Indian Patents. 213149:IMPROVED PROCESS FOR THE PREPARA... http://www.allindianpatents.com/patents/213149-improved-process-for-t...

Indian Patents (/)

Title of
Invention IMPROVED PROCESS FOR THE Patent Number 213149

Indian Patent 774/MUM/2005

PREPARATION OF SULPHANILIC ACID Application
Number
TECHNICAL GRADE
PG Journal 13/2008
Number
Abstract A fixed amount of Sulphanilic Acid Technical Grade 98.5% is Publication Date 28-Mar-2008
dissolved in water at elevated temperature & 0.1% activated
Grant Date 20-Dec-2007
carbon added & filter hot mother liquor in filter press to remove
water insoluble & then this filtrate is cooled to room temperature Date of Filing 30-Jun-2005
to re-crystallize White Sulphanilic Acid Purified Grade, this
Name of SANTOSH
material centrifuged & the wet cake is dried as finished goods.
Patentee PHULCHAND
The liquid portion is recycled for 30 cycles & after 30 cycles the
MEHTA
solution is treated by lime & filtrate is further used for recycling
there is no water effluent. Applicant HOUSE NO. 17,
Address NEAR SBI DAPOLI,
TAL: DAPOLI, DIST.
RATNAGIRI.

Inventors:

# Inventor's Inventor's
Name Address

1 SANTOSH HOUSE NO. 17,

PHULCHAND NEAR SBI
MEHTA DAPOLI, TAL:
DAPOLI, DIST.
RATNAGIRI.

PCT C07C 303/00

International
Classification
Number

PCT N/A
International
Application
Number

PCT
International
Filing date

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Full FORM - 2 PCT Conventions:

Text THE PATENTS ACT, 1970
(39 OF 1970) # PCT Date of Priority
& Application Convention Country
THE PATENTS RULES, 2003 Number
Provisional Specification (See Section 10 and rule 13)
1 NA
“AN IMPROVED PROCESS FOR THE PREPARATION OF
SULPHANILIC ACID TECHNICAL GRADE.”
Mr. Santosh P. Mehta
Indian National having
address at. House no. 18,
Dapoli- Harnai Road Tal: Dapoli,
Dist:- Ratnagiri
The following Specification describes the invention.

TITLE :- AN IMPROVED PROCESS FOR THE PREPARATION OF

SULPHANILIC ACID
TECHNICAL GRADE.
FIELD OF THE INVENTION
Present invention relates to a process for the preparation of
sulphanilic acid. More particularly present invention relates to a
process for the preparation of sulphanilic acid which gives about 98%
purity.
BACKGROUND OF THE INVENTION
In prior Art the process for the preparation of sulphanilic acid
comprising the steps of pouring sulphuric acid of commercial grade in
a ball mill and allowed to rotate the said ball mill and aniline is slowly
poured in the ball mill containing sulphuric acid of commercial grade in
the proper proportion of 1:1.05. Keeping the said ball mill rotating.
Heating the said rotating ball mill for about 2 hours by any heating
means preferably with the bio fuels, coal etc. After the heating is
completed the ball mill are continued to run for grinding. After the step
of grinding the said ball mills are unloaded to receive powder of
sulphanilic acid technical grade and the said received powder is
packed as per the requirement.
Since the balls of the ball mill are made up of mild iron
contamination/impurities of iron are seen in the end product i.e.
sulphanilic acid technical grade. It is also observed that the heating of
the ball mill is done at random and there is no control over the heating
because of the manual operation therefore the intermediate
temperature can not be measured which leads to variation in quality of
the finished product.
SUMMARY OF THE INVENTION
Object of the present invention aims at developing an improved
process for the preparation of sulphanilic acid technical grade.
Further object of the present invention is to eliminate the drawbacks
and shortfalls of the prior art.
It is also the object of the present invention to improve the purity of the
sulphanilic acid technical grade to about 98%.
An improved process for the preparation of sulphanilic acid technical
grade according to the present invention comprising the steps of

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Indian Patents. 213149:IMPROVED PROCESS FOR THE PREPARA... http://www.allindianpatents.com/patents/213149-improved-process-for-t...

preparing the slurry of aniline sulphate by taking the sulphuric acid of

commercial grade in a glass lined reactor, releasing aniline in the ratio
of 1:1.05 ( aniline and sulphuric acid commercial grade ) slowly in the
glass

lined reactor containing sulphuric acid of commercial grade over a

period of l hour under controlled temperature not exceeding 170° C.
This is very important because if the temperature increases above
170° C then there are chances that the slurry of aniline sulphate may
turn dry leaving behind the slumps in the glass lined reactor.
Adding oxalic acid, as a catalyst in the slurry of aniline sulphate in the
ratio of 1.5 to 2% of the aniline at the temperature of 90° C to 120° C
in order to maintain the temperature of the reaction below 170"C. It is
also important to note that if oxalic acid is added earlier at lower
temperature than 90°C it goes to the bottom of the reactor thereby
creating problems at the time of the discharge of the slurry of the
aniline sulphate. It is observed that addition of oxalic acid in the
proportion of 1.5 to 2% of aniline helps to improve the colour of aniline
sulphate slurry from dark blue to faint blue. There have been provided
various controls to monitor the temperature of the reaction.
After completion of this step the so formed slurry is released on the
marble floured surface and allowed it to settle for about 3 hours to
make it solid. Use of marble floured surface is particularly important
because use of another surface may cause reaction with the aniline
sulphate slurry and creates contamination in the final product.
After 3 hours the solid sulphomass is cut into pieces as per the
requirement with the help of cutting tool and placing the said cut
pieces in the M.S glass coated treys.
Such glass coated treys having pieces of solid sulphomass are baked
in the baker at a temperature of about 230°C to 270°C for about 6 to 8
hours to get sulphanilic acid technical grade of purity 98%
The said baked bricks are then pre crushed before pulverization of the
sulphanilic acid to obtain the powder of sulphnilic acid and packed as
per the requirement.
An improved process for (he preparation of sulphanilic acid technical
grade according to the present invention has following advantages:-
1. No contamination of iron or any other metal is observed.
2. Various checks and controls are possible which leads to the quality
of the product.
3. The quality of product is homogenous and purity is about 98.9%

COMPLETE AFTER PROVISIONAL

LEFT ON 29 MAY 2006
Patent Application File No. 774 / M / 2005 TITLE OF INVENTION
I) AN IMPROVED PROCESS FOR PREPARTION OF WHITE
SULPHANILIC ACID OF PURIFIED GRADE
II) EMPRIRIC FORMULA :
C6 H5 NH2 S03 H
MW =1 7 3 . 2
CAS NO. 121 -57-3.

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Ill) PREVIOUS PROCESS :

Sulphanilic Acid Technical Grade 98% dissolved in water Ammonia
Alkaline solutions (1Kg 5 Liters Solution), then 1% activated carbon is
added & filter the solution to remove impurities & adding Sulphuric
Acid in the mother liquor to precipitate Sulphanilic Acid Purified Grade
same is Centrifuged & Dried. The water effluents are treated with lime
& sent to common effluent treatment for discharge.

IV) NEW PROCESS:

A fixed amount of Sulphanilic Acid Technical Grade 98.5% is dissolved
in water at elevated temperature & 0.1% activated carbon added &
filter hot mother liquor in filter press to remove water insoluble & then
this filtrate is cooled to room temperature to re crystallize White
Sulphanilic Acid Purified Grade, this material centrifuged & the wet
cake is dried as finished goods.
The liquid portion is recycled for 30 cycles & after 30 cycles the
solution is treated by lime & filtrate is further used for recycling there is
no water effluent.
V) PROCESS FLOW CHART

VI) QUANTITY OF RAW MATERIALS & YIELD

1 kg of White Sulphanilic Acid Purified Grade needs 0.6 Kgs Aniline
Oil as per new process.
VII) MERITS OF INVENTION :

VIII) CLAIMS:
AN IMPROVED PROCESS FOR PREPARTION OF WHITE
SULPHANILIC ACID OF PURIFIED GRADE
1) Sulphanilic Acid Technical Grade 98.5% Dissolved in hot water &
insoluble Filter by Filter Press & recrystallized White Sulphanilic Acid
Purified Grade at room temperature by Cooling.
2) Water is recycled again & again
3) No Water Effluents.
4) The New Invention is Eco-Friendly.
5) The Present invention has very high quality of cleanliness with high
production efficiency & high product purity.

Documents:
774-mum-2005-abstract(31-10-2007).doc (http://ipindiaonline.gov.in
/patentsearch/GrantedSearch
/pdfviewer.aspx?AppNo=Nzc0LW11bS0yMDA1LWFic3RyYWN0KDMxLTEwLTIw
MDcpLmRvYw== )

774-mum-2005-abstract(31-10-2007).pdf (http://ipindiaonline.gov.in
/patentsearch/GrantedSearch
/pdfviewer.aspx?AppNo=Nzc0LW11bS0yMDA1LWFic3RyYWN0KDMxLTEwLTIw

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MDcpLnBkZg== )

774-mum-2005-claims(granted)-(31-10-2007).doc (http://ipindiaonline.gov.in
/patentsearch/GrantedSearch
/pdfviewer.aspx?AppNo=Nzc0LW11bS0yMDA1LWNsYWltcyhncmFudGVkKS0o
MzEtMTAtMjAwNykuZG9j )

774-mum-2005-claims(granted)-(31-10-2007).pdf (http://ipindiaonline.gov.in
/patentsearch/GrantedSearch
/pdfviewer.aspx?AppNo=Nzc0LW11bS0yMDA1LWNsYWltcyhncmFudGVkKS0o
MzEtMTAtMjAwNykucGRm )

774-mum-2005-claims.pdf (http://ipindiaonline.gov.in/patentsearch
/GrantedSearch
/pdfviewer.aspx?AppNo=Nzc0LW11bS0yMDA1LWNsYWltcy5wZGY= )

774-mum-2005-correspondence(31-10-2007).pdf (http://ipindiaonline.gov.in
/patentsearch/GrantedSearch
/pdfviewer.aspx?AppNo=Nzc0LW11bS0yMDA1LWNvcnJlc3BvbmRlbmNlKDMxL
TEwLTIwMDcpLnBkZg== )

774-mum-2005-correspondence(ipo)-(16-08-2007).pdf (http://ipindiaonline.gov.in
/patentsearch/GrantedSearch
/pdfviewer.aspx?AppNo=Nzc0LW11bS0yMDA1LWNvcnJlc3BvbmRlbmNlKGlwb
yktKDE2LTA4LTIwMDcp LnBkZg== )

774-mum-2005-correspondence-received-ver-101106.pdf
(http://ipindiaonline.gov.in/patentsearch/GrantedSearch
/pdfviewer.aspx?AppNo=Nzc0LW11bS0yMDA1LWNvcnJlc3BvbmRlbmNlLXJlY2
VpdmVkLXZlci0xMDEx MDYucGRm )

774-mum-2005-correspondence-received-ver-300605.pdf
(http://ipindiaonline.gov.in/patentsearch/GrantedSearch
/pdfviewer.aspx?AppNo=Nzc0LW11bS0yMDA1LWNvcnJlc3BvbmRlbmNlLXJlY2
VpdmVkLXZlci0zMDA2 MDUucGRm )

774-mum-2005-descripiton (provisional).pdf (http://ipindiaonline.gov.in

/patentsearch/GrantedSearch
/pdfviewer.aspx?AppNo=Nzc0LW11bS0yMDA1LWRlc2NyaXBpdG9uIChwcm92
aXNpb25hbCkucGRm )

774-mum-2005-form 1(31-10-2007).pdf (http://ipindiaonline.gov.in/patentsearch

/GrantedSearch
/pdfviewer.aspx?AppNo=Nzc0LW11bS0yMDA1LWZvcm0gMSgzMS0xMC0yMD
A3KS5wZGY= )

774-mum-2005-form 13(20-12-2007).pdf (http://ipindiaonline.gov.in/patentsearch

/GrantedSearch
/pdfviewer.aspx?AppNo=Nzc0LW11bS0yMDA1LWZvcm0gMTMoMjAtMTItMjAw
NykucGRm )

774-mum-2005-form 13(31-10-2007).pdf (http://ipindiaonline.gov.in/patentsearch

/GrantedSearch
/pdfviewer.aspx?AppNo=Nzc0LW11bS0yMDA1LWZvcm0gMTMoMzEtMTAtMjA
wNykucGRm )

774-mum-2005-form 18(10-11-2006).pdf (http://ipindiaonline.gov.in/patentsearch

/GrantedSearch
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/pdfviewer.aspx?AppNo=Nzc0LW11bS0yMDA1LWZvcm0gMTgoMTAtMTEtMjAw
NikucGRm )

774-mum-2005-form 2(granted)-(31-10-2007).doc (http://ipindiaonline.gov.in

/patentsearch/GrantedSearch
/pdfviewer.aspx?AppNo=Nzc0LW11bS0yMDA1LWZvcm0gMihncmFudGVkKS0o
MzEtMTAtMjAwNykuZG9j )

774-mum-2005-form 2(granted)-(31-10-2007).pdf (http://ipindiaonline.gov.in

/patentsearch/GrantedSearch
/pdfviewer.aspx?AppNo=Nzc0LW11bS0yMDA1LWZvcm0gMihncmFudGVkKS0o
MzEtMTAtMjAwNykucGRm )

774-mum-2005-form 3(31-10-2007).pdf (http://ipindiaonline.gov.in/patentsearch

/GrantedSearch
/pdfviewer.aspx?AppNo=Nzc0LW11bS0yMDA1LWZvcm0gMygzMS0xMC0yMD
A3KS5wZGY= )

774-mum-2005-form 5(31-10-2007).pdf (http://ipindiaonline.gov.in/patentsearch

/GrantedSearch
/pdfviewer.aspx?AppNo=Nzc0LW11bS0yMDA1LWZvcm0gNSgzMS0xMC0yMD
A3KS5wZGY= )

774-mum-2005-form 9(10-04-2006).pdf (http://ipindiaonline.gov.in/patentsearch

/GrantedSearch
/pdfviewer.aspx?AppNo=Nzc0LW11bS0yMDA1LWZvcm0gOSgxMC0wNC0yMD
A2KS5wZGY= )

774-mum-2005-form-1.pdf (http://ipindiaonline.gov.in/patentsearch
/GrantedSearch
/pdfviewer.aspx?AppNo=Nzc0LW11bS0yMDA1LWZvcm0tMS5wZGY= )

774-mum-2005-form-18.pdf (http://ipindiaonline.gov.in/patentsearch
/GrantedSearch
/pdfviewer.aspx?AppNo=Nzc0LW11bS0yMDA1LWZvcm0tMTgucGRm )

774-mum-2005-form-2.doc (http://ipindiaonline.gov.in/patentsearch
/GrantedSearch
/pdfviewer.aspx?AppNo=Nzc0LW11bS0yMDA1LWZvcm0tMi5kb2M= )

774-mum-2005-form-2.pdf (http://ipindiaonline.gov.in/patentsearch
/GrantedSearch
/pdfviewer.aspx?AppNo=Nzc0LW11bS0yMDA1LWZvcm0tMi5wZGY= )

774-mum-2005-form-26.pdf (http://ipindiaonline.gov.in/patentsearch
/GrantedSearch
/pdfviewer.aspx?AppNo=Nzc0LW11bS0yMDA1LWZvcm0tMjYucGRm )

774-mum-2005-form-9.pdf (http://ipindiaonline.gov.in/patentsearch
/GrantedSearch
/pdfviewer.aspx?AppNo=Nzc0LW11bS0yMDA1LWZvcm0tOS5wZGY= )

774-mum-2005-granted.pdf (http://ipindiaonline.gov.in/patentsearch
/GrantedSearch
/pdfviewer.aspx?AppNo=Nzc0LW11bS0yMDA1LWdyYW50ZWQucGRm )

774-mum-2005-power of attorney(17-05-2005).pdf (http://ipindiaonline.gov.in

/patentsearch/GrantedSearch

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