CN107987222A - A kind of preparation method of high water reducing type solid high-performance polycarboxylate water-reducer - Google Patents
A kind of preparation method of high water reducing type solid high-performance polycarboxylate water-reducer Download PDFInfo
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- CN107987222A CN107987222A CN201711216576.1A CN201711216576A CN107987222A CN 107987222 A CN107987222 A CN 107987222A CN 201711216576 A CN201711216576 A CN 201711216576A CN 107987222 A CN107987222 A CN 107987222A
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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
- C04B24/24—Macromolecular compounds
- C04B24/26—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
- C04B24/2605—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds containing polyether side chains
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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
- C08F2/00—Processes of polymerisation
- C08F2/46—Polymerisation initiated by wave energy or particle radiation
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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
-
- 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
Abstract
The present invention provides a kind of preparation method of high water reducing type solid high-performance polycarboxylate water-reducer, it is related to concrete admixture field.Heat simultaneously uniform stirring after 10 15 parts of 2000,30 40 parts of poly glycol monomethyl ether, 1000,58 parts of poly glycol monomethyl ether methacrylic acids, 12 parts of p-methyl benzenesulfonic acid and 0.5 1 parts of hydroquinones are mixed, after heating, material is taken out and is recovered to room temperature, up to macromonomer；Gained macromonomer, 0.5 0.8 parts of thioacetic acid, 10 15 parts of deionized waters are uniformly mixed, and heated, after cooling, up to No. 1 mixed solution；Gained mixed solution, 0.2 0.4 parts of vitamin c solution, 0.1 0.2 parts of initiators are uniformly mixed, and are stirred, up to No. 2 mixed solutions；Sodium hydroxide solution is added in No. 2 mixed solutions of gained, and it is 6.5 7 to adjust pH value, up to diminishing agent solution；Gained diminishing agent solution is subjected to frozen dried, to obtain the final product.The present invention can effectively reduce concrete viscosity, and concrete is had stronger retentivity.
Description
Technical field
The present invention relates to concrete admixture field, more particularly to a kind of high water reducing type solid high-performance polycarboxylate water-reducer
Preparation method.
Background technology
Concrete is that dosage is maximum in the world, most widely used construction material.Recent decades, concrete technology enter
New developing stage, its application range are also further expanding.Recently as the development of Building Trade in China, high-grade concrete
Just with its intensity height, good integrity, small dead weight the features such as, step into construction market.But as a result of relatively low water-cement ratio
With larger cementitious material amount, the problem of high-grade concrete is larger there are viscosity in the application, and flowing velocity is slow.
It is always the problem of perplexing normal construction that concrete slump declines excessive with the time.Polycarboxylate water-reducer is mixed in itself
Amount is very low, can consume substantial amounts of water-reducing agent initial stage in concrete mixing, cause the deficiency of actually active composition in later stage concrete,
The decline of its application performance is caused, particularly later-slump loss is serious, it is impossible to meets the requirement of normal construction.
The content of the invention
It is an object of the invention to provide a kind of preparation method of high water reducing type solid high-performance polycarboxylate water-reducer, with solution
Certainly above-mentioned technical problem.
The present invention using following technical scheme in order to solve the above technical problems, realized：
A kind of preparation method of high water reducing type solid high-performance polycarboxylate water-reducer, it is characterised in that comprise the following steps：
A. by weight, by 10-15 parts of poly glycol monomethyl ethers 2000,30-40 parts of poly glycol monomethyl ethers 1000,5-
After 8 parts of methacrylic acids, 1-2 parts of p-methyl benzenesulfonic acid and 0.5-1 parts of hydroquinone mixing heat and uniform stirring, heating are warm
Degree is arranged to 120-150 DEG C, when heating time is 6-8 small, after heating, and material is taken out and is recovered to room temperature, up to big
Molecule monomer；
B. gained macromonomer, 0.5-0.8 parts of thioacetic acid, 10-15 parts of deionized waters in A are uniformly mixed, gone forward side by side
Row heating, heating time is 15-20 minutes, after cooling, up to No. 1 mixed solution；
C. gained mixed solution, 0.2-0.4 parts of vitamin c solution, 0.1-0.2 parts of initiators in B are uniformly mixed, and
It is stirred under ultrasonic wave auxiliary, mixing time is 10-15 minutes, up to No. 2 mixed solutions；
Vitamin c solution and initiator are stirred under ultrasonic wave auxiliary, the effect of initiator can be effectively promoted
With so as to be effectively increased the retentivity of concrete.
D. No. 2 mixed solutions of gained add sodium hydroxide solution in C, and it is 6.5-7 to adjust pH value, molten up to water-reducing agent
Liquid；
E. gained diminishing agent solution in D is subjected to frozen dried, to obtain the final product.
Preferably, in the step B, mode of heating is to be heated using microwave.
The main chain of polycarboxylic acids is using polyethers as side chain, and the molecule heat endurance of this structure is poor, for a long time in higher temperature
Under conditions of molecular structure be easily destroyed so that performance is greatly reduced.Can effectively it be protected point by the way of microwave heating
Minor structure, so as to reduce concrete viscosity, and then strengthens the mobility of concrete.
Preferably, the power of microwave heating is 1000-1500w.
Preferably, in the step C, used initiator is the ammonium persulfate aqueous solution of concentration 4%-6%.
Preferably, in the step C, the power of used ultrasonic wave is 2000-2500w.
Preferably, in the step E, the temperature of frozen dried is -90~-80 DEG C.
The beneficial effects of the invention are as follows：The present invention provides a kind of system of high water reducing type solid high-performance polycarboxylate water-reducer
Preparation Method, can effectively reduce concrete viscosity, and concrete is had stronger retentivity.
Embodiment
In order to make the technical means, the creative features, the aims and the efficiencies achieved by the present invention easy to understand, tie below
Specific embodiment is closed, the present invention is further explained, but following embodiments are only the preferred embodiment of the present invention, and not all.
Based on the embodiment in embodiment, those skilled in the art obtain other realities on the premise of creative work is not made
Example is applied, belongs to protection scope of the present invention.Experimental method in following embodiments, is conventional method unless otherwise specified,
The materials, reagents and the like used in the following examples, is commercially available unless otherwise specified.
Embodiment 1
A. by weight, by 10 parts of 2000,30 parts of poly glycol monomethyl ether, 1000,5 parts of poly glycol monomethyl ether methyl
After acrylic acid, 1 part of p-methyl benzenesulfonic acid and 0.5 part of hydroquinone mixing heat and uniform stirring, heating-up temperature are arranged to 120
DEG C, when heating time is 6 small, after heating, material is taken out and is recovered to room temperature, up to macromonomer；
B. gained macromonomer, 0.5 part of thioacetic acid, 10 parts of deionized waters in A are uniformly mixed, and carries out microwave and add
Heat, the power of microwave heating is 1000w, and heating time is 15 minutes, after cooling, up to No. 1 mixed solution；
C. by gained mixed solution, 0.2 part of vitamin c solution, the ammonium persulfate aqueous solution that 0.1 part of concentration is 4% in B
Uniformly mixing, and be stirred under the ultrasonic wave auxiliary that power is 2000w, mixing time is 10 minutes, molten up to No. 2 mixing
Liquid；
D. No. 2 mixed solutions of gained add sodium hydroxide solution in C, and it is 6.5 to adjust pH value, molten up to water-reducing agent
Liquid；
E. gained diminishing agent solution in D is subjected to frozen dried, the temperature of frozen dried is -90 DEG C, to obtain the final product.
Embodiment 2
A. by weight, by 115 parts of 2000,40 parts of poly glycol monomethyl ether, 1000,8 parts of poly glycol monomethyl ether methyl
After acrylic acid, 2 parts of p-methyl benzenesulfonic acid and 1 part of hydroquinone mixing heat and uniform stirring, heating-up temperature are arranged to 150
DEG C, when heating time is 8 small, after heating, material is taken out and is recovered to room temperature, up to macromonomer；
B. gained macromonomer, 0.8 part of thioacetic acid, 15 parts of deionized waters in A are uniformly mixed, and carries out microwave and add
Heat, the power of microwave heating is 1500w, and heating time is 20 minutes, after cooling, up to No. 1 mixed solution；
C. by gained mixed solution, 0.4 part of vitamin c solution, the ammonium persulfate aqueous solution that 0.2 part of concentration is 6% in B
Uniformly mixing, and be stirred, mixing time 15 minutes, up to No. 2 mixed solutions；
D. No. 2 mixed solutions of gained add sodium hydroxide solution in C, and it is 7 to adjust pH value, up to diminishing agent solution；
E. gained diminishing agent solution in D is subjected to frozen dried, the temperature of frozen dried is -80 DEG C, to obtain the final product.
Embodiment 3
A. by weight, by 12 parts of 2000,34 parts of poly glycol monomethyl ether, 1000,6 parts of poly glycol monomethyl ether methyl
After acrylic acid, 1.4 parts of p-methyl benzenesulfonic acid and 0.7 part of hydroquinone mixing heat and uniform stirring, heating-up temperature are arranged to
130 DEG C, when heating time is 6.5 small, after heating, material is taken out and is recovered to room temperature, up to macromonomer；
B. gained macromonomer, 0.6 part of thioacetic acid, 12 parts of deionized waters in A are uniformly mixed, and heated, heated
Time is 16 minutes, after cooling, up to No. 1 mixed solution；
C. by gained mixed solution, 0.2 part of vitamin c solution, the ammonium persulfate aqueous solution that 0.1 part of concentration is 4% in B
Uniformly mixing, and be stirred under the ultrasonic wave auxiliary that power is 2000w, mixing time is 11 minutes, molten up to No. 2 mixing
Liquid；
D. No. 2 mixed solutions of gained add sodium hydroxide solution in C, and it is 6.5 to adjust pH value, molten up to water-reducing agent
Liquid；
E. gained diminishing agent solution in D is subjected to frozen dried, the temperature of frozen dried is -85 DEG C, to obtain the final product.
Embodiment 4
A. by weight, by 13 parts of 2000,35 parts of poly glycol monomethyl ether, 1000,8 parts of poly glycol monomethyl ether methyl
After acrylic acid, 2 parts of p-methyl benzenesulfonic acid and 1 part of hydroquinone mixing heat and uniform stirring, heating-up temperature are arranged to 150
DEG C, when heating time is 7 small, after heating, material is taken out and is recovered to room temperature, up to macromonomer；
B. gained macromonomer, 0.8 part of thioacetic acid, 15 parts of deionized waters in A are uniformly mixed, and heated,
Heating time is 20 minutes, after cooling, up to No. 1 mixed solution；
C. by gained mixed solution, 0.2 part of vitamin c solution, the ammonium persulfate aqueous solution that 0.1 part of concentration is 4% in B
Uniformly mixing, and be stirred, mixing time is 15 minutes, up to No. 2 mixed solutions；
D. No. 2 mixed solutions of gained add sodium hydroxide solution in C, and it is 7 to adjust pH value, up to diminishing agent solution；
E. gained diminishing agent solution in D is subjected to frozen dried, the temperature of frozen dried is -80 DEG C, to obtain the final product.
The slump and divergence of Statistics Implementation example 1-4, such as following table：
| Initial slump (mm) | 2 as a child after the slump (mm) | |
| Embodiment 1 | 240 | 247 |
| Embodiment 2 | 235 | 221 |
| Embodiment 3 | 240 | 243 |
| Embodiment 4 | 236 | 220 |
Table 1
| Initial extension degree (mm) | 2 as a child after divergence (mm) | |
| Embodiment 1 | 470 | 480 |
| Embodiment 2 | 470 | 477 |
| Embodiment 3 | 475 | 440 |
| Embodiment 4 | 468 | 432 |
Table 2
A kind of system of high water reducing type solid high-performance polycarboxylate water-reducer provided by the invention it can be seen from Tables 1 and 2
Preparation Method, can effectively reduce concrete viscosity, and concrete is had stronger retentivity.
Basic principle, main feature and the advantages of the present invention of the present invention has been shown and described above.The technology of the industry
For personnel it should be appreciated that the present invention is not limited to the above embodiments, described in the above embodiment and specification is only the present invention
Preference, be not intended to limit the present invention, without departing from the spirit and scope of the present invention, the present invention also have it is various
Changes and improvements, these changes and improvements all fall within the protetion scope of the claimed invention.The claimed scope of the invention is by institute
Attached claims and its equivalent thereof.
Claims (6)
1. a kind of preparation method of high water reducing type solid high-performance polycarboxylate water-reducer, it is characterised in that comprise the following steps：
A. by weight, by 10-15 parts of poly glycol monomethyl ethers 2000,30-40 parts of poly glycol monomethyl ethers 1000,5-8 parts
Heat simultaneously uniform stirring, heating-up temperature after methacrylic acid, 1-2 part p-methyl benzenesulfonic acid and 0.5-1 parts of hydroquinone mixing
120-150 DEG C, when heating time is 6-8 small, after heating is arranged to, material is taken out and is recovered to room temperature, up to big point
Sub- monomer；
B. gained macromonomer, 0.5-0.8 parts of thioacetic acid, 10-15 parts of deionized waters in A are uniformly mixed, and added
Heat, heating time is 15-20 minutes, after cooling, up to No. 1 mixed solution；
C. gained mixed solution, 0.2-0.4 parts of vitamin c solution, 0.1-0.2 parts of initiators in B are uniformly mixed, and super
It is stirred under sound wave auxiliary, mixing time is 10-15 minutes, up to No. 2 mixed solutions；
D. No. 2 mixed solutions of gained add sodium hydroxide solution in C, and it is 6.5-7 to adjust pH value, up to diminishing agent solution；
E. gained diminishing agent solution in D is subjected to frozen dried, to obtain the final product.
2. a kind of preparation method of high water reducing type solid high-performance polycarboxylate water-reducer according to claim 1, its feature
It is, in the step B, mode of heating is to be heated using microwave.
3. a kind of preparation method of high water reducing type solid high-performance polycarboxylate water-reducer according to claim 2, its feature
It is, the power of microwave heating is 1000-1500w.
4. a kind of preparation method of high water reducing type solid high-performance polycarboxylate water-reducer according to claim 1, its feature
It is, in the step C, used initiator is the ammonium persulfate aqueous solution of concentration 4%-6%.
5. a kind of preparation method of high water reducing type solid high-performance polycarboxylate water-reducer according to claim 1, its feature
It is, in the step C, the power of used ultrasonic wave is 2000-2500w.
6. a kind of preparation method of high water reducing type solid high-performance polycarboxylate water-reducer according to claim 1, its feature
It is, in the step E, the temperature of frozen dried is -90~-80 DEG C.
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| CN201711216576.1A CN107987222A (en) | 2017-11-28 | 2017-11-28 | A kind of preparation method of high water reducing type solid high-performance polycarboxylate water-reducer |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109678433A (en) * | 2019-02-22 | 2019-04-26 | 武汉理工大学 | Ultrahigh-strength self-compacting microdilatancy concrete filled steel tube and preparation method thereof |
| CN112430042A (en) * | 2020-12-11 | 2021-03-02 | 保利长大工程有限公司 | Low-rubber high-flow-state high-performance concrete and preparation method thereof |
-
2017
- 2017-11-28 CN CN201711216576.1A patent/CN107987222A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109678433A (en) * | 2019-02-22 | 2019-04-26 | 武汉理工大学 | Ultrahigh-strength self-compacting microdilatancy concrete filled steel tube and preparation method thereof |
| CN112430042A (en) * | 2020-12-11 | 2021-03-02 | 保利长大工程有限公司 | Low-rubber high-flow-state high-performance concrete and preparation method thereof |
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