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Infra-red synthesis of crosslinked carboxymethyl fecula

A technology of cross-linked carboxymethyl and synthesis method, which is applied in the field of infrared synthesis of cross-linked carboxymethyl starch, which can solve the problems of difficult product purification and recovery, uneven reaction, and high product cost, and achieve strong infrared penetration and reaction Easy and uniform effect

Inactive Publication Date: 2008-04-16
SOUTH CHINA UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The water-based method can only produce products with a degree of substitution of less than 0.07. This is because carboxymethyl starch with a higher degree of substitution is easy to gelatinize in cold water, and the product is difficult to purify and recover, and the amount of waste water is large, causing environmental pollution.
Adding organic solvents such as ethanol, propanol or isopropanol to the organic solvent method prevents the gelatinization of carboxymethyl starch in the reaction, and can prepare products with high substitution degree and high purity, which is a production method widely used in industry ; But the disadvantage is that more organic solvents are needed, the recovery is difficult and the recovery rate is low, and the product cost is high
The dry method does not use organic solvents, and the preparation time is short; but the equipment requirements are relatively high, it is difficult to control, and the reaction is uneven, and the product contains impurities such as residual reaction reagents.
The semi-dry method is between the organic solvent method and the dry method, saving cost, no pollution, uniform and easy to control the reaction, and the obtained product can still maintain the original starch granule structure, has good fluidity, is easy to dissolve in water and does not agglomerate; but the product still contains some impurities

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] Add 17 parts of monochloroacetic acid to the container, slowly neutralize with 44 parts of 30% sodium hydroxide, add 50 parts of ethanol solution with a volume ratio of 70% by volume and 3.0×10 -6 Parts of epichlorohydrin, mix well. Add 50 parts each of tapioca starch and potato starch, and stir evenly. Stir at room temperature for 30 min. Centrifuge the mixture in the container to remove a small amount of liquid. Crush the filter cake, place it in an infrared reactor, control the reaction temperature to 120°C, and complete the reaction within 40 minutes, while the material is dried. The product is obtained by crushing. The resulting 2% aqueous solution of cross-linked carboxymethyl starch has a viscosity of 2087±92 mPa·s measured by a rotational viscometer at 30° C. (measured 3 times).

Embodiment 2

[0034] Add 23 parts of monochloroacetic acid into the container, slowly add 52 parts of 30% sodium hydroxide for neutralization, add 50 parts of ethanol solution with 80% volume ratio after cooling, add 10 parts dropwise after stirring well -5 Parts of epichlorohydrin, mix well. Add 33.3 parts each of broad beans, plantain taro, and rice starch, and stir evenly. Stir continuously for 40 min at 20°C for pre-reaction. The pre-reacted starch material is centrifuged to remove excess liquid. Crush the filter cake and place it in an infrared reactor. The reaction temperature is controlled at 125-128° C. and the time is 35 minutes to complete the etherification and cross-linking reactions. The product is obtained by crushing. The resulting 2% aqueous solution of cross-linked carboxymethyl starch had a viscosity of 1867 mPa·s measured by a rotational viscometer at 30° C. (average value of three measurements).

Embodiment 3

[0036] Add 15 parts of monochloroacetic acid into the container, slowly add 58 parts of 30% sodium hydroxide for neutralization, add 50 parts of ethanol solution with volume ratio of 60% by volume and 6.6×10 -6 Parts of epichlorohydrin, mix well. Add 100 parts of pea starch, and continue stirring at 38°C for 20 minutes to carry out pre-reaction. After the pre-reaction is completed, centrifugal separation is carried out, and the resulting filter cake is crushed, placed in an infrared reactor at a reaction temperature of 130° C., and reacted for 30 minutes to complete the etherification and cross-linking reaction. The product is obtained by crushing. The resulting 2% aqueous solution of cross-linked carboxymethyl starch had a viscosity of 2293 mPa·s measured by a rotational viscometer at 30° C. (average value of three measurements).

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Abstract

The present invention relates to an infrared synthetic method of a cross-linked carboxymethyl starch, comprising (1) adding the monochloroacetic acid into the container, neutralizing the monochloroacetic acid by the sodium hydroxide, cooling the solution, adding the ethanol solution, dripping the chloroepoxy propane, and then adding the primary starch; (2) stirring and pre-reacting the materials in the container, then pouring the mixture out from the container, centrifuging the mixture to remove a little liquid, and then breaking the filter cake; (3) putting the broken filter cake into the infrared reactor, auto reacting at a constant temperature to obtain the modified starch, putting the starch out to crush. The invention uses the technology of infrared catalyzing and etherifying as well as heating and drying at the same time to accelerate the reaction, improve the product property, increase the viscosity of the aqueous solution of carboxymethyl starch and broaden the range of use of the product. And at the same time, the invention reduces the consumption of the organic solvent, has no need to recycle the alcohol, reduces the energy consumption, shortens the reaction time, raises efficiency, and reduces the production cost of the cross-linked carboxymethyl starch.

Description

technical field [0001] The invention relates to starch modification technology, in particular to an infrared synthesis method of cross-linked carboxymethyl starch. technical background [0002] Starch can be modified single-time or compound-modified. Starch carboxymethylation and crosslinking are two types of modification methods developed earlier. Carboxymethylation refers to the etherification reaction between starch and monochloroacetic acid in the presence of sodium hydroxide, which is a bimolecular nucleophilic substitution reaction. The alcoholic hydroxyl group in the glucose unit is replaced by carboxymethyl. The reaction process is as follows: [0003] (1) Starch-OH+NaOH→Starch-O-Na+H 2 o [0004] (2) Starch-O-Na+ClCH 2 COONa→starch-O-CH 2 COONa+NaCl [0005] After carboxymethylation of starch, the starch has strong hydrophilicity, and the degree of substitution above 0.1 can be dissolved in water at low temperature, and a clear and transparent sticky starch pa...

Claims

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Application Information

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IPC IPC(8): C08B31/04C08J3/24
Inventor 温其标黄国平王磊
Owner SOUTH CHINA UNIV OF TECH
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