CN104479082A - Slow-release type polycarboxylic acid water reducer and preparation method thereof - Google Patents
Slow-release type polycarboxylic acid water reducer and preparation method thereof Download PDFInfo
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- CN104479082A CN104479082A CN201410673575.XA CN201410673575A CN104479082A CN 104479082 A CN104479082 A CN 104479082A CN 201410673575 A CN201410673575 A CN 201410673575A CN 104479082 A CN104479082 A CN 104479082A
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 53
- 239000003638 chemical reducing agent Substances 0.000 title claims abstract description 41
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- 239000002253 acid Substances 0.000 title abstract description 8
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 33
- 239000007788 liquid Substances 0.000 claims abstract description 20
- PHOQVHQSTUBQQK-SQOUGZDYSA-N D-glucono-1,5-lactone Chemical compound OC[C@H]1OC(=O)[C@H](O)[C@@H](O)[C@@H]1O PHOQVHQSTUBQQK-SQOUGZDYSA-N 0.000 claims abstract description 18
- 235000012209 glucono delta-lactone Nutrition 0.000 claims abstract description 17
- 229960003681 gluconolactone Drugs 0.000 claims abstract description 17
- CERQOIWHTDAKMF-UHFFFAOYSA-N Methacrylic acid Chemical compound CC(=C)C(O)=O CERQOIWHTDAKMF-UHFFFAOYSA-N 0.000 claims abstract description 13
- 229920000056 polyoxyethylene ether Polymers 0.000 claims abstract description 13
- 229940051841 polyoxyethylene ether Drugs 0.000 claims abstract description 13
- 235000011121 sodium hydroxide Nutrition 0.000 claims abstract description 11
- 238000006243 chemical reaction Methods 0.000 claims abstract description 8
- 230000000694 effects Effects 0.000 claims abstract description 6
- 239000012986 chain transfer agent Substances 0.000 claims abstract description 5
- 239000000178 monomer Substances 0.000 claims abstract description 4
- 238000013268 sustained release Methods 0.000 claims description 27
- 239000012730 sustained-release form Substances 0.000 claims description 27
- XBDQKXXYIPTUBI-UHFFFAOYSA-N dimethylselenoniopropionate Natural products CCC(O)=O XBDQKXXYIPTUBI-UHFFFAOYSA-N 0.000 claims description 22
- 239000008367 deionised water Substances 0.000 claims description 15
- 229910021641 deionized water Inorganic materials 0.000 claims description 15
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 12
- QVDTXNVYSHVCGW-ONEGZZNKSA-N isopentenol Chemical compound CC(C)\C=C\O QVDTXNVYSHVCGW-ONEGZZNKSA-N 0.000 claims description 12
- 238000003756 stirring Methods 0.000 claims description 12
- 235000019260 propionic acid Nutrition 0.000 claims description 11
- IUVKMZGDUIUOCP-BTNSXGMBSA-N quinbolone Chemical compound O([C@H]1CC[C@H]2[C@H]3[C@@H]([C@]4(C=CC(=O)C=C4CC3)C)CC[C@@]21C)C1=CCCC1 IUVKMZGDUIUOCP-BTNSXGMBSA-N 0.000 claims description 11
- NIXOWILDQLNWCW-UHFFFAOYSA-N Acrylic acid Chemical compound OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims description 7
- 238000010526 radical polymerization reaction Methods 0.000 claims description 6
- 239000002994 raw material Substances 0.000 claims description 6
- 235000019154 vitamin C Nutrition 0.000 claims description 6
- 239000011718 vitamin C Substances 0.000 claims description 6
- 238000007334 copolymerization reaction Methods 0.000 claims description 2
- 239000004567 concrete Substances 0.000 abstract description 19
- 238000010276 construction Methods 0.000 abstract description 4
- 238000000034 method Methods 0.000 abstract description 4
- 239000003999 initiator Substances 0.000 abstract description 3
- 239000000654 additive Substances 0.000 abstract description 2
- 239000004566 building material Substances 0.000 abstract description 2
- 239000003795 chemical substances by application Substances 0.000 abstract description 2
- 238000005265 energy consumption Methods 0.000 abstract description 2
- 229920000570 polyether Polymers 0.000 abstract description 2
- 238000005086 pumping Methods 0.000 abstract description 2
- PHTQWCKDNZKARW-UHFFFAOYSA-N isoamylol Chemical compound CC(C)CCO PHTQWCKDNZKARW-UHFFFAOYSA-N 0.000 abstract 2
- 239000004721 Polyphenylene oxide Substances 0.000 abstract 1
- 230000003472 neutralizing effect Effects 0.000 abstract 1
- 238000006116 polymerization reaction Methods 0.000 abstract 1
- 230000000052 comparative effect Effects 0.000 description 6
- 229910052739 hydrogen Inorganic materials 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 3
- 229920005646 polycarboxylate Polymers 0.000 description 3
- 239000004568 cement Substances 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 2
- 150000002596 lactones Chemical class 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 description 1
- VVQNEPGJFQJSBK-UHFFFAOYSA-N Methyl methacrylate Chemical compound COC(=O)C(C)=C VVQNEPGJFQJSBK-UHFFFAOYSA-N 0.000 description 1
- AFCARXCZXQIEQB-UHFFFAOYSA-N N-[3-oxo-3-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)propyl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C(CCNC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)N1CC2=C(CC1)NN=N2 AFCARXCZXQIEQB-UHFFFAOYSA-N 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 150000001732 carboxylic acid derivatives Chemical class 0.000 description 1
- 230000003111 delayed effect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000008103 glucose Substances 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 102000004169 proteins and genes Human genes 0.000 description 1
- 108090000623 proteins and genes Proteins 0.000 description 1
- 238000005204 segregation Methods 0.000 description 1
- 239000003643 water by type Substances 0.000 description 1
Landscapes
- Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)
- Polymerisation Methods In General (AREA)
Abstract
The invention relates to the technical field of building material additives and in particular relates to a slow-release type polycarboxylic acid water reducer and a preparation method of the slow-release type polycarboxylic acid water reducer. The method comprises the following steps: on the basis of taking unsaturated polyether isoamyl alcohol polyoxyethylene ether, crylic acid, methacrylic acid and glucolactone as monomers, carrying out polymerization reaction at the room temperature in the presence of an initiator, a chain transfer agent and a reduction agent, and neutralizing a reaction system until the pH is 6-7 by using caustic soda liquid after the reaction is ended to prepare the slow-release type polycarboxylic acid water reducer. The water reducer synthesized by gluconolactone has high slump-retaining performance and has the effect of slowly releasing; the concrete state has high mobility; the completion of pumping construction in summer can be facilitated; meanwhile, the preparation process is simple, low in energy consumption and high in economic benefit.
Description
Technical field
The present invention relates to additive for building material technical field, especially relate to a kind of sustained-release polycarboxylic water reducer and preparation method thereof.
Background technology
Along with the development of building trade, in engineer applied, the requirement of water reducer is progressively improved.The advantages such as polycarboxylate water-reducer is high because of its water-reducing rate, adaptability is better, obtain great propagation and employment.Along with improving constantly of building level, require also more and more higher to concrete quality, in ready mixed concrete industry, the slump-loss problem of fresh concrete is a difficult problem for puzzlement construction always, particularly for a long time transport can cause concrete slump loss excessive, affects concrete serviceability, and retemper can make actual concrete intensity and the weather resistance such as impervious not reach index request, this a little measure complex operation, cost increases and easily causes the generation of accident.
Chinese patent (CN103723945A) discloses a kind of fast hydrolysis sustained-release polycarboxylic water reducer and preparation method thereof, pass through polyethers, double bond containing carboxylic acid monomer and water-soluble micro-crosslinked functional agent, in the presence of initiator and chain-transfer agent, polyreaction, this water reducer can reduce concrete segregation equivalent risk, but the method reaction process is loaded down with trivial details, temperature of reaction is higher, function of slump protection is undesirable, therefore, seek a kind of at room temperature can synthesize and to be delayed dissemination and the polycarboxylate water-reducer of high-thin arch dam performance is significant to concrete within a certain period of time.
Summary of the invention
For the problems referred to above, the invention provides a kind of sustained-release polycarboxylic water reducer, adding of monomeric glucose acid lactone, enable this water reducer postpone concrete dissemination and there is high-thin arch dam performance simultaneously.
Present invention also offers a kind of preparation method of sustained-release polycarboxylic water reducer, the method technique is simple, can synthesize under room temperature, environmental protection and economy.
The technical solution used in the present invention is:
The invention provides a kind of sustained-release polycarboxylic water reducer, it is characterized in that, be formed by radical polymerization by following parts by weight raw material: isopentenol polyoxyethylene ether 330-375 part, vinylformic acid (AA) 30-46 part, methacrylic acid (MAA) 5-10 part, Gluconolactone 8 parts, 30% hydrogen peroxide 2.5-4.5 part, vitamins C 0.7-1.2 part, thin base propionic acid 1.2-2.0 part;
Described isopentenol polyoxyethylene ether, vinylformic acid, methacrylic acid, gluconolactone are reaction monomers, under dredging the effect of base propionic acid, copolyreaction occur in redox system and chain-transfer agent.
Described isopentenol polyoxyethylene ether molecular weight is 2000-2400.
Present invention also offers a kind of preparation method of sustained-release polycarboxylic water reducer, comprise the following steps:
A. get isopentenol polyoxyethylene ether 330-375 part of weight part, 30% hydrogen peroxide 2.5-4.5 part joins in the deionized water of 200-270 weight part, be made into end liquid;
B. get vinylformic acid 30-46 part of weight part, methacrylic acid 5-10 part, Gluconolactone 8 parts mix, stir, wiring solution-forming A;
C. get vitamins C 0.7-1.2 part of weight part, thin base propionic acid 1.2-2.0 part joins in the deionized water of 150-210 weight part and mixes, stir, wiring solution-forming B;
D. under room temperature, drip the solution A in step b in end liquid, time for adding is 3 hours, and in end liquid, drip the solution B in step c, time for adding is 3.5 hours simultaneously;
E., after being added dropwise to complete, stirring and proceed copolymerization in 30 minutes, then add mass concentration be 32% liquid caustic soda regulate pH value to be 6-7, continue stirring 20 minutes, both described sustained-release polycarboxylic water reducer.
Described liquid caustic soda is aqueous sodium hydroxide solution.
30% described hydrogen peroxide (H
2o
2) to be mass concentration be 30% aqueous hydrogen peroxide solution.
The present invention's vitamins C is as initiator, dredge base propionic acid as chain-transfer agent, adjust suitable ratio, vitamins C is with 30% hydrogen peroxide composition redox system simultaneously, by adjustment proportioning, while can acting at normal temperatures, there is high conversion, invention introduces one there is guarantor to collapse genetic material Gluconolactone, ester bond in lactone structure can discharge slowly under the alkaline condition of ready mixed concrete, carboxyl is avoided to be adsorbed instantaneously by cement, cause a large amount of carboxyl to lose, thus be unfavorable for concrete retentivity; Gluconolactone has multiple hydroxyl simultaneously, hydroxyl has guarantor's effect of collapsing, and therefore, the existing good function of slump protection of the water reducer utilizing gluconolactone to synthesize can reach again the effect of slow releasing, make concrete state have good mobility always, be more conducive to completing of pumping construction in summer.
Advantage of the present invention and beneficial effect:
1. this water reducer at room temperature can synthesize, and energy consumption is little, economic environmental protection, reduces the production cost of polycarboxylate water-reducer.
2. the adding of Gluconolactone, improve concrete workability and make concrete have good retentivity, had good sustained release effect simultaneously, the polyhydric existence of Gluconolactone, make concrete slump retaining performance good.
Embodiment
Below by embodiment, the present invention will be further elaborated, and following explanation has been only explanation the present invention, do not limit its content.
Embodiment 1
A kind of sustained-release polycarboxylic water reducer is formed by radical polymerization by following parts by weight raw material:
Bed material: isopentenol polyoxyethylene ether: 330,30%H
2o
2: 2.5, deionized water: 210;
Solution A: AA:30, MAA:5, Gluconolactone: 8, deionized water: 120;
Solution B: VC:0.7, thin base propionic acid: 1.2, deionized water: 150.
A kind of preparation method of sustained-release polycarboxylic water reducer: under room temperature, drips solution A in end liquid, and time for adding is 3 hours, and in end liquid, drip solution B, time for adding is 3.5 hours simultaneously; After being added dropwise to complete, carry out copolyreaction 30 minutes, then add mass concentration be 32% aqueous sodium hydroxide solution regulate pH value to be 6, continue stirring 20 minutes, both described sustained-release polycarboxylic water reducer.
Embodiment 2
A kind of sustained-release polycarboxylic water reducer is formed by radical polymerization by following parts by weight raw material:
Bed material: isopentenol polyoxyethylene ether: 345,30%H
2o
2: 3.1, deionized water: 235;
Solution A: AA:34, MAA:6.5, Gluconolactone: 8, deionized water: 130;
Solution B: VC:0.85, thin base propionic acid: 1.6, deionized water: 170.
A kind of preparation method of sustained-release polycarboxylic water reducer: under room temperature, drips solution A in end liquid, and time for adding is 3 hours, and in end liquid, drip solution B, time for adding is 3.5 hours simultaneously; After being added dropwise to complete, carry out copolyreaction 30 minutes, then add mass concentration be 32% aqueous sodium hydroxide solution regulate pH value to be about 7, continue stirring 20 minutes, both described sustained-release polycarboxylic water reducer.
Embodiment 3
A kind of sustained-release polycarboxylic water reducer is formed by radical polymerization by following parts by weight raw material:
Bed material: isopentenol polyoxyethylene ether: 360,30%H
2o
2: 3.8, deionized water: 250;
Solution A: AA:40, MAA:8.2 Gluconolactone: 8 deionized waters: 142;
Solution B: VC:0.9, thin base propionic acid: 1.75, deionized water: 195.
A kind of preparation method of sustained-release polycarboxylic water reducer: under room temperature, drips solution A in end liquid, and time for adding is 3 hours, and in end liquid, drip solution B, time for adding is 3.5 hours simultaneously; After being added dropwise to complete, carry out copolyreaction 30 minutes, then add mass concentration be 32% aqueous sodium hydroxide solution regulate pH value to be 6, continue stirring 20 minutes, both described sustained-release polycarboxylic water reducer.
Embodiment 4
A kind of sustained-release polycarboxylic water reducer is formed by radical polymerization by following parts by weight raw material:
Bed material: isopentenol polyoxyethylene ether: 375,30%H
2o
2: 4.5, deionized water: 270;
Solution A: AA:46, MAA:10, Gluconolactone: 8, deionized water: 160
Solution B: VC:1.2, thin base propionic acid: 2, deionized water: 210.
The preparation method of sustained-release polycarboxylic water reducer: when end liquid temp is 17 DEG C ± 2 DEG C, drip solution A in end liquid, time for adding is 3 hours, in end liquid, drip solution B, time for adding is 3.5 hours simultaneously; After being added dropwise to complete, carry out copolyreaction 30 minutes, then add mass concentration be 32% aqueous sodium hydroxide solution regulate pH value to be 7, continue stirring 20 minutes, both described sustained-release polycarboxylic water reducer.
Comparative example 1: the methyl methacrylate of selecting announced according to CN103641959 replaces Gluconolactone in embodiment 2 and methacrylic acid, and other reactions steps are identical with embodiment 2.
Comparative example 2: contrast product is commercially available slow-setting polycarboxylic acid water reducing agent
The slow-setting polycarboxylic acid water reducing agent synthesize above embodiment 1-4 and comparative example 1-2 carry out following test respectively:
Adopt reference cement, according to the test request in " concrete admixture " (GB8076-2008), compare sustained-release polycarboxylic water reducer (embodiment 1-4) prepared by the present invention with comparative example 1, the water-reducing rate of comparative example 2, degree of mobilization, the slump, the results are shown in Table 1.
Table 1
As can be seen from above-mentioned experimental data, compare with comparative example, adopt sustained-release water reducing agent of the present invention while having high dispersion, there is again very strong slow releasing function, slow releasing carboxyl under the alkaline condition of ready mixed concrete, reduces and adsorbs instantaneously, decrease the problems such as slump-loss, improve concrete construction performance, and be applicable to long hauling operation.
Above-described embodiment is the present invention's preferably embodiment; but embodiments of the present invention are not by the restriction of embodiment; other is any do not deviate from spirit of the present invention and principle under make change, modification, combination, substitute, simplify and all should be equivalent substitute mode, be included within protection scope of the present invention.
Claims (4)
1. a sustained-release polycarboxylic water reducer, it is characterized in that, be formed by radical polymerization by following parts by weight raw material: isopentenol polyoxyethylene ether 330-375 part, vinylformic acid 30-46 part, methacrylic acid 5-10 part, Gluconolactone 8 parts, 30% hydrogen peroxide 2.5-4.5 part, vitamins C 0.7-1.2 part, thin base propionic acid 1.2-2.0 part;
Described isopentenol polyoxyethylene ether, vinylformic acid, methacrylic acid, gluconolactone are reaction monomers, under dredging the effect of base propionic acid, copolyreaction occur in redox system and chain-transfer agent.
2. sustained-release polycarboxylic water reducer according to claim 1, is characterized in that: described isopentenol polyoxyethylene ether molecular weight is 2000-2400.
3. the preparation method of the sustained-release polycarboxylic water reducer according to any one of claim 1-2, is characterized in that, comprises the following steps:
A. get isopentenol polyoxyethylene ether 330-375 part of weight part, 30% hydrogen peroxide 2.5-4.5 part joins in the deionized water of 200-270 weight part, be made into end liquid;
B. get vinylformic acid 30-46 part of weight part, methacrylic acid 5-10 part, Gluconolactone 8 parts mix, stir, wiring solution-forming A;
C. get vitamins C 0.7-1.2 part of weight part, thin base propionic acid 1.2-2.0 part joins in the deionized water of 150-210 weight part and mixes, stir, wiring solution-forming B;
D. under room temperature, drip the solution A in step b in end liquid, time for adding is 3 hours, and in end liquid, drip the solution B in step c, time for adding is 3.5 hours simultaneously;
E., after being added dropwise to complete, stirring and proceed copolymerization in 30 minutes, then add mass concentration be 32% liquid caustic soda regulate pH value to be 6-7, continue stirring 20 minutes, both described sustained-release polycarboxylic water reducer.
4. preparation method according to claim 3, is characterized in that: described liquid caustic soda is aqueous sodium hydroxide solution.
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| CN109906210A (en) * | 2016-10-31 | 2019-06-18 | 巴斯夫欧洲公司 | Additive for architectural chemistry composition |
| CN110003405A (en) * | 2019-04-24 | 2019-07-12 | 四川同舟化工科技有限公司 | Comprehensive high-performance polycarboxylic acids diminishing |
| CN110845673A (en) * | 2019-11-19 | 2020-02-28 | 安徽鑫固环保股份有限公司 | Comb-type coal water slurry dispersing agent prepared from glucolactone and preparation method thereof |
| CN111234131A (en) * | 2020-03-25 | 2020-06-05 | 陕西科技大学 | Gluconolactone-based polycarboxylic acid water reducing agent and preparation method thereof |
| CN112724340A (en) * | 2020-12-28 | 2021-04-30 | 江苏开放大学（江苏城市职业学院） | Viscosity-reducing composite polycarboxylate superplasticizer and preparation method thereof |
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| CN110845673A (en) * | 2019-11-19 | 2020-02-28 | 安徽鑫固环保股份有限公司 | Comb-type coal water slurry dispersing agent prepared from glucolactone and preparation method thereof |
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| CN112724340A (en) * | 2020-12-28 | 2021-04-30 | 江苏开放大学（江苏城市职业学院） | Viscosity-reducing composite polycarboxylate superplasticizer and preparation method thereof |
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| CN104479082B (en) | 2017-10-13 |
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