CN105036595A - High-liquidity polycarboxylic acid water reducing agent and preparation method thereof - Google Patents
High-liquidity polycarboxylic acid water reducing agent and preparation method thereof Download PDFInfo
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- CN105036595A CN105036595A CN201510461080.5A CN201510461080A CN105036595A CN 105036595 A CN105036595 A CN 105036595A CN 201510461080 A CN201510461080 A CN 201510461080A CN 105036595 A CN105036595 A CN 105036595A
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- deionized water
- transfer agent
- water
- add
- chain
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 30
- 239000003638 chemical reducing agent Substances 0.000 title claims abstract description 26
- 239000002253 acid Substances 0.000 title claims abstract description 8
- 238000002360 preparation method Methods 0.000 title claims abstract description 8
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 21
- 239000008367 deionised water Substances 0.000 claims abstract description 18
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 18
- 239000012986 chain transfer agent Substances 0.000 claims abstract description 16
- 238000003756 stirring Methods 0.000 claims abstract description 13
- 239000004721 Polyphenylene oxide Substances 0.000 claims abstract description 12
- 239000000178 monomer Substances 0.000 claims abstract description 12
- 229920000570 polyether Polymers 0.000 claims abstract description 12
- 238000006243 chemical reaction Methods 0.000 claims abstract description 8
- JTXMVXSTHSMVQF-UHFFFAOYSA-N 2-acetyloxyethyl acetate Chemical compound CC(=O)OCCOC(C)=O JTXMVXSTHSMVQF-UHFFFAOYSA-N 0.000 claims abstract description 7
- DWAQJAXMDSEUJJ-UHFFFAOYSA-M Sodium bisulfite Chemical compound [Na+].OS([O-])=O DWAQJAXMDSEUJJ-UHFFFAOYSA-M 0.000 claims abstract description 6
- 235000010267 sodium hydrogen sulphite Nutrition 0.000 claims abstract description 6
- 229920005646 polycarboxylate Polymers 0.000 claims description 14
- 238000010792 warming Methods 0.000 claims description 6
- 239000000470 constituent Substances 0.000 claims description 5
- 239000000463 material Substances 0.000 claims description 5
- VVWRJUBEIPHGQF-UHFFFAOYSA-N propan-2-yl n-propan-2-yloxycarbonyliminocarbamate Chemical compound CC(C)OC(=O)N=NC(=O)OC(C)C VVWRJUBEIPHGQF-UHFFFAOYSA-N 0.000 claims description 5
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 4
- 239000006185 dispersion Substances 0.000 claims description 3
- 125000003903 2-propenyl group Chemical group [H]C([*])([H])C([H])=C([H])[H] 0.000 claims description 2
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 2
- WCASXYBKJHWFMY-UHFFFAOYSA-N crotyl alcohol Chemical group CC=CCO WCASXYBKJHWFMY-UHFFFAOYSA-N 0.000 claims description 2
- DNJIEGIFACGWOD-UHFFFAOYSA-N ethyl mercaptane Natural products CCS DNJIEGIFACGWOD-UHFFFAOYSA-N 0.000 claims description 2
- 229920000056 polyoxyethylene ether Polymers 0.000 claims description 2
- 229940051841 polyoxyethylene ether Drugs 0.000 claims description 2
- CWERGRDVMFNCDR-UHFFFAOYSA-N thioglycolic acid Chemical compound OC(=O)CS CWERGRDVMFNCDR-UHFFFAOYSA-N 0.000 claims description 2
- DGVVWUTYPXICAM-UHFFFAOYSA-N β‐Mercaptoethanol Chemical compound OCCS DGVVWUTYPXICAM-UHFFFAOYSA-N 0.000 claims description 2
- OZAIFHULBGXAKX-UHFFFAOYSA-N 2-(2-cyanopropan-2-yldiazenyl)-2-methylpropanenitrile Chemical compound N#CC(C)(C)N=NC(C)(C)C#N OZAIFHULBGXAKX-UHFFFAOYSA-N 0.000 abstract 4
- 238000010438 heat treatment Methods 0.000 abstract 2
- 238000001816 cooling Methods 0.000 abstract 1
- LNOPIUAQISRISI-UHFFFAOYSA-N n'-hydroxy-2-propan-2-ylsulfonylethanimidamide Chemical compound CC(C)S(=O)(=O)CC(N)=NO LNOPIUAQISRISI-UHFFFAOYSA-N 0.000 abstract 1
- WBHQBSYUUJJSRZ-UHFFFAOYSA-M sodium bisulfate Chemical compound [Na+].OS([O-])(=O)=O WBHQBSYUUJJSRZ-UHFFFAOYSA-M 0.000 abstract 1
- 229910000342 sodium bisulfate Inorganic materials 0.000 abstract 1
- IIACRCGMVDHOTQ-UHFFFAOYSA-N sulfamic acid Chemical compound NS(O)(=O)=O IIACRCGMVDHOTQ-UHFFFAOYSA-N 0.000 abstract 1
- 239000004568 cement Substances 0.000 description 3
- 150000001732 carboxylic acid derivatives Chemical class 0.000 description 2
- 238000010276 construction Methods 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000006835 compression Effects 0.000 description 1
- 238000007906 compression Methods 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000010881 fly ash Substances 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 239000000203 mixture Substances 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
- 239000002245 particle Substances 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000004901 spalling Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 125000000542 sulfonic acid group Chemical group 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
Landscapes
- Curing Cements, Concrete, And Artificial Stone (AREA)
Abstract
The invention particularly relates to a high-liquidity polycarboxylic acid water reducing agent which comprises 15-20% of polyether monomer, 4-9% of ethylene glycol diacetate, 3-5% of a chain transfer agent, 4-9% of sulfamic acid, 2.5-5.5% of sodium bisulfite, 1-2% of azobisisobutyronitrile, 2-5% of sodium hydroxide and the balance of deionized water. A preparation method for the high-liquidity polycarboxylic acid water reducing agent comprises the following steps: (1), adding the polyether monomer and deionized water into a reaction kettle, uniformly stirring for completely dissolving, and heating to 60+/- 2 DEG C; (2), adding sodium bisulfate and ethylene glycol diacetate, continuously stirring for 30 min, after complete dispersing, adding azobisisobutyronitrile and sulphamic acid, heating to 80+/- 2 DEG C and reacting for 30 min; (3), adding the chain transfer agent, wherein the chain transfer agent is added into the reaction kettle for five times at the interval of 10 min; (4), continuously reacting for 3 h, cooling to room temperature, adding deionized water for dissolving sodium hydroxide so as to adjust pH to 7.0; finally, replenishing deionized water, and continuously stirring for 30 min so as to obtain the water reducing agent. By adopting the water reducing agent provided by the invention, the problem that concrete collapses due to high air temperature, long transport time and other factors is solved.
Description
Technical field
The invention belongs to research and the manufacturing technology field of concrete admixture, be specifically related to a kind of high anti-subsided polycarboxylate water-reducer and preparation method thereof.
Technical background
China from calendar year 2001 polycarboxylate water-reducer product application since Shanghai Magnet Suspension, from the usage quantity in technology and market can find out develop very fast.The application trend of poly carboxylic acid series water reducer be from the application of the Important Project keypoint part in past to general Important Project, common engineer applied, by high strength grade, special functional concrete progressively to application development in common engineering concrete.
Xinjiang is in construction of the West Region Rapid developing region, construction work large scale investment is built, concrete demand constantly increases, corresponding admixture usage quantity demand also constantly increases, along with improving constantly of national requirements for environmental protection, the using portion of polycarboxylate water-reducer also increases increasingly, and original naphthalene water reducer has become a kind of trend by poly carboxylic acid products substitution gradually.Due to the constraint of the factor such as Xinjiang weather, geographical environment, building-site distance stirring station scene is far away, and this just requires concrete guarantor to collapse time corresponding increase.
Summary of the invention
The object of the invention is to: a kind of high anti-subsided polycarboxylate water-reducer is provided, can effectively solve similar Xinjiang region due to temperature high, the slump that the unfavorable factors such as haulage time is long cause loses serious problem.
The object of the present invention is achieved like this: a kind of high anti-subsided polycarboxylate water-reducer, and described water reducer is formulated according to mass percent by following constituent materials: the deionized water of polyether monomer 15-20%, glycol diacetate 4-9%, chain-transfer agent 3-5%, thionamic acid 4-9%, sodium bisulfite 2.5-5.5%, Diisopropyl azodicarboxylate 1-2%, sodium hydroxide 2-5% and surplus.Described polyether monomer is methyl allyl alcohol polyoxyethylene ether TPEG or allyl polyethenoxy ether APEG.Described chain-transfer agent is the one in mercaptoethanol, Thiovanic acid, Virahol.
The preparation method of above-mentioned high anti-subsided polycarboxylate water-reducer comprises the steps: that polyether monomer and appropriate deionized water add in reactor by (1), uniform stirring, after making polyether monomer be dissolved in deionized water completely, be warming up to 60 ± 2 DEG C, for subsequent use;
(2) in step (1), add sodium bisulfite and glycol diacetate, continue to stir 30min, add Diisopropyl azodicarboxylate and thionamic acid after dispersion completely, be warming up to 80 ± 2 DEG C, reaction 30min, for subsequent use;
(3) in step (2), add chain-transfer agent, chain-transfer agent divides 5 times to add in reactor, and the timed interval is 10min;
(4) after adding chain-transfer agent in step (3), continue reaction 3h, then, be cooled to room temperature, add that to carry out regulator solution pH value with appropriate deionized water dissolving sodium hydroxide be 7.0; Finally, adding deionized water to each ratio of component sum of above-mentioned constituent materials is a hundred per cent, continues to stir 30min, can obtain high anti-subsided polycarboxylate water-reducer.
Beneficial effect: the high anti-subsided water reducer of the present invention's development; in its molecule, the sulfonic acid group of side chain forms layer protecting film at cement particle surface; effectively can stop aquation; extend cement setting time; when solid volume increase the crystallization pressure produced reach certain numerical value time; protective membrane will local spalling, the diffusion of water and ion loses obstruction, and aquation just can proceed.2.5-3h slump gradual loss can be controlled in 20-30mm, when ensureing that workability of concrete is constant, under effectively can solving hot conditions, and the problem that during long-distance transportation, loss of slump is serious.
Specific embodiment
Table 1 is the proportioning of embodiment A, B, C, D, E and F
Table 1
The preparation method of the high anti-subsided polycarboxylate water-reducer described in above-described embodiment A-F comprises the steps:
(1) polyether monomer and appropriate deionized water are added in reactor, uniform stirring, after making polyether monomer be dissolved in deionized water completely, be warming up to 60 ± 2 DEG C, for subsequent use;
(2) in step (1), add sodium bisulfite and glycol diacetate, continue to stir 30min, add Diisopropyl azodicarboxylate and thionamic acid after dispersion completely, be warming up to 80 ± 2 DEG C, reaction 30min, for subsequent use;
(3) in step (2), add chain-transfer agent, chain-transfer agent divides 5 times to add in reactor, and the timed interval is 10min;
(4) after adding chain-transfer agent in step (3), continue reaction 3h, then, be cooled to room temperature, add that to carry out regulator solution pH value with appropriate deionized water dissolving sodium hydroxide be 7.0; Finally, adding deionized water to each ratio of component sum of above-mentioned constituent materials is a hundred per cent, continues to stir 30min, can obtain high anti-subsided polycarboxylate water-reducer.
Implementation result is verified
P.042.5 cement is selected according to GBT8076-2008 " concrete admixture " test, flyash (one-level), breeze are two to be mixed, C30 concrete mix, product A of the present invention, B, C, D, E, F and commercially available polycarboxylate water-reducer carry out contrast experiment, initial slump and 1 hour, 2 hours, 3 hours slump results as shown in table 2.
Table 2
Conclusion: contrast experiment can see product consumption 0.2% of the present invention, during the consumption 0.25% of commercially available prod, product A of the present invention, B, C, D, E, F are in identical proportioning, when same raw materials, initial slump degree is identical, within 1 hour, product slump of the present invention is not lost, within 2 hours, loss of slump is not obvious, within 3 hours, loss of slump can be controlled in 20-30mm, illustrate that the guarantor of this product ability of collapsing is very remarkable, and 28 days ultimate compression strength can improve more than 20%, substantially increase concrete performance, ensure the quality of working-yard.
Claims (4)
1. a high anti-subsided polycarboxylate water-reducer, is characterized in that: described water reducer is formulated according to mass percent by following constituent materials: the deionized water of polyether monomer 15-20%, glycol diacetate 4-9%, chain-transfer agent 3-5%, thionamic acid 4-9%, sodium bisulfite 2.5-5.5%, Diisopropyl azodicarboxylate 1-2%, sodium hydroxide 2-5% and surplus.
2. water reducer according to claim 1, is characterized in that: described polyether monomer is methyl allyl alcohol polyoxyethylene ether TPEG or allyl polyethenoxy ether APEG.
3. water reducer according to claim 1, is characterized in that: described chain-transfer agent is the one in mercaptoethanol, Thiovanic acid, Virahol.
4. prepare a preparation method for high anti-subsided polycarboxylate water-reducer according to claim 1, it is characterized in that: this preparation method comprises the steps:
(1) polyether monomer and appropriate deionized water are added in reactor, uniform stirring, after making polyether monomer be dissolved in deionized water completely, be warming up to 60 ± 2 DEG C, for subsequent use;
(2) in step (1), add sodium bisulfite and glycol diacetate, continue to stir 30min, add Diisopropyl azodicarboxylate and thionamic acid after dispersion completely, be warming up to 80 ± 2 DEG C, reaction 30min, for subsequent use;
(3) in step (2), add chain-transfer agent, chain-transfer agent divides 5 times to add in reactor, and the timed interval is 10min;
(4) after adding chain-transfer agent in step (3), continue reaction 3h, then, be cooled to room temperature, add that to carry out regulator solution pH value with appropriate deionized water dissolving sodium hydroxide be 7.0; Finally, adding deionized water to each ratio of component sum of above-mentioned constituent materials is a hundred per cent, continues to stir 30min, can obtain high anti-subsided polycarboxylate water-reducer.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201510461080.5A CN105036595B (en) | 2015-07-30 | 2015-07-30 | High-liquidity polycarboxylic acid water reducing agent and preparation method thereof |
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| CN201510461080.5A CN105036595B (en) | 2015-07-30 | 2015-07-30 | High-liquidity polycarboxylic acid water reducing agent and preparation method thereof |
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| CN105036595B CN105036595B (en) | 2017-05-24 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109517115A (en) * | 2018-12-03 | 2019-03-26 | 广东科隆智谷新材料股份有限公司 | A kind of preparation method of polycarboxylate water-reducer |
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| CN101734879A (en) * | 2009-12-27 | 2010-06-16 | 长沙理工大学 | Polyurethane/polycarboxylic acid compound water reducer for concrete and preparation thereof |
| CN102199298A (en) * | 2011-03-23 | 2011-09-28 | 中国日用化学工业研究院 | Preparation method for polycarboxylic acid series comb-shaped surface active agent |
| CN102675557A (en) * | 2011-12-16 | 2012-09-19 | 天津冶建特种材料有限公司 | Slow-release type concrete slump retaining agent and preparation method thereof |
| CN102976655A (en) * | 2012-12-05 | 2013-03-20 | 江苏苏博特新材料股份有限公司 | Slump retaining polycarboxylic acid superplasticizer |
| CN104140503A (en) * | 2014-07-30 | 2014-11-12 | 江西格雷斯科技股份有限公司 | Method for synthesizing high-water-reduction high-slump-retaining high-performance polycarboxylate water reducer at normal temperature |
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- 2015-07-30 CN CN201510461080.5A patent/CN105036595B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101734879A (en) * | 2009-12-27 | 2010-06-16 | 长沙理工大学 | Polyurethane/polycarboxylic acid compound water reducer for concrete and preparation thereof |
| CN102199298A (en) * | 2011-03-23 | 2011-09-28 | 中国日用化学工业研究院 | Preparation method for polycarboxylic acid series comb-shaped surface active agent |
| CN102675557A (en) * | 2011-12-16 | 2012-09-19 | 天津冶建特种材料有限公司 | Slow-release type concrete slump retaining agent and preparation method thereof |
| CN102976655A (en) * | 2012-12-05 | 2013-03-20 | 江苏苏博特新材料股份有限公司 | Slump retaining polycarboxylic acid superplasticizer |
| CN104140503A (en) * | 2014-07-30 | 2014-11-12 | 江西格雷斯科技股份有限公司 | Method for synthesizing high-water-reduction high-slump-retaining high-performance polycarboxylate water reducer at normal temperature |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109517115A (en) * | 2018-12-03 | 2019-03-26 | 广东科隆智谷新材料股份有限公司 | A kind of preparation method of polycarboxylate water-reducer |
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Address after: 830013 Urumqi high tech Zone (new city) North Industrial Park, blue sky road, No. 216, No. Patentee after: DELAND WATER TECHNOLOGY Co.,Ltd. Address before: 830013, 216, Lantian Road, North Industrial Zone, hi tech Zone, the Xinjiang Uygur Autonomous Region, Urumqi Patentee before: XINJIANG DELAND Co.,Ltd. |
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Denomination of invention: A high collapse resistant polycarboxylate superplasticizer and its preparation method Granted publication date: 20170524 Pledgee: Beijing Bank Co.,Ltd. Urumqi Branch Pledgor: DELAND WATER TECHNOLOGY CO.,LTD. Registration number: Y2024650000002 |