Anti-mud amphoteric polycarboxylate superplasticizer and preparation method thereof

A technology of amphoteric polycarboxylic acid and water reducing agent, applied in the field of water reducing agent, can solve the problems of large slump loss, pollution, low sensitivity and the like

Pending Publication Date: 2020-10-30
中科广化(重庆)新材料研究院有限公司 +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] Chinese patent CN103897116 uses vinyl polyoxyethylene ether, sodium styrene sulfonate, acrylic acid and acrylamide compounds as monomers to synthesize a mud-resistant polycarboxylate water reducer. The water reducer is sensitive to mud content Lower, and better adaptability to cement and various muds, but the production cost is higher
Chinese patent CN103467670 has announced a kind of anti-mud type amphoteric polycarboxylate superplasticizer, and this patent first prepares quaternary ammonium salt oligomer with epibromohydrin and tertiary amine compound, then this quaternary ammonium salt oligomer and Prenyl alcohol polyoxyethylene ether, unsaturated carboxylic acid and its derivatives, and amino trimethylene phosphonic acid are free radically polymerized to obtain a mud-resistant polycarboxy...

Method used

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  • Anti-mud amphoteric polycarboxylate superplasticizer and preparation method thereof
  • Anti-mud amphoteric polycarboxylate superplasticizer and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0054] (1) Preparation of methacrylate-6-dimethylaminohexyl ester intermediate: add 21.9732g of 6-dimethylamino-1-hexanol and 100mL ether to a three-necked round-bottomed flask, and control the temperature to 0°C; Add methacryloyl chloride dropwise to the three-necked round-bottomed flask for 40 minutes, react for 3 hours, and stop the reaction; wash the oil layer with deionized water for 3 times, then add desiccant anhydrous calcium chloride, and dry overnight , filtered, and the filtrate was rotary evaporated at 35°C, and the organic solvent ether was removed to obtain the intermediate of 6-dimethylaminohexyl methacrylate, which was set aside.

[0055] (2) Preparation of amphoteric monomer: add 2.7670g of 6-dimethylaminohexyl methacrylate intermediate prepared in step (1), 0.0390g of hydroquinone and 30mL of acetone into a three-neck round bottom flask, Stir to dissolve and heat up to 50°C; add 1.2203g 1,3-propane sultone into 10mL acetone to obtain 1,3-propane sultone dropw...

Embodiment 2

[0058] (1) The preparation of 6-dimethylaminohexyl methacrylate intermediate and amphoteric monomer is the same as in Example 1.

[0059] (2) Add 35mL of deionized water, 24.06g of methacryl alcohol polyoxyethylene ether (molecular weight: 2400) and 0.1178g of hydrogen peroxide into a 150mL three-neck round bottom flask, stir and dissolve, and heat up to 65°C to obtain a mixed solution; 2.1796g of acrylic acid and 0.6745g of the amphoteric monomer prepared in step (1) were dissolved in 10mL of deionized water to prepare drop solution A; 0.0332g of ascorbic acid and 0.1007g of thioglycolic acid were dissolved in 15mL of deionized water to prepare Obtain dropwise solution B; then begin to dropwise add A and B in the mixed solution under the condition of constant temperature oil bath 65 ℃ and stirring, wherein the dropwise addition time of solution A, B is 3 hours and 3.5 hours respectively, dropwise After completion, keep the reaction for 1 hour. After cooling to room temperatur...

Embodiment 3

[0061] (1) The preparation of 6-dimethylaminohexyl methacrylate intermediate and amphoteric monomer is the same as in Example 1.

[0062] (2) Add 40 mL of deionized water, 24.47 g of methacryl alcohol polyoxyethylene ether (molecular weight: 2400) and 0.1207 g of hydrogen peroxide into a 150 mL three-neck round bottom flask, stir and dissolve, and heat up to 60 ° C to obtain a mixed solution; 3.2034g of acrylic acid and 1.0479g of the amphoteric monomer prepared in step (1) were dissolved in 10mL of deionized water to prepare drop solution A; 0.0351g of ascorbic acid and 0.1172g of thioglycolic acid were dissolved in 15mL of deionized water to prepare Obtain dropwise liquid B; then begin to drip A and B in the mixed solution under the condition of constant temperature oil bath 60 ℃ and stirring, wherein the time for adding dropwise liquid A, B is 3 hours and 3.5 hours respectively, dropwise After completion, keep the reaction for 1 hour. After cooling to room temperature, adju...

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Abstract

The invention discloses an anti-mud amphoteric polycarboxylate superplasticizer and a preparation method thereof. The preparation method comprises the following steps: reacting 6-dimethylamino-1-hexanol with methacryloyl chloride in an organic solvent to obtain a methacrylic acid-6-dimethylaminohexyl ester intermediate, adding the methacrylic acid-6-dimethylaminohexyl ester intermediate and a polymerization inhibitor into the organic solvent, adding a 1, 3-propane sultone dropwise-adding solution, reacting, and purifying to obtain an amphoteric monomer; mixing an unsaturated polyether macromonomer, an initiator, an unsaturated carboxylic acid monomer and an amphoteric monomer, reacting, and regulating the pH value to 6.5-7.5 to obtain the anti-mud amphoteric polycarboxylate superplasticizer. Compared with a traditional anionic polycarboxylic acid water reducing agent, the mud-resistant functional monomer is introduced into the molecular structure of the prepared anti-mud amphoteric polycarboxylate superplasticizer, the sensitivity of the water reducing agent to mud is reduced, the water reducing agent does not contain chloride ions, potential hazards caused by corrosion of the chloride ions to reinforced concrete can be eliminated, the preparation method is simple, and the cost is low.

Description

technical field [0001] The invention relates to the field of water reducers, in particular to a mud-resistant amphoteric polycarboxylate water reducer and a preparation method thereof. Background technique [0002] Polycarboxylate superplasticizer has the advantages of low dosage, high water reducing rate, good slump retention, good dispersion of cement particles, strong molecular structure adjustability and environmental protection, and is more and more widely used in concrete engineering. However, the polycarboxylate superplasticizer has the problem of adaptability to concrete materials in different regions. In recent years, with the extensive use of natural sand and gravel, sand and gravel with a large mud content have been more and more used in concrete. Ordinary polycarboxylate superplasticizers are sensitive to soil, so when the concrete contains mud, the superplasticizer is easily absorbed by the soil, that is, the water reducing agent that really plays a role in red...

Claims

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Application Information

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IPC IPC(8): C08F283/06C08F220/06C08F220/38C04B24/16C04B103/30
CPCC08F283/065C04B24/165C04B2103/302C08F220/06
Inventor 庞浩张静斐廖兵黄健恒蒙业云李思敏林秀菊
Owner 中科广化(重庆)新材料研究院有限公司
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