CN103865007A - Preparation method of viscosity-reduction type polycarboxylate water reducer - Google Patents
Preparation method of viscosity-reduction type polycarboxylate water reducer Download PDFInfo
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- CN103865007A CN103865007A CN201410097467.2A CN201410097467A CN103865007A CN 103865007 A CN103865007 A CN 103865007A CN 201410097467 A CN201410097467 A CN 201410097467A CN 103865007 A CN103865007 A CN 103865007A
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 50
- 239000003638 chemical reducing agent Substances 0.000 title claims abstract description 38
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- 229920005646 polycarboxylate Polymers 0.000 title abstract description 3
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims abstract description 20
- 239000002253 acid Substances 0.000 claims abstract description 13
- 239000003999 initiator Substances 0.000 claims abstract description 10
- 238000006386 neutralization reaction Methods 0.000 claims abstract description 9
- 125000005907 alkyl ester group Chemical group 0.000 claims abstract description 7
- 150000002148 esters Chemical class 0.000 claims abstract description 6
- 239000007864 aqueous solution Substances 0.000 claims abstract description 5
- 239000003513 alkali Substances 0.000 claims abstract description 4
- 238000007334 copolymerization reaction Methods 0.000 claims abstract description 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 21
- 238000003756 stirring Methods 0.000 claims description 17
- 230000009467 reduction Effects 0.000 claims description 16
- 230000000694 effects Effects 0.000 claims description 14
- 125000004432 carbon atom Chemical group C* 0.000 claims description 10
- 238000009413 insulation Methods 0.000 claims description 7
- 239000007788 liquid Substances 0.000 claims description 7
- 239000000203 mixture Substances 0.000 claims description 7
- 235000019394 potassium persulphate Nutrition 0.000 claims description 7
- 235000011121 sodium hydroxide Nutrition 0.000 claims description 7
- 239000000243 solution Substances 0.000 claims description 7
- LDHQCZJRKDOVOX-UHFFFAOYSA-N 2-butenoic acid Chemical compound CC=CC(O)=O LDHQCZJRKDOVOX-UHFFFAOYSA-N 0.000 claims description 6
- 125000001118 alkylidene group Chemical group 0.000 claims description 6
- 230000001105 regulatory effect Effects 0.000 claims description 6
- 238000012986 modification Methods 0.000 claims description 5
- 230000004048 modification Effects 0.000 claims description 5
- 125000000217 alkyl group Chemical group 0.000 claims description 4
- DNJIEGIFACGWOD-UHFFFAOYSA-N ethyl mercaptane Natural products CCS DNJIEGIFACGWOD-UHFFFAOYSA-N 0.000 claims description 3
- 238000010792 warming Methods 0.000 claims description 3
- DGVVWUTYPXICAM-UHFFFAOYSA-N β‐Mercaptoethanol Chemical compound OCCS DGVVWUTYPXICAM-UHFFFAOYSA-N 0.000 claims description 3
- DKIDEFUBRARXTE-UHFFFAOYSA-N 3-mercaptopropanoic acid Chemical compound OC(=O)CCS DKIDEFUBRARXTE-UHFFFAOYSA-N 0.000 claims description 2
- 239000004160 Ammonium persulphate Substances 0.000 claims description 2
- 239000004159 Potassium persulphate Substances 0.000 claims description 2
- 125000002877 alkyl aryl group Chemical group 0.000 claims description 2
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 claims description 2
- 235000019395 ammonium persulphate Nutrition 0.000 claims description 2
- 125000003118 aryl group Chemical group 0.000 claims description 2
- 239000003795 chemical substances by application Substances 0.000 claims description 2
- USHAGKDGDHPEEY-UHFFFAOYSA-L potassium persulfate Chemical compound [K+].[K+].[O-]S(=O)(=O)OOS([O-])(=O)=O USHAGKDGDHPEEY-UHFFFAOYSA-L 0.000 claims description 2
- CWERGRDVMFNCDR-UHFFFAOYSA-N thioglycolic acid Chemical compound OC(=O)CS CWERGRDVMFNCDR-UHFFFAOYSA-N 0.000 claims description 2
- 150000001735 carboxylic acids Chemical class 0.000 claims 4
- 239000004567 concrete Substances 0.000 abstract description 19
- 239000004568 cement Substances 0.000 abstract description 9
- 239000011372 high-strength concrete Substances 0.000 abstract description 7
- 230000002209 hydrophobic effect Effects 0.000 abstract description 7
- 238000000034 method Methods 0.000 abstract description 6
- 230000008901 benefit Effects 0.000 abstract description 5
- 229910052500 inorganic mineral Inorganic materials 0.000 abstract description 4
- 239000000463 material Substances 0.000 abstract description 4
- 239000011707 mineral Substances 0.000 abstract description 4
- 230000001603 reducing effect Effects 0.000 abstract description 4
- 239000011376 self-consolidating concrete Substances 0.000 abstract description 3
- CERQOIWHTDAKMF-UHFFFAOYSA-N alpha-methacrylic acid Natural products CC(=C)C(O)=O CERQOIWHTDAKMF-UHFFFAOYSA-N 0.000 abstract 2
- 229920001577 copolymer Polymers 0.000 abstract 1
- 125000001165 hydrophobic group Chemical group 0.000 abstract 1
- 229940051841 polyoxyethylene ether Drugs 0.000 abstract 1
- 229920000056 polyoxyethylene ether Polymers 0.000 abstract 1
- 150000001732 carboxylic acid derivatives Chemical class 0.000 description 19
- -1 polyoxyethylene Polymers 0.000 description 17
- 239000003643 water by type Substances 0.000 description 10
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 6
- 239000011230 binding agent Substances 0.000 description 6
- NIXOWILDQLNWCW-UHFFFAOYSA-M Acrylate Chemical compound [O-]C(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-M 0.000 description 4
- 229920003171 Poly (ethylene oxide) Polymers 0.000 description 4
- 239000002585 base Substances 0.000 description 4
- CQEYYJKEWSMYFG-UHFFFAOYSA-N butyl acrylate Chemical class CCCCOC(=O)C=C CQEYYJKEWSMYFG-UHFFFAOYSA-N 0.000 description 4
- GHKCSRZBNZQHKW-UHFFFAOYSA-N 1-sulfanylethanol Chemical class CC(O)S GHKCSRZBNZQHKW-UHFFFAOYSA-N 0.000 description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 235000010755 mineral Nutrition 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- 125000002769 thiazolinyl group Chemical group 0.000 description 3
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 2
- 230000001276 controlling effect Effects 0.000 description 2
- 238000013461 design Methods 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 229920000642 polymer Polymers 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 description 1
- XNWFRZJHXBZDAG-UHFFFAOYSA-N 2-METHOXYETHANOL Chemical compound COCCO XNWFRZJHXBZDAG-UHFFFAOYSA-N 0.000 description 1
- UATRONWBYDQKSQ-UHFFFAOYSA-N 3-methyl-1-(3-methylbut-2-enoxy)but-2-ene Chemical compound CC(C)=CCOCC=C(C)C UATRONWBYDQKSQ-UHFFFAOYSA-N 0.000 description 1
- WSNSMPZJJIYZCV-UHFFFAOYSA-N [Na]C Chemical compound [Na]C WSNSMPZJJIYZCV-UHFFFAOYSA-N 0.000 description 1
- 150000007513 acids Chemical class 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 239000004566 building material Substances 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 230000003467 diminishing effect Effects 0.000 description 1
- 235000013312 flour Nutrition 0.000 description 1
- 238000007306 functionalization reaction Methods 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- 239000004574 high-performance concrete Substances 0.000 description 1
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 description 1
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 239000012452 mother liquor Substances 0.000 description 1
- 229920000151 polyglycol Polymers 0.000 description 1
- 239000010695 polyglycol Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 239000004576 sand Substances 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 239000004575 stone Substances 0.000 description 1
- 150000005846 sugar alcohols Polymers 0.000 description 1
Landscapes
- Curing Cements, Concrete, And Artificial Stone (AREA)
- Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)
Abstract
The invention discloses a preparation method of a viscosity-reduction type polycarboxylate water reducer, which belongs to the field of concrete admixtures. The water reducer is prepared from random polyoxyalkyl ether unsaturated acid ester, unsaturated modified polyoxyethylene ether, unsaturated acid alkyl ester, and (methyl) acrylic acid, by means of copolymerization with an aqueous solution and then adding alkali for neutralization, under the presence of an initiator and a molecular weight regulator. By a certain quantity of hydrophobic units and hydrophobic groups which are introduced into and controlled in carboxylic acid copolymer molecule structures, the viscosity of a cement-based material is reduced under the presence of the water reducer. The water reducer prepared by the method has the advantages of high viscosity reducing effect, high dispersibility, good adaptability to cement, and the like; the water reducer is especially applicable to preparation of high-strength concrete, self-compacting concrete, low-water-binder-ratio high-dosage mineral admixture concrete, and the like.
Description
Technical field
The invention belongs to concrete additives in building materials field.Be specifically related to a kind of viscosity reduction type poly carboxylic acid series water reducer preparation method.
Background technology
Poly carboxylic acid series water reducer is along with functionalized design research gos deep into, and its low-dosage, high diminishing, the high advantage such as collapse, early strong of protecting are progressively embodied, and have now been widely used in the fields such as civil engineering work.At present, the poly carboxylic acid series water reducer on market all has excellent dispersing property, conventionally can meet the requirement of low water binder ratio concrete to water-reducing rate, but a difficult problem for the concrete construction aspect of performance can not fine solution low water binder ratio bringing.The development of technology of high performance concrete be unable to do without exploitation and the application of poly carboxylic acid series water reducer, along with concrete technology is to high-strength, high durable, gravity flow equality functionalization future development, due to the reduction of water-binder ratio, and the mixing and the raising of ratio of some mineral admixtures, concrete viscosity increases, affect concrete workability, there is the novel poly carboxylic acid series water reducer of viscosity reduction effect in the urgent need to exploitation, solved its engineering application difficult problem.
CN101805146A discloses a kind of poly carboxylic acid series water reducer and preparation method thereof, the carboxylic acid polyalcohol having synthesized take poly glycol monomethyl ether (methyl) acrylate, (methyl) vinylformic acid, (methyl) esters of acrylic acid, (methyl) sodium allylsulfonate as raw material have dispersed high, protect the advantages such as the ability of collapsing is strong, bleed is low, reinforced effects is obvious, viscosity-reducing performance is good.Though this invention has related to viscosity-reducing performance, mainly from disperseing, protecting over-all properties considerations such as collapse, there is no specific aim to introduce hydrophobic units and hydrophobic grouping to play the effect of reduction cement-based material viscosity.
CN101475338A discloses a kind of fragment-free track slab high-early strength type polycarboxylate compositional water reducing agent, and by accelerating component, viscosity reduction component, reduce component and poly carboxylic acid series water reducer mother liquor is composited, wherein the viscosity reduction component of composite use is polyoxyethylene glycol.This invention does not relate to from polymers of carboxylic acid Molecular Structure Design starts with, and solves the large problem of viscosity of low water binder ratio cement-based material.
Summary of the invention
Technical problem: the object of this invention is to provide a kind of viscosity reduction type poly carboxylic acid series water reducer preparation method.By introducing and controlling a certain amount of hydrophobic units (oxypropylene group, oxybutylene base) and hydrophobic grouping (alkyl ester), play the effect that reduces cement-based material viscosity under this water reducer effect in polymers of carboxylic acid molecular structure.Under initiator and molecular weight regulator effect, again add in alkali and preparation by aqueous solution copolymerization with random polyoxyalkylenes ether unsaturated acid ester, unsaturated modification Soxylat A 25-7, unsaturated acid alkyl ester, (methyl) vinylformic acid.The viscosity reduction type poly carboxylic acid series water reducer of preparing by the present invention have viscosity reducing effect obviously, dispersed high, with the advantage such as cement adaptability is good, be particularly useful for preparing high-strength concrete, self-compacting concrete, and the high volume mineral admixture concrete of low water binder ratio etc.
Technical scheme: a kind of viscosity reduction type poly carboxylic acid series water reducer preparation method provided by the invention, be with random polyoxyalkylenes ether unsaturated acid ester, unsaturated modification Soxylat A 25-7, unsaturated acid alkyl ester, (methyl) vinylformic acid under initiator and molecular weight regulator effect, add alkali neutralization by aqueous solution copolymerization again and be prepared from, this water reducer molecular structure is as shown in general formula (1):
Wherein, R
1, R
2, R
3identical or different, represent separately H or CH
3;
R
4represent alkyl or aryl or the alkylaryl of H or 1～10 C atom;
X represents the alkyl of 1～4 C atom;
Y
1represent the alkylidene group of 2 C atoms;
Y
2represent the alkylidene group of 3 C atoms;
Y
3represent the alkylidene group of 4 C atoms;
M is 1～100 integer, the integer that n is 20～100, and the integer that q is 0～50, the integer that z is 0～50, and (m+q+z) be 1～200 integer.
A kind of viscosity reduction type poly carboxylic acid series water reducer preparation method provided by the invention, is characterized in that the preparation method of this water reducer comprises the following steps:
1) unsaturated modification Soxylat A 25-7 is dissolved in the water, is warming up to 50 ℃～70 ℃, add random polyoxyalkylenes ether unsaturated acid ester and unsaturated acid alkyl ester, then stir;
2) temperature control, at 50 ℃～70 ℃, drops into initiator in still, stirs 10min;
3) temperature control, at 50 ℃～70 ℃, drips the mixing solutions of (methyl) vinylformic acid and molecular weight regulator, and time for adding is 2h～3h;
4) continue insulation 1h～2h;
5) be cooled to 35 ℃～40 ℃, and add liquid caustic soda neutralization, regulating pH value is 5～7.
Described initiator is a kind of or its mixture in ammonium persulphate, Potassium Persulphate, and the consumption of initiator (weight percent) is 1%～5% of comonomer gross weight.
Described molecular weight regulator is a kind of or its mixture in Thiovanic acid, thiohydracrylic acid, mercaptoethanol, and the consumption of molecular regulation agent (weight percent) is 0.5%～3% of comonomer gross weight.
Beneficial effect: the viscosity reduction type poly carboxylic acid series water reducer of preparing by the present invention have viscosity reducing effect obviously, dispersed high, with the advantage such as cement adaptability is good, be particularly useful for preparing high-strength concrete, self-compacting concrete, and the high volume mineral admixture concrete of low water binder ratio etc.
Embodiment
Below in conjunction with embodiment and comparative example, process of the present invention and effect are described further.
Embodiment 1
1) by methyl thiazolinyl Soxylat A 25-7, (molecular structure is shown in general formula 1, n=50) at the bottom of 100 parts of input stills, add 100 parts of deionized waters, be warmed up to 60 ℃, stirring and dissolving, then (molecular structure is shown in general formula 1 to drop into 70 parts of 10 parts of butyl acrylates, random polyoxyethylene thiazolinyl oxypropylene group ether acrylate, m=50, q=10, z=0), stir;
2) temperature control, at 60 ℃, adds 3.5 parts of Potassium Persulphates in still, stirs 10min;
3) temperature control, at 60 ℃, drips the mixing solutions containing 15 parts of vinylformic acid, 1.2 parts of mercaptoethanols and 15 parts of deionized waters, and time for adding is 3h;
4) continue insulation 2h
5) be cooled to 35 ℃～40 ℃, and add 30% liquid caustic soda neutralization, regulating pH value is 5.Be diluted with water to 40% concentration, obtain product VPC-1 of the present invention.
Embodiment 2
1) by methyl thiazolinyl Soxylat A 25-7, (molecular structure is shown in general formula 1, n=50) at the bottom of 100 parts of input stills, add 100 parts of deionized waters, be warmed up to 60 ℃, stirring and dissolving, then (molecular structure is shown in general formula 1 to drop into 70 parts of 5 parts of butyl acrylates, the random polyoxyethylene thiazolinyl of methoxyl group oxypropylene group ether acrylate, m=50, q=20, z=0), stir;
2) temperature control, at 60 ℃, adds 3.5 parts of Potassium Persulphates in still, stirs 10min;
3) temperature control, at 60 ℃, drips the mixing solutions containing 15 parts of vinylformic acid, 1.2 parts of mercaptoethanols and 15 parts of deionized waters, and time for adding is 3h;
4) continue insulation 2h
5) be cooled to 35 ℃～40 ℃, and add 30% liquid caustic soda neutralization, regulating pH value is 5.Be diluted with water to 40% concentration, obtain product VPC-2 of the present invention.
Embodiment 3
1) by methyl thiazolinyl Soxylat A 25-7, (molecular structure is shown in general formula 1, n=50) at the bottom of 100 parts of input stills, add 100 parts of deionized waters, be warmed up to 60 ℃, stirring and dissolving, then (molecular structure is shown in general formula 1 to drop into 70 parts of 5 parts of butyl acrylates, the random polyoxyethylene thiazolinyl of methoxyl group oxypropylene group oxybutylene base ether acrylate, m=50, q=20, z=20), stir;
2) temperature control, at 60 ℃, adds 3.5 parts of Potassium Persulphates in still, stirs 10min;
3) temperature control, at 60 ℃, drips the mixing solutions containing 15 parts of vinylformic acid, 1.2 parts of mercaptoethanols and 15 parts of deionized waters, and time for adding is 3h;
4) continue insulation 2h
5) be cooled to 35 ℃～40 ℃, and add 30% liquid caustic soda neutralization, regulating pH value is 5.Be diluted with water to 40% concentration, obtain product VPC-3 of the present invention.
Embodiment 4
1) by methyl thiazolinyl Soxylat A 25-7, (molecular structure is shown in general formula 1, n=50) at the bottom of 100 parts of input stills, add 100 parts of deionized waters, be warmed up to 60 ℃, stirring and dissolving, then (molecular structure is shown in general formula 1 to drop into 70 parts of 10 parts of butyl acrylates, the random polyoxyethylene thiazolinyl of methoxyl group oxypropylene group ether acrylate, m=50, q=20, z=0), stir;
2) temperature control, at 60 ℃, adds 3.5 parts of Potassium Persulphates in still, stirs 10min;
3) temperature control, at 60 ℃, drips the mixing solutions containing 10 parts of vinylformic acid, 0.9 part of mercaptoethanol and 15 parts of deionized waters, and time for adding is 3h;
4) continue insulation 2h
5) be cooled to 35 ℃～40 ℃, and add 30% liquid caustic soda neutralization, regulating pH value is 5.Be diluted with water to 40% concentration, obtain product VPC-4 of the present invention.
Comparative example 1
In four-hole boiling flask, add 100 parts, prenyl ether, add 100 parts of deionized waters simultaneously, stir rising temperature for dissolving, and be warming up to 60 ℃.Add 2 parts of Potassium Persulphates, then drip respectively the mixed solution of 10 parts of vinylformic acid, 20 parts of deionized waters simultaneously, 50 parts of mixed aqueous solutions that contain 2 parts of 3-thiohydracrylic acids, the about 3h of time for adding.Dropwise rear insulation reaction 2h.Be cooled to 40 ℃, it is 6.5 that the liquid caustic soda that adds 30% concentration is neutralized to pH, makes water reducer PCM.
Comparative example 2
Japan famous brand name product poly carboxylic acid series water reducer HW.
Implementation result
Water reducer of the present invention has been carried out to concrete application performance simultaneous test.
The mix proportion of high-strength concrete that simultaneous test adopts is in table 1, and concrete air content is controlled at 2.0～2.5%, and concrete divergence is controlled at 500～550mm.The method of falling slump cone of employing is tested concrete viscosity, and decay used time of degree of falling cylinder of concrete outflow is less, means that concrete viscosity is less.Under water reducer effect, Properties of High Strength Concrete test-results is in table 2.
Table 2 result shows: controlling under concrete initialization performance uniform condition, with respect to conventional poly carboxylic acid series water reducer PCM and HW, it is significantly less that under the water reducer effect of preparing by the inventive method, concrete flows out the used time of degree of falling cylinder of decaying, and illustrates that the poly carboxylic acid series water reducer of preparing by the inventive method can effectively reduce concrete viscosity.In molecular structure, introduce a certain amount of hydrophobic units polyoxytrimethylene base, polyoxybutylene base, and improve the ratio of hydrophobic grouping, all can play good viscosity reducing effect.
Table 1 mix proportion of high-strength concrete (kg/m
3)
| Water-cement ratio | Cement | Silica flour | Sand | Middle stone | Gravelstone | Water |
| 0.24 | 495 | 55 | 740 | 666 | 444 | 130 |
Properties of High Strength Concrete test under the effect of table 2 water reducer
Although the present invention has enumerated part embodiment openly as above; but they are not for limiting the present invention; anyly be familiar with this skill person; without departing from the spirit and scope of the invention; can make various changes or retouch from working as; for example certain part of feed composition or process time are done to increase or reduce, but the effect of product may not can be produced to substantial effect, within so this change belongs to the scope that the application's claim protection domain defines equally.
Claims (4)
1. a viscosity reduction type poly carboxylic acid series water reducer preparation method, it is characterized in that: this water reducer be with random polyoxyalkylenes ether unsaturated acid ester, unsaturated modification Soxylat A 25-7, unsaturated acid alkyl ester, (methyl) vinylformic acid under initiator and molecular weight regulator effect, add alkali neutralization by aqueous solution copolymerization again and be prepared from, this water reducer molecular structure is as shown in general formula (1):
Wherein, R
1, R
2, R
3identical or different, represent separately H or CH
3;
R
4represent alkyl or aryl or the alkylaryl of H or 1～10 C atom;
X represents the alkyl of 1～4 C atom;
Y
1represent the alkylidene group of 2 C atoms;
Y
2represent the alkylidene group of 3 C atoms;
Y
3represent the alkylidene group of 4 C atoms;
M is 1～100 integer, the integer that n is 20～100, and the integer that q is 0～50, the integer that z is 0～50, and (m+q+z) be 1～200 integer.
2. viscosity reduction type poly carboxylic acid series water reducer preparation method according to claim 1, is characterized in that: the preparation method of this water reducer comprises the following steps:
1) unsaturated modification Soxylat A 25-7 is dissolved in the water, is warming up to 50 ℃～70 ℃, add random polyoxyalkylenes ether unsaturated acid ester and unsaturated acid alkyl ester, then stir;
2) temperature control, at 50 ℃～70 ℃, drops into initiator in still, stirs 10min;
3) temperature control, at 50 ℃～70 ℃, drips the mixing solutions of (methyl) vinylformic acid and molecular weight regulator, and time for adding is 2h～3h;
4) continue insulation 1h～2h;
5) be cooled to 35 ℃～40 ℃, and add liquid caustic soda neutralization, regulating pH value is 5～7.
3. viscosity reduction type poly carboxylic acid series water reducer preparation method according to claim 1 and 2, it is characterized in that: initiator is a kind of or its mixture in ammonium persulphate, Potassium Persulphate, and the consumption weight percent of initiator is 1%～5% of comonomer gross weight.
4. viscosity reduction type poly carboxylic acid series water reducer preparation method according to claim 1 and 2, it is characterized in that: molecular weight regulator is a kind of or its mixture in Thiovanic acid, thiohydracrylic acid, mercaptoethanol, and the consumption of molecular regulation agent (weight percent) is 0.5%～3% of comonomer gross weight.
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Cited By (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105461866A (en) * | 2014-09-05 | 2016-04-06 | 深圳市迈地砼外加剂有限公司 | Viscosity-reducing type polycarboxylic-acid water-reducing agent and preparation method thereof |
| CN105732911A (en) * | 2016-01-15 | 2016-07-06 | 江苏苏博特新材料股份有限公司 | Preparation method and application of viscosity-reducing polycarboxylate superplasticizer |
| CN105924592A (en) * | 2016-06-04 | 2016-09-07 | 石家庄市长安育才建材有限公司 | Viscosity-reduction type polycarboxylate water reducer and preparation method thereof |
| CN106380550A (en) * | 2016-08-27 | 2017-02-08 | 广东红墙新材料股份有限公司 | Surface tension adjustment reduction type polycarboxylate superplasticizer and preparation method thereof |
| CN106496445A (en) * | 2016-11-15 | 2017-03-15 | 湖北工业大学 | A kind of hydrophobic minor comonomer modification viscosity reduction type polycarboxylate water-reducer masterbatch |
| CN106632889A (en) * | 2016-12-27 | 2017-05-10 | 陕西友邦新材料科技有限公司 | Low air-entrained and viscosity-reduced slow-release polycarboxylate water reducer and preparation method thereof |
| CN106927751A (en) * | 2017-03-28 | 2017-07-07 | 南宁市嘉大混凝土有限公司 | A kind of GHPC |
| CN106967200A (en) * | 2017-03-31 | 2017-07-21 | 刘翠芬 | It is a kind of to have poly carboxylic acid series water reducer that guarantor is collapsed with viscosity-reducing performance and preparation method thereof concurrently |
| CN107082891A (en) * | 2017-05-23 | 2017-08-22 | 中国矿业大学 | A kind of hyperbranched poly carboxylic acid water reducer and preparation method |
| CN108003301A (en) * | 2017-11-14 | 2018-05-08 | 佳化化学（茂名）有限公司 | A kind of preparation method of viscosity reduction type polycarboxylate water-reducer |
| CN108084357A (en) * | 2017-11-14 | 2018-05-29 | 佳化化学（茂名）有限公司 | A kind of preparation method of liquid polycarboxylate water-reducer |
| CN108084358A (en) * | 2017-11-14 | 2018-05-29 | 佳化化学（茂名）有限公司 | A kind of preparation method of collapse-preventing type polycarboxylate water-reducer |
| CN112521045A (en) * | 2020-12-10 | 2021-03-19 | 联泓(江苏)新材料研究院有限公司 | Viscosity-reducing liquid phase composition and preparation method and application thereof |
| CN113929837A (en) * | 2021-11-03 | 2022-01-14 | 同济大学 | Shrinkage-reducing polycarboxylic acid water reducer and preparation method and application thereof |
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| CN105461866B (en) * | 2014-09-05 | 2018-04-06 | 深圳市迈地砼外加剂有限公司 | A kind of viscosity reduction type polycarboxylate water-reducer and preparation method thereof |
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| CN105924592A (en) * | 2016-06-04 | 2016-09-07 | 石家庄市长安育才建材有限公司 | Viscosity-reduction type polycarboxylate water reducer and preparation method thereof |
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| CN106927751A (en) * | 2017-03-28 | 2017-07-07 | 南宁市嘉大混凝土有限公司 | A kind of GHPC |
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| CN106967200A (en) * | 2017-03-31 | 2017-07-21 | 刘翠芬 | It is a kind of to have poly carboxylic acid series water reducer that guarantor is collapsed with viscosity-reducing performance and preparation method thereof concurrently |
| CN107082891A (en) * | 2017-05-23 | 2017-08-22 | 中国矿业大学 | A kind of hyperbranched poly carboxylic acid water reducer and preparation method |
| CN108084358A (en) * | 2017-11-14 | 2018-05-29 | 佳化化学（茂名）有限公司 | A kind of preparation method of collapse-preventing type polycarboxylate water-reducer |
| CN108084357A (en) * | 2017-11-14 | 2018-05-29 | 佳化化学（茂名）有限公司 | A kind of preparation method of liquid polycarboxylate water-reducer |
| CN108003301A (en) * | 2017-11-14 | 2018-05-08 | 佳化化学（茂名）有限公司 | A kind of preparation method of viscosity reduction type polycarboxylate water-reducer |
| CN112521045A (en) * | 2020-12-10 | 2021-03-19 | 联泓(江苏)新材料研究院有限公司 | Viscosity-reducing liquid phase composition and preparation method and application thereof |
| CN113929837A (en) * | 2021-11-03 | 2022-01-14 | 同济大学 | Shrinkage-reducing polycarboxylic acid water reducer and preparation method and application thereof |
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Application publication date: 20140618 |