Polycarboxylic acid slump retaining agent based on alkylamido halide modification, and ATRP preparation method thereof

A technology based on halides and alkylamides, which is applied in the preparation of polycarboxylate slump-retaining agents based on alkylamide-based halides and its ATRP preparation, and the preparation of polycarboxylate slump-retaining agents, which can solve the problem of large losses, etc. problems, to achieve the effect of strong flexibility, enhanced dispersion ability and long-lasting slump performance

Inactive Publication Date: 2020-02-25
HUBEI UNIV OF TECH
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] 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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  • Polycarboxylic acid slump retaining agent based on alkylamido halide modification, and ATRP preparation method thereof

Examples

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Effect test

example 1

[0038] An ATRP preparation method based on alkyl amide halide modified polycarboxylic acid slump retention agent, the total mass of raw materials is 1000 parts, the mass fraction is about 40%, and it is mainly prepared from the following components:

[0039] Vinyl butyl ether polyoxyethylene ether: 360 parts

[0040] Hydroxyethyl acrylate: 22 parts

[0041] Methacrylane: 8 parts

[0042] Acrylamide: 9 parts

[0043] Ammonium persulfate: 0.9 parts

[0044] Mercaptoethanol: 0.8 parts

[0045] N,N,N',N'-tetramethylethylenediamine: 1.4 parts

[0046] Cuprous bromide: 0.06 parts

[0047] The rest is water.

[0048] Step 1: Put 8 parts of methacrylane, 9 parts of acrylamide, and 200 parts of deionized water on the bottom of No. 1 reactor, add A and B dropwise at 40℃, add dropwise A and B for 3h, and add dropwise B 2.5h, where material A is a mixture of 0.9 parts of ammonium persulfate and 50 parts of deionized water, and material B is a mixture of 0.8 parts of mercaptoethanol and 50 parts of deio...

example 2

[0051] An ATRP preparation method based on alkyl amide halide modified polycarboxylic acid slump retention agent, the total mass of raw materials is 1000 parts, the mass fraction is about 40%, and it is mainly prepared from the following components:

[0052] Vinyl butyl ether polyoxyethylene ether: 362 parts

[0053] Hydroxypropyl acrylate: 20 parts

[0054] Pentenane: 6 parts

[0055] 4-(acrylamide)benzoic acid: 10 parts

[0056] Azobisisobutyronitrile: 0.8 parts

[0057] Mercaptopropanol: 0.7 parts

[0058] N,N,N',N″,N'-pentamethylmethacrylate divinyltriamine: 1.2 parts

[0059] Cuprous chloride: 0.03 parts

[0060] The rest is water.

[0061] Step 1: 6 parts of pentenane, 10 parts of 4-(acrylamide) benzoic acid, and 200 parts of deionized water are placed at the bottom of No. 1 reactor, and the A and B materials are added dropwise at 55℃, and the A material is added dropwise for 2 hours , B material is added dropwise for 3h, of which material A is 0.8 parts of azobisisobutyronitrile and ...

example 3

[0064] An ATRP preparation method based on alkyl amide halide modified polycarboxylic acid slump retention agent, the total mass of raw materials is 1000 parts, the mass fraction is about 40%, and it is mainly prepared from the following components:

[0065] Vinyl butyl ether polyoxyethylene ether: 364 parts

[0066] Hydroxyethyl acrylate: 18 parts

[0067] Isopentenane: 7 parts

[0068] 2-acrylamide phenylboronic acid: 8 parts

[0069] Azobisisoheptonitrile: 0.9 parts

[0070] Mercaptoethanol: 0.6 parts

[0071] N,N,N',N',N",N"-hexamethacrylate n-butyl trivinyltetraamine: 1.1 parts

[0072] Ferrous bromide: 0.08 parts

[0073] The rest is water.

[0074] Step 1: 7 parts of isopentenane, 8 parts of 2-acrylamide phenylboronic acid, and 200 parts of deionized water are placed at the bottom of No. 1 reactor, and the A and B materials are added dropwise at 55°C, and the A material is added dropwise for 2.5 hours , Material B is added dropwise for 3h, where material A is a mixture of 0.9 parts o...

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Abstract

The invention discloses a polycarboxylic acid slump retaining agent based on alkylamido halide modification, and an ATRP preparation method thereof. Raw materials of the polycarboxylic acid slump retaining agent comprise, by weight, 360-370 parts of a polyether macromonomer, 16-22 parts of alkyl acrylate, 3-8 parts of an unsaturated alkyl monomer, 8-12 parts of an amide monomer, 0.8-1.1 parts of an initiator, 0.6-0.8 part of a chain transfer agent, 0.8-1.6 parts of a ligand, 0.03-0.1 part of a catalyst, and the balance of water. The preparation method comprises the following steps: firstly carrying out free radical polymerization on the unsaturated alkyl monomer, the amide monomer, the initiator and the chain transfer agent at 40-55 DEG C, introducing nitrogen for 5 min after the reactionis finished, introducing bromine gas, and halogenating the obtained reaction product under an illumination condition so as to obtain a halogenated polymer I; and then putting the polyether macromonomer, the alkyl acrylate, the ligand and the catalyst at the bottom of a second reaction kettle, dropwise adding the halogenated polymer I into the second reaction kettle under the protection of an inertgas atmosphere for 2-3 h, and carrying out heat insulation for 1 h after the drop-by-drop addition is finished in order to obtain the polycarboxylic acid slump retaining agent after the reaction is completed. The prepared polycarboxylic acid slump retaining agent has the advantages of narrow molecular mass distribution, high effective component content and high 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 polycarboxylic acid slump retaining agent, in particular to a polycarboxylic acid slump retaining agent modified based on alkyl amide halide and an ATRP preparation method thereof. Background technique [0002] With the vigorous development of the commercial concrete industry for construction, my country’s concrete admixtures have been widely used in recent years. Among them, the naphthalene sulfonate formaldehyde condensate type superplasticizer, the melamine sulfonate formaldehyde condensate type superplasticizer The amount of water agent, lignosulfonate series water reducing agent, etc. is large. These water-reducing agents give fresh concrete better fluidity and strength. For on-site mixing, it can basically meet the construction requirements. However, for commercial concrete, there are generally problems of large slump and excessive loss. At pre...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F283/06C08F220/20C08F8/22C08F220/54C08F212/14C08F230/06C08F220/58C08F220/56C04B24/26C04B103/30
CPCC04B24/2647C04B2103/308C08F8/22C08F283/065C08F2438/01C08F220/20C08F220/56C08F220/58C08F230/06C08F212/14C08F220/54
Inventor 柯凯徐洪飞姚恒
Owner HUBEI UNIV OF TECH
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