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Preparation of carboxymethylstach sodium by microwave alcohol-free solid-phase one-step alkali-adding method

A technology of sodium carboxymethyl starch and microwave is applied in the field of preparing sodium carboxymethyl starch by one-step alkali addition method in microwave-free solid phase, which can solve the problems of unbalanced microwave energy of starch, uneven heating inside and outside, and inaccurate temperature control. , to achieve the effect of easier control of reaction temperature, high reaction thermal efficiency and simplified process

Inactive Publication Date: 2010-01-27
SOUTHWEST UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The wet method takes a long time to react, consumes a large amount of organic solvent, and the production cost is high; while the dry method adds alkali twice, which takes a long time and has low efficiency. Pre-drying is required, and when using microwave heating, due to the uneven distribution and volatilization of the dispersant, the starch absorbs microwave energy unevenly, the temperature control is not accurate, and it is easy to produce uneven heating inside and outside, resulting in starch burnt

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0011] Weigh 2 kg of starch and put it into a vertical high-speed mixer at 1400 rpm, add 20 g of sodium chloride, and add 100 g of sodium hydroxide to the starch, stir and mix for 5 minutes, take it out and put it in an oven for alkalization at 20°C 20 minutes; after alkalization of starch, add 60 grams of chloroacetic acid, stir and mix for 8 minutes, place in a microwave reactor of 2 kilowatts for microwave heating etherification reaction, etherification reaction temperature is 55 ° C, reaction time is 8 minutes; after the reaction is completed Take out and pulverize, wash twice with 74%-86% ethanol, and adjust the pH value of sodium carboxymethyl starch to 6.5 with hydrochloric acid, filter and dry at 30°C for 5 hours, and pulverize through a 80-120 mesh sieve to obtain the product. The degree of substitution of the obtained carboxymethyl starch was 0.3.

Embodiment 2

[0013] Weigh 20 kg of starch and put it into a vertical high-speed mixer at 1400 rpm, add 600 g of sodium chloride, and add 4 kg of sodium hydroxide into the starch, stir and mix for 10 minutes, take it out and put it in an oven for alkalization at 30°C 40 minutes; after alkalization of starch, add 2 kg of chloroacetic acid, stir and mix for 15 minutes, place in a 20 kilowatt microwave reactor for microwave heating etherification reaction, etherification reaction temperature 85 ° C, reaction time 6 minutes; after the reaction Take out and pulverize, wash 3 times with 74%-86% ethanol, and adjust the pH value of sodium carboxymethyl starch to 7 with hydrochloric acid, filter and dry at 40°C for 4 hours, and pulverize through a 80-120 mesh sieve to obtain the product. The degree of substitution of the obtained carboxymethyl starch was 0.8.

Embodiment 3

[0015] Weigh 50 kg of starch and put it into a vertical high-speed mixer at 1400 rpm, add 2.5 kg of sodium chloride, and add 15 kg of sodium hydroxide into the starch, stir and mix for 20 minutes, take it out and put it in an oven for alkalization at 40 °C 80 minutes; after alkalization of starch, add 12.5 kg of chloroacetic acid, stir and mix for 25 minutes, place in a microwave reactor of 40 kilowatts for microwave heating etherification reaction, etherification reaction temperature is 105 ° C, reaction time is 10 minutes; the reaction is completed Finally, take out and pulverize, wash 3 times with 74%~86% ethanol, and adjust the pH value of sodium carboxymethyl starch with hydrochloric acid to be 8, filter and dry at 45°C for 3 hours, pulverize through a 80~120 mesh sieve to obtain the product. The degree of substitution of the obtained carboxymethyl starch was 0.4.

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Abstract

The invention provides a method for preparing carboxymethyl starch sodium by the microwave non-alcohol solid phase one step alkalizing method, which makes creative improvements based on the prior dry-process production technique. The method uses micro waves to heat, thereby the reaction efficiency is high, the reaction time is short and the production efficiency is high; moreover, no dispersant is used, thereby while microwave heating, the charring of starches due to overheat does not happen, and the reaction temperature is easier to control; the alkali and chloroactic acid are both respectively added once, thereby simplifying the technological process; organic solvents such as ethanol, etc. are not used in the reaction process, thereby lowering production costs.

Description

Technical field: [0001] The invention relates to the technical field of agricultural product processing, in particular to a method for preparing sodium carboxymethyl starch by a microwave-free alcohol-free solid-phase one-step alkali addition method. Products are widely used in food, textile chemical industry, papermaking, printing and dyeing, petroleum and other fields. Background technique: [0002] Sodium Carboxymethyl Starch (CMS) is one of the main varieties of modified starch, which belongs to ether starch and is a water-soluble anionic polymer compound. Usually used is its sodium salt, also known as CMS-Na, which is characterized by: white or yellow powder, odorless, tasteless, non-toxic, easy to absorb moisture. Soluble in water to form a colloidal solution, stable to light and heat. Insoluble in ethanol, ether, chloroform and other organic solvents. It can be used as an emulsifier, thickener, dispersant, stabilizer, sizing agent, film-forming agent, water-retaini...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08B31/12
Inventor 钟耕张运芳
Owner SOUTHWEST UNIV
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