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New method for synthesis and purification of sucrose octasulfate potassium salt

A technology of eight sulfonate esters and a new method, which is applied in the direction of chemical instruments and methods, esterified saccharides, sugar derivatives, etc., can solve the problem that there are no literature and patent reports on the synthesis method of potassium sucrose octasulfonate, and achieve reduction Post-processing difficulty, high yield, good quality effect

Inactive Publication Date: 2018-09-14
FARMASINO PHARMA ANHUI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0002] The synthetic method of potassium sucrose octasulfonate has no literature and patent reports so far

Method used

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] The invention provides a new method for the synthesis and purification of potassium sucrose octasulfonate, comprising the following steps:

[0020] (1) Add 5g sucrose into 150ml triethylamine at 60°C and stir to dissolve, then add 25.6g triethylamine-sulfur trioxide and stir to dissolve, keep warm at 60-65°C for three hours, add 25% potassium hydroxide solution to adjust pH8-9 , and then cooled to 0-5°C for suction filtration;

[0021] (2) Add 30ml of purified water to the filter cake, stir and dissolve at 30-35°C for 20 minutes, cool to 0-5°C, and precipitate powder. This crystallization is repeated three times, and the finished product is white. Vacuum dried to obtain 14.2 g of white powder. The yield is 85%, and the melting point is 160-161°C.

Embodiment 2

[0023] The invention provides a new method for the synthesis and purification of potassium sucrose octasulfonate, the preparation method comprising the following steps:

[0024] (1) Add 5g of sucrose into 150ml triethylamine at 60°C and stir to dissolve, then add 25.6g of triethylamine-sulfur trioxide and stir to dissolve, keep warm at 75-80°C for two hours, add 25% potassium hydroxide solution to adjust the pH to 8- 9, then cool to 0-5 °C and filter with suction.

[0025] (2) Add 30ml of purified water to the filter cake, stir and dissolve at 30-35°C for 20 minutes, cool to 0-5°C, and precipitate powder. This crystallization is repeated three times, and the finished product is white. Vacuum dried to obtain 14.2 g of white powder. The yield is 85%, and the melting point is 160-161°C.

Embodiment 3

[0027] The invention provides a new method for the synthesis and purification of potassium sucrose octasulfonate, the preparation method comprising the following steps:

[0028] (1) Add 5g of sucrose into 150ml triethylamine at 60°C and stir to dissolve, then add 25.6g of triethylamine-sulfur trioxide and stir to dissolve, keep warm at 40-50°C for five hours, add 25% potassium hydroxide solution to adjust the pH to 8- 9, then cool to 0-5 °C and filter with suction.

[0029] (2) Add 30ml of purified water to the filter cake, stir and dissolve at 30-35°C for 20 minutes, cool to 0-5°C, and precipitate powder. So repeated crystallization twice, the finished product is white. Vacuum dried to obtain 15.2 g of white powder. Yield 91%, melting point 160-162°C.

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PUM

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Abstract

The invention discloses a new method for synthesis and purification of sucrose octasulfate potassium salt. The method is as follows: dissolving sucrose in triethylamine, adding a triethylamine-sulphurtrioxide complex for reaction under certain conditions, adjusting pH, cooling, filtering by suction, repeatedly crystallizing with purified water, and drying under vacuum to obtain a pure product. The preparation process disclosed by the invention has mild reaction conditions, simple operation and high yield, and fills the blank of the domestic process.

Description

technical field [0001] The invention relates to the field of synthesis and purification of organic matter, in particular to a new method for the synthesis and purification of potassium sucrose octasulfonate. Background technique [0002] The synthetic method of potassium sucrose octasulfonate has no literature and patent reports so far. This project belongs to the research and development category of the latest cosmetics and food additives. Sucrose ester (SE) is a general term for a class of nonionic surfactants synthesized from sucrose and higher fatty acids, generally in the form of white to ivory powder, block, and wax Solid, or colorless to light yellow viscous or resinous liquid. No odor and peculiar smell, good emulsifying, dispersing, wetting, foaming and washing properties, as well as viscosity adjustment, anti-aging, anti-crystallization and other functions. It is easily absorbed by the human body, non-allergenic, and can be well compounded with many anionic, noni...

Claims

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Application Information

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IPC IPC(8): C07H11/00C07H1/00C07H1/06
CPCC07H1/00C07H1/06C07H11/00
Inventor 燕立波燕立兵王丽
Owner FARMASINO PHARMA ANHUI
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