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ATRP preparation method for polycarboxylate slump retaining agent based on phenyl-hydroxyl halogenation polymerization

A phenylhydroxyl, halogenated polymer technology, applied in the preparation of polycarboxylic acid slump-retaining agent, the field of ATRP preparation of polycarboxylic acid slump-retaining agent, can solve the problems of excessive loss, large slump, etc., to achieve the reaction conditions The effect of smoothing, dispersing ability is enhanced, and the effect of reducing the generation of closed chains

Inactive Publication Date: 2020-03-31
HUBEI UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

These superplasticizers endow fresh concrete with better fluidity and strength. For on-site mixing, they can basically meet the construction requirements. However, for commercial concrete, there are generally problems of large slump and excessive loss.

Method used

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  • ATRP preparation method for polycarboxylate slump retaining agent based on phenyl-hydroxyl halogenation polymerization

Examples

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Effect test

example 1

[0039] An ATRP preparation method of polycarboxylic acid slump retention agent based on phenylhydroxyl halogenation polymerization, the total mass of raw materials is 1000 parts, the mass fraction is about 40%, and it is mainly prepared from the following components:

[0040] Vinyl butyl ether polyoxyethylene ether: 345 parts

[0041] Hydroxyethyl acrylate: 28 parts

[0042] 1-allyl-2-fluorobenzene: 5 parts

[0043] Propylene hydroxy: 18 parts

[0044] Ammonium persulfate: 1.2 parts

[0045] Mercaptopropanol: 0.9 parts

[0046] N,N,N',N'-tetramethylethylenediamine: 0.8 parts

[0047] Cuprous bromide: 0.1 part

[0048] The rest is water.

[0049] Step 1: Put 5 parts of 1-allyl-2-fluorobenzene, 18 parts of propylene hydroxy, and 100 parts of deionized water in the No. 1 reaction kettle, and drop materials A and B. The dropping time is 2h, of which material A 1.2 parts of ammonium persulfate, 50 parts of deionized water mixed liquid; B material is 0.9 parts of mercaptopropanol, 50 parts of dei...

example 2

[0052] An ATRP preparation method of polycarboxylic acid slump retention agent based on phenylhydroxyl halogenation polymerization, the total mass of raw materials is 1000 parts, the mass fraction is about 40%, and it is mainly prepared from the following components:

[0053] Vinyl butyl ether polyoxyethylene ether: 347 parts

[0054] Hydroxypropyl acrylate: 27 parts

[0055] 1-allyl-4-fluorobenzene: 10 parts

[0056] 4-(propylene hydroxy)benzoic acid: 12 parts

[0057] Azobisisobutyronitrile: 1.5 parts

[0058] Mercaptoethanol: 0.6 parts

[0059] N,N,N',N″,N'-pentamethylmethacrylate divinyltriamine: 1.1 parts

[0060] Cuprous chloride: 0.05 parts

[0061] The rest is water.

[0062] Step 1: Put 10 parts of 1-allyl-4-fluorobenzene, 12 parts of 4-(propylene hydroxy)benzoic acid, and 100 parts of deionized water in the No. 1 reaction kettle, drop materials A and B, and add time It is 1.5h, where material A is 1.5 parts of azobisisobutyronitrile and 50 parts of deionized water; material B is 0...

example 3

[0065] An ATRP preparation method of polycarboxylic acid slump retention agent based on phenylhydroxyl halogenation polymerization, the total mass of raw materials is 1000 parts, the mass fraction is about 40%, and it is mainly prepared from the following components:

[0066] Vinyl butyl ether polyoxyethylene ether: 349 parts

[0067] Hydroxyethyl acrylate: 26 parts

[0068] Styrene: 7 parts

[0069] 2-propylene hydroxyphenyl boric acid: 13 parts

[0070] Azobisisoheptanonitrile: 1.3 parts

[0071] Mercaptopropanol: 0.8 parts

[0072] N,N,N',N',N",N"-hexamethacrylate n-butyl trivinyltetraamine: 1.5 parts

[0073] Cuprous bromide: 0.02 parts

[0074] The rest is water.

[0075] Step 1: Put 7 parts of styrene, 13 parts of 2-propenylhydroxyphenylboronic acid, and 100 parts of deionized water in the No. 1 reaction kettle, and add materials A and B dropwise for 1 hour, of which material A is 1.3 parts even Nitrogen diisohepta nitrile, 50 parts of deionized water mixed liquid; B material is 0.8 p...

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Abstract

The invention discloses an ATRP preparation method for polycarboxylate slump retaining agent based on phenyl-hydroxyl halogenation polymerization. The polycarboxylate water reducing agent is preparedfrom: 345-355 parts of a polyether macromonomer, 20-28 parts of alkyl acrylate, 5-10 parts of a phenyl monomer, 12-18 parts of a hydroxyl monomer, 0.8-1.5 parts of an initiator, 0.6-0.9 parts of a chain transfer agent, 0.8-1.5 parts of a ligand, 0.02-0.1 parts of a catalyst, and the balance being water. The preparation method comprises: performing free radical polymerization on the phenyl monomer,the hydroxyl monomer, the initiator and the chain transfer agent at 60-70 DEG C, then performing heat preservation for 1 h after the reaction is finished and feeding nitrogen gas for 5 min, then feeding chlorine gas for halogenation under light to obtain a halogenated polymer (I); then placing the polyether macromonomer, the alkyl acrylate, 0.8-1.5 parts of the ligand and 0.02-0.1 parts of the catalyst on the bottom of the 2# reaction kettle, dropwise adding the halogenated polymer (I) into the 2# reaction kettle with temperature controlled at 40-50 DEG C, and performing heat preservation for1 h after the dropwise addition is finished, thus obtaining the polycarboxylate slump retaining agent after the reaction is completed. The molecular mass distribution of the polycarboxylate slump retaining agent is narrow, effective component content is high and slump retaining capability is excellent.

Description

Technical field [0001] The invention belongs to the technical field of building materials, and relates to a preparation method of a polycarboxylic acid slump retaining agent, in particular to an ATRP preparation method of a polycarboxylic acid slump retaining agent based on phenyl hydroxy halogenation polymerization. Background technique [0002] Concrete admixtures refer to substances added to improve and adjust the performance of concrete, which can control the rheological properties of concrete, improve mechanical properties and increase durability, and provide a strong guarantee for the quality of large-scale projects. Therefore, its wide application is It is regarded as the third major breakthrough in concrete technology after reinforced concrete and prestressed concrete. Concrete is the most widely used and most used building material in contemporary civil engineering. With the large-scale application of commercial concrete, centralized mixing and commercial supply have be...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F293/00C08F283/06C08F220/20C08F220/34C08F8/22C08F212/14C08F230/06C08F212/08C08F4/26C08F4/10C08F2/38C04B24/26
CPCC08F293/005C08F283/065C08F220/20C08F220/34C08F8/22C08F4/26C08F4/10C08F2/38C04B24/2694C08F2438/01
Inventor 柯凯姚恒
Owner HUBEI UNIV OF TECH
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