CN104479082B - A kind of sustained-release polycarboxylic water reducer and preparation method thereof - Google Patents
A kind of sustained-release polycarboxylic water reducer and preparation method thereof Download PDFInfo
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 51
- 239000003638 chemical reducing agent Substances 0.000 title claims abstract description 40
- 238000013268 sustained release Methods 0.000 title claims abstract description 28
- 239000012730 sustained-release form Substances 0.000 title claims abstract description 28
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 28
- PHTQWCKDNZKARW-UHFFFAOYSA-N isoamylol Chemical compound CC(C)CCO PHTQWCKDNZKARW-UHFFFAOYSA-N 0.000 claims abstract description 22
- 239000007788 liquid Substances 0.000 claims abstract description 18
- 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 16
- 229920000056 polyoxyethylene ether Polymers 0.000 claims abstract description 12
- 229940051841 polyoxyethylene ether Drugs 0.000 claims abstract description 12
- 235000011121 sodium hydroxide Nutrition 0.000 claims abstract description 11
- CERQOIWHTDAKMF-UHFFFAOYSA-N Methacrylic acid Chemical compound CC(=C)C(O)=O CERQOIWHTDAKMF-UHFFFAOYSA-N 0.000 claims abstract description 7
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims abstract description 6
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 claims abstract description 5
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 16
- 239000008367 deionised water Substances 0.000 claims description 14
- 229910021641 deionized water Inorganic materials 0.000 claims description 14
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 claims description 10
- 238000003756 stirring Methods 0.000 claims description 10
- 238000010526 radical polymerization reaction Methods 0.000 claims description 6
- 239000002994 raw material Substances 0.000 claims description 6
- ZZZCUOFIHGPKAK-UHFFFAOYSA-N D-erythro-ascorbic acid Natural products OCC1OC(=O)C(O)=C1O ZZZCUOFIHGPKAK-UHFFFAOYSA-N 0.000 claims description 5
- 229930003268 Vitamin C Natural products 0.000 claims description 5
- 235000019154 vitamin C Nutrition 0.000 claims description 5
- 239000011718 vitamin C Substances 0.000 claims description 5
- 238000007334 copolymerization reaction Methods 0.000 claims description 2
- DKIDEFUBRARXTE-UHFFFAOYSA-N 3-mercaptopropanoic acid Chemical compound OC(=O)CCS DKIDEFUBRARXTE-UHFFFAOYSA-N 0.000 claims 2
- ASUAYTHWZCLXAN-UHFFFAOYSA-N prenol Chemical compound CC(C)=CCO ASUAYTHWZCLXAN-UHFFFAOYSA-N 0.000 claims 1
- 239000004567 concrete Substances 0.000 abstract description 19
- 238000006243 chemical reaction Methods 0.000 abstract description 7
- 239000003795 chemical substances by application Substances 0.000 abstract description 4
- 238000010276 construction Methods 0.000 abstract description 4
- 235000012209 glucono delta-lactone Nutrition 0.000 abstract description 4
- 229960003681 gluconolactone Drugs 0.000 abstract description 4
- 238000000034 method Methods 0.000 abstract description 4
- 239000000654 additive Substances 0.000 abstract description 3
- 230000000996 additive effect Effects 0.000 abstract description 3
- 230000000694 effects Effects 0.000 abstract description 3
- 239000003999 initiator Substances 0.000 abstract description 3
- 239000000178 monomer Substances 0.000 abstract description 3
- 239000004566 building material Substances 0.000 abstract description 2
- 238000005265 energy consumption Methods 0.000 abstract description 2
- 238000005516 engineering process Methods 0.000 abstract description 2
- 229920000570 polyether Polymers 0.000 abstract description 2
- 238000005086 pumping Methods 0.000 abstract description 2
- 239000004721 Polyphenylene oxide Substances 0.000 abstract 1
- 238000006386 neutralization reaction Methods 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 17
- XBDQKXXYIPTUBI-UHFFFAOYSA-N dimethylselenoniopropionate Natural products CCC(O)=O XBDQKXXYIPTUBI-UHFFFAOYSA-N 0.000 description 16
- 235000019260 propionic acid Nutrition 0.000 description 8
- 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 description 8
- 230000000052 comparative effect Effects 0.000 description 6
- 229920005646 polycarboxylate Polymers 0.000 description 6
- 239000007864 aqueous solution Substances 0.000 description 5
- 239000002253 acid Substances 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 3
- 150000002596 lactones Chemical class 0.000 description 3
- 230000002035 prolonged effect Effects 0.000 description 3
- 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 2
- 239000004568 cement Substances 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 239000008103 glucose Substances 0.000 description 2
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 2
- 239000006193 liquid solution Substances 0.000 description 2
- VVQNEPGJFQJSBK-UHFFFAOYSA-N Methyl methacrylate Chemical group COC(=O)C(C)=C VVQNEPGJFQJSBK-UHFFFAOYSA-N 0.000 description 1
- MKYBYDHXWVHEJW-UHFFFAOYSA-N N-[1-oxo-1-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)propan-2-yl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C(C(C)NC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)N1CC2=C(CC1)NN=N2 MKYBYDHXWVHEJW-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
- 229940114077 acrylic acid Drugs 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 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
- 238000004132 cross linking Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 235000013399 edible fruits Nutrition 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000000686 essence Substances 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000002955 isolation Methods 0.000 description 1
- 229940063559 methacrylic acid Drugs 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 102000004169 proteins and genes Human genes 0.000 description 1
- 108090000623 proteins and genes Proteins 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000007634 remodeling Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000008030 superplasticizer Substances 0.000 description 1
- 230000002459 sustained effect Effects 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 239000003643 water by type Substances 0.000 description 1
Abstract
The present invention relates to additive for building material technical field, more particularly, to a kind of sustained-release polycarboxylic water reducer and preparation method thereof.This method is using unsaturated polyether isoamyl alcohol polyoxyethylene ether, acrylic acid and methacrylic acid, glucolactone as monomer, acted on by initiator and chain-transferring agent, reducing agent, room temperature carries out polymerisation, after reaction terminates, it is 67 with liquid caustic soda neutralization reaction system PH, produce sustained-release polycarboxylic water reducer, the existing good function of slump protection of water reducer that the present invention is synthesized using gluconolactone can reach the effect slowly discharged again, make concrete state that there is the completion of good mobility, more conducively summer pumping construction always.The preparation technology of the present invention is simple simultaneously, and energy consumption is small, with good economic benefit.
Description
Technical field
The present invention relates to additive for building material technical field, more particularly, to a kind of sustained-release polycarboxylic water reducer and its
Preparation method.
Background technology
With the development of building trade, the requirement in engineer applied to water reducer is stepped up.Polycarboxylate water-reducer because
The advantages of its water-reducing rate is high, adaptability is preferable, has obtained great popularization and application.It is right with the continuous improvement of building level
Concrete quality requires also more and more higher, and in ready-mixed concrete industry, the slump-loss problem of fresh concrete is always
Perplex the problem of construction, particularly prolonged transport can cause concrete slump loss excessive, influence the work of concrete
Performance, and the remodeling that adds water can make the intensity and the durability such as impervious of actual concrete not reach index request, this little measures operation
Cumbersome, cost increases and is easily caused the generation of accident.
Chinese patent（CN103723945A）A kind of fast hydrolyzable slow releasing polycarboxylate superplasticizer and preparation method thereof is disclosed,
By polyethers, double bond containing carboxylic acid monomer and water-soluble micro- crosslinking function additive, in the presence of initiator and chain-transferring agent, gather
Reaction is closed, the water reducer can reduce the isolation equivalent risk of concrete, but this method course of reaction is cumbersome, and reaction temperature is higher,
Function of slump protection is undesirable, therefore, seeks a kind of can synthesizing at room temperature and concrete generation can be prolonged within a certain period of time
The polycarboxylate water-reducer of slow peptizaiton and high-collapse-retentivity energy is significant.
The content of the invention
In view of the above-mentioned problems, the invention provides a kind of sustained-release polycarboxylic water reducer, monomeric glucose acid lactone plus
Enter, the water reducer is postponed the peptizaiton of concrete while having high-collapse-retentivity energy.
Present invention also offers a kind of preparation method of sustained-release polycarboxylic water reducer, this method technique is simply, at room temperature
It can synthesize, environmental protection and economy.
The technical solution adopted by the present invention is：
The invention provides a kind of sustained-release polycarboxylic water reducer, it is characterised in that is led to by following parts by weight raw material
Radical polymerization is crossed to form：330-375 parts of isoamyl alcohol polyoxyethylene ether, acrylic acid（AA）30-46 parts, methacrylic acid
（MAA）5-10 parts, 8 parts of glucolactone, 2.5-4.5 parts of 30% hydrogen peroxide, 0.7-1.2 parts of vitamin C, dredge base propionic acid
1.2-2.0 part；
Described isoamyl alcohol polyoxyethylene ether, acrylic acid, methacrylic acid, gluconolactone are reaction monomers, in oxygen
Change in the presence of reduction system and the thin base propionic acid of chain-transferring agent, be copolymerized.
Described isoamyl alcohol 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. 330-375 parts of the isoamyl alcohol polyoxyethylene ether of parts by weight, 2.5-4.5 parts of 30% hydrogen peroxide is taken to be added to
In the deionized water of 200-270 parts by weight, bottom liquid is made into；
B. take 8 parts of 5-10 parts of 30-46 parts of acrylic acid, methacrylic acid, the glucolactone of parts by weight to be mixed, stir
Mix uniform, wiring solution-forming A；
C. 0.7-1.2 parts of the vitamin C of parts by weight, thin 1.2-2.0 parts of base propionic acid is taken to be added to 150-210 parts by weight
Mixed, stirred in deionized water, wiring solution-forming B；
D. at room temperature, the solution A in step b is added dropwise into bottom liquid, time for adding is 3 hours, while being added dropwise into bottom liquid
Solution B in step c, time for adding is 3.5 hours；
E. after being added dropwise to complete, stirring proceeds copolymerization in 30 minutes, then adds mass concentration and is adjusted for 32% liquid caustic soda
PH value is 6-7, continues to stir 20 minutes, both obtains described sustained-release polycarboxylic water reducer.
Described liquid caustic soda is sodium hydrate aqueous solution.
30% described hydrogen peroxide（H2O2）It is the aqueous hydrogen peroxide solution that mass concentration is 30%.
Present invention vitamin C dredges base propionic acid as chain-transferring agent, adjusts suitable ratio, tie up simultaneously as initiator
Raw element C constitutes redox system with 30% hydrogen peroxide, is matched, had while can acting at normal temperatures by adjusting
High conversion, invention introduces one there is guarantor to collapse genetic material glucolactone, and the ester bond in lactone structure can be slow
Discharged under the alkalescence condition of ready-mixed concrete, it is to avoid carboxyl is adsorbed by cement moment, causes a large amount of carboxyls to lose, from
And it is unfavorable for the retentivity of concrete；Gluconolactone has multiple hydroxyls simultaneously, and hydroxyl has guarantor's effect of collapsing, therefore, utilizes
The existing good function of slump protection of water reducer of gluconolactone synthesis can reach the effect slowly discharged again, make concrete state
There is the completion of good mobility, more conducively summer pumping construction always.
Advantages of the present invention and beneficial effect：
1. the water reducer can be synthesized at room temperature, energy consumption is small, economic and environment-friendly, reduces the life of polycarboxylate water-reducer
Produce cost.
2. the addition of glucolactone, improve concrete workability makes concrete have good retentivity simultaneously, is sustained
Effect is good, the presence of glucolactone polyhydroxy, makes concrete slump retaining performance good.
Embodiment
Below by embodiment, the present invention will be further elaborated, and the description below is only for explaining the present invention, not
Its content is defined.
Embodiment 1
A kind of sustained-release polycarboxylic water reducer, is to be formed by following parts by weight raw material by radical polymerization：
Bed material：Isoamyl alcohol polyoxyethylene ether：330、30%H2O2：2.5th, deionized water：210；
Solution A： AA：30、MAA：5th, glucolactone：8th, deionized water：120；
Solution B：VC：0.7th, base propionic acid is dredged：1.2nd, deionized water：150.
A kind of preparation method of sustained-release polycarboxylic water reducer：At room temperature, solution A is added dropwise into bottom liquid, time for adding is 3
Hour, while solution B is added dropwise into bottom liquid, time for adding is 3.5 hours；After being added dropwise to complete, copolyreaction 30 minutes is carried out,
Then add mass concentration be 32% sodium hydrate aqueous solution regulation pH value be 6, continue stir 20 minutes, both the sustained release
Type polycarboxylate water-reducer.
Embodiment 2
A kind of sustained-release polycarboxylic water reducer, is to be formed by following parts by weight raw material by radical polymerization：
Bed material：Isoamyl alcohol polyoxyethylene ether：345、30%H2O2：3.1st, deionized water：235；
Solution A：AA：34、MAA：6.5th, glucolactone：8th, deionized water：130；
Solution B：VC：0.85th, base propionic acid is dredged：1.6th, deionized water：170.
A kind of preparation method of sustained-release polycarboxylic water reducer：At room temperature, solution A is added dropwise into bottom liquid, time for adding is 3
Hour, while solution B is added dropwise into bottom liquid, time for adding is 3.5 hours；After being added dropwise to complete, copolyreaction 30 minutes is carried out,
Then it is 7 or so to add the sodium hydrate aqueous solution regulation pH value that mass concentration is 32%, continues to stir 20 minutes, had both obtained described
Sustained-release polycarboxylic water reducer.
Embodiment 3
A kind of sustained-release polycarboxylic water reducer, is to be formed by following parts by weight raw material by radical polymerization：
Bed material：Isoamyl alcohol polyoxyethylene ether：360、30%H2O2：3.8th, deionized water：250；
Solution A：AA：40、MAA：8.2 glucolactone：8 deionized waters：142；
Solution B：VC：0.9th, base propionic acid is dredged：1.75, deionized water：195.
A kind of preparation method of sustained-release polycarboxylic water reducer：At room temperature, solution A is added dropwise into bottom liquid, time for adding is 3
Hour, while solution B is added dropwise into bottom liquid, time for adding is 3.5 hours；After being added dropwise to complete, copolyreaction 30 minutes is carried out,
Then add mass concentration be 32% sodium hydrate aqueous solution regulation pH value be 6, continue stir 20 minutes, both the sustained release
Type polycarboxylate water-reducer.
Embodiment 4
A kind of sustained-release polycarboxylic water reducer, is to be formed by following parts by weight raw material by radical polymerization：
Bed material：Isoamyl alcohol polyoxyethylene ether：375、30%H2O2：4.5th, deionized water：270；
Solution A：AA：46、MAA：10th, glucolactone：8th, deionized water：160
Solution B：VC：1.2nd, base propionic acid is dredged：2nd, deionized water：210.
A kind of preparation method of sustained-release polycarboxylic water reducer：When bottom liquid temperature degree is 17 DEG C ± 2 DEG C, it is added dropwise into bottom liquid
Solution A, time for adding is 3 hours, while solution B is added dropwise into bottom liquid, time for adding is 3.5 hours；After being added dropwise to complete, enter
Row copolyreaction 30 minutes, it is 7 then to add the sodium hydrate aqueous solution regulation pH value that mass concentration is 32%, continues to stir 20
Minute, both the sustained-release polycarboxylic water reducer.
Comparative example 1：Glucose in the selection methyl methacrylate substitution embodiment 2 announced according to CN103641959
Acid lactone and methacrylic acid, other reactions steps be the same as Examples 2 are identical.
Comparative example 2：Contrast product is commercially available slow-setting polycarboxylic acid water reducing agent
Following experiment is carried out respectively to the above example 1-4 slow-setting polycarboxylic acid water reducing agents synthesized and comparative example 1-2：
Using reference cement, according to《Concrete admixture》（GB8076-2008）In test request, compare the present invention
The sustained-release polycarboxylic water reducer of preparation（Embodiment 1-4）With comparative example 1, the water-reducing rate of comparative example 2, fluidity, the slump, knot
Fruit is shown in Table 1.
Table 1
It can be seen from above-mentioned experimental data compared with comparative example, using the sustained-release water reducing agent of the present invention with height
While degree dispersiveness, there is very strong slow releasing function again, slow release carboxyl, is reduced under the alkalescence condition of ready-mixed concrete
Moment is adsorbed, the problems such as reducing slump-loss, improves concrete construction performance, and be adapted to prolonged hauling operation.
Above-described embodiment is not limited for the present invention preferably embodiment, but embodiments of the present invention by embodiment
System, other any Spirit Essences and the change made under principle, modifications without departing from the present invention, combines, substitutes, simplifying and should be
Equivalence replacement mode, is included within protection scope of the present invention.
Claims (3)
1. a kind of sustained-release polycarboxylic water reducer, it is characterised in that be by radical polymerization by following parts by weight raw material
Into：330-375 parts of isoamyl alcohol polyoxyethylene ether, 30-46 parts of acrylic acid, 5-10 parts of methacrylic acid, glucolactone 8
Part, 2.5-4.5 parts of 30% hydrogen peroxide, 0.7-1.2 parts of vitamin C, 1.2-2.0 parts of mercaptopropionic acid；
Preparation method is as follows：
A. 330-375 parts of the isoamyl alcohol polyoxyethylene ether of parts by weight, 2.5-4.5 parts of 30% hydrogen peroxide is taken to be added to 200-270
In the deionized water of parts by weight, bottom liquid is made into；
B. 8 parts of 5-10 parts of 30-46 parts of acrylic acid, methacrylic acid, the glucolactone of parts by weight is taken to be mixed, stirring is equal
It is even, wiring solution-forming A；
C. take parts by weight 1.2-2.0 parts of 0.7-1.2 parts of vitamin C, mercaptopropionic acid be added to 150-210 parts by weight go from
Mixed, stirred in sub- water, wiring solution-forming B；
D. at room temperature, the solution A in step b is added dropwise into bottom liquid, time for adding is 3 hours, while step c is added dropwise into bottom liquid
In solution B, time for adding be 3.5 hours；
E. after being added dropwise to complete, stirring proceeds copolymerization in 30 minutes, and it is 32% liquid caustic soda regulation pH values then to add mass concentration
For 6-7, continue to stir 20 minutes, both obtain described sustained-release polycarboxylic water reducer.
2. sustained-release polycarboxylic water reducer according to claim 1, it is characterised in that：Described prenol polyoxyethylene
Ether molecular weight is 2000-2400.
3. sustained-release polycarboxylic water reducer according to claim 1, it is characterised in that：Described liquid caustic soda is sodium hydroxide water
Solution.
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| JP7060592B2 (en) * | 2016-10-31 | 2022-04-26 | ビーエーエスエフ ソシエタス・ヨーロピア | Additives for chemical compositions for construction |
| CN106893047A (en) * | 2017-02-08 | 2017-06-27 | 山东卓星化工有限公司 | The method that solid polycarboxylic acid water reducing agent is prepared using organic oxidation reduction system |
| 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 |
| CN111234131B (en) * | 2020-03-25 | 2023-08-08 | 山东易和建材科技有限公司 | Glucolactone-based polycarboxylate water reducer 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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| CN103992443A (en) * | 2014-05-19 | 2014-08-20 | 科之杰新材料集团有限公司 | Method for preparing polycarboxylate water reducing agent by normal-temperature mixing process |
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