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Saccharin green environmental-protection production process

A technology of cyclization and raw materials, applied in the direction of organic chemistry, can solve the problems of difficult separation of methanol and inert solvents, energy consumption, and influence on the yield of saccharin

Inactive Publication Date: 2013-07-03
HENAN UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

As far as this step reaction is concerned, the advantage of this method is that no ammonium salt and water are produced, but a part of the methanol removed is mixed with the inert solvent, which makes it difficult to separate methanol from the inert solvent; rectification is required to separate, which is more Consumes energy, increases costs
At the same time, saccharin has a certain solubility in methanol, which affects the yield of saccharin
In short, the process is not yet mature, so most companies in the industry have not adopted it.

Method used

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  • Saccharin green environmental-protection production process
  • Saccharin green environmental-protection production process

Examples

Experimental program
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Effect test

Embodiment 1

[0022] Take 4.000g of methyl o-sulfonate ammonium benzoate and add it to a 50mL three-necked flask, and add 20mL of trimethylbenzene solvent, and fix the three-necked flask on a VDF-101S collector-type constant temperature heating magnetic stirrer. One neck of the three-necked flask Insert a thermometer, install a condensation receiving device on the other neck, start stirring, pass cooling water, and heat. When the temperature of the liquid in the three-necked flask rose to 135°C, it was found that liquid fractions appeared in the condenser, and no fractions were produced after 40 minutes of constant temperature reaction. Then the temperature was raised slowly up to 140°C, during which no distillate was produced, so the heating was stopped and cooled to room temperature.

[0023] Add saturated NaHCO into the three-neck flask 3 When the solids in the solution bottle are completely dissolved and the pH=5, stop adding alkali, transfer and stand still for liquid separation. The...

Embodiment 2

[0027] Take 5.000g of methyl o-sulfonate ammonium benzoate and add it to a 50mL three-necked flask, and add 25mL of trimethylbenzene solvent, and fix the three-necked flask on the VDF-101S collector-type constant temperature heating magnetic stirrer. One neck of the three-necked flask Insert a thermometer, install a condensation receiving device on the other neck, start stirring, pass cooling water, and heat. When the temperature of the liquid in the three-necked flask rose to 135°C, it was found that there was a liquid fraction in the condenser, and no fraction was produced after 40 minutes of constant temperature reaction. Then the temperature was raised slowly up to 140°C, during which no distillate was produced, so the heating was stopped and cooled to room temperature.

[0028] Add saturated NaHCO into the three-neck flask 3 When the solids in the solution bottle are completely dissolved and the pH=5, stop adding alkali, transfer and stand still for liquid separation. T...

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Abstract

The invention relates to a green environmental-protection synthetic route of benzosulfimide, an intermediate of sodium saccharin green environmental-protection production process. According to the process route, o-ammonium sulfonate methyl benzoate mixed in an assigned solvent or its dry material is used as a raw material; a three-in-one reaction of dehydration, cyclization, and dealcoholization is completed in one step in a reactor at a certain temperature to finally synthesize saccharin, and further to produce sodium saccharin. Methanol and water obtained after dehydration and dealcoholization are condensed and recovered together without rectification for recycle in esterification reactions, which reaches the effects of consumption reduction, emission reduction, and environmental protection. Therefore, the invention has high application value in sodium saccharin green environmental-protection production process.

Description

technical field [0001] The invention relates to a green and environment-friendly production process route of o-sulfonylbenzimide (ie, saccharin). The process route uses a new compound o-sulfonate ammonium benzoate as a raw material, and through a special reaction, one-step synthesis of o-sulfonylbenzimide. Background technique [0002] In the 134 years since Constantin Fahlberg and Ira Remsen invented saccharin in 1877, although many experts have been conducting research on the production process of saccharin, and achieved a lot of results, there are mainly two major process routes: one is The "toluene method" process route invented by Constantin Fahlberg and Ira Rensen; the other is the "phthalic anhydride method" process route created by Chinese scientists. There are different degrees of problems in the environmental protection of these two kinds of process routes. There is also a process invented in recent years to generate saccharin from methyl o-sulfonamide benzoate t...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D275/06
Inventor 赵文善张磊齐化多崔元臣刘红张滨楚楠楠赵恩旭常守欣齐天勤机
Owner HENAN UNIVERSITY