CN110818857A - High slump loss resistant polycarboxylate superplasticizer and preparation method thereof - Google Patents

High slump loss resistant polycarboxylate superplasticizer and preparation method thereof Download PDF

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Publication number
CN110818857A
CN110818857A CN201911149577.8A CN201911149577A CN110818857A CN 110818857 A CN110818857 A CN 110818857A CN 201911149577 A CN201911149577 A CN 201911149577A CN 110818857 A CN110818857 A CN 110818857A
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parts
solution
reducing agent
mass
preparation
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陈世学
刘允伟
邹锋
廖思淘
陈华君
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Sichuan Yu Concrete Building Materials Co Ltd
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Sichuan Yu Concrete Building Materials Co Ltd
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    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F283/00—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G
    • C08F283/06—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G on to polyethers, polyoxymethylenes or polyacetals
    • C08F283/065—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G on to polyethers, polyoxymethylenes or polyacetals on to unsaturated polyethers, polyoxymethylenes or polyacetals
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B24/00—Use of organic materials as active ingredients for mortars, concrete or artificial stone, e.g. plasticisers
    • C04B24/24—Macromolecular compounds
    • C04B24/26—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
    • C04B24/2688—Copolymers containing at least three different monomers
    • C04B24/2694—Copolymers containing at least three different monomers containing polyether side chains
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F4/00—Polymerisation catalysts
    • C08F4/40—Redox systems
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2103/00—Function or property of ingredients for mortars, concrete or artificial stone
    • C04B2103/30—Water reducers, plasticisers, air-entrainers, flow improvers
    • C04B2103/302—Water reducers

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Organic Chemistry (AREA)
  • Ceramic Engineering (AREA)
  • Materials Engineering (AREA)
  • Health & Medical Sciences (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Structural Engineering (AREA)
  • Curing Cements, Concrete, And Artificial Stone (AREA)

Abstract

The application relates to the field of concrete admixtures, in particular to a high slump loss resistant type polycarboxylic acid water reducing agent and a preparation method thereof. The high slump-retaining polycarboxylate superplasticizer is prepared by carrying out a series of chemical reactions on methyl allyl polyoxyethylene ether, organic acid, organic salt, a reducing agent, an oxidizing agent and other raw materials, and controlling the molecular weight of a product by a molecular weight regulator. The high slump-retaining type polycarboxylate superplasticizer can obviously improve the slump retention performance of concrete under the condition of basically not influencing the strength of the concrete, thereby improving the workability and the applicability of the concrete. In addition, the preparation method of the high slump loss resistant polycarboxylic acid high-performance water reducing agent has the advantages of convenient and easily obtained raw materials, simple production process and no pollution, so that the finished product cost and the production environmental protection pressure of the high slump loss resistant polycarboxylic acid high-performance water reducing agent are reduced.

Description

High slump loss resistant polycarboxylate superplasticizer and preparation method thereof
Technical Field
The application relates to the field of concrete admixtures, in particular to a high slump loss resistant type polycarboxylic acid water reducing agent and a preparation method thereof.
Background
The water reducing agent is an additive of concrete, which can reduce the mixing water consumption and improve the strength of the concrete on the premise of not changing the cement consumption of the concrete and the workability of the concrete. The polycarboxylate superplasticizer as a concrete water reducer has the advantages of low mixing amount, high water reducing rate and the like, the market share is continuously promoted, and along with the rapid development of the current infrastructure, the requirements and the yield of the polycarboxylate superplasticizer are higher and higher, so that the polycarboxylate superplasticizer is an important direction for the research of concrete admixtures in the future.
However, in the prior art, in practical application of concrete using the polycarboxylate superplasticizer, the problems of too fast concrete slump loss and poor concrete workability caused by long-distance concrete transportation and the like exist, and in addition, the conventional polycarboxylate superplasticizer has high production cost, complex process and great pollution, so the use of the polycarboxylate superplasticizer is limited.
Disclosure of Invention
In order to solve the problems, the application provides a preparation method of a high slump retaining type polycarboxylate superplasticizer, which is characterized by comprising the following steps:
1) mixing water, unsaturated organic acid and unsaturated ester to prepare a solution A;
2) mixing water and an oxidant to prepare a solution B;
3) mixing water and a first reducing agent to prepare a solution C;
4) sequentially adding organic salt, a second reducing agent and a molecular weight regulating agent into the methyl allyl polyoxyethylene ether aqueous solution until the materials are completely dissolved to obtain a solution D;
5) dropwise adding the solution A into the solution D according to 15% of the weight to obtain a solution E;
6) simultaneously dripping the solution B, the rest solution A and the solution C into the solution E to obtain a solution F; the solution F is a solution of a high slump retaining type polycarboxylate superplasticizer;
optionally, in the solution a, the components include water in parts by mass: 10-12 parts of unsaturated organic acid: 3-5 parts of unsaturated ester: 6-8 parts;
in the solution B, the components comprise water in parts by mass: 3-4 parts of an oxidant: 0.6-0.8 part;
in the solution C, the components comprise water in parts by mass: 3-4 parts of a first reducing agent: 0.4-0.5 part;
in the solution D, the components comprise water in parts by mass: 40-44 parts of methyl allyl polyoxyethylene ether: 28-31 parts of organic salt: 2-3 parts of a second reducing agent: 0.04-0.09 part of a molecular weight regulator: 1.5 to 2.5 portions.
Optionally, the dropping time of the solution B in the step 6) is 95 min; the dropping time of the solution A is 90 min; and (3) dropwise adding the solution C for 100min, and stirring for 30min after dropwise adding the solution C to obtain a solution F, wherein the solution F is a high slump retaining type polycarboxylate superplasticizer solution.
Optionally, in the step 1), the unsaturated organic acid is acrylic acid, and the unsaturated ester is hydroxypropyl acrylate.
Optionally, the oxidant in the step 2) is hydrogen peroxide.
Optionally, the first reducing agent in step 3) is a mixture of vitamin C and sodium bisulfite.
Optionally, the mixture is vitamin C: sodium bisulfite ═ 1: (2.2-6).
Optionally, in the step 3), the organic salt is sodium citrate, the second reducing agent is ammonium ferrous sulfate, the molecular regulator is amide phosphate, and the molecular formula of the methallyl polyoxyethylene ether is as follows:
CH2＝C(CH3)CH2O(CH2CH2O)nH，n＝10～60。
in addition, the high slump-retaining type polycarboxylate water reducer prepared by the preparation method is also provided.
The preparation method of the high slump retaining type polycarboxylate water reducer is simple in process, the adopted raw materials are common materials which can be purchased conveniently in the market, no waste gas or waste water is discharged in the whole process, and the production cost and the environmental protection pressure of the polycarboxylate water reducer are well reduced. In addition, the polycarboxylate superplasticizer prepared by the preparation method has the performance of keeping excellent slump for a long time under the condition of basically not influencing the compressive strength of concrete, so that the workability and the applicability of the concrete are improved.
Detailed Description
The present solution is illustrated below with reference to examples.
The invention provides a preparation method of a high slump retaining type polycarboxylate superplasticizer. The method mainly comprises the following steps:
1) mixing water, unsaturated organic acid and unsaturated ester to prepare a solution A;
2) mixing water and an oxidant to prepare a solution B;
3) mixing water and a first reducing agent to prepare a solution C;
4) sequentially adding organic salt, a second reducing agent and a molecular weight regulating agent into the methyl allyl polyoxyethylene ether aqueous solution until the materials are completely dissolved to obtain a solution D;
5) dropwise adding the solution A into the solution D according to 15% of the weight to obtain a solution E;
6) simultaneously dripping the solution B, the rest solution A and the solution C into the solution E to obtain a solution F; and the solution F is a high slump retaining type polycarboxylate superplasticizer solution.
More specifically, a preparation method of the high slump loss resistant type polycarboxylate superplasticizer. The method mainly comprises the following steps:
1) adding unsaturated organic acid and unsaturated ester into water, and fully stirring to form a completely dispersed mixed solution A, wherein the water can be tap water which is common and qualified in the market, the unsaturated organic acid is preferably acrylic acid, and the unsaturated ester is preferably hydroxypropyl acrylate;
2) adding an oxidant into water, and fully stirring to form a completely dispersed mixed solution B, wherein the water can be common and qualified tap water on the market, and the oxidant is preferably hydrogen peroxide;
3) adding a first reducing agent into water, and fully stirring to form a completely dispersed mixed solution C, wherein the water can adopt commercially common and qualified tap water, the first reducing agent preferably adopts a mixture of vitamin C and sodium bisulfite, and the mixture comprises the following components in percentage by mass: sodium bisulfite ═ 1: (2.2-6);
4) putting methyl allyl polyoxyethylene ether into a four-neck flask, adding water, stirring at normal temperature until the methyl allyl polyoxyethylene ether is completely dissolved, sequentially adding organic salt and a second reducing agent into the four-neck flask, and stirring a molecular weight regulator until the materials are completely dissolved to obtain a solution D, wherein the water can adopt common and qualified tap water on the market, the organic salt is preferably sodium citrate, the second reducing agent is preferably ammonium ferrous sulfate, the molecular weight regulator is preferably amide phosphate, and the molecular formula of the methyl allyl polyoxyethylene ether is as follows:
CH2＝C(CH3)CH2O(CH2CH2O)nH，n＝10～60；
5) dropwise adding the solution A into the solution D according to 15% of the weight of the solution A, and uniformly stirring to obtain a solution E, wherein the dropwise adding time of the solution A is 15 min;
6) dripping the solution B, the rest solution A and the rest solution C into the solution E at a constant speed, wherein the dripping time of the solution B is 95 min; the dropping time of the solution A is 90 min; and (3) dropwise adding the solution C for 100min, and stirring for 30min after dropwise adding the solution C to obtain a solution F, wherein the solution F is a high slump retaining type polycarboxylate superplasticizer solution.
Wherein in the solution A, the components comprise water in parts by mass: 10-12 parts of unsaturated organic acid: 3-5 parts of unsaturated ester: 6-8 parts;
in the solution B, the components comprise water in parts by mass: 3-4 parts of an oxidant: 0.6-0.8 part;
in the solution C, the components comprise water in parts by mass: 3-4 parts of a first reducing agent: 0.4-0.5 part;
in the solution D, the components comprise water in parts by mass: 40-44 parts of methyl allyl polyoxyethylene ether: 28-31 parts of organic salt: 2-3 parts of a second reducing agent: 0.04-0.09 part of a molecular weight regulator: 1.5 to 2.5 portions.
The application a preparation method of high slump retaining type polycarboxylate water reducing agent adopts common material on the market, and these materials all can be directly bought from the market to no special model or performance requirement, water is the running water, consequently in the aspect of raw and other materials, the raw materials cost of this preparation method of high slump retaining type polycarboxylate water reducing agent is very little, and the production technology of this preparation method of high slump retaining type polycarboxylate water reducing agent is also comparatively simple in addition, and does not have waste gas waste water discharge, has further reduced manufacturing cost, and accords with the requirement of industrial production to the feature of environmental protection now.
The application also provides a high slump retaining type polycarboxylate superplasticizer which is prepared by the preparation method.
Practical properties of the high slump loss resistant type polycarboxylate water reducer prepared by the preparation method are illustrated by the following examples.
Example 1
The high slump retaining type polycarboxylate superplasticizer is prepared by the preparation method, wherein:
in the solution A, the components comprise water in parts by mass: 11 parts of unsaturated organic acid: 4 parts of unsaturated ester: 7 parts;
in the solution B, the components comprise water in parts by mass: 3.5 parts of an oxidant: 0.7 part;
in the solution C, the components comprise water in parts by mass: 3.5 parts of a first reducing agent: 0.45 part;
in the solution D, the components comprise water in parts by mass: 42 parts of methyl allyl polyoxyethylene ether: 29.5 parts of organic salt: 2.5 parts of a second reducing agent: 0.065 part of molecular weight regulator: and 2 parts.
The first reducing agent is prepared from vitamin C and sodium bisulfite according to the mass ratio of vitamin C: sodium bisulfite is 1: 4.1 of the mixture.
Example 2
The high slump loss resistant polycarboxylate water reducer of the embodiment is prepared by the preparation method, and is different from the polycarboxylate water reducer of the embodiment 1 in that:
and in the solution A, the mass part of the unsaturated organic acid is 3 parts.
Specifically, in the solution A, the components comprise water in parts by mass: 11 parts of unsaturated organic acid: 3 parts of unsaturated ester: 7 parts;
in the solution B, the components comprise water in parts by mass: 3.5 parts of an oxidant: 0.7 part;
in the solution C, the components comprise water in parts by mass: 3.5 parts of a first reducing agent: 0.45 part;
in the solution D, the components comprise water in parts by mass: 42 parts of methyl allyl polyoxyethylene ether: 29.5 parts of organic salt: 2.5 parts of a second reducing agent: 0.065 part of molecular weight regulator: and 2 parts.
The first reducing agent is prepared from vitamin C and sodium bisulfite according to the mass ratio of vitamin C: sodium bisulfite is 1: 4.1 of the mixture.
Example 3
The high slump loss resistant polycarboxylate water reducer of the embodiment is prepared by the preparation method, and is different from the polycarboxylate water reducer of the embodiment 1 in that:
and in the solution A, the mass part of the unsaturated organic acid is 5 parts.
Specifically, in the solution A, the components comprise water in parts by mass: 11 parts of unsaturated organic acid: 5 parts of unsaturated ester: 7 parts;
in the solution B, the components comprise water in parts by mass: 3.5 parts of an oxidant: 0.7 part;
in the solution C, the components comprise water in parts by mass: 3.5 parts of a first reducing agent: 0.45 part;
in the solution D, the components comprise water in parts by mass: 42 parts of methyl allyl polyoxyethylene ether: 29.5 parts of organic salt: 2.5 parts of a second reducing agent: 0.065 part of molecular weight regulator: and 2 parts.
The first reducing agent is prepared from vitamin C and sodium bisulfite according to the mass ratio of vitamin C: sodium bisulfite is 1: 4.1 of the mixture.
Example 4
The high slump loss resistant polycarboxylate water reducer of the embodiment is prepared by the preparation method, and is different from the polycarboxylate water reducer of the embodiment 1 in that:
in the solution A, the mass part of the unsaturated ester is 6 parts.
Specifically, in the solution A, the components comprise water in parts by mass: 11 parts of unsaturated organic acid: 4 parts of unsaturated ester: 6 parts of (1);
in the solution B, the components comprise water in parts by mass: 3.5 parts of an oxidant: 0.7 part;
in the solution C, the components comprise water in parts by mass: 3.5 parts of a first reducing agent: 0.45 part;
in the solution D, the components comprise water in parts by mass: 42 parts of methyl allyl polyoxyethylene ether: 29.5 parts of organic salt: 2.5 parts of a second reducing agent: 0.065 part of molecular weight regulator: and 2 parts.
The first reducing agent is prepared from vitamin C and sodium bisulfite according to the mass ratio of vitamin C: sodium bisulfite is 1: 4.1 of the mixture.
Example 5
The high slump loss resistant polycarboxylate water reducer of the embodiment is prepared by the preparation method, and is different from the polycarboxylate water reducer of the embodiment 1 in that:
in the solution A, the mass part of the unsaturated ester is 8 parts.
Specifically, in the solution A, the components comprise water in parts by mass: 11 parts of unsaturated organic acid: 4 parts of unsaturated ester: 0.8 part;
in the solution B, the components comprise water in parts by mass: 3.5 parts of an oxidant: 0.7 part;
in the solution C, the components comprise water in parts by mass: 3.5 parts of a first reducing agent: 0.45 part;
in the solution D, the components comprise water in parts by mass: 42 parts of methyl allyl polyoxyethylene ether: 29.5 parts of organic salt: 2.5 parts of a second reducing agent: 0.065 part of molecular weight regulator: and 2 parts.
The first reducing agent is prepared from vitamin C and sodium bisulfite according to the mass ratio of vitamin C: sodium bisulfite is 1: 4.1 of the mixture.
Example 6
The high slump loss resistant polycarboxylate water reducer of the embodiment is prepared by the preparation method, and is different from the polycarboxylate water reducer of the embodiment 1 in that:
and in the solution B, the mass part of the oxidant is 0.6 part.
Specifically, in the solution A, the components comprise water in parts by mass: 11 parts of unsaturated organic acid: 4 parts of unsaturated ester: 7 parts;
in the solution B, the components comprise water in parts by mass: 3.5 parts of an oxidant: 0.6 part;
in the solution C, the components comprise water in parts by mass: 3.5 parts of a first reducing agent: 0.45 part;
in the solution D, the components comprise water in parts by mass: 42 parts of methyl allyl polyoxyethylene ether: 29.5 parts of organic salt: 2.5 parts of a second reducing agent: 0.065 part of molecular weight regulator: and 2 parts.
The first reducing agent is prepared from vitamin C and sodium bisulfite according to the mass ratio of vitamin C: sodium bisulfite is 1: 4.1 of the mixture.
Example 7
The high slump loss resistant polycarboxylate water reducer of the embodiment is prepared by the preparation method, and is different from the polycarboxylate water reducer of the embodiment 1 in that:
and in the solution B, the mass part of the oxidant is 0.8 part.
Specifically, in the solution A, the components comprise water in parts by mass: 11 parts of unsaturated organic acid: 4 parts of unsaturated ester: 7 parts;
in the solution B, the components comprise water in parts by mass: 3.5 parts of an oxidant: 0.8 part;
in the solution C, the components comprise water in parts by mass: 3.5 parts of a first reducing agent: 0.45 part;
in the solution D, the components comprise water in parts by mass: 42 parts of methyl allyl polyoxyethylene ether: 29.5 parts of organic salt: 2.5 parts of a second reducing agent: 0.065 part of molecular weight regulator: and 2 parts.
The first reducing agent is prepared from vitamin C and sodium bisulfite according to the mass ratio of vitamin C: sodium bisulfite is 1: 4.1 of the mixture.
Example 8
The high slump loss resistant polycarboxylate water reducer of the embodiment is prepared by the preparation method, and is different from the polycarboxylate water reducer of the embodiment 1 in that:
in the solution C, the mass part of the first reducing agent is 0.4 part.
Specifically, in the solution A, the components comprise water in parts by mass: 11 parts of unsaturated organic acid: 4 parts of unsaturated ester: 7 parts;
in the solution B, the components comprise water in parts by mass: 3.5 parts of an oxidant: 0.7 part;
in the solution C, the components comprise water in parts by mass: 3.5 parts of a first reducing agent: 0.4 part;
in the solution D, the components comprise water in parts by mass: 42 parts of methyl allyl polyoxyethylene ether: 29.5 parts of organic salt: 2.5 parts of a second reducing agent: 0.065 part of molecular weight regulator: and 2 parts.
The first reducing agent is prepared from vitamin C and sodium bisulfite according to the mass ratio of vitamin C: sodium bisulfite is 1: 4.1 of the mixture.
Example 9
The high slump loss resistant polycarboxylate water reducer of the embodiment is prepared by the preparation method, and is different from the polycarboxylate water reducer of the embodiment 1 in that:
in the solution C, the mass part of the first reducing agent is 0.5 part.
Specifically, in the solution A, the components comprise water in parts by mass: 11 parts of unsaturated organic acid: 4 parts of unsaturated ester: 7 parts;
in the solution B, the components comprise water in parts by mass: 3.5 parts of an oxidant: 0.7 part;
in the solution C, the components comprise water in parts by mass: 3.5 parts of a first reducing agent: 0.5 part;
in the solution D, the components comprise water in parts by mass: 42 parts of methyl allyl polyoxyethylene ether: 29.5 parts of organic salt: 2.5 parts of a second reducing agent: 0.065 part of molecular weight regulator: and 2 parts.
The first reducing agent is prepared from vitamin C and sodium bisulfite according to the mass ratio of vitamin C: sodium bisulfite is 1: 4.1 of the mixture.
Example 10
The high slump loss resistant polycarboxylate water reducer of the embodiment is prepared by the preparation method, and is different from the polycarboxylate water reducer of the embodiment 1 in that:
in the solution D, the mass part of the methyl allyl polyoxyethylene ether is 28 parts.
Specifically, in the solution A, the components comprise water in parts by mass: 11 parts of unsaturated organic acid: 4 parts of unsaturated ester: 7 parts;
in the solution B, the components comprise water in parts by mass: 3.5 parts of an oxidant: 0.7 part;
in the solution C, the components comprise water in parts by mass: 3.5 parts of a first reducing agent: 0.45 part;
in the solution D, the components comprise water in parts by mass: 42 parts of methyl allyl polyoxyethylene ether: 28 parts of organic salt: 2.5 parts of a second reducing agent: 0.065 part of molecular weight regulator: and 2 parts.
The first reducing agent is prepared from vitamin C and sodium bisulfite according to the mass ratio of vitamin C: sodium bisulfite is 1: 4.1 of the mixture.
Example 11
The high slump loss resistant polycarboxylate water reducer of the embodiment is prepared by the preparation method, and is different from the polycarboxylate water reducer of the embodiment 1 in that:
and in the solution D, the mass part of the methyl allyl polyoxyethylene ether is 31 parts.
Specifically, in the solution A, the components comprise water in parts by mass: 11 parts of unsaturated organic acid: 4 parts of unsaturated ester: 7 parts;
in the solution B, the components comprise water in parts by mass: 3.5 parts of an oxidant: 0.7 part;
in the solution C, the components comprise water in parts by mass: 3.5 parts of a first reducing agent: 0.45 part;
in the solution D, the components comprise water in parts by mass: 42 parts of methyl allyl polyoxyethylene ether: 31 parts of organic salt: 2.5 parts of a second reducing agent: 0.065 part of molecular weight regulator: and 2 parts.
The first reducing agent is prepared from vitamin C and sodium bisulfite according to the mass ratio of vitamin C: sodium bisulfite is 1: 4.1 of the mixture.
Example 12
The high slump loss resistant polycarboxylate water reducer of the embodiment is prepared by the preparation method, and is different from the polycarboxylate water reducer of the embodiment 1 in that:
and in the solution D, the mass part of the organic salt is 2 parts.
Specifically, in the solution A, the components comprise water in parts by mass: 11 parts of unsaturated organic acid: 4 parts of unsaturated ester: 7 parts;
in the solution B, the components comprise water in parts by mass: 3.5 parts of an oxidant: 0.7 part;
in the solution C, the components comprise water in parts by mass: 3.5 parts of a first reducing agent: 0.45 part;
in the solution D, the components comprise water in parts by mass: 42 parts of methyl allyl polyoxyethylene ether: 29.5 parts of organic salt: 2 parts of a second reducing agent: 0.065 part of molecular weight regulator: and 2 parts.
The first reducing agent is prepared from vitamin C and sodium bisulfite according to the mass ratio of vitamin C: sodium bisulfite is 1: 4.1 of the mixture.
Example 13
The high slump loss resistant polycarboxylate water reducer of the embodiment is prepared by the preparation method, and is different from the polycarboxylate water reducer of the embodiment 1 in that:
and in the solution D, the mass part of the organic salt is 3 parts.
Specifically, in the solution A, the components comprise water in parts by mass: 11 parts of unsaturated organic acid: 4 parts of unsaturated ester: 7 parts;
in the solution B, the components comprise water in parts by mass: 3.5 parts of an oxidant: 0.7 part;
in the solution C, the components comprise water in parts by mass: 3.5 parts of a first reducing agent: 0.45 part;
in the solution D, the components comprise water in parts by mass: 42 parts of methyl allyl polyoxyethylene ether: 29.5 parts of organic salt: 3 parts of a second reducing agent: 0.065 part of molecular weight regulator: and 2 parts.
The first reducing agent is prepared from vitamin C and sodium bisulfite according to the mass ratio of vitamin C: sodium bisulfite is 1: 4.1 of the mixture.
Example 14
The high slump loss resistant polycarboxylate water reducer of the embodiment is prepared by the preparation method, and is different from the polycarboxylate water reducer of the embodiment 1 in that:
and in the solution D, the mass part of the second reducing agent is 0.04 part.
Specifically, in the solution A, the components comprise water in parts by mass: 11 parts of unsaturated organic acid: 4 parts of unsaturated ester: 7 parts;
in the solution B, the components comprise water in parts by mass: 3.5 parts of an oxidant: 0.7 part;
in the solution C, the components comprise water in parts by mass: 3.5 parts of a first reducing agent: 0.45 part;
in the solution D, the components comprise water in parts by mass: 42 parts of methyl allyl polyoxyethylene ether: 29.5 parts of organic salt: 2.5 parts of a second reducing agent: 0.04 parts of a molecular weight regulator: and 2 parts.
The first reducing agent is prepared from vitamin C and sodium bisulfite according to the mass ratio of vitamin C: sodium bisulfite is 1: 4.1 of the mixture.
Example 15
The high slump loss resistant polycarboxylate water reducer of the embodiment is prepared by the preparation method, and is different from the polycarboxylate water reducer of the embodiment 1 in that:
in the solution D, the mass part of the second reducing agent is 0.09 part.
Specifically, in the solution A, the components comprise water in parts by mass: 11 parts of unsaturated organic acid: 4 parts of unsaturated ester: 7 parts;
in the solution B, the components comprise water in parts by mass: 3.5 parts of an oxidant: 0.7 part;
in the solution C, the components comprise water in parts by mass: 3.5 parts of a first reducing agent: 0.45 part;
in the solution D, the components comprise water in parts by mass: 42 parts of methyl allyl polyoxyethylene ether: 29.5 parts of organic salt: 2.5 parts of a second reducing agent: 0.09 part of molecular weight regulator: and 2 parts.
The first reducing agent is prepared from vitamin C and sodium bisulfite according to the mass ratio of vitamin C: sodium bisulfite is 1: 4.1 of the mixture.
Example 16
The high slump loss resistant polycarboxylate water reducer of the embodiment is prepared by the preparation method, and is different from the polycarboxylate water reducer of the embodiment 1 in that:
and in the solution D, the mass part of the molecular weight regulator is 1.5 parts.
Specifically, in the solution A, the components comprise water in parts by mass: 11 parts of unsaturated organic acid: 4 parts of unsaturated ester: 7 parts;
in the solution B, the components comprise water in parts by mass: 3.5 parts of an oxidant: 0.7 part;
in the solution C, the components comprise water in parts by mass: 3.5 parts of a first reducing agent: 0.45 part;
in the solution D, the components comprise water in parts by mass: 42 parts of methyl allyl polyoxyethylene ether: 29.5 parts of organic salt: 2.5 parts of a second reducing agent: 0.65 part of molecular weight regulator: 1.5 parts.
The first reducing agent is prepared from vitamin C and sodium bisulfite according to the mass ratio of vitamin C: sodium bisulfite is 1: 4.1 of the mixture.
Example 17
The high slump loss resistant polycarboxylate water reducer of the embodiment is prepared by the preparation method, and is different from the polycarboxylate water reducer of the embodiment 1 in that:
and in the solution D, the mass part of the molecular weight regulator is 2.5 parts.
Specifically, in the solution A, the components comprise water in parts by mass: 11 parts of unsaturated organic acid: 4 parts of unsaturated ester: 7 parts;
in the solution B, the components comprise water in parts by mass: 3.5 parts of an oxidant: 0.7 part;
in the solution C, the components comprise water in parts by mass: 3.5 parts of a first reducing agent: 0.45 part;
in the solution D, the components comprise water in parts by mass: 42 parts of methyl allyl polyoxyethylene ether: 29.5 parts of organic salt: 2.5 parts of a second reducing agent: 0.65 part of molecular weight regulator: 2.5 parts.
The first reducing agent is prepared from vitamin C and sodium bisulfite according to the mass ratio of vitamin C: sodium bisulfite is 1: 4.1 of the mixture.
Example 18
The high slump loss resistant polycarboxylate water reducer of the embodiment is prepared by the preparation method, and is different from the polycarboxylate water reducer of the embodiment 1 in that:
in the solution C, the first reducing agent adopts vitamin C and sodium bisulfite in a mass ratio of vitamin C: sodium bisulfite is 1: 2.2.
Specifically, in the solution A, the components comprise water in parts by mass: 11 parts of unsaturated organic acid: 4 parts of unsaturated ester: 7 parts;
in the solution B, the components comprise water in parts by mass: 3.5 parts of an oxidant: 0.7 part;
in the solution C, the components comprise water in parts by mass: 3.5 parts of a first reducing agent: 0.45 part;
in the solution D, the components comprise water in parts by mass: 42 parts of methyl allyl polyoxyethylene ether: 29.5 parts of organic salt: 2.5 parts of a second reducing agent: 0.65 part of molecular weight regulator: 2.5 parts.
Example 19
The high slump loss resistant polycarboxylate water reducer of the embodiment is prepared by the preparation method, and is different from the polycarboxylate water reducer of the embodiment 1 in that:
in the solution C, the first reducing agent adopts vitamin C and sodium bisulfite in a mass ratio of vitamin C: sodium bisulfite is 1: 6.
And in the solution D, the mass part of the molecular weight regulator is 2.5 parts.
Specifically, in the solution A, the components comprise water in parts by mass: 11 parts of unsaturated organic acid: 4 parts of unsaturated ester: 7 parts;
in the solution B, the components comprise water in parts by mass: 3.5 parts of an oxidant: 0.7 part;
in the solution C, the components comprise water in parts by mass: 3.5 parts of a first reducing agent: 0.45 part;
in the solution D, the components comprise water in parts by mass: 42 parts of methyl allyl polyoxyethylene ether: 29.5 parts of organic salt: 2.5 parts of a second reducing agent: 0.65 part of molecular weight regulator: 2.5 parts.
It should be noted that the raw materials used in the above examples are the same raw materials, and the differences between the examples are only the differences in the mass parts of a certain component. Specifically, the water is tap water which is common and qualified in the market; the unsaturated organic acid is acrylic acid; the unsaturated ester adopts hydroxypropyl acrylate; the oxidant is hydrogen peroxide; the first reducing agent is a mixture of vitamin C and sodium bisulfite, and the mixture is a mixture of vitamin C and sodium bisulfite; the organic salt is sodium citrate; the second reducing agent adopts ammonium ferrous sulfate; the molecular weight regulator adopts amide phosphate; the molecular formula of the methyl allyl polyoxyethylene ether is as follows:
CH2＝C(CH3)CH2O(CH2CH2O)nH，n＝10～60。
the experimental concrete is prepared by mixing the high slump retaining type polycarboxylate superplasticizer with different component ratios obtained in the embodiment with other components, wherein the experimental concrete adopts a cement type of P.O42.5R, and the dosage of the concrete is 280kg/m3And other components also comprise:
the using amount of the fly ash is 50kg/m3；
The amount of the machine sand is 750kg/m3；
Fine sand in an amount of 150kg/m3；
Stone in 1050kg/m3；
Water in an amount of 160kg/m3。
The materials are common commercial materials which can be purchased in the market, wherein water is common qualified tap water, and the mixing amount of the high slump loss resistant type polycarboxylate superplasticizer in concrete is 1.5%. The final test results are given in the following table, wherein the gas content is 2.8%:
Figure BDA0002283165040000161
Figure BDA0002283165040000171
wherein, the water reducing agent adopted by the control experiment group is other common conventional slump-retaining water reducing agents in the market; in addition, the 0h, 1h, 2h, 3h and 4h refer to the time measured from the time of adding water in the process of stirring concrete in the concrete slump test, and it is noted that after the concrete is stirred, the concrete needs to be placed in a specific container for standing. Can derive through above-mentioned experimental data, this application high slump retaining type polycarboxylate water reducing agent can obviously promote the slump retaining performance of concrete under the condition that does not reduce concrete compressive strength basically to make the concrete also can keep good slump under the complex condition, guaranteed the workability of concrete.
The same and similar parts among the various embodiments in the specification of the present application may be referred to each other. Especially, for the system and terminal embodiments, since the method therein is basically similar to the method embodiments, the description is relatively simple, and the relevant points can be referred to the description in the method embodiments.
It is noted that, in this document, relational terms such as "first" and "second," and the like, may be used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Also, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus. Without further limitation, an element defined by the phrase "comprising an … …" does not exclude the presence of other identical elements in a process, method, article, or apparatus that comprises the element.
Of course, the above description is not limited to the above examples, and technical features that are not described in this application may be implemented by or using the prior art, and are not described herein again; the above examples are merely illustrative of the technical solutions of the present application and are not intended to limit the present application, and the present application is only described in detail with reference to the preferred embodiments, and those skilled in the art should understand that changes, additions or substitutions which are made by those skilled in the art within the spirit of the present application are also within the scope of the claims of the present application.

Claims (9)

1. A preparation method of a high slump retaining type polycarboxylate superplasticizer is characterized by comprising the following steps:
1) mixing water, unsaturated organic acid and unsaturated ester to prepare a solution A;
2) mixing water and an oxidant to prepare a solution B;
3) mixing water and a first reducing agent to prepare a solution C;
4) sequentially adding organic salt, a second reducing agent and a molecular weight regulating agent into the methyl allyl polyoxyethylene ether aqueous solution until the materials are completely dissolved to obtain a solution D;
5) dropwise adding the solution A into the solution D according to 15% of the weight to obtain a solution E;
6) simultaneously dripping the solution B, the rest solution A and the solution C into the solution E to obtain a solution F;
and the solution F is a high slump retaining type polycarboxylate superplasticizer solution.
2. The preparation method of the high slump retaining type polycarboxylate water reducer as claimed in claim 1,
in the solution A, the components comprise water in parts by mass: 10-12 parts of unsaturated organic acid: 3-5 parts of unsaturated ester: 6-8 parts;
in the solution B, the components comprise water in parts by mass: 3-4 parts of an oxidant: 0.6-0.8 part;
in the solution C, the components comprise water in parts by mass: 3-4 parts of a first reducing agent: 0.4-0.5 part;
in the solution D, the components comprise water in parts by mass: 40-44 parts of methyl allyl polyoxyethylene ether: 28-31 parts of organic salt: 2-3 parts of a second reducing agent: 0.04-0.09 part of a molecular weight regulator: 1.5 to 2.5 portions.
3. The preparation method of the high slump retaining type polycarboxylate water reducer as claimed in claim 1, wherein the dropping time of the solution B in the step 6) is 95 min; the dropping time of the solution A is 90 min; and (3) dropwise adding the solution C for 100min, and stirring for 30min after dropwise adding the solution C to obtain a solution F, wherein the solution F is a high slump retaining type polycarboxylate superplasticizer solution.
4. The preparation method of the high slump loss resistant polycarboxylic acid water reducing agent according to claim 1, wherein the unsaturated organic acid in the step 1) is acrylic acid, and the unsaturated ester is hydroxypropyl acrylate.
5. The preparation method of the high slump retaining type polycarboxylate water reducer according to claim 1, wherein an oxidant in the step 2) is hydrogen peroxide.
6. The preparation method of the high slump retaining type polycarboxylate water reducer as claimed in claim 1, wherein the first reducing agent in the step 3) is a mixture of vitamin C and sodium bisulfite.
7. The preparation method of the high slump retaining type polycarboxylate water reducer as claimed in claim 6, wherein the mixture is prepared from the following components in percentage by mass: sodium bisulfite ═ 1: (2.2-6).
8. The preparation method of the high slump loss resistant type polycarboxylate water reducer according to claim 1, wherein the organic salt in the step 3) is sodium citrate, the second reducing agent is ammonium ferrous sulfate, the molecular regulator is amide phosphate, and the molecular formula of the methallyl polyoxyethylene ether is as follows:
CH2＝C(CH3)CH2O(CH2CH2O)nH，n＝10～60。
9. a high slump retaining type polycarboxylate water reducer is characterized by being prepared by the preparation method of any one of claims 1-8.
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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20150291716A1 (en) * 2012-12-05 2015-10-15 Sobute New Materials Co., Ltd. Slump retaining polycarboxylic acid superplasticizer
CN108484838A (en) * 2018-03-21 2018-09-04 江苏诚意水泥有限公司 A kind of super collapse protective poly-carboxylic acid series high-performance dehydragent and preparation method thereof
CN110003402A (en) * 2019-04-23 2019-07-12 四川同舟化工科技有限公司 A kind of anti-mud collapse protective poly-carboxylic acid water reducing agent and its low temperature preparation method of lower shrinkage high-adaptability

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20150291716A1 (en) * 2012-12-05 2015-10-15 Sobute New Materials Co., Ltd. Slump retaining polycarboxylic acid superplasticizer
CN108484838A (en) * 2018-03-21 2018-09-04 江苏诚意水泥有限公司 A kind of super collapse protective poly-carboxylic acid series high-performance dehydragent and preparation method thereof
CN110003402A (en) * 2019-04-23 2019-07-12 四川同舟化工科技有限公司 A kind of anti-mud collapse protective poly-carboxylic acid water reducing agent and its low temperature preparation method of lower shrinkage high-adaptability

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