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A low-valence variable valence cation-modified polycarboxylate water-reducing agent masterbatch and a low-temperature preparation method thereof

A technology of polycarboxylic acid and water reducing agent, applied in the field of polycarboxylate water reducing agent, can solve the problems of short half-life, molecular disorder of water reducing agent, poor effect of water reducing agent, etc., and achieve poor high temperature stability and side chain distribution. The effect of uniform, high polymerization activity

Active Publication Date: 2018-11-13
HUBEI UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

When the temperature is lower than 15°C, the common oxidation-reduction system is not enough to ensure the initiation effect. At this time, strong reducing agents such as chalk and sodium bicarbonate that can release a large amount of heat when contacting with water are often used, but the oxidizing agent-strong reducing agent system is in A large number of free radicals will be released in a short period of time, and the polymerization rate and chain growth rate are significantly greater than the chain termination rate. The mismatch between the above three will easily lead to the formation of disordered structures in the water reducer molecules. Due to the short half-life of the strong reducing agent in the middle and later stages of synthesis and the large consumption of acrylic acid in the early stage, the grafting of branch chains is chaotic and disorderly, and the effect of water reducing agent becomes poor.

Method used

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  • A low-valence variable valence cation-modified polycarboxylate water-reducing agent masterbatch and a low-temperature preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] A low-valence variable cation modified polycarboxylate superplasticizer masterbatch, which is formed by polymerizing the following components by mass percentage. The total mass of raw materials is 1000 parts. The components and process parameters are as follows:

[0038] Primer: 2400 molecular weight isopentenol polyoxyethylene ether: 352, water: 200;

[0039] Oxidant solution: hydrogen peroxide: 5, water: 5;

[0040] The temperature of the base material: 10°C;

[0041] Within 10 minutes after adding the oxidant solution, add the initiator and the small monomer solution dropwise in sequence. After adding the initiator dropwise for 5 minutes, add ferric sulfite heptahydrate at one time; after another 5 minutes, start adding the small monomer solution dropwise;

[0042] Iron sulfate heptahydrate: 0.035;

[0043] Initiator: thioglycolic acid: 1.5, ascorbic acid: 0.85, water: 120;

[0044] Small monomer solution: acrylic acid: 39.5, water: 50;

[0045] Initiator dropping ...

Embodiment 2

[0053] Primer: 2400 molecular weight vinyl butyl ether polyoxyethylene ether: 355, water: 220;

[0054] Oxidant solution: peracetic acid: 5.0, water: 10;

[0055] The temperature of the bottom material: 7 ℃;

[0056] Within 10 minutes after adding the oxidant solution, add the initiator and the small monomer solution dropwise in sequence. After adding the initiator dropwise for 5 minutes, add ferric sulfite heptahydrate at one time; after another 5 minutes, start adding the small monomer solution dropwise;

[0057] Ferric sulfate heptahydrate: 0.057;

[0058] Initiator: sodium methacrylate sulfonate: 2.7, glucose monohydrate: 3.5, water: 120;

[0059] Small monomer solution: acrylic acid: 36.2, water: 50;

[0060] Initiator dropping time: 4.0h;

[0061] The small monomer solution dripping time is 3.5h;

[0062] Adjust the opening of the cooling water valve to ensure that the reaction temperature during the dropping process is controlled at 20-30°C;

[0063] After the dro...

Embodiment 3

[0068] Primer: 2400 molecular weight vinyl butyl ether polyoxyethylene ether: 342, water: 250;

[0069] Oxidant solution: hydrogen peroxide: 4.5, water: 15;

[0070] The temperature of the base material: 13°C;

[0071] Within 10 minutes after adding the oxidant solution, add the initiator and the small monomer solution dropwise in sequence. After adding the initiator dropwise for 5 minutes, add ferric sulfite heptahydrate at one time; after another 5 minutes, start adding the small monomer solution dropwise;

[0072] Cobalt sulfate heptahydrate: 0.065;

[0073] Initiator: sodium hypophosphite: 3.0, sodium bisulfite: 1.5, fructose: 1.5, water: 120;

[0074] Small monomer solution: acrylic acid: 48.5, water: 50;

[0075] Initiator dropping time: 3.5h;

[0076] The small monomer solution dripping time is 3.0h;

[0077] Adjust the opening of the cooling water valve to ensure that the reaction temperature during the dropping process is controlled at 20-30°C;

[0078] After th...

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Abstract

The invention discloses a low-valence variable-valence cation modification polycarboxylate superplasticizer master batch and a low temperature preparation method thereof. The modification master batch is used for an enterprise of additives in the non-heating production condition or a cold region, and with the limit of 40% of the mass of the master batch, the master batch is prepared from, by mass, 340-360 parts of a polyether macromonomer, 32.0-50.0 parts of acrylic acid, 1.3-3.0 parts of a chain transfer agent, 3.0-5.0 parts of an oxidizing agent, 0.55-3.50 parts of a reducing agent, 0.020-0.070 part of a low-valence variable-valence cation compound, 0.1-0.5 part of a stabilizer, 10-15 parts of sodium hydroxide and the balance water, wherein the total mass of all the synthesis raw materials is 1,000 parts. The synthesis polycarboxylate superplasticizer has the advantages that the polycarboxylate superplasticizer can be polymerized under the low temperature, side chain distribution is uniform, the molecular weight distribution range is wide, the water reduction rate of the master batch is high, and the adaptability is wide.

Description

technical field [0001] The invention relates to a polycarboxylate water-reducer for cement-based cementitious materials, which is suitable for non-heating production conditions or cold regional climates, and specifically relates to a low-valence variable cation modified polycarboxylate water-reducer parent very low temperature preparation method. Background technique [0002] With the proposal of the national green building materials strategy, the normal temperature synthesis technology of polycarboxylate superplasticizers has tended to be mature. The peroxide used in the synthetic heating process is abandoned as an initiator. The normal temperature synthesis mostly uses an oxidation-reduction system to reduce the activation energy of decomposition. The concept usually refers to 15 ~ 25 ℃. When the temperature is lower than 15°C, the common oxidation-reduction system is not enough to ensure the initiation effect. At this time, strong reducing agents such as chalk and sodium...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F283/06C08F220/06C08F2/38C08F4/40C04B24/26C04B103/30
CPCC04B24/2605C04B2103/302C08F2/38C08F4/40C08F283/065C08F220/06
Inventor 柯凯贺行洋李学锋苏英王迎斌常鹰
Owner HUBEI UNIV OF TECH
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