CN108793810A - A kind of preparation method of polycarboxylate water-reducer - Google Patents
A kind of preparation method of polycarboxylate water-reducer Download PDFInfo
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- 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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Classifications
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- 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
- C04B24/16—Sulfur-containing compounds
- C04B24/161—Macromolecular compounds comprising sulfonate or sulfate groups
- C04B24/163—Macromolecular compounds comprising sulfonate or sulfate groups obtained by reactions only involving carbon-to-carbon unsaturated bonds
- C04B24/165—Macromolecular compounds comprising sulfonate or sulfate groups obtained by reactions only involving carbon-to-carbon unsaturated bonds 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
- C08F220/00—Copolymers 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
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/04—Acids; Metal salts or ammonium salts thereof
- C08F220/06—Acrylic acid; Methacrylic acid; Metal salts or ammonium salts thereof
-
- 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)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Curing Cements, Concrete, And Artificial Stone (AREA)
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
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%.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN117682787A (en) * | 2023-12-14 | 2024-03-12 | 四川嘉兆丰新材料科技有限公司 | Low-temperature-resistant polycarboxylate superplasticizer and preparation method thereof |
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Application publication date: 20181113 |