CN104448156A - Room-temperature preparation method for high-efficiency polycarboxylic acid water reducing agent - Google Patents
Room-temperature preparation method for high-efficiency polycarboxylic acid water reducing agent Download PDFInfo
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- CN104448156A CN104448156A CN201410673602.3A CN201410673602A CN104448156A CN 104448156 A CN104448156 A CN 104448156A CN 201410673602 A CN201410673602 A CN 201410673602A CN 104448156 A CN104448156 A CN 104448156A
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- polycarboxylic acid
- water
- room temperature
- efficiency polycarboxylic
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 65
- 239000003638 chemical reducing agent Substances 0.000 title claims abstract description 46
- 239000002253 acid Substances 0.000 title claims abstract description 27
- 238000002360 preparation method Methods 0.000 title claims abstract description 20
- 239000008367 deionised water Substances 0.000 claims abstract description 24
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 24
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims abstract description 15
- XWGJFPHUCFXLBL-UHFFFAOYSA-M rongalite Chemical compound [Na+].OCS([O-])=O XWGJFPHUCFXLBL-UHFFFAOYSA-M 0.000 claims abstract description 13
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 6
- 238000010526 radical polymerization reaction Methods 0.000 claims abstract description 6
- 239000000178 monomer Substances 0.000 claims abstract description 5
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 33
- XBDQKXXYIPTUBI-UHFFFAOYSA-N dimethylselenoniopropionate Natural products CCC(O)=O XBDQKXXYIPTUBI-UHFFFAOYSA-N 0.000 claims description 18
- 239000007788 liquid Substances 0.000 claims description 14
- 238000006243 chemical reaction Methods 0.000 claims description 11
- 125000005395 methacrylic acid group Chemical group 0.000 claims description 11
- 239000002994 raw material Substances 0.000 claims description 11
- 235000011121 sodium hydroxide Nutrition 0.000 claims description 11
- 239000000463 material Substances 0.000 claims description 9
- 235000019260 propionic acid Nutrition 0.000 claims description 9
- 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 9
- 238000003756 stirring Methods 0.000 claims description 9
- 230000002829 reductive effect Effects 0.000 claims description 4
- 239000012986 chain transfer agent Substances 0.000 claims description 2
- 238000002156 mixing Methods 0.000 claims description 2
- 238000005516 engineering process Methods 0.000 abstract description 3
- 230000015572 biosynthetic process Effects 0.000 abstract description 2
- 239000004566 building material Substances 0.000 abstract description 2
- 238000005265 energy consumption Methods 0.000 abstract description 2
- 238000003786 synthesis reaction Methods 0.000 abstract description 2
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 abstract 4
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 abstract 2
- 230000033116 oxidation-reduction process Effects 0.000 abstract 1
- 238000010189 synthetic method Methods 0.000 abstract 1
- 229920005646 polycarboxylate Polymers 0.000 description 8
- 229910052739 hydrogen Inorganic materials 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 5
- 239000003599 detergent Substances 0.000 description 5
- 238000009413 insulation Methods 0.000 description 5
- 230000001603 reducing effect Effects 0.000 description 4
- UFWIBTONFRDIAS-UHFFFAOYSA-N Naphthalene Chemical compound C1=CC=CC2=CC=CC=C21 UFWIBTONFRDIAS-UHFFFAOYSA-N 0.000 description 2
- 150000001735 carboxylic acids Chemical class 0.000 description 2
- 239000004568 cement Substances 0.000 description 2
- 238000000034 method Methods 0.000 description 2
- 230000035484 reaction time Effects 0.000 description 2
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- 239000004721 Polyphenylene oxide Substances 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000011575 calcium Substances 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 235000003891 ferrous sulphate Nutrition 0.000 description 1
- 239000011790 ferrous sulphate Substances 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- BAUYGSIQEAFULO-UHFFFAOYSA-L iron(2+) sulfate (anhydrous) Chemical compound [Fe+2].[O-]S([O-])(=O)=O BAUYGSIQEAFULO-UHFFFAOYSA-L 0.000 description 1
- 229910000359 iron(II) sulfate Inorganic materials 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229920000570 polyether Polymers 0.000 description 1
- 238000010517 secondary reaction Methods 0.000 description 1
- 238000001308 synthesis method Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Landscapes
- Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)
- Macromonomer-Based Addition Polymer (AREA)
Abstract
The invention relates to the technical field of building material admixtures, in particular to a room-temperature preparation method for a high-efficiency polycarboxylic acid water reducing agent. The preparation method adopts methyl allyl polyethenoxy ether and acrylic acid as reactive monomers, and adopts hydrogen peroxide as an oxide agent and sodium formaldehyde sulfoxylate as a reducing agent to build an oxidation-reduction system. The specific synthetic method comprises the following steps: adopting methyl allyl polyethenoxy ether, hydrogen peroxide and deionized water as a base solution; dropwise adding a water solution A of acrylic acid and a chain transferring agent, and a water solution B of sodium formaldehyde sulfoxylate; enabling radical polymerization reaction at room temperature. The preparation method can be carried out for synthesis at the room temperature, and is economical, environment-friendly, low in energy consumption and simple in preparation technology, and the synthesized water reducing agent is high in water-reducing rate, good in fluidity and good in slump retaining performance.
Description
Technical field
The present invention relates to additive for building material technical field, especially relate to a kind of room temperature preparation method of High-efficiency polycarboxylic acid water reducer.
Background technology
Along with the development of building trade, in engineer applied, the requirement of water reducer is progressively improved.The poly carboxylic acid series water reducer grown up in recent years is known as both at home and abroad continue the first-generation water reducer being representative with wooden calcium and the third generation high-performance water reducing agent grown up after with naphthalene being the s-generation water reducer of representative.The advantages such as polycarboxylate water-reducer is high because of its water-reducing rate, adaptability is better, obtain great propagation and employment.
Chinese patent (CN103275280A) discloses a kind of normal temperature synthesis method of polyocarboxy acid type high-thin arch dam water reducer, be raw material by unsaturated polyether, unsaturated carboxylic acid, by the foundation of redox system, polycarboxylic acid water reducing agent has been synthesized under room temperature, but the low conversion rate of the method product, long reaction time.Therefore, seek a kind ofly at room temperature can to synthesize, technique is simply controlled and preparation method that is High-efficiency polycarboxylic acid water reducer efficiently is extremely urgent.
Summary of the invention
For the problems referred to above, the invention provides a kind of room temperature preparation method of High-efficiency polycarboxylic acid water reducer, this water reducer at room temperature can synthesize, and reaction required time is short, and products obtained therefrom water-reducing rate is high, function of slump protection good, product performance are stable.
Technical scheme of the present invention is:
The invention provides a kind of room temperature preparation method of High-efficiency polycarboxylic acid water reducer, reaction monomers is carried out according to the following steps by radical polymerization:
A. monomer methacrylic Soxylat A 25-7, oxygenant 30% hydrogen peroxide and deionized water are dropped in reactor as bed material, be stirred to and dissolve completely;
B. bed material drips the good solution A of configured in advance and solution B after dissolving simultaneously, and solution A was added dropwise to complete through 1 hour, and solution B was added dropwise to complete through 1.5 hours, and solution B continues stirring reaction 30 minutes after dripping and terminating;
C. by above-mentioned mixing solutions mass concentration be 32% liquid caustic soda regulate pH value be 6-7, rear continuation stirs 20 minutes, obtains described High-efficiency polycarboxylic acid water reducer;
Described solution A is monomeric acrylic, chain-transfer agent dredges base propionic acid and deionized water;
Described solution B is reductive agent rongalite and deionized water.
Described radical polymerization system is made up of following raw material: methacrylic Soxylat A 25-7 280-330,30% hydrogen peroxide (30%H
2o
2) 2.5-4.5 part, vinylformic acid (AA) 40-52 part, dredge base propionic acid 1.2-2.0, rongalite 1.2-2;
Described deionized water quality is 1.5-2.5 times of each raw material total mass.
The molecular weight of described methacrylic Soxylat A 25-7 is 2000-2400.
Described liquid caustic soda is aqueous sodium hydroxide solution.
30% described hydrogen peroxide to be mass concentration be 30% aqueous hydrogen peroxide solution.
The present invention is by adopting redox system, cause radical polymerization, reaction can at room temperature be carried out, rongalite has strong reducing property, can prevent hydroxyl too much in water reducer from causing cement to be adsorbed instantaneously, improve concrete slump retention ability, by the proportion relation of adjustment oxygenant with reductive agent, determine each monomer consumption, improve transformation efficiency, prevent the waste of raw material from also effectively controlling the generation of high temperature secondary reaction.This water reducer has high water reducing rate, and function of slump protection is good, applied widely, is applicable to industrialization scale operation.
Advantage of the present invention and beneficial effect:
1. the present invention is by the foundation of redox system, adds strong reducing property rongalite, and at room temperature can synthesize, energy consumption is little, economic environmental protection.
2. preparation technology of the present invention is simple, and the water reducer of synthesis has high water reducing rate, and degree of mobilization, function of slump protection are 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 High-efficiency polycarboxylic acid water reducer, is made up of the raw material of following weight part:
Bed material: methacrylic Soxylat A 25-7: 280,30%H
2o
2: 2.6, deionized water: 280;
Solution A: AA:40, thin base propionic acid: 1.2, deionized water: 65;
Solution B: rongalite: 1.25, deionized water: 165.
A kind of preparation method of High-efficiency polycarboxylic acid water reducer: under room temperature condition, drips solution A in end liquid, and time for adding is 1 hour, and in end liquid, drip solution B, time for adding is 1.5 hours simultaneously; After being added dropwise to complete, insulation continues reaction 30 minutes, the mass concentration then adding 22-30 weight part be 32% aqueous sodium hydroxide solution regulate pH value to be 6-7, continue stirring 20 minutes, both described heavy duty detergent polycarboxylate water-reducer.
Embodiment 2
A kind of High-efficiency polycarboxylic acid water reducer, is made up of the raw material of following weight part:
Bed material: methacrylic Soxylat A 25-7: 293,30%H
2o
2: 3.0, deionized water: 300;
Solution A: AA:43.5, thin base propionic acid: 1.45, deionized water: 75;
Solution B: rongalite: 1.5, deionized water: 170.
A kind of preparation method of High-efficiency polycarboxylic acid water reducer: under room temperature condition, drips solution A in end liquid, and time for adding is 1 hour, and in end liquid, drip solution B, time for adding is 1.5 hours simultaneously; After being added dropwise to complete, insulation continues reaction 30 minutes, the mass concentration then adding 22-30 weight part be 32% aqueous sodium hydroxide solution regulate pH value to be 6-7, continue stirring 20 minutes, both described heavy duty detergent polycarboxylate water-reducer.
Embodiment 3
A kind of High-efficiency polycarboxylic acid water reducer, is made up of the raw material of following weight part:
Bed material: methacrylic Soxylat A 25-7: 306,30%H
2o
2: 3.56, deionized water: 315;
Solution A: AA:46.8, thin base propionic acid: 1.7, deionized water: 88;
Solution B: rongalite: 1.63, deionized water: 182.
A kind of preparation method of High-efficiency polycarboxylic acid water reducer: under room temperature condition, drips solution A in end liquid, and time for adding is 1 hour, and in end liquid, drip solution B, time for adding is 1.5 hours simultaneously; After being added dropwise to complete, insulation continues reaction 30 minutes, the mass concentration then adding 22-30 weight part be 32% aqueous sodium hydroxide solution regulate pH value to be 6-7, continue stirring 20 minutes, both described heavy duty detergent polycarboxylate water-reducer.
Embodiment 4
A kind of High-efficiency polycarboxylic acid water reducer, is made up of the raw material of following weight part:
Bed material: methacrylic Soxylat A 25-7: 319,30%H
2o
2: 4.2, deionized water: 335;
Solution A: AA:49.2, thin base propionic acid: 1.85, deionized water: 95;
Solution B: rongalite: 1.79, deionized water: 200.
A kind of preparation method of High-efficiency polycarboxylic acid water reducer: under room temperature condition, drips solution A in end liquid, and time for adding is 1 hour, and in end liquid, drip solution B, time for adding is 1.5 hours simultaneously; After being added dropwise to complete, insulation continues reaction 30 minutes, the mass concentration then adding 22-30 weight part be 32% aqueous sodium hydroxide solution regulate pH value to be 6-7, continue stirring 20 minutes, both described heavy duty detergent polycarboxylate water-reducer.
Embodiment 5
A kind of High-efficiency polycarboxylic acid water reducer, is made up of the raw material of following weight part:
Bed material: methacrylic Soxylat A 25-7: 330,30%H
2o
2: 4.45, deionized water: 350;
Solution A: AA:52, thin base propionic acid: 1.9, deionized water: 110;
Solution B: rongalite: 2.0, deionized water: 210.
A kind of preparation method of High-efficiency polycarboxylic acid water reducer: under room temperature condition, drips solution A in end liquid, and time for adding is 1 hour, and in end liquid, drip solution B, time for adding is 1.5 hours simultaneously; After being added dropwise to complete, insulation continues reaction 30 minutes, then add mass concentration be 32% aqueous sodium hydroxide solution regulate pH value to be 6-7, continue stirring 20 minutes, both described heavy duty detergent polycarboxylate water-reducer.
Comparative example 1: this polycarboxylate water-reducer adopts ferrous sulfate as reductive agent, and other steps are identical with embodiment 3.
Comparative example 2: contrast product is commercially available polycarboxylate water-reducer
Find through Experimental Comparison, 3 hours longer than the present invention of reaction times needed for comparative example 1, product income rate is low.
Application Example
Adopt reference cement, according to the test request in " concrete admixture " (GB8076-2008), compare High-efficiency polycarboxylic acid water reducer (embodiment 1-5) 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 the table, High-efficiency polycarboxylic acid water reducer prepared by the present invention has that degree of mobilization is large, water-reducing rate is high, the excellent feature of function of slump protection.
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 room temperature preparation method for High-efficiency polycarboxylic acid water reducer, is characterized in that, is carried out according to the following steps by radical polymerization:
A. monomer methacrylic Soxylat A 25-7, oxygenant 30% hydrogen peroxide and deionized water are dropped in reactor as bed material, be stirred to and dissolve completely;
B. bed material drips the good solution A of configured in advance and solution B after dissolving simultaneously, and solution A was added dropwise to complete through 1 hour, and solution B was added dropwise to complete through 1.5 hours, and solution B continues stirring reaction 30 minutes after dripping and terminating;
C. by above-mentioned mixing solutions mass concentration be 32% liquid caustic soda regulate pH value be 6-7, rear continuation stirs 20 minutes, obtains described High-efficiency polycarboxylic acid water reducer;
Described solution A is monomeric acrylic, chain-transfer agent dredges base propionic acid and deionized water;
Described solution B is reductive agent rongalite and deionized water.
2. the room temperature preparation method of High-efficiency polycarboxylic acid water reducer according to claim 1, it is characterized in that, described radical polymerization system is made up of the raw material of following weight part:: methacrylic Soxylat A 25-7 280-330,30% hydrogen peroxide 2.5-4.5 part, vinylformic acid (AA) 40-52 part, thin base propionic acid 1.2-2.0, rongalite 1.2-2;
Described deionized water quality is 1.5-2.5 times of each raw material total mass.
3. the room temperature preparation method of the High-efficiency polycarboxylic acid water reducer according to any one of claim 1-2, is characterized in that: the molecular weight of described methacrylic Soxylat A 25-7 is 2000-2400.
4. the room temperature preparation method of High-efficiency polycarboxylic acid water reducer according to claim 1, is characterized in that: described liquid caustic soda is aqueous sodium hydroxide solution.
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| CN105037648A (en) * | 2015-08-25 | 2015-11-11 | 科之杰新材料集团有限公司 | Slump-retaining water-reducing polycarboxylic acid water reducing agent and low-temperature quick preparation method thereof |
| CN105330193A (en) * | 2015-11-24 | 2016-02-17 | 同济大学 | Polycarboxylate water reducer for ultra-compact concrete for nuclear power and preparation method of polycarboxylate water reducer |
| CN105418856A (en) * | 2015-12-18 | 2016-03-23 | 中建商品混凝土有限公司 | Preparation method of synthesis of polycarboxylate superplasticizer at room temperature in wide temperature range |
| CN105524230A (en) * | 2015-12-24 | 2016-04-27 | 湖南铭煌科技发展有限公司 | Preparation method of polycarboxylate superplasticizer |
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| CN106632742A (en) * | 2016-12-30 | 2017-05-10 | 长沙加美乐素化工有限公司 | Composite activator system and method for preparing concrete water-reducing admixture from same |
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