CN108793810A - A kind of preparation method of polycarboxylate water-reducer - Google Patents

A kind of preparation method of polycarboxylate water-reducer Download PDF

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Publication number
CN108793810A
CN108793810A CN201810685272.8A CN201810685272A CN108793810A CN 108793810 A CN108793810 A CN 108793810A CN 201810685272 A CN201810685272 A CN 201810685272A CN 108793810 A CN108793810 A CN 108793810A
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China
Prior art keywords
solution
water
stirring
polymeric monomer
added
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CN201810685272.8A
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Chinese (zh)
Inventor
余协平
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Wuhan Chong Chong Technology Co Ltd
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Wuhan Chong Chong Technology Co Ltd
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Priority to CN201810685272.8A priority Critical patent/CN108793810A/en
Publication of CN108793810A publication Critical patent/CN108793810A/en
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    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B24/00Use of organic materials as active ingredients for mortars, concrete or artificial stone, e.g. plasticisers
    • C04B24/16Sulfur-containing compounds
    • C04B24/161Macromolecular compounds comprising sulfonate or sulfate groups
    • C04B24/163Macromolecular compounds comprising sulfonate or sulfate groups obtained by reactions only involving carbon-to-carbon unsaturated bonds
    • C04B24/165Macromolecular compounds comprising sulfonate or sulfate groups obtained by reactions only involving carbon-to-carbon unsaturated bonds containing polyether side chains
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08FMACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F220/00Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
    • C08F220/02Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
    • C08F220/04Acids; Metal salts or ammonium salts thereof
    • C08F220/06Acrylic acid; Methacrylic acid; Metal salts or ammonium salts thereof
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2103/00Function or property of ingredients for mortars, concrete or artificial stone
    • C04B2103/30Water reducers, plasticisers, air-entrainers, flow improvers
    • C04B2103/302Water reducers

Abstract

The invention discloses a kind of preparation methods of polycarboxylate water-reducer, belong to water-reducing agent technical field.Include the following steps:S1, polymeric monomer and 2- acrylamidos -2- methyl-1s-propane sulfonic acid are added, stirring is to being completely dissolved, then is warming up to 60 DEG C, oxidant is added, bottom liquid is made in stirring and dissolving;S2, unsaturated acids, beta-unsaturated esters and chain conversion agent are add to deionized water, stirring and dissolving, solution A is made;S3, reducing agent is add to deionized water, stirring and dissolving, B solution is made;S4, at a temperature of 60~70 DEG C, solution A and B solution is added dropwise respectively simultaneously into bottom liquid;After S5, completion of dropwise addition, continue constant temperature and stir 1~2h, then be cooled to 20~40 DEG C, 30% sodium hydroxide solution is added and adjusts pH to 6~7, obtains polycarboxylate water-reducer.Water-reducing agent water-reducing rate made from polycarboxylate water-reducer produced by the present invention is high, function of slump protection is good.

Description

A kind of preparation method of polycarboxylate water-reducer
Technical field
The invention belongs to water-reducing agent technical fields, and in particular to a kind of preparation method of polycarboxylate water-reducer.
Background technology
Polycarboxylate water-reducer is a kind of high-performance water reducing agent, is a kind of cement dispersants during cement concrete uses, Be at present in the world generally acknowledged research with application prospect preferably and the optimal water-reducing agent of comprehensive performance, be widely used in highway, The engineerings such as bridge, dam, tunnel, skyscraper.
The molecular structure of polycarboxylate water-reducer is designed for the cement mechanism of action, has that ultra-dispersed property, volume be low, slump retaining Can be good the advantages that.It is in recent years, domestic unprecedentedly active to the research of water-reducing agent because of the significant economic benefit of polycarboxylate water-reducer, And there is certain improvement in its preparation process.But it is poor to still remain polycarboxylate water-reducer comprehensive performance, and slump retaining is insufficient The problem of.
Invention content
For the above-mentioned prior art the problem of, the present invention provides a kind of preparation method of polycarboxylate water-reducer, Water-reducing agent water-reducing rate obtained is high, function of slump protection is good.
The invention is realized in this way:
S1, deionized water is warming up to 58 DEG C, polymeric monomer and 2- acrylamidos -2- methyl-1s-propane sulfonic acid is added, stirring is extremely It is completely dissolved, then is warming up to 60 DEG C, oxidant is added, bottom liquid is made in stirring and dissolving;
S2, unsaturated acids, beta-unsaturated esters and chain conversion agent are add to deionized water, stirring and dissolving, solution A is made;
S3, reducing agent is add to deionized water, stirring and dissolving, B solution is made;
S4, at a temperature of 60~70 DEG C, solution A and B solution is added dropwise respectively simultaneously into bottom liquid, wherein the time for adding of solution A For 3.5h, mode is added dropwise and is added dropwise for speed change, the time for adding of B solution is 3h, and dropwise addition mode is at the uniform velocity to be added dropwise;
After S5, completion of dropwise addition, continue constant temperature and stir 1~2h, then be cooled to 20~40 DEG C, 30% sodium hydroxide solution is added and adjusts PH to 6~7, obtains polycarboxylate water-reducer;
Wherein, the polymeric monomer is any one in methyl allyl polyoxyethylene ether, own pentenyl polyoxyethylene ether, described Unsaturated acids is alkyl acrylic or acrylic acid, and the beta-unsaturated esters are ethyl methacrylate, propyl methacrylate, propylene Any one in acetoacetic ester, propyl acrylate, the polymeric monomer, unsaturated acids, beta-unsaturated esters molar ratio be(1~ 1.25):(3~5.5):(1.0~1.5).
Preferably, in step S1, the addition of the 2- acrylamidos -2- methyl-1s-propane sulfonic acid is the big list The 5% of body weight.
Preferably, in step S1, the oxidant is hydrogen peroxide, ammonium persulfate, sodium peroxydisulfate and tert-butyl hydroperoxide At least one of hydrogen, the addition of the oxidant be the polymeric monomer, unsaturated acids, beta-unsaturated esters gross mass 8~ 13%。
Preferably, in step S2, the chain conversion agent is thioacetic acid or mercaptopropionic acid, the addition of the chain conversion agent For the polymeric monomer, unsaturated acids, beta-unsaturated esters gross mass 0.4~4%.
Preferably, in step S3, the reducing agent be ascorbic acid, vitamin C, sodium sulfite and hypophosphites in extremely Few one kind, the addition of the reducing agent be the polymeric monomer, unsaturated acids, beta-unsaturated esters gross mass 6.5~10%.
Preferably, in step S4, it is by time for adding three equal parts, when the solution A is added dropwise at three sections that the speed change, which is added dropwise, Between the mass percent of middle dropwise addition be respectively 40~60%, 30~40%, 5~15%.
The invention has the advantages that:The present invention introduces sulfonic acid group in the molecular structure, enhances dispersion effect Fruit, while amide group is introduced, so that the speed that it discharges adsorption group is slowed down, increases its dispersion effect.In addition, being protected reaching Collapsing property, water-reducing rate and paste flowing degree three are with optimizing production technology under conditions of excellent, the poly- carboxylic for making it produce Not only water-reducing rate has reached 30% to sour water-reducing agent, and paste flowing degree and the slump in one hour is also made to influence to reduce.
Specific implementation mode
The embodiment of the present invention is described below in detail, the examples of the embodiments are intended to be used to explain the present invention, and cannot It is interpreted as limitation of the present invention.
Embodiment 1
A kind of preparation method of polycarboxylate water-reducer, includes the following steps:
S1, deionized water is warming up to 58 DEG C, polymeric monomer and 2- acrylamidos -2- methyl-1s-propane sulfonic acid is added, stirring is extremely It is completely dissolved, then is warming up to 60 DEG C, oxidant is added, bottom liquid is made in stirring and dissolving;
S2, unsaturated acids, beta-unsaturated esters and chain conversion agent are add to deionized water, stirring and dissolving, solution A is made;
S3, reducing agent is add to deionized water, stirring and dissolving, B solution is made;
S4, at a temperature of 60~70 DEG C, solution A and B solution is added dropwise respectively simultaneously into bottom liquid, wherein the time for adding of solution A For 3.5h, mode is added dropwise and is added dropwise for speed change, the time for adding of B solution is 3h, and dropwise addition mode is at the uniform velocity to be added dropwise;
After S5, completion of dropwise addition, continue constant temperature and stir 1~2h, then be cooled to 20~40 DEG C, 30% sodium hydroxide solution is added and adjusts PH to 6~7, obtains polycarboxylate water-reducer;
Wherein, polymeric monomer is methyl allyl polyoxyethylene ether, and unsaturated acids is acrylic acid, and beta-unsaturated esters are ethyl acrylate, Polymeric monomer, unsaturated acids, beta-unsaturated esters molar ratio be 1.25:5:1.5,2- acrylamido -2- methyl-1s-propane sulfonic acid Addition is the 5% of polymeric monomer weight.
Preferably, oxidant is hydrogen peroxide, and addition is polymeric monomer, unsaturated acids, beta-unsaturated esters gross mass 10%;Chain conversion agent is mercaptopropionic acid, addition be polymeric monomer, unsaturated acids, beta-unsaturated esters gross mass 1%;Reducing agent is anti- Bad hematic acid, addition be polymeric monomer, unsaturated acids, beta-unsaturated esters gross mass 6.5%.
More preferred, in step S4, speed change is added dropwise as by time for adding three equal parts, solution A is in three sections of time for adding The mass percent of dropwise addition is respectively 50%, 35%, 15%.
Embodiment 2
A kind of preparation method of polycarboxylate water-reducer, includes the following steps:
S1, deionized water is warming up to 58 DEG C, polymeric monomer and 2- acrylamidos -2- methyl-1s-propane sulfonic acid is added, stirring is extremely It is completely dissolved, then is warming up to 60 DEG C, oxidant is added, bottom liquid is made in stirring and dissolving;
S2, unsaturated acids, beta-unsaturated esters and chain conversion agent are add to deionized water, stirring and dissolving, solution A is made;
S3, reducing agent is add to deionized water, stirring and dissolving, B solution is made;
S4, at a temperature of 60~70 DEG C, solution A and B solution is added dropwise respectively simultaneously into bottom liquid, wherein the time for adding of solution A For 3.5h, mode is added dropwise and is added dropwise for speed change, the time for adding of B solution is 3h, and dropwise addition mode is at the uniform velocity to be added dropwise;
After S5, completion of dropwise addition, continue constant temperature and stir 1~2h, then be cooled to 20~40 DEG C, 30% sodium hydroxide solution is added and adjusts PH to 6~7, obtains polycarboxylate water-reducer;
Wherein, polymeric monomer is own pentenyl polyoxyethylene ether, and unsaturated acids is methacrylic acid, and beta-unsaturated esters are acrylic acid second Ester, polymeric monomer, unsaturated acids, beta-unsaturated esters molar ratio be 1:3:1,2- acrylamido -2- methyl-1s-propane sulfonic acid adds Enter 5% that amount is polymeric monomer weight.
Preferably, oxidant is sodium peroxydisulfate, addition be polymeric monomer, unsaturated acids, beta-unsaturated esters gross mass 8%; Chain conversion agent is thioacetic acid, addition be polymeric monomer, unsaturated acids, beta-unsaturated esters gross mass 0.4%;Reducing agent is that dimension is given birth to Plain C, addition be polymeric monomer, unsaturated acids, beta-unsaturated esters gross mass 10%.
More preferred, in step S4, speed change is added dropwise as by time for adding three equal parts, solution A is in three sections of time for adding The mass percent of dropwise addition is respectively 60%, 30%, 10%.
Embodiment 3
A kind of preparation method of polycarboxylate water-reducer, includes the following steps:
S1, deionized water is warming up to 58 DEG C, polymeric monomer and 2- acrylamidos -2- methyl-1s-propane sulfonic acid is added, stirring is extremely It is completely dissolved, then is warming up to 60 DEG C, oxidant is added, bottom liquid is made in stirring and dissolving;
S2, unsaturated acids, beta-unsaturated esters and chain conversion agent are add to deionized water, stirring and dissolving, solution A is made;
S3, reducing agent is add to deionized water, stirring and dissolving, B solution is made;
S4, at a temperature of 60~70 DEG C, solution A and B solution is added dropwise respectively simultaneously into bottom liquid, wherein the time for adding of solution A For 3.5h, mode is added dropwise and is added dropwise for speed change, the time for adding of B solution is 3h, and dropwise addition mode is at the uniform velocity to be added dropwise;
After S5, completion of dropwise addition, continue constant temperature and stir 1~2h, then be cooled to 20~40 DEG C, 30% sodium hydroxide solution is added and adjusts PH to 6~7, obtains polycarboxylate water-reducer;
Wherein, polymeric monomer is own pentenyl polyoxyethylene ether, and unsaturated acids is methacrylic acid, and beta-unsaturated esters are methacrylic acid Ethyl ester, polymeric monomer, unsaturated acids, beta-unsaturated esters molar ratio be 1.25:5.5:1.5,2- acrylamido -2- methyl-1s-the third The addition of alkyl sulfonic acid is the 5% of polymeric monomer weight.
Preferably, oxidant is ammonium persulfate, and addition is polymeric monomer, unsaturated acids, beta-unsaturated esters gross mass 13%;Chain conversion agent is thioacetic acid, addition be polymeric monomer, unsaturated acids, beta-unsaturated esters gross mass 4%;Reducing agent is secondary Sodium phosphate, addition be polymeric monomer, unsaturated acids, beta-unsaturated esters gross mass 8%.
More preferred, in step S4, speed change is added dropwise as by time for adding three equal parts, solution A is in three sections of time for adding The mass percent of dropwise addition is respectively 45%, 40%, 15%.
Certain ratio of mud is kept, above-described embodiment of 0.5% volume is added, by GB8077-2000《Concrete admixture is even Matter test method》The paste flowing degree test for carrying out cement, as a result such as table 1
Table 1
From the data in the table, the water-reducing agent function admirable produced through the present invention, with water-reducing rate height, fluidity is big, protects The good advantage of performance of collapsing.
Certainly, described above is only presently preferred embodiments of the present invention, not limitation of the present invention, the art Those of ordinary skill in the essential scope of the present invention variations, modifications, additions or substitutions made, also belong to the present invention's Protection domain.

Claims (6)

1. a kind of preparation method of polycarboxylate water-reducer, which is characterized in that include the following steps:
S1, deionized water is warming up to 58 DEG C, polymeric monomer and 2- acrylamidos -2- methyl-1s-propane sulfonic acid is added, stirring is extremely It is completely dissolved, then is warming up to 60 DEG C, oxidant is added, bottom liquid is made in stirring and dissolving;
S2, unsaturated acids, beta-unsaturated esters and chain conversion agent are add to deionized water, stirring and dissolving, solution A is made;
S3, reducing agent is add to deionized water, stirring and dissolving, B solution is made;
S4, at a temperature of 60~70 DEG C, solution A and B solution is added dropwise respectively simultaneously into bottom liquid, wherein the time for adding of solution A For 3.5h, mode is added dropwise and is added dropwise for speed change, the time for adding of B solution is 3h, and dropwise addition mode is at the uniform velocity to be added dropwise;
After S5, completion of dropwise addition, continue constant temperature and stir 1~2h, then be cooled to 20~40 DEG C, 30% sodium hydroxide solution is added and adjusts PH to 6~7, obtains polycarboxylate water-reducer;
Wherein, the polymeric monomer is any one in methyl allyl polyoxyethylene ether, own pentenyl polyoxyethylene ether, described Unsaturated acids is alkyl acrylic or acrylic acid, and the beta-unsaturated esters are ethyl methacrylate, propyl methacrylate, propylene Any one in acetoacetic ester, propyl acrylate, the polymeric monomer, unsaturated acids, beta-unsaturated esters molar ratio be(1~ 1.25):(3~5.5):(1.0~1.5).
2. a kind of preparation method of polycarboxylate water-reducer according to claim 1, it is characterised in that:It is described in step S1 The addition of 2- acrylamidos -2- methyl-1s-propane sulfonic acid is the 5% of the polymeric monomer weight.
3. a kind of preparation method of polycarboxylate water-reducer according to claim 1, it is characterised in that:It is described in step S1 Oxidant is at least one of hydrogen peroxide, ammonium persulfate, sodium peroxydisulfate and tert-butyl hydroperoxide, and the oxidant adds Enter amount be the polymeric monomer, unsaturated acids, beta-unsaturated esters gross mass 8~13%.
4. a kind of preparation method of polycarboxylate water-reducer according to claim 1, it is characterised in that:It is described in step S2 Chain conversion agent is thioacetic acid or mercaptopropionic acid, and the addition of the chain conversion agent is the polymeric monomer, unsaturated acids, unsaturation The 0.4~4% of ester gross mass.
5. a kind of preparation method of polycarboxylate water-reducer according to claim 1, it is characterised in that:It is described in step S3 Reducing agent is at least one of ascorbic acid, vitamin C, sodium sulfite and hypophosphites, and the addition of the reducing agent is The 6.5~10% of the polymeric monomer, unsaturated acids, beta-unsaturated esters gross mass.
6. a kind of preparation method of polycarboxylate water-reducer according to claim 1, it is characterised in that:It is described in step S4 Speed change is added dropwise as by time for adding three equal parts, the mass percent that the solution A is added dropwise in three sections of time for adding is respectively 40 ~60%, 30~40%, 5~15%.
CN201810685272.8A 2018-06-28 2018-06-28 A kind of preparation method of polycarboxylate water-reducer Pending CN108793810A (en)

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Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102358768A (en) * 2011-07-22 2012-02-22 广州市建筑科学研究院有限公司 Modified ether polycarboxylic acid water reducing agent and preparation method thereof
CN102503226A (en) * 2011-10-19 2012-06-20 中建商品混凝土有限公司 High slump retaining type polycarboxylic acid water reducing agent with sustained-release effect and preparation method thereof
CN103965414A (en) * 2014-05-23 2014-08-06 同济大学 High-early-strength polycarboxylate water reducer as well as synthesis method and application method of polycarboxylate water reducer
CN103992443A (en) * 2014-05-19 2014-08-20 科之杰新材料集团有限公司 Method for preparing polycarboxylate water reducing agent by normal-temperature mixing process
CN105645810A (en) * 2016-01-05 2016-06-08 河南新汉材料科技有限公司 Early-strength polycarboxylate type high-performance water reducing agent and preparation method
CN106397681A (en) * 2016-08-24 2017-02-15 安徽鑫固环保股份有限公司 Early-strength-type polycarboxylic high-performance water reducing agent and preparation method thereof
CN106866895A (en) * 2017-03-27 2017-06-20 南宁新泰瑞科建材有限公司 A kind of high-performance poly carboxylic acid series water reducer and preparation method thereof

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102358768A (en) * 2011-07-22 2012-02-22 广州市建筑科学研究院有限公司 Modified ether polycarboxylic acid water reducing agent and preparation method thereof
CN102503226A (en) * 2011-10-19 2012-06-20 中建商品混凝土有限公司 High slump retaining type polycarboxylic acid water reducing agent with sustained-release effect and preparation method thereof
CN103992443A (en) * 2014-05-19 2014-08-20 科之杰新材料集团有限公司 Method for preparing polycarboxylate water reducing agent by normal-temperature mixing process
CN103965414A (en) * 2014-05-23 2014-08-06 同济大学 High-early-strength polycarboxylate water reducer as well as synthesis method and application method of polycarboxylate water reducer
CN105645810A (en) * 2016-01-05 2016-06-08 河南新汉材料科技有限公司 Early-strength polycarboxylate type high-performance water reducing agent and preparation method
CN106397681A (en) * 2016-08-24 2017-02-15 安徽鑫固环保股份有限公司 Early-strength-type polycarboxylic high-performance water reducing agent and preparation method thereof
CN106866895A (en) * 2017-03-27 2017-06-20 南宁新泰瑞科建材有限公司 A kind of high-performance poly carboxylic acid series water reducer and preparation method thereof

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Application publication date: 20181113