature in the range of 60-110°C for a time period in the range of 10-20 hrs, cooling to ambient temperature ranging from 25°-35°C and neutralizing the condensation product with alkali metal hydroxide such as herein described , followed by drying to obtain formaldehyde condensate of toluene-naphthalene sulphonates. In an embodiment of the present invention toluene and naphthalene are first sulphonated separately with 98% sulphuric acid and then the toluene sulphonic acid and naphthalene sulphonic acid are condensed with formaldehyde at a temperature in the range of 60°-110°C, for time period in the range of 10-20 hours. In another embodiment of the present invention the formaldehyde condensate of toluene sulphonic acid is neutralized with alkali metal hydroxide to a pH of 7.0-9.0. In this process toluene is sulphonated with 98% sulphuric acid in the temperature range 90°-130°C for 2-8 hours. Similarly, naphthalene is sulphonated with sulphuric acid in the temperature range of 130°-165°C for 2-8 hours. The toluene sulphonic acid and naphthalene sulphonic acid are then taken together and condensed with formaldehyde at 60°-110°C for 10-20 hours. The condensed mass is neutralized with alkali metal hydroxide to a pH 7.0-9.0 and then dried to obtain formaldehyde condensate of toluene-naphthalene sulphonates which is used as an additive in the formulation of coal-water slurry. The novelty of the present invention with respect to the prior art lies in that the process provides a state of the art technology for the production of a toluene - naphthalene based additive which apart from being cost - effective is very efficient and environmentally safe agent and is also most suited to the low-grade Indian coals for the production of coal water slurry fuels. This new additive is capable of incorporating high coal-loadings(60-70%) in the aqueous medium providing desirable viscosity and stability to the slurry fuel. The inventive steps are-- 1. The process which is apart from cost effective is very efficient and environmentally safe agent. 2. The process is most suited for to the low grade Indian coals for the production of coal water slurry fuels. 3. The additive used is capable of incorporating high coal- loadings(60-70%) in the aqueous medium providing desirable viscosity and stability to the fuel. The following example is given by way of illustration of the present invention and therefore should not be construed to limit the scope of the present invention. EXAMPLE-1 186 gms of toluene is sulphonated by adding 225 gms of 98% sulphuric acid at 110°C for 5 hours. In another reaction vessel, 400 gms. of naphthalene is melted, 330 gms. of 98% sulphuric acid is added gradually to it and temperature of sulphonation reaction maintained at 160°C for 5 hours. The sulphonated toluene and naphthalene obtained as above are mixed together and 225 ml water is added. To this mixture 304 ml formaldehyde solution (37%) is added slowly, the temperature is raised to 70°C and the reaction is carried out for 15 hours. At the end of this period the mixture is gradually heated to 100°C.The reaction product is cooled to ambient temperature and then neutralised with aqueous sodium hydroxide solution. The neutralised mass is dried to get formaldehyde condensate of sodium toluene-naphthalene sulphonate which functions as an excellent additive in the formulation of coal water slurry fuels. The invention has led to a simple process for the production of formaldehyde condensate of toluene-naphthalene sulphonates which apart from being cost-effective, is an environmentally safe agent for use as an additive in the formulation of coal water slurry fuel. Secondly, the process steps have been reduced to a minimum and no by-products or any effluent are produced in the process. Thirdly, the reactions are carried out at relatively lower ranges of temperatures, thereby leading to considerable savings in energy consumption in the process. The salient features of the invention which have an edge over the known processes are-- 1. That the feedstock (toluene and naphthalene) constitute mainly carbo-chemicals. These chemicals as well as other reactants are easily and cheaply available. 2. The consumption of raw materials are considerably less. 3. The reactions are carried out at relatively lower ranges of temperatures thereby reducing the energy consumption. 4. No effluent is produced in the process making it an eco-friendly. 5. The developed additive package functions excellently at concentration of 0.6- 1.0%(on dry coal basis) with low- rank Indian coals incorporating high coal- loadings (60-70%) in aqueous slurry and providing desirable flow property/viscosity as well as stability to the slurry fuel. 6. The additive has a shelf life / stability of 9-22 days and viscosity in the range of 400-1000 mPas at 128 sec"1 We Claim: 1. A process for the production of condensate of toluene-naphthalene sulphonates, an additive for coal-water slurry, which comprises sulphonation of toluene at a temperature in the range of 90°-130°C, for a time period in the range of 2-8 hrs and naphthalene at a temperature in the range of 130°-165°C, for a time period in the range of 2-8 hrs, then condensing together toluene sulphonic acid and naphthalene sulphonic acid with formaldehyde at a temperature in the range of 60-110°C for a time period in the range of 10-20 hrs, cooling to ambient temperature ranging from 25°-35°C and neutralizing the condensation product with alkali metal hydroxide such as herein described , followed by drying to obtain formaldehyde condensate of toluene-naphthalene sulphonates. 2. A process as claimed in claim 1 wherein toluene and naphthalene are sulphonated separately with 98% sulphuric acid then the toluene sulphonic acid and naphthalene sulphonic acid are condensed with formaldehyde . 3. A process as claimed in claims 1 & 2 wherein metal hydroxide used for neutralizing formaldehyde condensate of toluene sulphonic acid and naphthalene sulphonic acid is sodium hydroxide at a pH of 7.0-9.0. 4. A process for the production of condensate of toluene naphthalene sulphonates, an additive for coal water slurry substantially as herein described with reference to the example.

Full Text

The present invention relates to a process for the production of condensate of toluene -naphthalene sulphonates, an additive for coal -water slurry.
The main usage of the invention is in the preparation of high concentration coal-water slurry fuel achieving desirable flow property and stability.
Reference may be made to patent No.JP 1062392 dated 08.03.1989, wherein additives for coal water slurry (CWS) containing compounds prepared by sulphonating (alkyl) naphthalene, anthracene and biphenyl and condensing with formaldehyde & fatty acids, have been described.
Reference may also be made to Japanese Patent Nos.JP1062391 dt. 08.03.1989, JP 1054097 dt.01.03.1989, JP 1182392 dt.20.07.1989 and JP 63156891 dt.29.06.1988, wherein additives for coal water slurry - containing formaldehyde condensates of naphthalene/(alkyl) naphthalene sulphonic acids, fatty acids and polyethylene polyamine fatty acid amide compounds or compounds obtained from ethylene oxide and alkyl phenol/ polyhydric alcohols etc, have been described.
The drawbacks of the above processes are that reactions have to be carried out in several stages with various types of specific compounds and the final additive package requires extensive pretreatment and selective purification methods, thus making the process tedious and uneconomical. Besides, the performance of the additive packages was not upto the desired level. Owing to these disadvantages of naphthalene based additives, the Japanese developed an efficient additive, namely sodium polystyrene sulphonate (PSS) which is used for commercial production of coal-water slurry (Ref. H.Arai and T.Ukigaki, Proc.16 Int. Tech. Conference of Coal Utilisation and Fuel System, Florida(1991) 423-433 ). PSS being the proprietary additive package of a
Japanese company, its preparation method are fully guarded and the additive is highly expensive.
Reference may also be made to work of J.L. Morrison, B.G. miller and A.W. Scaroni, proc. 18 Int. Tech. Conf. Coal Utilisation and Fuel Systems, April 26-29(1993) 361-368, Florida, U.S.A., wherein an ammonium based sulphonated naphthalene condensate has been used as the dispersant for coal-water slurry fuels. However, the slurry formulation with this dispersant requires a pH modifier & a stabliser.
The main object of the present invention is to provide a process for the production of condensate of toluene-naphthalene sulphonates, an additive for Coal-water slurry, which obviates the drawbacks as detailed above.
Another object of the present invention is to remove the tedious pretreatment and purification steps involved in itherto known processes for the preparation of sulphonated naphthalene/alkyl naphthalene based additives.
Still another object of the present invention is to develop a new additive most suited to low-rank Indian coals for production of Coal water-slurry fuels having desired viscosity and stability.
Yet another object of the present invention is to develop a low-cost, environmentally safe additive package based on coal carbonization products.
Accordingly the present invention provides, a process for the production of condensate of toluene-naphthalene sulphonates, an additive for coal-water slurry, which comprises sulphonation of toluene at a temperature in the range of 90°-130°C, for a time period in the range of 2-8 hrs and naphthalene at a temperature in the range of 130°-165°C, for a time period in the range of 2-8 hrs, then condensing together toluene sulphonic acid and naphthalene
sulphonic acid with formaldehyde at a temperature in the range of 60-110°C for a time period in the range of 10-20 hrs, cooling to ambient temperature ranging from 25°-35°C and neutralizing the condensation product with alkali metal hydroxide such as herein described , followed by drying to obtain formaldehyde condensate of toluene-naphthalene sulphonates.
In an embodiment of the present invention toluene and naphthalene are first sulphonated separately with 98% sulphuric acid and then the toluene sulphonic acid and naphthalene sulphonic acid are condensed with formaldehyde at a temperature in the range of 60°-110°C, for time period in the range of 10-20 hours.
In another embodiment of the present invention the formaldehyde condensate of toluene sulphonic acid is neutralized with alkali metal hydroxide to a pH of 7.0-9.0.
In this process toluene is sulphonated with 98% sulphuric acid in the temperature range 90°-130°C for 2-8 hours. Similarly, naphthalene is sulphonated with sulphuric acid in the temperature range of 130°-165°C for 2-8 hours. The toluene sulphonic acid and naphthalene sulphonic acid are then taken together and condensed with formaldehyde at 60°-110°C for 10-20 hours. The condensed mass is neutralized with alkali metal hydroxide to a pH 7.0-9.0 and then dried to obtain formaldehyde condensate of toluene-naphthalene sulphonates which is used as an additive in the formulation of coal-water slurry.
The novelty of the present invention with respect to the prior art lies in that the process provides a state of the art technology for the production of a toluene - naphthalene based additive which apart from being cost - effective is very efficient and environmentally safe

agent and is also most suited to the low-grade Indian coals for the production of coal water slurry fuels. This new additive is capable of incorporating high coal-loadings(60-70%) in the aqueous medium providing desirable viscosity and stability to the slurry fuel. The inventive steps are--
1. The process which is apart from cost effective is very efficient and environmentally
safe agent.
2. The process is most suited for to the low grade Indian coals for the production of coal
water slurry fuels.
3. The additive used is capable of incorporating high coal- loadings(60-70%) in the
aqueous medium providing desirable viscosity and stability to the fuel.
The following example is given by way of illustration of the present invention and therefore should not be construed to limit the scope of the present invention.
EXAMPLE-1
186 gms of toluene is sulphonated by adding 225 gms of 98% sulphuric acid at 110°C for 5 hours. In another reaction vessel, 400 gms. of naphthalene is melted, 330 gms. of 98% sulphuric acid is added gradually to it and temperature of sulphonation reaction maintained at 160°C for 5 hours. The sulphonated toluene and naphthalene obtained as above are mixed together and 225 ml water is added. To this mixture 304 ml formaldehyde solution (37%) is added slowly, the temperature is raised to 70°C and the reaction is carried out for 15 hours. At the end of this period the mixture is gradually heated to 100°C.The reaction product is cooled to ambient temperature and then neutralised with aqueous sodium hydroxide solution. The neutralised mass is dried to get formaldehyde condensate of sodium toluene-naphthalene sulphonate which functions as an excellent additive in the formulation of coal water slurry fuels.

The invention has led to a simple process for the production of formaldehyde condensate of toluene-naphthalene sulphonates which apart from being cost-effective, is an environmentally safe agent for use as an additive in the formulation of coal water slurry fuel. Secondly, the process steps have been reduced to a minimum and no by-products or any effluent are produced in the process. Thirdly, the reactions are carried out at relatively lower ranges of temperatures, thereby leading to considerable savings in energy consumption in the process.
The salient features of the invention which have an edge over the known processes are--
1. That the feedstock (toluene and naphthalene) constitute mainly carbo-chemicals.
These chemicals as well as other reactants are easily and cheaply available.
2. The consumption of raw materials are considerably less.
3. The reactions are carried out at relatively lower ranges of temperatures thereby
reducing the energy consumption.
4. No effluent is produced in the process making it an eco-friendly.
5. The developed additive package functions excellently at concentration of 0.6-
1.0%(on dry coal basis) with low- rank Indian coals incorporating high coal-
loadings (60-70%) in aqueous slurry and providing desirable flow
property/viscosity as well as stability to the slurry fuel.
6. The additive has a shelf life / stability of 9-22 days and viscosity in the range of
400-1000 mPas at 128 sec"1

We Claim:
1. A process for the production of condensate of toluene-naphthalene
sulphonates, an additive for coal-water slurry, which comprises
sulphonation of toluene at a temperature in the range of 90°-130°C,
for a time period in the range of 2-8 hrs and naphthalene at a
temperature in the range of 130°-165°C, for a time period in the
range of 2-8 hrs, then condensing together toluene sulphonic acid
and naphthalene sulphonic acid with formaldehyde at a
temperature in the range of 60-110°C for a time period in the range
of 10-20 hrs, cooling to ambient temperature ranging from 25°-35°C
and neutralizing the condensation product with alkali metal
hydroxide such as herein described , followed by drying to obtain
formaldehyde condensate of toluene-naphthalene sulphonates.
2. A process as claimed in claim 1 wherein toluene and naphthalene
are sulphonated separately with 98% sulphuric acid then the
toluene sulphonic acid and naphthalene sulphonic acid are
condensed with formaldehyde .
3. A process as claimed in claims 1 & 2 wherein metal hydroxide used
for neutralizing formaldehyde condensate of toluene sulphonic
acid and naphthalene sulphonic acid is sodium hydroxide at a pH
of 7.0-9.0.
4. A process for the production of condensate of toluene naphthalene sulphonates, an additive for coal water slurry substantially as herein described with reference to the example.

Documents:

156-del-2001-abstract.pdf

156-del-2001-claims.pdf

156-del-2001-correspondence-others.pdf

156-del-2001-correspondence-po.pdf

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

156-del-2001-form-1.pdf

156-del-2001-form-19.pdf

156-del-2001-form-2.pdf

156-del-2001-form-3.pdf

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Patent Number

232875

Indian Patent Application Number

156/DEL/2001

PG Journal Number

13/2009

Publication Date

27-Mar-2009

Grant Date

21-Mar-2009

Date of Filing

16-Feb-2001

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	KAUSHAL KISHORE TIWARI	SCIENTIST, CENTRAL FUEL RESEARCH INSTITUTE, P.O. F.R.I-828108. DIST: DHANBAD. (BIHAR)
2	KUMARES CHANDRA BIT.	SCIENTIST, CENTRAL FUEL RESEARCH INSTITUTE,P.O. F.R.I-828108. DIST. DHANBAD (BIHAR)
3	SOMNATH BANERJI	SCIENTIST, CENTRAL FUEL RESEARCH INSTITUTE,P.O. F.R.I-828108. DIST. DHANBAD (BIHAR)
4	KAMLESH KUMAR MISHRA	SCIENTIST, CENTRAL FUEL RESEARCH INSTITUTE,P.O. F.R.I-828108. DIST. DHANBAD (BIHAR)

PCT International Classification Number

B01F 17/00

PCT International Application Number

N/A

PCT International Filing date

PCT Conventions:

#	PCT Application Number	Date of Convention	Priority Country
1			NA