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Method for producing saccharin sodium

A production method and technology of sodium saccharin, applied in the field of food additive production, can solve the problems of polluted air, high labor intensity, fast heating, etc., and achieve the effects of stable reaction process, improved working environment, and reduced labor intensity.

Active Publication Date: 2005-09-07
天津北方食品有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method is labor-intensive, and a large amount of 25 kilograms of raw materials per bag needs to be put into a height of two meters; at the same time, the cost is high, and the current market price of 31% hydrochloric acid is 550 yuan / ton, especially when solid sodium bicarbonate is added, the local heating is fast and the temperature is high. , the reaction speed is fast and the reaction is violent, resulting in the rapid evaporation of the toxic substance toluene to pollute the air, it is difficult to ensure a good working environment for the operator, and at the same time the pH value is difficult to measure and control, which affects the preparation quality of the intermediate product of sodium saccharin

Method used

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  • Method for producing saccharin sodium
  • Method for producing saccharin sodium
  • Method for producing saccharin sodium

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] A method for producing sodium saccharin, comprising the reaction steps of amidation, Hofmann degradation, lipidation, diazotization, replacement, chlorination, ammoniation, acid precipitation, alkalization, and decolorization, followed by filtration, concentration, crystallization, and drying to get the finished product. The production method of sodium saccharin mainly improves the preparation steps of acid analysis and alkalization reaction, and obtains an intermediate ammoniated solution from the ammoniation reaction as the main component of the acid analysis and alkalization reaction;

[0019] The ammoniation reaction formula is:

[0020]

[0021] Acid analysis, alkalization reaction steps are as follows:

[0022] (1) The ammoniated solution and the toluene washing water prepared after the ammoniation reaction are pumped into the acid analysis and alkalization reaction kettle and fully stirred evenly;

[0023] (2) Add water to adjust the concentration of ammonia...

Embodiment 2

[0037] Acid analysis, alkalization reaction steps are as follows:

[0038] (1) The ammoniated solution and the toluene washing water prepared after the ammoniation reaction are pumped into the acid analysis and alkalization reaction kettle and fully stirred evenly;

[0039] (2) Add water to adjust the concentration of ammoniated solution and toluene washing solution to 1.05~1.06kg / m 3 , measure the volume of the ammoniated solution, the ammoniated solution is 1500L according to the ratio, add 375L of toluene and continue to stir, the temperature is 18°C-20°C;

[0040] (3) Add 375L of sulfuric acid with a concentration of 15% in the stirring, the time is 10-15 minutes, the temperature is below 15-30°C, the measured pH is between 1-4, and the insoluble colloidal particles are precipitated under sufficient stirring, and the insoluble particles are observed. The surface of the colloidal particles should be smooth and about the size of red bean grains; the end point of acid precip...

Embodiment 3

[0050] Acid analysis, alkalization reaction steps are as follows:

[0051] (1) The ammoniated solution and the toluene washing water prepared after the ammoniation reaction are pumped into the acid analysis and alkalization reactor and fully stirred evenly;

[0052] (2) Add water to adjust the concentration of ammoniated solution and toluene washing solution to 1.05~1.06kg / m 3 , measure the volume of the ammoniated solution, the ammoniated solution is 1700L according to the ratio, add 425L of toluene and continue to stir, the temperature is 18°C-20°C;

[0053](3) Add 425 L of sulfuric acid with a concentration of 30% in the stirring, the time is 10-15 minutes, the temperature is 15-30 ° C, the measured pH is between 1 and 4, the insoluble colloidal particles are precipitated under sufficient stirring, and the insoluble colloids are observed. The grain surface should be smooth and about the size of a red bean grain; the end point of acid precipitation should be clarified by ac...

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Abstract

The invention relates to a method for producing saccharin sodium comprising the steps of acyl ammonization, Hofmann degradation, diazotization, displacement, chloridization, ammonization, acid out, alkalization, de-coloration, filtering, concentrating, crystallization and drying, wherein the acid out and quaternization mainly include, charging 15-30% sulfuric, chaging toluene for balling up the insoluble, rinshing till the sour water is clear, charging 10-30% edible sodium carbonate solution into insoluble colloidal particles, elevated temperature simultaneously, stirring and stewing for stratification.

Description

technical field [0001] The invention relates to a method for producing a food additive, in particular to a method for producing sodium saccharin. Background technique [0002] At present, sodium saccharin is used as a food additive in a wide range of applications. The production method mainly includes amidation, Hoffman degradation lipidation, diazotization, replacement, chlorination, ammoniation, acid analysis, alkalization and decolorization reaction steps, and then the finished product is obtained through filtration, concentration, crystallization and drying. Wherein the acid analysis and alkalization production method generally adopted now is to use 31% hydrochloric acid to precipitate the insoluble, and utilize solid sodium bicarbonate to neutralize the insoluble colloidal particles. This method is labor-intensive, and a large amount of 25 kilograms of raw materials per bag needs to be put into a height of two meters; at the same time, the cost is high, and the current...

Claims

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Application Information

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IPC IPC(8): A23L29/00C07D275/06
Inventor 刘立杰马近贤陈树武刘玉斌
Owner 天津北方食品有限公司
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