CN102060464B - Polycarboxylate water reducing agent by using water as solvent and preparation method thereof - Google Patents
Polycarboxylate water reducing agent by using water as solvent 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 45
- 229920005646 polycarboxylate Polymers 0.000 title claims abstract description 31
- 238000002360 preparation method Methods 0.000 title claims abstract description 29
- 239000003638 chemical reducing agent Substances 0.000 title abstract description 18
- 239000002904 solvent Substances 0.000 title description 4
- 239000000178 monomer Substances 0.000 claims abstract description 42
- 239000003999 initiator Substances 0.000 claims abstract description 20
- 238000000034 method Methods 0.000 claims abstract description 13
- 239000008367 deionised water Substances 0.000 claims description 18
- 229910021641 deionized water Inorganic materials 0.000 claims description 18
- 125000004435 hydrogen atom Chemical group [H]* 0.000 claims description 13
- 238000009835 boiling Methods 0.000 claims description 10
- -1 alkali metal cation Chemical class 0.000 claims description 8
- FPYJFEHAWHCUMM-UHFFFAOYSA-N maleic anhydride Chemical compound O=C1OC(=O)C=C1 FPYJFEHAWHCUMM-UHFFFAOYSA-N 0.000 claims description 7
- NIXOWILDQLNWCW-UHFFFAOYSA-N acrylic acid group Chemical group C(C=C)(=O)O NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims description 6
- JPAOMENBKRZQDR-UHFFFAOYSA-N CC=CC.[Na] Chemical group CC=CC.[Na] JPAOMENBKRZQDR-UHFFFAOYSA-N 0.000 claims description 4
- CERQOIWHTDAKMF-UHFFFAOYSA-N Methacrylic acid Chemical group CC(=C)C(O)=O CERQOIWHTDAKMF-UHFFFAOYSA-N 0.000 claims description 4
- 239000002253 acid Substances 0.000 claims description 4
- 239000003513 alkali Substances 0.000 claims description 4
- BDHFUVZGWQCTTF-UHFFFAOYSA-M sulfonate Chemical compound [O-]S(=O)=O BDHFUVZGWQCTTF-UHFFFAOYSA-M 0.000 claims description 4
- JHUFGBSGINLPOW-UHFFFAOYSA-N 3-chloro-4-(trifluoromethoxy)benzoyl cyanide Chemical compound FC(F)(F)OC1=CC=C(C(=O)C#N)C=C1Cl JHUFGBSGINLPOW-UHFFFAOYSA-N 0.000 claims description 3
- 229910052783 alkali metal Inorganic materials 0.000 claims description 3
- 238000009413 insulation Methods 0.000 claims description 3
- JRZJOMJEPLMPRA-UHFFFAOYSA-N olefin Natural products CCCCCCCC=C JRZJOMJEPLMPRA-UHFFFAOYSA-N 0.000 claims description 3
- ATVJXMYDOSMEPO-UHFFFAOYSA-N 3-prop-2-enoxyprop-1-ene Chemical class C=CCOCC=C ATVJXMYDOSMEPO-UHFFFAOYSA-N 0.000 claims description 2
- 150000001875 compounds Chemical class 0.000 claims description 2
- 230000000694 effects Effects 0.000 claims description 2
- 125000000864 peroxy group Chemical group O(O*)* 0.000 claims description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims 1
- 125000000217 alkyl group Chemical group 0.000 claims 1
- 239000004567 concrete Substances 0.000 abstract description 14
- 230000008901 benefit Effects 0.000 abstract description 4
- 239000004566 building material Substances 0.000 abstract description 2
- 238000006116 polymerization reaction Methods 0.000 abstract 1
- 238000003786 synthesis reaction Methods 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 23
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 22
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 18
- 125000003903 2-propenyl group Chemical group [H]C([*])([H])C([H])=C([H])[H] 0.000 description 11
- 229920000151 polyglycol Polymers 0.000 description 10
- 239000010695 polyglycol Substances 0.000 description 10
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 description 9
- 239000004568 cement Substances 0.000 description 9
- 238000005516 engineering process Methods 0.000 description 6
- 239000004570 mortar (masonry) Substances 0.000 description 6
- 238000012360 testing method Methods 0.000 description 6
- 239000004160 Ammonium persulphate Substances 0.000 description 5
- 235000019395 ammonium persulphate Nutrition 0.000 description 5
- HRPVXLWXLXDGHG-UHFFFAOYSA-N Acrylamide Chemical compound NC(=O)C=C HRPVXLWXLXDGHG-UHFFFAOYSA-N 0.000 description 4
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- 239000000047 product Substances 0.000 description 4
- 239000007787 solid Substances 0.000 description 4
- 239000007864 aqueous solution Substances 0.000 description 3
- 150000001732 carboxylic acid derivatives Chemical class 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 3
- 238000003756 stirring Methods 0.000 description 3
- LDHQCZJRKDOVOX-UHFFFAOYSA-N 2-butenoic acid Chemical compound CC=CC(O)=O LDHQCZJRKDOVOX-UHFFFAOYSA-N 0.000 description 2
- 150000007513 acids Chemical class 0.000 description 2
- 229910001870 ammonium persulfate Inorganic materials 0.000 description 2
- LYCAIKOWRPUZTN-UHFFFAOYSA-N ethylene glycol Natural products OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 2
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 description 2
- 229920001427 mPEG Polymers 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 229920000098 polyolefin Polymers 0.000 description 2
- 238000010926 purge Methods 0.000 description 2
- 239000004576 sand Substances 0.000 description 2
- 239000002002 slurry Substances 0.000 description 2
- 0 *C(C(N*)=O)=C Chemical compound *C(C(N*)=O)=C 0.000 description 1
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 description 1
- OMIGHNLMNHATMP-UHFFFAOYSA-N 2-hydroxyethyl prop-2-enoate Chemical compound OCCOC(=O)C=C OMIGHNLMNHATMP-UHFFFAOYSA-N 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- BAPJBEWLBFYGME-UHFFFAOYSA-N Methyl acrylate Chemical compound COC(=O)C=C BAPJBEWLBFYGME-UHFFFAOYSA-N 0.000 description 1
- 229920002472 Starch Polymers 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 239000012986 chain transfer agent Substances 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 230000015271 coagulation Effects 0.000 description 1
- 238000005345 coagulation Methods 0.000 description 1
- 230000006835 compression Effects 0.000 description 1
- 238000007906 compression Methods 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 230000001143 conditioned effect Effects 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 229920001577 copolymer Polymers 0.000 description 1
- 238000007334 copolymerization reaction Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 239000002612 dispersion medium Substances 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 230000032050 esterification Effects 0.000 description 1
- 238000005886 esterification reaction Methods 0.000 description 1
- DNJIEGIFACGWOD-UHFFFAOYSA-N ethyl mercaptane Natural products CCS DNJIEGIFACGWOD-UHFFFAOYSA-N 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 238000010528 free radical solution polymerization reaction Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000002440 industrial waste Substances 0.000 description 1
- 230000000977 initiatory effect Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 1
- JRKICGRDRMAZLK-UHFFFAOYSA-L persulfate group Chemical group S(=O)(=O)([O-])OOS(=O)(=O)[O-] JRKICGRDRMAZLK-UHFFFAOYSA-L 0.000 description 1
- 229920001515 polyalkylene glycol Polymers 0.000 description 1
- 230000037048 polymerization activity Effects 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- UIIIBRHUICCMAI-UHFFFAOYSA-N prop-2-ene-1-sulfonic acid Chemical class OS(=O)(=O)CC=C UIIIBRHUICCMAI-UHFFFAOYSA-N 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000012266 salt solution Substances 0.000 description 1
- 235000019698 starch Nutrition 0.000 description 1
- 239000008107 starch Substances 0.000 description 1
- 238000010025 steaming Methods 0.000 description 1
- 239000004575 stone Substances 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 238000010792 warming Methods 0.000 description 1
- DGVVWUTYPXICAM-UHFFFAOYSA-N β‐Mercaptoethanol Chemical compound OCCS DGVVWUTYPXICAM-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B24/00—Use of organic materials as active ingredients for mortars, concrete or artificial stone, e.g. plasticisers
- C04B24/24—Macromolecular compounds
- C04B24/26—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
- C04B24/2641—Polyacrylates; Polymethacrylates
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Organic Chemistry (AREA)
- Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)
Abstract
The invention belongs to the technical fields of building materials and chemical synthesis, and particularly relates to a polycarboxylate water reducing agent prepared by a one-step method and a preparation process thereof. The efficient polycarboxylate water reducing agent is obtained by directly dripping monomers a, b, c, d and e and performing polymerization reaction on initiator solution. The water reducing agent can be widely applied in various concrete projects, and has the advantages of high water reducing rate, good slump holding performance and the like. The method is simple, environmentally-friendly and easy to control, and has good social and economic benefits.
Description
Technical field:
The invention belongs to additive for building material and chemosynthesis technical field, be specifically related to a kind of polycarboxylate dehydragent and preparation technology thereof by the single stage method preparation.
Background technology:
Water reducer is consumption maximum application admixture kind the most widely in the concrete works, and its consumption accounts for more than 80% of the total consumption of admixture.Polycarboxylate dehydragent is little because of its volume, water-reducing rate is high, protect the extensive approval that the advantages such as performance is good of collapsing are received the coagulation pedosphere gradually.Particularly since 2005, be accompanied by railway to the appearance with the admixture regulation of motorway, Line for Passenger Transportation, polycarboxylate dehydragent has all been used in this field, its year usage quantity reach 500,000 tons.In China's other engineering of fundamental construction concrete, also begin to promote the use of polycarboxylate dehydragent as water power, highway, concrete civilian, Industrial buildings at present.Because its excellent performance, market outlook are wide, also become in recent years focus about the research of polycarboxylate dehydragent.Polycarboxylate water-reducer generally all is methoxy poly (ethylene glycol) (methyl) acrylate that obtains to have polymerization activity by methoxy poly (ethylene glycol) and (methyl) vinylformic acid elder generation esterification at present, adopt solution polymerization process and the copolymerization of (methyl) vinylformic acid isoreactivity group to form again, there is complicated process of preparation, influence factor is more, the cost height, shortcomings such as quality instability.Patent CN 101041571A discloses a kind of air entrained collapse-preventing type polycarboxylate concrete high efficiency water reducing agent and preparation thereof, polyalkylene glycol mono body and carboxylic-acid monomer are joined in the reactor that the condensation part flow arrangement is housed, add stopper, catalyzer, solvent, stir, be warming up to 85-125 ℃, reacted 5-15 hour, desolventize and reclaim by the underpressure distillation steaming, namely get the polyalkene glycol acrylates class monomer that contains excess carboxylic acid class monomer, with gained polyalkene glycol acrylates class monomer, the mixture of carboxylic-acid monomer and allyl sulphonic acid class monomer adds water and is made into the aqueous solution, persulphate adds water and is made into initiator solution, in reactor, add water and be dispersion medium, stir, be warmed up to 75-95 ℃, add monomer solution and initiator solution, reacted 4-8 hour, cooling adds alkali with the gained multipolymer and is neutralized to 6.5-8, namely gets copolymer salt solution.Make in the big monomer process in the first step, add catalyzer, stopper and band aqua, not only increase cost and can bring the impurity complex process into restive; CN 101353397A has introduced a kind of water-soluble grafting polycarboxylic acids dehydragent and preparation method thereof, at first allyl polyethenoxy alcohol ether monomer is added in the reactor, add deionized water and make its dissolving, use the nitrogen purging reactor while stirring to heat up, when being warmed up to 60-120 ℃, mixed aqueous solution and 10% ammonium persulfate aqueous solution of while dropwise addition of acrylic acid monomer and Hydroxyethyl acrylate monomer, dropwise insulation 1-3 hour, cool to 25-55 ℃, adding alkali accent pH value is that 6.0-7.0 namely gets described product, the raw materials used cost of this method is higher, and reaction process needs nitrogen purging, the technology relative complex.CN 101215119A discloses a kind of high-performance polycarboxylic acids water reducing agent that adopts the single stage method preparation, in inert atmosphere, monomer A and monomers B in water, are reacted under the initiation of initiator, the pH value that adopts sodium hydroxide conditioned reaction product then is 4.5-7, get final product target product.Though reaction process is simple, as chain-transfer agent, has unpleasant irritating smell with mercaptoethanol.
Summary of the invention:
The objective of the invention is the problem at existing water reducer technology of preparing existence, a kind of polycarboxylate dehydragent and method preparation technology simple, with low cost of excellent performance is provided.
For achieving the above object, the present invention is by the following technical solutions:
Polycarboxylate dehydragent of the present invention is characterized in that: by following a, b, c, d, five kinds of monomers of e according to a certain ratio under the initiator effect copolyreaction make:
The a maleic anhydride:
The b acrylic monomer:
R wherein
1Expression hydrogen atom or methyl.
C allyl ether series monomer
R3 represents hydrogen atom or C
1-3Alkyl, n represents number of repeat unit, its value is for 10-80;
The d aminated compounds
R
4Expression hydrogen atom or C
1-3Alkane; R
5Expression hydrogen atom or C
1-3Alkyl or C
1-8Alkylsulphonic acid;
E olefin sulfonic acid class monomer
R
6Expression hydrogen atom or C
1-3Alkyl, M represents hydrogen atom or alkali metal cation;
Above-mentioned monomer molar proportioning: a: b: c: d: e is 1: 0.5-2.0: 0.3-2.0: 0.3-1.5: 0.1-0.5.
The preparation method of polycarboxylate dehydragent of the present invention is as follows:
(1) in four-hole boiling flask, adds monomer a, e and a part of monomer c, add a certain amount of deionized water and make its dissolving and be heated to 50-100 ℃.
(2) drip monomer b, c, d solution and the initiator solution for preparing in advance respectively in four-hole boiling flask, 2-6h drips off, insulation 1-5h.
(3) be cooled to 25-45 ℃, add alkali and be neutralized to PH=7.0 ± 0.5, both described polycarboxylate dehydragent.Described initiator is inorganic peroxy class initiator, initiator system of ammonium persulfate, and consumption is the 1-8% of monomer total amount.The monomer solution concentration of preparation is 30-80%, and initiator solution concentration is 1-20%.
Polycarboxylate dehydragent of the present invention, it is 0.2% o'clock of gelling material at the solid volume of folding, concrete water-reducing ratio can reach more than 30%, 28d ultimate compression strength can be brought up to more than 140, the product cement adaptability is good, be applicable to the cement of multiple different manufacturers, specification, model, stable performance, long storage does not have precipitation, not stratified.
Polycarboxylate dehydragent preparation technology of the present invention is very simple, and reaction conditions is easy to control, and production process does not produce three industrial wastes, and directly water is as solvent, and cost is low, energy consumption is low, has both guaranteed economic benefit, again non-environmental-pollution.
Embodiment:
Embodiment 1
Add 19.61g maleic anhydride, 100g molecular weight in the four-hole boiling flask and be 2000 allyl polyglycol ether and the sodium allyl sulfonate of 5.76g, add deionized water dissolving.Heat to 75 ℃, drip respectively by the 100g molecular weight is the monomer solution of 2000 allyl polyglycol ether, 17.22g methacrylic acid and 14.2g acrylamide and deionized water preparation, with the initiator solution by 3g ammonium persulphate and deionized water preparation, dropwised in 3 hours, be incubated after 2 hours, cool to 30 ℃, with the 30% sodium hydroxide solution Ph=7.0 that neutralizes, namely get polycarboxylate dehydragent PC-1.
Embodiment 2
Add 19.61g maleic anhydride, 100g molecular weight in the four-hole boiling flask and be 2000 allyl polyglycol ether and the sodium allyl sulfonate of 14.4g, add deionized water dissolving.Heat to 85 ℃, drip respectively by the 100g molecular weight is the monomer solution of 2000 allyl polyglycol ether, 14.4g vinylformic acid and 20.07g2-acrylamido-2-methyl propane sulfonic acid and deionized water preparation, with the initiator solution by 5g ammonium persulphate and deionized water preparation, dropwised in 3 hours, be incubated after 2 hours, cool to 30 ℃, with the 40% sodium hydroxide solution Ph=7.0 that neutralizes, namely get polycarboxylate dehydragent PC-2.
Embodiment 3
Add 19.61g maleic anhydride, 120g molecular weight in the four-hole boiling flask and be 2400 allyl polyglycol ether and the methylpropene sodium sulfonate of 12.6g, add deionized water dissolving.Heat to 70 ℃, drip respectively by the 120g molecular weight is the monomer solution of 2400 allyl polyglycol ether, 17.29g vinylformic acid and 5.68g acrylamide and deionized water preparation, with the initiator solution by 8g ammonium persulphate and deionized water preparation, dropwised in 2 hours, be incubated after 2 hours, cool to 30 ℃, with the 40% sodium hydroxide solution Ph=7.0 that neutralizes, namely get polycarboxylate dehydragent PC-3.
Embodiment 4
Add 19.61g maleic anhydride, 72g molecular weight in the four-hole boiling flask and be 2400 allyl polyglycol ether and the methylpropene sodium sulfonate of 9.49g, add deionized water dissolving.Heat to 90 ℃, drip respectively by the 72g molecular weight is the monomer solution of 2400 allyl polyglycol ether, 25.8g methacrylic acid and 7.1g acrylamide and deionized water preparation, with the initiator solution by 10g ammonium persulphate and deionized water preparation, dropwised in 3 hours, be incubated after 1 hour, cool to 30 ℃, with the 40% sodium hydroxide solution Ph=7.0 that neutralizes, namely get polycarboxylate dehydragent PC-4.
Embodiment 5
Add 19.61g maleic anhydride, 144g molecular weight in the four-hole boiling flask and be 4800 allyl polyglycol ether and the methylpropene sodium sulfonate of 9.49g, add deionized water dissolving.Heat to 95 ℃, drip respectively by the 144g molecular weight is the monomer solution of 4800 allyl polyglycol ether, 25.8g methacrylic acid and 7.1g acrylamide and deionized water preparation, with the initiator solution by 10g ammonium persulphate and deionized water preparation, dropwised in 3 hours, be incubated after 1 hour, cool to 30 ℃, with the 40% sodium hydroxide solution Ph=7.0 that neutralizes, namely get polycarboxylate dehydragent PC-5.
Test example 1
Water reducer PC-1, the PC-2 that the present invention is made, PC-3, PC-4, PC-5 and two kinds of commercially available water reducer SS-1, SS-2 measure indexs such as their clean slurry degree of mobilization, mortar water-reducing rate, concrete water-reducing ratio respectively, flowing degree of net paste of cement is with reference to GB/T8077-2000 " Methods for testing uniformity of concrete admixture ", water reducer volume (by solid content) is cement total amount 0.2%, water 87g (comprising the institute of water reducer water content own).The mortar water-reducing rate is controlled mortar degree of mobilization (180 ± 5) mm with reference to GB/T8077-2000 " Methods for testing uniformity of concrete admixture ", and water reducer volume (by solid content) is cement total amount 0.2%.Concrete test is with reference to GB8076-1997 " concrete admixture " standard detection.Every side's cement consumption for the 330kg/m3 concrete mix is: m (cement): m (sand): m (stone)=1: 2.34: 3.50, and sand coarse aggregate ratio 40%, water reducer volume (by solid content) is cement total amount 0.2%.Test-results such as following table 1 and table 2.
The different water reducers of table 1 are to the influence of flowing degree of net paste of cement and mortar water-reducing rate
| The water reducer model | Clean slurry degree of mobilization/mm | Mortar water-reducing rate/% |
| PC-1 | 260 | 19.86 |
| PC-2 | 265 | 20.04 |
| PC-3 | 240 | 18.54 |
| PC-4 | 255 | 18.60 |
| PC-5 | 268 | 20.70 |
| SS-1 | 235 | 18.60 |
| SS-2 | 255 | 17.83 |
Table 2 concrete test result
Test shows, adopt the polycarboxylate dehydragent of preparation in example 1 of the present invention and the example 4, starch degree of mobilization and mortar water-reducing rate only and all be higher than commercially available two kinds of products, the concrete amount of air entrainment is lower, water-reducing rate and each phase intensity are all higher, say that totally performance is better than commercially available water reducer SS-1, SS-2.
Claims (7)
1. polycarboxylate dehydragent that adopts single stage method preparation is characterized in that: by following a, b, c, d, five kinds of monomers of e according to a certain ratio under the initiator effect copolyreaction make:
The a maleic anhydride:
The b acrylic monomer:
R wherein
1Expression hydrogen atom or C
1-3Alkyl, R
2Expression hydrogen atom, alkali metal cation, ammonium or C
1-4Aliphatic alkyl;
C allyl ether series monomer
R3 represents hydrogen atom or C
1-3Alkyl, n represents number of repeat unit, its value is for 10-80;
The d aminated compounds
R
4Expression hydrogen atom or C
1-3Alkane; R
5Expression hydrogen atom or C
1-3Alkyl or C
1-8Alkylsulphonic acid;
E olefin sulfonic acid class monomer
R
6Expression hydrogen atom or C
1-3Alkyl, M represents hydrogen atom or alkali metal cation;
Described olefin sulfonic acid class monomer is methylpropene sodium sulfonate or sodium allyl sulfonate;
Above-mentioned monomer molar proportioning: a:b:c:d:e is 1:0.5-2.0:0.3-2.0:0.3-1.5:0.1-0.5.
2. polycarboxylate dehydragent according to claim 1 is characterized in that, described monomer b is acrylic or methacrylic acid.
3. polycarboxylate dehydragent according to claim 1 is characterized in that, the molecular weight of described monomer c is 1000-5000.
4. the preparation method of polycarboxylate dehydragent according to claim 1 is characterized in that, may further comprise the steps:
(1) in four-hole boiling flask, adds monomer a, e and a part of monomer c, add a certain amount of deionized water and make its dissolving and be heated to 50-100 ℃;
(2) drip monomer b, c, d solution and the initiator solution for preparing in advance respectively in four-hole boiling flask, 2-6h drips off, insulation 1-5h;
(3) be cooled to 25-45 ℃, add alkali and be neutralized to PH=7.0 ± 0.5, both described polycarboxylate dehydragent.
5. the preparation method of polycarboxylate dehydragent according to claim 4 is characterized in that, the amount of the monomer c of the first step adding four-hole boiling flask accounts for the 10-80% of total amount.
6. the preparation method of polycarboxylate dehydragent according to claim 4 is characterized in that, described initiator is inorganic peroxy class initiator.
7. the preparation method of polycarboxylate dehydragent according to claim 4 is characterized in that, described initiator amount is the 1-8% of monomer total amount.
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| CN102250295A (en) * | 2011-05-24 | 2011-11-23 | 中建商品混凝土天津有限公司 | Concrete super plasticizer for machine-made sand and preparation method thereof |
| CN102675557A (en) * | 2011-12-16 | 2012-09-19 | 天津冶建特种材料有限公司 | Slow-release type concrete slump retaining agent and preparation method thereof |
| CN110003403A (en) * | 2019-04-23 | 2019-07-12 | 长沙加美乐素化工有限公司 | A kind of anti-mud early-strength water-reducing agent and preparation method thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP1247824A2 (en) * | 1997-06-10 | 2002-10-09 | Nippon Shokubai Co., Ltd. | Process for producing a polycarboxylic acid as an effective compound for a cement admixture |
| WO2006129883A1 (en) * | 2005-06-01 | 2006-12-07 | Nippon Shokubai Co., Ltd. | Powdery cement dispersant |
| CN101538134A (en) * | 2009-04-14 | 2009-09-23 | 大连市建筑科学研究设计院股份有限公司 | Polyether class polycarboxylic acid high-efficiency water reducing agent and preparation method thereof |
-
2009
- 2009-11-17 CN CN 200910230447 patent/CN102060464B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP1247824A2 (en) * | 1997-06-10 | 2002-10-09 | Nippon Shokubai Co., Ltd. | Process for producing a polycarboxylic acid as an effective compound for a cement admixture |
| WO2006129883A1 (en) * | 2005-06-01 | 2006-12-07 | Nippon Shokubai Co., Ltd. | Powdery cement dispersant |
| CN101538134A (en) * | 2009-04-14 | 2009-09-23 | 大连市建筑科学研究设计院股份有限公司 | Polyether class polycarboxylic acid high-efficiency water reducing agent and preparation method thereof |
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