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Polycarboxylate superplasticizer with modified cyclodextrin side chain structure and preparation method of polycarboxylate superplasticizer with modified cyclodextrin side chain structure

A technology of cyclodextrin and polycarboxylic acid, which is applied in the field of concrete, can solve the problems of difficulty in guaranteeing the quality of concrete, reduction of water retention and viscosity increase effect, and impact on concrete strength, etc., achieving no effect on setting time, excellent stability, and clean slurry flow The effect of small degree changes

Active Publication Date: 2018-08-07
CCCC SHEC WUHAN PORT NEW MATERIALS +1
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  • Abstract
  • Description
  • Claims
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Problems solved by technology

[0006] These patents have successfully prepared polycarboxylate superplasticizers with cyclodextrin side chains. The cyclodextrin side chains in the molecule are connected to the main chain through ester groups, and the ester groups are in the alkalinity of concrete. It is easy to hydrolyze in the environment and release cyclodextrin molecules. Cyclodextrin molecules have a retarding effect, and the rate of hydrolysis release cyclodextrin molecules is related to the pH and temperature of concrete. With the difference of pH and temperature, the hydrolysis rate is inconsistent. The amount of cyclodextrin molecules released is more or less, which makes the setting time of concrete longer or shorter, affects the formation of concrete strength, and the quality of concrete is difficult to guarantee; in addition, the hydrogen bond between polycarboxylic acid molecules is weakened, and water retention is increased. sticky effect reduction

Method used

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  • Polycarboxylate superplasticizer with modified cyclodextrin side chain structure and preparation method of polycarboxylate superplasticizer with modified cyclodextrin side chain structure
  • Polycarboxylate superplasticizer with modified cyclodextrin side chain structure and preparation method of polycarboxylate superplasticizer with modified cyclodextrin side chain structure
  • Polycarboxylate superplasticizer with modified cyclodextrin side chain structure and preparation method of polycarboxylate superplasticizer with modified cyclodextrin side chain structure

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preparation example Construction

[0026] A kind of preparation method of the polycarboxylate water-reducer of modified cyclodextrin side chain structure of the present invention, comprises the following steps:

[0027] 1) Add prenyl alcohol polyoxyethylene ether, allyl polyethylene glycol and deionized water into the reaction kettle, heat and dissolve at a temperature of 20-80°C to obtain a solution;

[0028] 2) Add the deionized aqueous solution of persulfate and the deionized water mixed solution of methacrylic acid and cyclodextrin allyl etherified monomer dropwise to the solution A at the same time, and carry out the heat preservation reaction at a temperature of 60-80°C 1.0~2.0h and cooling to room temperature to obtain solution B; the persulfate is selected from sodium persulfate, potassium persulfate or ammonium persulfate;

[0029] 3) Add liquid caustic soda with a mass fraction of 30% in solution B, adjust the pH value to 6-8, and obtain a polycarboxylate water reducer with a modified cyclodextrin sid...

Embodiment 1

[0031] (1) Synthesis of cyclodextrin allyl etherified monomer: use N, N-dimethylformamide (DMF) as solvent, add β-cyclodextrin into the reaction kettle, heat and dissolve completely, and then add to the reaction Add sodium hydroxide (NaOH) into the kettle as a catalyst, and after stirring for 1 hour, slowly add bromopropylene into the reaction kettle, react for 48 hours in an ice-water bath at 0°C, precipitate with acetone, and wash several times with absolute ethanol, vacuum Remove the solvent by suction filtration, and finally vacuum-dry to obtain the cyclodextrin allyl etherified monomer in the form of white powder. Wherein, the molar ratio of bromopropene and β-cyclodextrin is 1:1.

[0032] (2) Polymerization reaction: add isopentenol polyoxyethylene ether with a molecular weight of 2080, allyl polyethylene glycol with a molecular weight of 454 and deionized water into the reaction kettle, heat and dissolve at a temperature of 20-80°C Obtain A solution; add the deionized ...

Embodiment 2

[0034](1) Synthesis of cyclodextrin allyl etherification monomer: use pyridine as solvent, add β-cyclodextrin into the reaction kettle, after heating and dissolving completely, add potassium hydroxide as catalyst into the reaction kettle, stir thoroughly After 1 hour, slowly add allyl bromide into the reaction kettle, react at 10°C for 24 hours, precipitate with acetone, wash repeatedly with absolute ethanol several times, remove the solvent by vacuum filtration, and finally obtain a white powdery ring by vacuum drying. Dextrin allyl etherified monomer, wherein the molar ratio of bromopropene and β-cyclodextrin is 1:1.

[0035] (2) Polymerization reaction: add isopentenol polyoxyethylene ether with a molecular weight of 2432, allyl polyethylene glycol with a molecular weight of 586 and deionized water into the reaction kettle, heat and dissolve at a temperature of 20-80°C Obtain A solution; dropwise add the deionized aqueous solution of sodium persulfate and the deionized wate...

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Abstract

The invention discloses a polycarboxylate superplasticizer with a modified cyclodextrin side chain structure. The polycarboxylate superplasticizer has a structural general formula as shown in the description, in the structural general formula, a, b, c, d, m and n are degrees of polymerization and positive integers, wherein a is equal to 15-20, b is equal to 1-5, c is equal to 55-90, d is equal to1-5, m is equal to 45-90, and n is equal to 9-27. The invention further discloses a preparation method of the polycarboxylate superplasticizer with the modified cyclodextrin side chain structure. Themolecule of the polycarboxylate superplasticizer synthesized in the invention has an etherified cyclodextrin side chain structure, compared with an esterified cyclodextrin side chain structure, the etherified cyclodextrin side chain structure is more stable in the alkaline environment of concrete, the hydrolysis reaction is avoided, after the polycarboxylate superplasticizer is added in the concrete, the stability is good, the water retaining, slump retaining and tackability are excellent, and the change of cement paste fluidity is small after 120min.

Description

technical field [0001] The invention relates to the technical field of concrete, in particular to a modified cyclodextrin side chain structure polycarboxylate water reducer and a preparation method thereof. Background technique [0002] As the third-generation high-performance water-reducer, polycarboxylate superplasticizer has strong designability of molecular structure and great potential for high-performance. It can prepare multi-functional products by selecting monomers with different functions for copolymerization. . The polycarboxylate superplasticizer modified by cyclodextrin has the advantages of high slump retention, high water retention and viscosity increase, etc. It has good adaptability to different cement and mineral admixtures, inferior sand and gravel materials, etc., and has broad market application prospects , a variety of products have come out. [0003] Patent CN 103819637 A uses β-cyclodextrin and lignin to perform esterification with maleic anhydride ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F283/06C08F220/06C08F251/00C08B37/16C04B24/26C04B103/30
CPCC04B24/2694C04B2103/302C08B37/0012C08F251/00C08F283/065C08F220/06
Inventor 高玉军李顺凯明阳王文荣韦鹏亮陈雍雍
Owner CCCC SHEC WUHAN PORT NEW MATERIALS
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