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Chitosan oligosaccharide intermediate, preparation method thereof and application of chitosan oligosaccharide intermediate in preparation of phosphonate water reducing agent

A technology of chitosan oligosaccharide and intermediate, which is applied in the field of concrete admixtures, can solve the problems of water-soluble and water-reducing performance decline of water-reducing agent, application limitation, etc.

Active Publication Date: 2020-07-07
JIANGSU SOBUTE NEW MATERIALS +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] However, due to the large molecular weight of chitosan itself, the viscosity-average molecular weight of chitosan with better water solubility is between 50,000 and 190,000, and the molecular weight of the prepared water reducer is larger, and the larger molecular weight is likely to cause water solubility of the water reducer. And the decline of water reducing performance, so the application of this kind of polyhydroxyl and polyamine-based chitosan in water reducing agent is greatly restricted

Method used

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  • Chitosan oligosaccharide intermediate, preparation method thereof and application of chitosan oligosaccharide intermediate in preparation of phosphonate water reducing agent
  • Chitosan oligosaccharide intermediate, preparation method thereof and application of chitosan oligosaccharide intermediate in preparation of phosphonate water reducing agent
  • Chitosan oligosaccharide intermediate, preparation method thereof and application of chitosan oligosaccharide intermediate in preparation of phosphonate water reducing agent

Examples

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preparation example 1

[0049] Weigh 100.0 parts of ethanol as an initiator, add 0.02 part of catalyst DMC, seal the reaction vessel, and replace with nitrogen for 3 times. Raise the temperature to 100°C, and feed 20.0 parts of propylene oxide. After the induced reaction occurs (the temperature in the kettle rises and the pressure drops), continue to feed 230.0 parts of propylene oxide, and control the reaction temperature between 120 and 140°C. ≤0.4MPa, heat preservation reaction for 10 minutes after feeding, then feed 1820.0 parts of ethylene oxide, heat insulation reaction for 10 minutes after feeding, finally feed 200.0 parts of epichlorohydrin, heat insulation reaction for 30 minutes after feeding, and cool down to After discharge at 80°C, 2693.0 parts of colorless and transparent polyether was obtained, denoted as P-1. After testing, the number average molecular weight of the polyether was Mn=1035, and the molecular weight distribution PDI=1.08.

[0050] Similarly, the following chlorinated pol...

preparation example 2

[0059] Weigh 100.0 parts of chitosan oligosaccharide with number average molecular weight Mn=483, add 40.0 parts of solvent water, 5.0 parts of catalyst solid heteropolyacid, and 67.9 parts of phosphorous acid, and start stirring. Raise the temperature to 80°C, stir until the materials are fully mixed, add 24.8 parts of paraformaldehyde, seal the reaction kettle, raise the temperature to 100°C, and keep it warm for 15 hours. After the reaction was completed, the catalyst solid heteropolyacid was separated by vacuum filtration, and 103.5 parts of 32% NaOH aqueous solution was added to the filtered liquid to obtain the chitosan oligosaccharide intermediate.

[0060] Add 1029.6 parts of P-5 polyether to the chitosan oligosaccharide intermediate, raise the temperature to 150°C, and keep warm for 15 hours to obtain the finished product of phosphonic acid-based water reducer, which is denoted as PCA-1. After testing, the weight average molecular weight of the water reducer Mw= 5672,...

preparation example 3

[0062] Weigh 100.0 parts of chitosan oligosaccharide with number average molecular weight Mn=1610, add 50.0 parts of solvent water, 8.0 parts of catalyst solid superacid, and 50.9 parts of phosphorous acid, and start stirring. Raise the temperature to 80°C, stir until the materials are fully mixed, add 60.4 parts of 37% formaldehyde, seal the reaction kettle, raise the temperature to 120°C, and keep it warm for 10 hours. After the reaction was completed, the catalyst solid superacid was separated by vacuum filtration, and 77.6 parts of 32% NaOH aqueous solution was added to the filtered liquid to obtain a wine-red oligochitosan intermediate solution.

[0063] Add 1246.3 parts of P-4 polyether to the chitosan oligosaccharide intermediate, raise the temperature to 130°C, and keep it warm for 10 hours to obtain a tan phosphonic acid-based water reducer, which is denoted as PCA-2. After testing, the weight average of the water reducer is Molecular weight Mw=21014, molecular weight...

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Abstract

The invention provides a chitosan oligosaccharide intermediate, a preparation method thereof and an application of the chitosan oligosaccharide intermediate in synthesis of a phosphate-based water reducing agent. The chitosan oligosaccharide intermediate is structurally characterized in that a main chain structure is a-C-O-bonded six-membered oxygen-containing heterocyclic ring structure, whereinthe six-membered oxygen-containing heterocyclic ring structure is provided with polyhydroxy and amido, and the amido is provided with a phosphorous acid group bridged through methylene. The phosphate-based water reducing agent takes chitosan oligosaccharide as a main chain; a phosphonic acid-based adsorption group and a polyether side chain are grafted on the chitosan oligosaccharide; the main chain structure is a six-membered ring structure connected through a C-O bond, and the ring structure has a polyhydroxy group. The phosphate-based water reducing agent has workability improvement and retarding performance.

Description

technical field [0001] The invention relates to a chitosan oligosaccharide intermediate, a preparation method thereof and an application thereof for preparing a phosphonate water reducer, belonging to the field of concrete admixtures. Background technique [0002] Chitosan, also known as deacetylated chitin, is obtained by deacetylation of chitin (chitin), which exists widely in nature, and its chemical name is polyglucosamine (1-4)-2-amino-B-D glucose. Used in medicine, food industry, daily chemical industry, agriculture, biotechnology and sewage treatment and other fields. The molecular structure of chitosan contains polyhydroxyl and amino groups, which provides more possibilities for the chemical modification and research of chitosan, and has gradually attracted the attention and research of researchers in the concrete superplasticizer industry. [0003] Patent CN108383956A reports a preparation method of polycarboxylate water reducer containing chitosan. First react th...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08B37/08C08G65/335C08G81/00C07H5/06C07H1/00C04B24/32C04B24/38C04B103/30
CPCC08B37/003C08G65/3356C08G81/00C07H5/06C07H1/00C04B24/246C04B2103/302
Inventor 马建峰刘加平王涛亓帅范士敏王兵韩正王衍伟
Owner JIANGSU SOBUTE NEW MATERIALS
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