CN102757539B - Preparation method of polycarboxylic acid high-performance water reducing agent - Google Patents
Preparation method of polycarboxylic acid high-performance water reducing agent Download PDFInfo
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- CN102757539B CN102757539B CN2011101219648A CN201110121964A CN102757539B CN 102757539 B CN102757539 B CN 102757539B CN 2011101219648 A CN2011101219648 A CN 2011101219648A CN 201110121964 A CN201110121964 A CN 201110121964A CN 102757539 B CN102757539 B CN 102757539B
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 37
- 239000003638 chemical reducing agent Substances 0.000 title claims abstract description 22
- 239000002253 acid Substances 0.000 title claims abstract description 16
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 15
- 239000008367 deionised water Substances 0.000 claims abstract description 13
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 13
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 7
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 claims abstract description 6
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims abstract description 5
- 125000003903 2-propenyl group Chemical group [H]C([*])([H])C([H])=C([H])[H] 0.000 claims abstract description 5
- FPYJFEHAWHCUMM-UHFFFAOYSA-N maleic anhydride Chemical compound O=C1OC(=O)C=C1 FPYJFEHAWHCUMM-UHFFFAOYSA-N 0.000 claims abstract description 5
- 239000000463 material Substances 0.000 claims description 33
- 239000000243 solution Substances 0.000 claims description 9
- 238000009413 insulation Methods 0.000 claims description 8
- 239000004160 Ammonium persulphate Substances 0.000 claims description 4
- 235000019395 ammonium persulphate Nutrition 0.000 claims description 4
- 230000003750 conditioning effect Effects 0.000 claims description 4
- 229920000151 polyglycol Polymers 0.000 claims description 4
- 239000010695 polyglycol Substances 0.000 claims description 4
- 238000002791 soaking Methods 0.000 claims description 4
- 238000003756 stirring Methods 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims description 3
- 239000002994 raw material Substances 0.000 claims description 3
- 239000007864 aqueous solution Substances 0.000 claims description 2
- 238000006386 neutralization reaction Methods 0.000 claims description 2
- 230000000740 bleeding effect Effects 0.000 abstract description 2
- 230000008602 contraction Effects 0.000 abstract description 2
- 238000000034 method Methods 0.000 abstract description 2
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 abstract 1
- 239000002202 Polyethylene glycol Substances 0.000 abstract 1
- 229910001870 ammonium persulfate Inorganic materials 0.000 abstract 1
- 238000006243 chemical reaction Methods 0.000 abstract 1
- 230000003472 neutralizing effect Effects 0.000 abstract 1
- 238000002464 physical blending Methods 0.000 abstract 1
- 229920001223 polyethylene glycol Polymers 0.000 abstract 1
- 238000006116 polymerization reaction Methods 0.000 abstract 1
- 230000001105 regulatory effect Effects 0.000 abstract 1
- 239000004567 concrete Substances 0.000 description 11
- 239000004568 cement Substances 0.000 description 4
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 238000010276 construction Methods 0.000 description 2
- 229920000877 Melamine resin Polymers 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 150000001732 carboxylic acid derivatives Chemical class 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- NVVZQXQBYZPMLJ-UHFFFAOYSA-N formaldehyde;naphthalene-1-sulfonic acid Chemical compound O=C.C1=CC=C2C(S(=O)(=O)O)=CC=CC2=C1 NVVZQXQBYZPMLJ-UHFFFAOYSA-N 0.000 description 1
- 239000004574 high-performance concrete Substances 0.000 description 1
- JDSHMPZPIAZGSV-UHFFFAOYSA-N melamine Chemical compound NC1=NC(N)=NC(N)=N1 JDSHMPZPIAZGSV-UHFFFAOYSA-N 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- DGVVJWXRCWCCOD-UHFFFAOYSA-N naphthalene;hydrate Chemical compound O.C1=CC=CC2=CC=CC=C21 DGVVJWXRCWCCOD-UHFFFAOYSA-N 0.000 description 1
- BDHFUVZGWQCTTF-UHFFFAOYSA-M sulfonate Chemical compound [O-]S(=O)=O BDHFUVZGWQCTTF-UHFFFAOYSA-M 0.000 description 1
- 239000008030 superplasticizer Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 239000011374 ultra-high-performance concrete Substances 0.000 description 1
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- Curing Cements, Concrete, And Artificial Stone (AREA)
Abstract
The invention discloses a preparation method of a polycarboxylic acid high-performance water reducing agent. The polycarboxylic acid high-performance water reducing agent TJ-98 is prepared from 45-50 percent by weight of allyl polyethyleneglycol, 1.5-3.5 percent by weight of acrylic acid, 1.5-3.5 percent by weight of maleic anhydride, 0.5-0.7 percent by weight of ammonium persulfate, 41-48 percent by weight of deionized water, 2.1-2.5 percent by weight of sodium hydroxide and 0.1-0.3 percent by weight of a TC-1 regulating agent by performing a polymerization reaction, a neutralizing reaction and physical blending. The preparation method has the advantages of simple process, multiple molecular structure variable factors and environment friendliness; the obtained product has high adaptability, water reducing rate of over 35 percent and high workability during application; and compared with the conventional commercially-available products of the same type, the polycarboxylic acid high-performance water reducing agent has the characteristics of high early compressive strength, small slump loss, low bleeding rate, low contraction ratio and the like.
Description
Technical field
The present invention relates to a kind of preparation method of water reducer, especially a kind of preparation method of high performance water reducing agent of polyocarboxy acid.
Background technology
Concrete is the material of construction of consumption maximum in the world, and admixture is again the requisite component of concrete.Since the thirties in last century,, along with the progress of science and technology, several times to update and developed into this up-to-date scientific and technological achievement of polycarboxylic acid series high-performance admixture, it not only is used as concrete high efficiency water reducing agent, and can be used as water-resisting agent and concrete pump-feed agent.
Water reducer refers under concrete workability and cement consumption permanence condition, can reduce the mixing water amount, improve concrete strength; Or under workability and intensity permanence condition, save the admixture of cement consumption.High efficiency water reducing agent claims again superplasticizer, and it is improved the concrete construction performance, reduces water cement ratio, improves concrete intensity and weather resistance, saving cement, reduces the effects such as concrete initial imperfection.The high efficiency water reducing agent main products of the sixties in last century has naphthalenesulfonate formaldehyde condensation compound NSF and melamine sulfonate and formaldehyde condenses MSF, although this series products water-reducing rate is higher, but the slump loss is fast, weather resistance is poor and can not reach the purpose of preparation high-performance and ultra-high performance concrete, and polycarboxylic acid series high efficiency water reducing agent has the function of larger water-reducing rate and control concrete slump loss than naphthalene water reducer, and the raising of its performance has promoted the development of modern concrete technology.Synthesis mechanism research to poly carboxylic acid series water reducer is at home and abroad also received and is paid special attention to.
Summary of the invention
The preparation method who the purpose of this invention is to provide a kind of high performance water reducing agent of polyocarboxy acid.
Technical solution of the present invention is as follows:
The preparation method of high performance water reducing agent of polyocarboxy acid of the present invention, comprise the following steps:
The aqueous solution that allyl polyglycol, deionized water is made into 50% concentration under a normal temperature, as the still bed material, heats up simultaneously;
When b is raised to 80～85 ℃ when temperature, drip simultaneously A, B material, the A material is the solution that ammonium persulphate and deionized water are made into, the solution that the B material is made into for vinylformic acid, MALEIC ANHYDRIDE and deionized water, the time for adding of A, B material is all 2～4 hours, while dripping A, B material, temperature is controlled at 80～85 ℃, after A, B material adds, start insulation, holding temperature is controlled at 80～85 ℃ equally, and soaking time is 1～2 hour;
After the c insulation finishes, cool to 50～60 ℃ and add sodium hydroxide to neutralize, make material PH=7 ± 1;
After the d neutralization reaction is complete, adds the TC-1 conditioning agent to stir rear and obtain high performance water reducing agent of polyocarboxy acid TJ-9B;
Composition of raw materials (being more excellent proportioning in weight ratio, bracket) is:
The invention has the beneficial effects as follows:
It is simple that this preparation method has technique, and the molecular structure variable factor is many, environmental protection; Products obtained therefrom has in application that adaptability is good, water-reducing rate up to more than 35%, workability is good; Compare with existing like product on market have that early anti pressured intension is high, little loss of slump, the characteristics such as bleeding rate is little and contraction ratio is little.
Embodiment
Embodiment 1
A dropped into reactor with allyl polyglycol, deionized water by weight 1.3: 1 interior as the still bed material, heated up simultaneously;
When b is raised to 80 ℃ when temperature, drip simultaneously A, B material; The A material is the solution that ammonium persulphate and deionized water are made into; The solution that the B material is made into for vinylformic acid, MALEIC ANHYDRIDE and deionized water; The time for adding of A, B material is all 3 hours, and while dripping A, B material, temperature is controlled at 80～85 ℃, after A, B material adds, starts insulation, and holding temperature is controlled at 80～85 ℃ equally, and soaking time is 1.0 hours;
After the c insulation finishes, cool to 50 ℃ and add sodium hydroxide to neutralize, make material PH=6;
In d and after complete, add the TC-1 conditioning agent to stir rear and obtain high performance water reducing agent of polyocarboxy acid TJ-9B.
Embodiment 2
A dropped into reactor with allyl polyglycol, deionized water by weight 1.25: 1 interior as the still bed material, heated up simultaneously;
When b is raised to 85 ℃ when temperature, drip simultaneously A, B material, the A material is the solution that ammonium persulphate and deionized water are made into, the solution that the B material is made into for vinylformic acid, MALEIC ANHYDRIDE and deionized water, the time for adding of A, B material is all 4 hours, while dripping A, B material, temperature is controlled at 80～85 ℃, after A, B material adds, start insulation, holding temperature is controlled at 80～85 ℃ equally, and soaking time is 2.0 hours;
After the c insulation finishes, cool to 60 ℃ and add sodium hydroxide to neutralize, make material PH=7;
In d and after complete, add the TC-1 conditioning agent to stir rear and obtain high performance water reducing agent of polyocarboxy acid TJ-9B.
Claims (2)
1. the preparation method of a high performance water reducing agent of polyocarboxy acid, comprise the following steps:
The aqueous solution that allyl polyglycol, deionized water is made into 50% concentration under a normal temperature, as the still bed material, heats up simultaneously;
When b is raised to 80～85 ℃ when temperature, drip simultaneously A, B material, the A material is the solution that ammonium persulphate and deionized water are made into, the solution that the B material is made into for vinylformic acid, MALEIC ANHYDRIDE and deionized water, the time for adding of A, B material is all 2～4 hours, while dripping A, B material, temperature is controlled at 80～85 ℃, after A, B material adds, start insulation, holding temperature is controlled at 80～85 ℃ equally, and soaking time is 1～2 hour;
After the c insulation finishes, cool to 50～60 ℃ and add sodium hydroxide to neutralize, make material pH=7 ± 1;
After the d neutralization reaction is complete, adds the TC-1 conditioning agent to stir rear and obtain high performance water reducing agent of polyocarboxy acid TJ-9B;
The composition of raw materials weight ratio is:
2. the preparation method of high performance water reducing agent of polyocarboxy acid according to claim 1 is characterized in that the composition of raw materials weight ratio is:
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| Application Number | Priority Date | Filing Date | Title |
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| CN2011101219648A CN102757539B (en) | 2011-04-26 | 2011-04-26 | Preparation method of polycarboxylic acid high-performance water reducing agent |
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| Application Number | Priority Date | Filing Date | Title |
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| CN2011101219648A CN102757539B (en) | 2011-04-26 | 2011-04-26 | Preparation method of polycarboxylic acid high-performance water reducing agent |
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| Publication Number | Publication Date |
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| CN102757539A CN102757539A (en) | 2012-10-31 |
| CN102757539B true CN102757539B (en) | 2013-11-13 |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103641363B (en) * | 2013-12-06 | 2015-11-18 | 广州市鲁班建筑工程技术有限公司 | A kind of selfreparing vinylon waterproof polymer mortar admixture and preparation method thereof |
| CN110540620A (en) * | 2019-01-09 | 2019-12-06 | 咸阳鸿鑫建材有限公司 | polycarboxylate superplasticizer and preparation method thereof |
| CN111647115A (en) * | 2020-06-15 | 2020-09-11 | 安徽海螺新材料科技有限公司 | Polycarboxylate superplasticizer mother liquor and preparation method thereof, and polycarboxylate superplasticizer and preparation method thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP1016638A2 (en) * | 1998-12-28 | 2000-07-05 | Nippon Shokubai Co., Ltd. | Cement additive, cement composition and polycarboxylic acid polymer |
| CN101186460A (en) * | 2007-11-22 | 2008-05-28 | 同济大学 | Polycarboxylate water reducer using allyl polyethylene glycol as raw material and its synthesis method |
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2011
- 2011-04-26 CN CN2011101219648A patent/CN102757539B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP1016638A2 (en) * | 1998-12-28 | 2000-07-05 | Nippon Shokubai Co., Ltd. | Cement additive, cement composition and polycarboxylic acid polymer |
| CN101186460A (en) * | 2007-11-22 | 2008-05-28 | 同济大学 | Polycarboxylate water reducer using allyl polyethylene glycol as raw material and its synthesis method |
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| CN102757539A (en) | 2012-10-31 |
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