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A kind of preparation method of starch sulfate ammonium salt

A technology of ester ammonium salt and starch, which is applied in the field of starch sulfate ammonium salt and its preparation, can solve the problems of high cost of sulfonating agent and solvent, low degree of substitution of sulfonic acid groups in the product, strong corrosiveness of sulfonating agent, etc. Achieve low raw material cost and equipment requirements, no odor to human body toxicity, and reduce environmental pollution

Inactive Publication Date: 2018-06-26
殷鸽
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The biggest disadvantages of these three methods are: the strong corrosiveness or toxicity of the sulfonating agent; the serious degradation of starch molecules and complicated post-treatment;
Although the maximum degree of substitution of the product sulfonic acid group has been improved by these two methods, the cost of the sulfonating agent and solvent used is all expensive, and the toxicity of the pyridine used is also very high.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] In the kneader, first put in sulfamic acid according to the molar ratio of starch sugar unit and sulfamic acid as 1:1.2, then put in urea according to the molar ratio of starch sugar unit and urea as 1:0.8, mix and heat to 150°C After it is completely melted, put in cornstarch with a starch sugar unit molar ratio of 1:1 and a purity of 87%. After constant temperature reaction until no water vapor is generated in the kettle, cool down to room temperature and use ammonia water to neutralize the residual acid in the reaction system to pH 8. Add ethanol with a purity of 95% to precipitate a precipitate, centrifuge at a centrifugal speed of 3500 rpm, and dry at 40°C to obtain a starch sulfate ammonium salt product with a sulfonic acid group substitution degree of 1.0.

Embodiment 2

[0024] Put sulfamic acid into the kneader according to the molar ratio of starch sugar unit and sulfamic acid as 1:1.0, then put urea into the kneader according to the molar ratio of starch sugar unit and urea as 1:1.2, mix and heat to 120°C, After it is completely melted, put in rice starch with a molar ratio of starch and sugar units of 1:1 and a purity of 90.2%, and react at a constant temperature until no water vapor is generated in the kettle, then cool down to room temperature and use ammonia water to neutralize the residual acid in the reaction system to pH 10 , add purity 95% ethanol to precipitate out, centrifuge at a centrifugal speed of 5000 rpm, and dry at 50°C to obtain a starch sulfate ammonium salt product with a sulfonic acid group substitution degree of 0.96.

Embodiment 3

[0026] Put sulfamic acid in the kneader according to the molar ratio of starch sugar unit to sulfamic acid as 1:1.5, then put urea into the kneader according to the molar ratio of starch sugar unit to urea as 1:1.0, mix and heat to 140°C, After it is completely melted, put in tapioca starch with a molar ratio of 1:1 and a purity of 96.5% tapioca starch, and react at a constant temperature until no water vapor is generated in the kettle, then cool down to room temperature and use ammonia water to neutralize the residual acid in the reaction system to pH 10 , add 95% pure ethanol to precipitate out the precipitate, centrifuge at a centrifugal speed of 6000 rpm, and dry at 45°C to obtain a starch sulfate ammonium salt product with a degree of substitution of 0.98.

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PUM

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Abstract

The invention relates to a preparing method for starch sulphate ammonium salt.The preparing method specifically comprises the steps that in a kneading machine, a starch sugar unit is put into sulfamic acid at the mole ratio of the starch sugar unit to sulfamic acid being 1:0.5-1:1.5, and a catalyst is put into the mixture at the mole ratio of the starch sugar unit to the catalyst being 1:0.25-1:1.5; the mixture is mixed and heated to 100-150 DEG C, starch is put into the mixture after the mixture is completely melt at the mole ratio of the starch sugar unit to starch being 1:1, a reaction is carried out at a constant temperature until no water vapor is generated in a reaction kettle, and then the mixture is cooled to the room temperature; ammonium hydroxide is used for neutralizing acid remaining in the reaction system to reach the pH of 8-10, ethyl alcohol with the purity of 95% is added to separate precipitate out, centrifugal separation is carried out at the centrifugal speed of 3500-9000 turns / min, drying is carried out at 40-50 DEG C, and a starch sulphate ammonium salt product is obtained.By means of the preparing method, the sulfonation degree of the product is increased, strong degradation on starch and the strong corrosion effect on equipment can be avoided by means of the adopted raw materials, and the preparing method has the advantages that operation is convenient, production cost is reduced while environment pollution is relieved, and the raw material cost and the requirement for equipment are low.

Description

technical field [0001] The invention belongs to the technical field of preparation of modified starch, in particular to a starch sulfate ammonium salt and a preparation method thereof. Background technique [0002] Starch sulfate, also known as sulfonated starch, is the introduction of sulfonic acid groups -SO 3 A starch derivative obtained from H. Starch sulfate has a variety of characteristics different from other modified starches, and has been well used in many fields, especially in food, medicine and other fields. For example, the hydrosol formed by starch sulfate still shows good stability below the freezing temperature, and can be used as a thickener for frozen foods and certain pharmaceuticals. The most interesting property of starch sulfate is the biological activity discovered in recent years. For example, some starch sulfates have a strong affinity for proteins and have a heparin-like anticoagulant effect, which can be used as a cheap substitute for natural hep...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08B31/06
CPCC08B31/06C08B31/063
Inventor 殷鸽
Owner 殷鸽
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