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Method for preparing telechelic polycarboxylic acid water reducer

A technology of telechelic polycarboxylic acid and water reducing agent is applied in the application field of concrete admixture, which can solve the problems of large application limitation and single functional group, and achieves enhancement of early strength and toughness, simple process, and increased molecular weight. The effect of polarity and steric hindrance

Active Publication Date: 2019-03-01
江苏博西瑞新材料科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, its single functional group has great limitations on application

Method used

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  • Method for preparing telechelic polycarboxylic acid water reducer

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example 1

[0024] (1) Preparation of nitrogen and oxygen stable free radicals: 1 mol of pentaerythritol and 10 mol of N-methyl-4-hydroxypiperidine were reacted at 35°C for 4 hours under the action of 0.015 mol of sodium hydroxide to obtain the initiator nitrogen and oxygen stable free radicals. base.

[0025] (2) Preparation of unsaturated polyether macromonomer: After adding 0.01mol melamine-amide and 0.003mol sodium methoxide to the reaction kettle, vacuumize, replace with nitrogen, heat to 130°C, and then continuously add 1mol epoxy Ethane undergoes ring-opening polymerization reaction to prepare unsaturated polyether macromonomer with number average molecular weight of 800.

[0026] (3) Preparation of telechelic polycarboxylate water-reducer: 1 mol step (2) unsaturated polyether macromonomer, 2.5 mol cyanovinylaniline and 0.15 mol 2,4-diphenyl-4-methyl Under the action of 0.06 mol of nitroxide stabilized free radicals in step (1), NMRP reaction occurs at 65° C., and the reaction tim...

example 2

[0028] (1) Preparation of nitrogen and oxygen stable free radicals: Under the action of 1mol tripentaerythritol and 12mol 2,2,6,6-tetramethylpiperidine and 0.005mol potassium hydroxide, carry out a catalytic reaction at 40°C for 3h to obtain the initiator nitrogen Oxygen stabilizes free radicals.

[0029] (2) Preparation of unsaturated polyether macromonomer: After adding 0.02mol triallyl cyanurate and 0.004mol sodium hydride into the reaction kettle, vacuumize, replace with nitrogen, heat to 140°C, and then Continuously add 1 mol of propylene oxide to carry out ring-opening polymerization reaction to prepare an unsaturated polyether macromonomer with a number average molecular weight of 1400.

[0030] (3) Preparation of telechelic polycarboxylate water reducer: 1mol step (2) unsaturated polyether macromonomer, 3mol styryl triphenylamine and 0.05mol dodecyl mercaptan in 0.23mol step (1 ) NMRP reaction occurs at 70°C under the action of nitrogen and oxygen stable free radicals...

example 3

[0032] (1) Preparation of nitrogen-oxygen stable free radicals: 1 mol of neopentyl glycol and 14 mol of 2,2,6,6-tetramethylpiperidine were reacted at 45°C for 5 hours under the action of 0.01 mol of potassium hydride to obtain Nitrogen stabilizes free radicals.

[0033] (2) Preparation of unsaturated polyether macromonomer: After adding 0.004mol trimethylcyanurate and 0.005mol potassium hydride into the reaction kettle, vacuumize, replace with nitrogen, heat to 150°C, and then continuously Add 1 mol of butylene oxide to carry out ring-opening polymerization reaction to prepare an unsaturated polyether macromonomer with a number average molecular weight of 1400.

[0034] (3) Preparation of telechelic polycarboxylate water-reducer: 1 mol step (2) unsaturated polyether macromonomer, 3.5 mol N,N-diphenyl-4-vinylaniline and 0.08 mol 2-mercapto Under the action of 0.08 mol of ethanesulfonic acid stable free radicals in step (1), NMRP reaction occurs at 75° C., and the reaction time...

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Abstract

The invention relates to a method for preparing a telechelic polycarboxylic acid water reducer. The method comprises the following specific steps: preparing a compound containing polyol hydroxyl and amethylpiperidine type compound into an initiator nitroxide stable free radical under the action of a catalyst; then adding a cyanuric acid type derivative and a catalyst into alkyl ethylene oxide andcarrying out polymerization reaction to prepare an unsaturated polyether macromonomer; finally, taking the unsaturated polyether macromonomer, an unsaturated aniline type monomer and a chain transferagent to be subjected to NMRP (Nitroxide Mediated Radical Polymerization) reaction under the action of the nitroxide stable free radical, so as to obtain the telechelic polycarboxylic acid water reducer. The method provided by the invention has the advantage that one nitroxide stable free radical initiator is prepared; one interpenetrating network type double-end amino telechelic polymer is prepared through an NMRP method, is used as the functional polycarboxylic acid water reducer and has the characteristics of improving the early strength and toughening performance of concrete.

Description

technical field [0001] The invention relates to the application field of concrete admixtures, in particular to a method for preparing a telechelic polycarboxylate water reducer. Background technique [0002] The chemical composition of various molecular structures can be realized through polymer synthesis technology, and the molecular weight and its distribution can be controlled. At present, the most studied polymerization reactions include free radical copolymerization, emulsion polymerization, anionic living polymerization, and cationic living polymerization. However, it is difficult to effectively control the molecular weight of the structure designed for a specific molecule. The conditions of ion living polymerization are also relatively harsh, and are more sensitive to the selection of functional groups. The use of living radical polymerization is easier to control chain growth and stabilize free radicals during the polymerization process, which is a remedy for the sh...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C04B24/26C08F283/06C08F212/14C08F212/32C08G65/26C04B103/30
CPCC04B24/2605C04B24/2694C04B2103/302C08F283/065C08G65/2618C08G65/2633C08F212/14C08F212/32
Inventor 于浩沈学涛
Owner 江苏博西瑞新材料科技有限公司
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