Title of Invention

IMPROVED PROCESS FOR THE PREPARATION OF SULPHANILIC ACID TECHNICAL GRADE

Abstract

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.

Full Text

FORM - 2 THE PATENTS ACT, 1970 (39 OF 1970) & THE PATENTS RULES, 2003 Provisional Specification (See Section 10 and rule 13) “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 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. 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

774-mum-2005-abstract(31-10-2007).pdf

774-mum-2005-claims(granted)-(31-10-2007).doc

774-mum-2005-claims(granted)-(31-10-2007).pdf

774-mum-2005-claims.pdf

774-mum-2005-correspondence(31-10-2007).pdf

774-mum-2005-correspondence(ipo)-(16-08-2007).pdf

774-mum-2005-correspondence-received-ver-101106.pdf

774-mum-2005-correspondence-received-ver-300605.pdf

774-mum-2005-descripiton (provisional).pdf

774-mum-2005-form 1(31-10-2007).pdf

774-mum-2005-form 13(20-12-2007).pdf

774-mum-2005-form 13(31-10-2007).pdf

774-mum-2005-form 18(10-11-2006).pdf

774-mum-2005-form 2(granted)-(31-10-2007).doc

774-mum-2005-form 2(granted)-(31-10-2007).pdf

774-mum-2005-form 3(31-10-2007).pdf

774-mum-2005-form 5(31-10-2007).pdf

774-mum-2005-form 9(10-04-2006).pdf

774-mum-2005-form-1.pdf

774-mum-2005-form-18.pdf

774-mum-2005-form-2.doc

774-mum-2005-form-2.pdf

774-mum-2005-form-26.pdf

774-mum-2005-form-9.pdf

774-mum-2005-granted.pdf

774-mum-2005-power of attorney(17-05-2005).pdf