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Hydroxyalkyl composite halogenated polycarboxylate slump retaining agent and ATRP preparation method thereof

A technology of hydroxyalkyl and polycarboxylic acid, which is applied in the preparation of polycarboxylic acid slump-retaining agent, hydroxyalkyl complex halogenated polycarboxylic acid slump-retaining agent and its ATRP preparation field, which can solve the problem of difficult industrial production and long production cycle , high energy consumption and other issues, to achieve the effect of gentle reaction conditions, enhanced dispersion ability, and single molecular weight distribution

Inactive Publication Date: 2020-04-03
HUBEI UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] Patent CN2010617174.4 discloses a preparation method of polycarboxylic acid high slump retention agent. The advantage of this invention is that the esterification of maleic anhydride and polyethylene glycol avoids the need to add a polymerization inhibitor when esterifying traditional acrylic acid, but this The invention requires a two-step synthesis method, and the production cycle is longer
In addition, it needs to be heated to 100-130°C, which consumes a lot of energy and is not easy for industrial production.
[0004] Patent CN201710851324.X discloses a maleate-based polycarboxylate-based concrete slump-retaining agent and its preparation method, aiming to solve the problem of large loss when the existing polycarboxylate-based slump-retaining agent is used in concrete

Method used

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  • Hydroxyalkyl composite halogenated polycarboxylate slump retaining agent and ATRP preparation method thereof

Examples

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Effect test

example 1

[0038] A kind of ATRP preparation method of polycarboxylic acid slump-retaining agent of hydroxyalkyl compound halogenation, the total mass of raw materials is 1000 parts, the mass fraction is about 40%, mainly prepared from the following components:

[0039] Vinyl butyl ether polyoxyethylene ether: 362 parts

[0040] Hydroxyethyl acrylate: 22 parts

[0041] Methacrylic: 3 parts

[0042] Propyl alcohol: 10 parts

[0043] Azobisisoheptanonitrile: 0.8 parts

[0044] Mercaptoethanol: 0.7 parts

[0045] N,N,N',N'-Tetramethylethylenediamine: 0.8 parts

[0046] Cuprous bromide: 0.06 parts

[0047] The rest is water.

[0048] Step 1: Put 3 parts of methacrylic alkane, 10 parts of propylene alcohol, and 100 parts of deionized water in the No. 1 reactor, add A and B materials dropwise, and the dropping time is 2-3 hours, of which A material is 0.8 parts of distilled water A mixture of nitrogen diisoheptanonitrile and 50 parts of deionized water; material B is a mixture of 0.7 part...

example 2

[0051] A kind of ATRP preparation method of polycarboxylic acid slump-retaining agent of hydroxyalkyl compound halogenation, the total mass of raw materials is 1000 parts, the mass fraction is about 40%, mainly prepared from the following components:

[0052] Vinyl butyl ether polyoxyethylene ether: 360 parts

[0053] Hydroxypropyl acrylate: 20 parts

[0054] Pentenane: 6 parts

[0055] Methacryl alcohol: 8 parts

[0056] Dibenzoyl peroxide: 1.2 parts

[0057] Mercaptopropanol: 0.6 parts

[0058] N,N,N',N",N'-pentamethacrylate divinyltriamine: 0.6 parts

[0059] Ferrous bromide: 0.08 parts

[0060] The rest is water.

[0061] Step 1: Put 6 parts of pentene, 8 parts of methacryl alcohol, and 100 parts of deionized water in the No. 1 reactor, add A and B materials dropwise, and the dropping time is 2-3 hours, of which A material is 1.2 parts A mixture of dibenzoyl peroxide and 50 parts of deionized water; material B is a mixture of 0.6-0.8 parts of mercaptopropanol and 50...

example 3

[0064] A kind of ATRP preparation method of polycarboxylic acid slump-retaining agent of hydroxyalkyl compound halogenation, the total mass of raw materials is 1000 parts, the mass fraction is about 40%, mainly prepared from the following components:

[0065] Vinyl butyl ether polyoxyethylene ether: 364 parts

[0066] Hydroxyethyl acrylate: 19 parts

[0067] Isopentenane: 8 parts

[0068] Propyl alcohol: 7 parts

[0069] Azobisisovaleronitrile: 1.1 parts

[0070] Mercaptoethanol: 0.8 parts

[0071] N,N,N',N',N",N"-n-butylhexamethacrylate triethylenetetramine: 1.4 parts

[0072] Cuprous bromide: 0.03 parts

[0073] The rest is water.

[0074] Step 1: Put 8 parts of isopentane, 7 parts of propylene alcohol, and 100 parts of deionized water in the No. 1 reactor, add A and B materials dropwise, and the dropping time is 2-3 hours, of which A material is 1.1 parts of distilled water A mixture of nitrogen diisovaleronitrile and 50 parts of deionized water; material B is a mixt...

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Abstract

The invention provides a hydroxyalkyl composite halogenated polycarboxylate slump retaining agent and an ATRP preparation method thereof. The polycarboxylate slump retaining agent is prepared from thefollowing materials: 360-375 parts of a polyether macromonomer, 15-22 parts of alkyl acrylate, 3-8 parts of an unsaturated alkyl monomer, 5-10 parts of a hydroxyl monomer, 0.8-1.2 parts of an initiator, 0.6-0.8 parts of a chain transfer agent, 0.6-1.4 parts of an ATRP method ligand, 0.02-0.1 parts of an ATRP method catalyst and the balance of water. The preparation method comprises the followingsteps: first, carrying out free radical polymerization on an unsaturated alkyl monomer, a hydroxyl monomer, an initiator and a chain transfer agent at 40-50 DEG C, preserving the heat for 1 hour afterthe reaction is finished, introducing nitrogen for 5 minutes, introducing chlorine, and carrying out halogenation under an illumination condition to obtain a halogenated polymer I; and then, puttinga polyether macromonomer, alkyl acrylate, an ATRP method ligand and an ATRP method catalyst at the bottom of a second reaction kettle, dropwise adding the halogenated polymer I into the second reaction kettle, keeping the temperature for 1 hour after dropwise adding is finished, and carrying out reaction completely to obtain the polycarboxylate slump retaining agent. The prepared polycarboxylate slump retaining agent is narrow in molecular mass distribution, high in effective component content and high in slump retaining capacity.

Description

technical field [0001] The invention belongs to the technical field of building materials, and relates to a preparation method of a polycarboxylate slump retaining agent, in particular to a hydroxyalkyl complex halogenated polycarboxylate slump retainer and a preparation method thereof. Background technique [0002] With the rapid development of the construction industry, the commercial concrete market is in short supply, and the development of concrete admixtures has also entered a new era. Polycarboxylate slump-retaining agents can not only significantly improve the anisotropic indicators of concrete, but also have strong design and easy operation and preparation. It has become an essential and important component in the construction industry. At present, many concrete admixtures and cement have adaptability problems, such as insufficient concrete dispersion performance and short slump retention time, etc., which bring great inconvenience to engineering construction. In t...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F293/00C08F2/38C04B24/26
CPCC04B24/2647C08F2/38C08F293/00C08F2438/01
Inventor 柯凯徐洪飞姚恒
Owner HUBEI UNIV OF TECH
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