Preparation method of oxidized starch containing aldehyde group on C6 position of glucose unit

A technology for oxidizing starch and glucose, which is applied to the preparation of oxidized starch containing aldehyde groups in the 6-position of starch molecules. Effect of poor oxidation selectivity, reduced nitric acid consumption, high content of aldehyde and carboxyl groups

Inactive Publication Date: 2014-02-05
TIANJIN VOCATIONAL INST
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Problems solved by technology

[0008] The purpose of the present invention is to provide a method for preparing aldehyde group-containing oxidized starch on the C6 position of glucose unit in starch molecules, which can control the content of aldehyde groups and carboxyl groups in oxidized starch, prevent a large number of starch molecules from breaking and degrading, and overcome the existing preparation method of oxidized starch Poor process oxidation selectivity, large consumption of oxidant and high production cost

Method used

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  • Preparation method of oxidized starch containing aldehyde group on C6 position of glucose unit
  • Preparation method of oxidized starch containing aldehyde group on C6 position of glucose unit
  • Preparation method of oxidized starch containing aldehyde group on C6 position of glucose unit

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Experimental program
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Effect test

Embodiment 1-4

[0031] Add 5mL, 10mL, 15mL, and 20mL of concentrated hydrochloric acid to four parts of 30% starch milk (270g) respectively, so that the concentration of hydrochloric acid is 0.25, 0.50, 0.75, and 1.0mol / L respectively, and slowly introduce air at 45°C , 28.5 mL of 65% nitric acid was added dropwise within 3 hours, and the oxidized starch was prepared by reacting for 4 hours. The content of carboxyl and aldehyde groups in oxidized starch and the viscosity of the solution were determined by sampling as shown in Table 1.

[0032] Table 1 Effect of hydrochloric acid concentration on carboxyl and aldehyde content in oxidized starch

[0033]

Embodiment 5-9

[0035] Add 15mL of concentrated hydrochloric acid to five parts of 30% starch milk (270g) respectively to make the concentration of hydrochloric acid 0.75mol / L, slowly pass air at 45°C, add 65% nitric acid 22mL, 25mL, 28.5mL, 32mL and 35.7mL, so that the molar ratio of nitric acid to starch was 0.6, 0.7, 0.8, 0.9 and 1.0 respectively, reacted for 4h to prepare oxidized starch, and sampled to determine the content of carboxyl and aldehyde groups in oxidized starch as shown in Table 2.

[0036] Table 2 Effect of nitric acid dosage on carboxyl and aldehyde content in oxidized starch

[0037]

Embodiment 10-15

[0039] Add 15 mL of concentrated hydrochloric acid to six parts of 30% starch milk (270 g) to make the concentration of hydrochloric acid 0.75 mol / L, and slowly introduce air at 45 ° C, within 1, 2, 3, 4, and 5 hours respectively 28.5mL of 65% nitric acid was added dropwise, so that the molar ratio of nitric acid to starch was 0.8, and the oxidized starch was prepared by reacting for 4h, and the content of carboxyl and aldehyde groups in the oxidized starch was sampled and determined as shown in Table 3.

[0040] Table 3 Effect of reaction time on carboxyl and aldehyde content in oxidized starch

[0041]

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Abstract

The invention discloses a preparation method of oxidized starch containing an aldehyde group in a starch molecule. The preparation method comprises the steps: mixing nitric acid and diluted hydrochloric acid to generate a nitryl chloride strong oxidizer, and oxidizing 40-85% of primary hydroxy on C6 positions of glucose units in the starch molecule with the nitryl chloride strong oxidizer, wherein the mole number of the aldehyde group in the generated oxidized starch is 0.15-0.25, and the mole number of the carboxyl group is 0.25-0.60; and in the oxidation process, air is introduced to a reactor, and nitrosyl chloride generated by reduction of nitryl chloride is oxidized by oxygen to regenerate nitryl chloride, so that starch oxidation process is repeatedly performed. The preparation method has the advantages that the aldehyde group and carboxyl group contents in the oxidized starch can be controlled, the application range of the oxidized starch is widened, the problems of poor oxidation selectivity, large oxidizer consumption and high production cost in the traditional preparation process of the oxidized starch are overcome, and the preparation method has wide application prospects.

Description

technical field [0001] The invention relates to a preparation method of oxidized starch, in particular to a preparation method of oxidized starch containing aldehyde groups in the 6-position of starch molecules, which belongs to the field of fine chemical industry. Background technique [0002] Starch is a kind of biodegradable natural macromolecular compound with wide sources, low price and semi-crystalline granular polymer. The glucose units that make up starch have hydroxyl groups at the C2, C3 and C6 positions, and their oxidation can change the properties of starch a lot. Starch has the advantages of environmental protection and low price, and has been widely used in the fields of papermaking, textiles, adhesives and building interior wall coatings. In order to expand the application range of starch and improve its performance, a series of oxidized starches with different structures and properties have been developed at home and abroad. Oxidized starch generally refer...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08B31/18
Inventor 宋超先于韶梅李建生朱虹鲍辰刘彦峰
Owner TIANJIN VOCATIONAL INST
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