CN109111551A - A kind of anti-chamotte mould polycarboxylate water-reducer preparation method of 3000 molecular weight polyethers - Google Patents
A kind of anti-chamotte mould polycarboxylate water-reducer preparation method of 3000 molecular weight polyethers Download PDFInfo
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- CN109111551A CN109111551A CN201810743412.2A CN201810743412A CN109111551A CN 109111551 A CN109111551 A CN 109111551A CN 201810743412 A CN201810743412 A CN 201810743412A CN 109111551 A CN109111551 A CN 109111551A
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- 239000003638 chemical reducing agent Substances 0.000 title claims abstract description 59
- 238000002360 preparation method Methods 0.000 title claims abstract description 48
- 229920000570 polyether Polymers 0.000 title claims abstract description 43
- 229920005646 polycarboxylate Polymers 0.000 title claims abstract description 30
- 239000000178 monomer Substances 0.000 claims abstract description 45
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 44
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 44
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims abstract description 40
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 claims abstract description 38
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims abstract description 20
- 238000006243 chemical reaction Methods 0.000 claims abstract description 18
- 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 17
- 235000010323 ascorbic acid Nutrition 0.000 claims abstract description 17
- 239000011668 ascorbic acid Substances 0.000 claims abstract description 17
- 229960005070 ascorbic acid Drugs 0.000 claims abstract description 17
- WPYMKLBDIGXBTP-UHFFFAOYSA-N benzoic acid Chemical group OC(=O)C1=CC=CC=C1 WPYMKLBDIGXBTP-UHFFFAOYSA-N 0.000 claims abstract description 17
- 239000004721 Polyphenylene oxide Substances 0.000 claims abstract description 16
- 150000003460 sulfonic acids Chemical class 0.000 claims abstract description 14
- 125000002467 phosphate group Chemical group [H]OP(=O)(O[H])O[*] 0.000 claims abstract description 12
- 238000004090 dissolution Methods 0.000 claims abstract description 9
- 238000010438 heat treatment Methods 0.000 claims abstract description 9
- 230000003020 moisturizing effect Effects 0.000 claims abstract description 9
- 239000000203 mixture Substances 0.000 claims description 39
- 230000003467 diminishing effect Effects 0.000 claims description 26
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 claims description 21
- 229910019142 PO4 Inorganic materials 0.000 claims description 17
- 239000010452 phosphate Substances 0.000 claims description 17
- -1 polyoxy Polymers 0.000 claims description 15
- 229920000056 polyoxyethylene ether Polymers 0.000 claims description 15
- 229940051841 polyoxyethylene ether Drugs 0.000 claims description 15
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 claims description 13
- 239000002253 acid Substances 0.000 claims description 12
- 150000007513 acids Chemical class 0.000 claims description 11
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 9
- WQDUMFSSJAZKTM-UHFFFAOYSA-N Sodium methoxide Chemical compound [Na+].[O-]C WQDUMFSSJAZKTM-UHFFFAOYSA-N 0.000 claims description 8
- PHTQWCKDNZKARW-UHFFFAOYSA-N isoamylol Chemical compound CC(C)CCO PHTQWCKDNZKARW-UHFFFAOYSA-N 0.000 claims description 8
- 239000011734 sodium Substances 0.000 claims description 8
- 229910052708 sodium Inorganic materials 0.000 claims description 8
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 7
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 6
- BDHFUVZGWQCTTF-UHFFFAOYSA-M sulfonate Chemical compound [O-]S(=O)=O BDHFUVZGWQCTTF-UHFFFAOYSA-M 0.000 claims description 6
- DKIDEFUBRARXTE-UHFFFAOYSA-N 3-mercaptopropanoic acid Chemical compound OC(=O)CCS DKIDEFUBRARXTE-UHFFFAOYSA-N 0.000 claims description 5
- KOUKXHPPRFNWPP-UHFFFAOYSA-N pyrazine-2,5-dicarboxylic acid;hydrate Chemical compound O.OC(=O)C1=CN=C(C(O)=O)C=N1 KOUKXHPPRFNWPP-UHFFFAOYSA-N 0.000 claims description 5
- HZAXFHJVJLSVMW-UHFFFAOYSA-N 2-Aminoethan-1-ol Chemical compound NCCO HZAXFHJVJLSVMW-UHFFFAOYSA-N 0.000 claims description 4
- SLINHMUFWFWBMU-UHFFFAOYSA-N Triisopropanolamine Chemical compound CC(O)CN(CC(C)O)CC(C)O SLINHMUFWFWBMU-UHFFFAOYSA-N 0.000 claims description 4
- GTDPSWPPOUPBNX-UHFFFAOYSA-N ac1mqpva Chemical compound CC12C(=O)OC(=O)C1(C)C1(C)C2(C)C(=O)OC1=O GTDPSWPPOUPBNX-UHFFFAOYSA-N 0.000 claims description 4
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Chemical compound [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 claims description 4
- 229920002818 (Hydroxyethyl)methacrylate Polymers 0.000 claims description 3
- JPAOMENBKRZQDR-UHFFFAOYSA-N CC=CC.[Na] Chemical compound CC=CC.[Na] JPAOMENBKRZQDR-UHFFFAOYSA-N 0.000 claims description 3
- WOBHKFSMXKNTIM-UHFFFAOYSA-N Hydroxyethyl methacrylate Chemical compound CC(=C)C(=O)OCCO WOBHKFSMXKNTIM-UHFFFAOYSA-N 0.000 claims description 3
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical compound OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 claims description 3
- MNCGMVDMOKPCSQ-UHFFFAOYSA-M sodium;2-phenylethenesulfonate Chemical compound [Na+].[O-]S(=O)(=O)C=CC1=CC=CC=C1 MNCGMVDMOKPCSQ-UHFFFAOYSA-M 0.000 claims description 3
- BWYYYTVSBPRQCN-UHFFFAOYSA-M sodium;ethenesulfonate Chemical compound [Na+].[O-]S(=O)(=O)C=C BWYYYTVSBPRQCN-UHFFFAOYSA-M 0.000 claims description 3
- UZKWTJUDCOPSNM-UHFFFAOYSA-N 1-ethenoxybutane Chemical compound CCCCOC=C UZKWTJUDCOPSNM-UHFFFAOYSA-N 0.000 claims description 2
- 125000003903 2-propenyl group Chemical group [H]C([*])([H])C([H])=C([H])[H] 0.000 claims description 2
- UIIMBOGNXHQVGW-DEQYMQKBSA-M Sodium bicarbonate-14C Chemical compound [Na+].O[14C]([O-])=O UIIMBOGNXHQVGW-DEQYMQKBSA-M 0.000 claims description 2
- 150000001336 alkenes Chemical class 0.000 claims description 2
- ZBCBWPMODOFKDW-UHFFFAOYSA-N diethanolamine Chemical compound OCCNCCO ZBCBWPMODOFKDW-UHFFFAOYSA-N 0.000 claims description 2
- 229940043237 diethanolamine Drugs 0.000 claims description 2
- 229940031098 ethanolamine Drugs 0.000 claims description 2
- JRZJOMJEPLMPRA-UHFFFAOYSA-N olefin Natural products CCCCCCCC=C JRZJOMJEPLMPRA-UHFFFAOYSA-N 0.000 claims description 2
- 229910000027 potassium carbonate Inorganic materials 0.000 claims description 2
- QDRKDTQENPPHOJ-UHFFFAOYSA-N sodium ethoxide Chemical compound [Na+].CC[O-] QDRKDTQENPPHOJ-UHFFFAOYSA-N 0.000 claims description 2
- 125000003396 thiol group Chemical class [H]S* 0.000 claims description 2
- 229960004418 trolamine Drugs 0.000 claims description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims 2
- QYKIQEUNHZKYBP-UHFFFAOYSA-N Vinyl ether Chemical compound C=COC=C QYKIQEUNHZKYBP-UHFFFAOYSA-N 0.000 claims 1
- BVKZGUZCCUSVTD-UHFFFAOYSA-N carbonic acid Chemical compound OC(O)=O BVKZGUZCCUSVTD-UHFFFAOYSA-N 0.000 claims 1
- 235000019441 ethanol Nutrition 0.000 claims 1
- 239000004927 clay Substances 0.000 description 24
- 230000000694 effects Effects 0.000 description 16
- 239000011229 interlayer Substances 0.000 description 15
- 239000004568 cement Substances 0.000 description 14
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 13
- 239000000463 material Substances 0.000 description 13
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 12
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 12
- 239000004567 concrete Substances 0.000 description 11
- 239000002156 adsorbate Substances 0.000 description 8
- 238000013461 design Methods 0.000 description 7
- 239000012467 final product Substances 0.000 description 7
- 239000008187 granular material Substances 0.000 description 7
- 239000002994 raw material Substances 0.000 description 6
- 230000002708 enhancing effect Effects 0.000 description 5
- 150000004965 peroxy acids Chemical class 0.000 description 5
- 238000001179 sorption measurement Methods 0.000 description 5
- 239000011398 Portland cement Substances 0.000 description 4
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 4
- 150000001732 carboxylic acid derivatives Chemical class 0.000 description 4
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 4
- WDHYRUBXLGOLKR-UHFFFAOYSA-N phosphoric acid;prop-2-enoic acid Chemical compound OC(=O)C=C.OP(O)(O)=O WDHYRUBXLGOLKR-UHFFFAOYSA-N 0.000 description 4
- SUBDBMMJDZJVOS-UHFFFAOYSA-N 5-methoxy-2-{[(4-methoxy-3,5-dimethylpyridin-2-yl)methyl]sulfinyl}-1H-benzimidazole Chemical compound N=1C2=CC(OC)=CC=C2NC=1S(=O)CC1=NC=C(C)C(OC)=C1C SUBDBMMJDZJVOS-UHFFFAOYSA-N 0.000 description 3
- 238000004873 anchoring Methods 0.000 description 3
- 238000013459 approach Methods 0.000 description 3
- 150000002148 esters Chemical class 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- SRPWOOOHEPICQU-UHFFFAOYSA-N trimellitic anhydride Chemical compound OC(=O)C1=CC=C2C(=O)OC(=O)C2=C1 SRPWOOOHEPICQU-UHFFFAOYSA-N 0.000 description 3
- ZZZCUOFIHGPKAK-UHFFFAOYSA-N D-erythro-ascorbic acid Natural products OCC1OC(=O)C(O)=C1O ZZZCUOFIHGPKAK-UHFFFAOYSA-N 0.000 description 2
- VKEQBMCRQDSRET-UHFFFAOYSA-N Methylone Chemical compound CNC(C)C(=O)C1=CC=C2OCOC2=C1 VKEQBMCRQDSRET-UHFFFAOYSA-N 0.000 description 2
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 2
- 239000005864 Sulphur Substances 0.000 description 2
- 229930003268 Vitamin C Natural products 0.000 description 2
- 150000002169 ethanolamines Chemical class 0.000 description 2
- DNJIEGIFACGWOD-UHFFFAOYSA-N ethyl mercaptane Natural products CCS DNJIEGIFACGWOD-UHFFFAOYSA-N 0.000 description 2
- BPMFZUMJYQTVII-UHFFFAOYSA-N guanidinoacetic acid Chemical group NC(=N)NCC(O)=O BPMFZUMJYQTVII-UHFFFAOYSA-N 0.000 description 2
- 238000000034 method Methods 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 239000002002 slurry Substances 0.000 description 2
- 229910000029 sodium carbonate Inorganic materials 0.000 description 2
- 239000002689 soil Substances 0.000 description 2
- 235000019154 vitamin C Nutrition 0.000 description 2
- 239000011718 vitamin C Substances 0.000 description 2
- DGVVWUTYPXICAM-UHFFFAOYSA-N β‐Mercaptoethanol Chemical compound OCCS DGVVWUTYPXICAM-UHFFFAOYSA-N 0.000 description 2
- HMBNQNDUEFFFNZ-UHFFFAOYSA-N 4-ethenoxybutan-1-ol Chemical compound OCCCCOC=C HMBNQNDUEFFFNZ-UHFFFAOYSA-N 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- 150000008065 acid anhydrides Chemical group 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 150000008064 anhydrides Chemical class 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000033228 biological regulation Effects 0.000 description 1
- 239000004566 building material Substances 0.000 description 1
- 125000002843 carboxylic acid group Chemical group 0.000 description 1
- 150000001768 cations Chemical class 0.000 description 1
- 238000007334 copolymerization reaction Methods 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 125000006159 dianhydride group Chemical group 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000004574 high-performance concrete Substances 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 239000003999 initiator Substances 0.000 description 1
- 239000010410 layer Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 125000005641 methacryl group Chemical group 0.000 description 1
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 1
- 239000007800 oxidant agent Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 150000003014 phosphoric acid esters Chemical group 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 229920001281 polyalkylene Polymers 0.000 description 1
- ASUAYTHWZCLXAN-UHFFFAOYSA-N prenol Chemical compound CC(C)=CCO ASUAYTHWZCLXAN-UHFFFAOYSA-N 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 239000004576 sand Substances 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 239000004575 stone Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F283/00—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G
- C08F283/06—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G on to polyethers, polyoxymethylenes or polyacetals
- C08F283/065—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G on to polyethers, polyoxymethylenes or polyacetals on to unsaturated polyethers, polyoxymethylenes or polyacetals
-
- 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
- C04B24/2688—Copolymers containing at least three different monomers
- C04B24/2694—Copolymers containing at least three different monomers containing polyether side chains
-
- 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
- C04B2103/00—Function or property of ingredients for mortars, concrete or artificial stone
- C04B2103/30—Water reducers, plasticisers, air-entrainers, flow improvers
- C04B2103/302—Water reducers
Abstract
The present invention provides a kind of 3000 molecular weight polyethers anti-chamotte mould polycarboxylate water-reducer preparation method, the following steps are included: 1) 3000 molecular weight polyether polymeric monomers, phenyl carboxylic acid's function monomer, phosphate function monomer and the water of certain mass ratio are added in reaction kettle, agitating and heating waits for its dissolution；2) control temperature is initially added into a certain amount of hydrogen peroxide at 46-52 DEG C；3) after 5min, start that solution B is added dropwise；Start that solution A is added dropwise after solution B is added dropwise, in 10min, solution A time for adding is a hours, and a value is 2-4, and solution B time for adding is a+0.5 hours；Solution A is made of the acrylic acid, unsaturated sulfonic acid salt and water of certain mass ratio, and solution B is made of the ascorbic acid, chain-transferring agent and water of certain mass ratio；4) after completion of dropwise addition, keep temperature constant, cure 1-3 hour, when reaction solution temperature is lower than 30 DEG C, be slowly added to a certain amount of neutralizer, moisturizing to 1000 parts to get mass fraction for 40% the anti-chamotte mould polycarboxylate water-reducer of 3000 molecular weight polyethers.
Description
Technical field
The invention belongs to building material technical fields, are related to concrete admixture field, specifically a kind of 3000 molecule
Measure the anti-chamotte mould polycarboxylate water-reducer preparation method of polyethers.
Background technique
Water-reducing agent is as the important component in high performance concrete, and development is very fast, with the continuous expansion of scale
Greatly, to the water-reducing rate of water-reducing agent, more stringent requirements are proposed for slump retaining and adaptability etc..Nowadays quality sand and stone resources subtract
The sandstone usage amount of few problem, secondary material constantly increases, and the clay content in sandstone material has ever-increasing trend, general
Logical polycarboxylate water-reducer product occurs more and more being not suitable with situation in use, it would be highly desirable to there is new mentality of designing, newly
The product of molecular configuration is supplemented.The high sandstone material of clay content, often there is stratiforms for the strong adsorbate of clay class therein
Structure, its main chain and side chain lengths are difficult to play effect, the side chain of normal length common polycarboxylate water-reducer in this case
The entire segment of meeting enters in the interlayer hole of clay, can not play steric hindrance effect；The backbone length of ordinary water-reducing agent and
The configuration of side chain density also makes diminishing agent molecule be easy to be restrained and entire diminishing agent molecule is made to be difficult to shake off by strong adsorbate,
Lose dispersion effect.
The present invention passes through the ratio for improving the hydrophilic radicals such as carboxyl, sulfonic group, phosphate first, and it is long to improve main chain
Degree increases diminishing agent molecule in cement particle surface to improve diminishing agent molecule to the initial adsorption ability of cement particle surface
Sticking probability.Use 3000 molecular weight polyethers as raw material, obtain longer side chain, side chain is longer to bring side chain to disturb to make up
Spend it is larger, cause two cement granules due to the intermolecular mutual steric hindrance effect of water-reducing agent is unobvious too close to the problem of,
Longer main chain and peracid ether are prepared than design, obtains the carboxyl density for being higher than general polycarboxylate water-reducer, it is close using high carboxyl
Two cement granules are separated into long side chain by the powerful electrostatic repulsion of degree bring can play the position of steric hindrance effect；Containing
In the higher hydrated environment of mud amount, side chain is longer to allow side chain not lose whole steric hindrances into adsorbate interlayer
Effect, and side chain is longer and side chain density is smaller, causes when having side chain to be adsorbed on clay interlayer, into the side of interlayer
Chain can make adsorbate that can not further influence entire diminishing because detent is caused there are differential seat angle in approach axis and interlayer direction
Agent molecule.Phenyl carboxylic acid's function monomer is introduced, while enhancing steric hindrance effect, phenyl ring can also be contradicted at lamellar clay end
Face prevents side chain from entering clay interlayer.
Patent CN107337766A discloses a kind of high-adaptability polycarboxylate water-reducer and preparation method thereof, described in the invention
High-adaptability polycarboxylate water-reducer by carboxylic acid monomer A, high molecular weight polyether polymeric monomer B, functional polyalkylene cation polymeric monomer C with not
Phosphate ester monomer D progress free radicals copolymerization reaction is saturated to be made.The high-adaptability polycarboxylate water-reducer of the invention is suitable for sandstone
The high area of aggregate clay content, and have the advantages that low-dosage, high water reduction and high-thin arch dam；High-adaptability polycarboxylic acids of the invention
The preparation process of water-reducing agent is simple, and production process is environmentally protective, at low cost.
Patent CN107011489A discloses a kind of preparation method of the peracid ether than protecting the polycarboxylate water-reducer that collapses, invention tool
Body includes kettle base solution, A1 material solution, A2 material solution and B material solution；S1, terminal double bond polyoxyethylene ether, double bond monomer, oxidation are provided
Agent, beta-unsaturated esters, chain-transferring agent, reducing agent vitamin C；The preparation of S2, kettle base solution: by terminal double bond polyoxyethylene ether, double bond list
Body, oxidant and water mixing are made into kettle base solution；The preparation of S3, A1 material solution: the A1 material solution is that double bond monomer is mixed with water
It forms；The preparation of S4, A2 material solution: A2 material solution is made of beta-unsaturated esters and double bond monomer and water；The preparation of S5, B material solution:
B material solution is made of reducing agent vitamin C, chain-transferring agent and water.Sour ether is than protecting the polycarboxylic acids diminishing that collapses proposed in the present invention
In agent, terminal double bond polyoxyethylene ether dosage is less, reduces cost, while keeping preferable diminishing and function of slump protection, preparation method
Simple process is suitble to industrial production.
Patent CN107325236A discloses a kind of non-soil responsive type polycarboxylate water-reducer and preparation method thereof, specifically with
4- hydroxy butyl vinyl ether polymeric monomer, unsaturated carboxylic acid, unsaturated sulfonic acid salt, unsaturated esters minor comonomer are comonomer, with
Initiator, chain-transferring agent carry out copolyreaction as molecular regulation agent and manufactured.The water-reducing agent of the invention is in concrete
Sandstone material clay content is insensitive, is applied in the high concrete of clay content, has more than traditional polycarboxylate water-reducer
High water reducing ability and lesser slump-loss, solve traditional polycarboxylate water-reducer concrete application present in it is right
The problem of sandstone raw material soil sensibility.
It is different from the above patent, the present invention uses the polyether macromonomer of 3000 molecular weight, and peracid ether ratio, low chain-transferring agent are used
The formula of amount designs, and introduces sulfonic group, phosphate etc. compared with the stronger group of carboxylic acid group's adsorption capacity, enhances anchoring group to band
The adsorption capacity and sticking probability of the cement granules of positive electricity, and phenyl carboxylic acid's function monomer is introduced, it can be contradicted using phenyl ring in layer
Shape clay end face is to prevent side chain from entering clay interlayer.The final backbone length that obtains is longer, carboxyl, sulfonic group, phosphate ratio
Example and density are larger, and electrostatic repulsion is stronger, and steric hindrance acts on more obviously anti-chamotte mould polycarboxylate water-reducer.
Summary of the invention
Technical problem to be solved by the present invention lies in provide a kind of 3000 molecular weight polyethers anti-chamotte mould polycarboxylic acids diminishing
Agent and preparation method thereof.
In order to obtain target molecule configuration, uses 3000 molecular weight polyethers as raw material, obtain longer side chain, to make up
Side chain is longer to bring side chain degree of disturbing larger, causes two cement granules unobvious because of the intermolecular mutual steric hindrance effect of water-reducing agent
And too close to the problem of, prepare longer main chain and peracid ether than design, obtain the carboxyl for being higher than general polycarboxylate water-reducer
Density is intersected the intermolecular long side chain of two water-reducing agents using the powerful electrostatic repulsion of high carboxyl density bring, commissure shape
State repulsion contradicts state to chain end of drawing money on credit, this conflict state can preferably play the steric hindrance effect of diminishing agent molecule；
In addition, the carboxyl density design point of the diminishing agent molecule is 1.5-2 times of normality water-reducing agent carboxyl density, sulfonic group, phosphorus are matched
The strong anchoring group of acidic group, adsorption capacity and sticking probability of the enhancing diminishing agent molecule to positively charged cement granules.Introduce phenyl
Carboxylic acid functional monomer, enhancing steric hindrance effect, and phenyl ring can be contradicted in lamellar clay end face, and side chain is prevented to enter argillic horizon
Between.
Longer side chain can promote main chain is longer to promote to form thicker hydrated sheath, and diminishing agent molecule is made to play good point
Dissipate property.In the higher hydrated environment of clay content, side chain is longer to allow side chain not lose whole into adsorbate interlayer
Steric hindrance effect, and side chain is longer and side chain density is smaller, causes when having side chain to be adsorbed on clay interlayer, into
The side chain for entering interlayer can make adsorbate can not further shadow because detent is caused there are differential seat angle in approach axis and interlayer direction
Ring entire diminishing agent molecule.The structure of long side chain, downside chain density can also reduce diminishing agent molecule in adjacent domain by clay
Grain adsorbs the probability of a large amount of side chains simultaneously.
In conclusion preparing a kind of water-reducing rate height, anti-mud effect using the multiple design for high clay content situation
Good polycarboxylate water-reducer.
Technical scheme is as follows:
A kind of anti-chamotte mould polycarboxylate water-reducer preparation method of 3000 molecular weight polyethers, the water-reducing agent is mainly by following components
It is prepared: 3000 molecular weight polyether polymeric monomers, hydrogen peroxide, acrylic acid, unsaturated sulfonic acid salt, ascorbic acid, phenyl carboxylic acid's function
It can monomer, phosphate function monomer, chain-transferring agent, neutralizer and water；1000 parts of gross mass, final product quality score is after preparation
40%, preparation method the following steps are included:
1) by 3000 molecular weight polyether polymeric monomer of 335-350 part, 2-7 parts of phenyl carboxylic acid's function monomers, 1.5-5.5 parts of phosphoric acid
Ester function monomer and 180-220 parts of water are added in reaction kettle, and agitating and heating waits for its dissolution；
2) temperature in the kettle is measured, control temperature after temperature is stablized, is added at one time 0.8-1.5 parts of dioxygens at 46-52 DEG C
Water；
3) after 5min, start that solution B is added dropwise, start that solution A, solution A drop is added dropwise after solution B is added dropwise, in 10min
It is a hours between added-time, a value is 2-4, and solution B time for adding is a+0.5 hours；Solution B by 0.35-0.55 parts of ascorbic acid,
0.3-0.6 parts of chain-transferring agents and 80-100 parts of water composition, solution A by 33-40 parts of acrylic acid, 1.5-5 portions of unsaturated sulfonic acid salt and
50-70 parts of water compositions；
4) it after completion of dropwise addition, keeps temperature constant, cures 1-3 hours, when reaction solution temperature is lower than 30 DEG C, slowly add
Enter 6-12 parts of neutralizers, moisturizing to 1000 parts be 40% to get mass fraction the anti-chamotte mould polycarboxylic acids of 3000 molecular weight polyethers
Water-reducing agent.
In above-mentioned preparation method, the 3000 molecular weight polyether polymeric monomer by 3000 molecular weight allyl polyethenoxy
One of ether, methyl allyl polyoxyethylene ether, isoamyl alcohol polyoxyethylene ether, vinyl butyl ether polyoxyethylene ether are several
Kind composition；Preferably the isoamyl alcohol polyoxyethylene ether of 3000 molecular weight, 3000 molecular weight methyl allyl polyoxyethylene ether,
One or more of methyl allyl polyoxyethylene ether of 3000 molecular weight composition；The preferably prenol of 3000 molecular weight
Polyoxyethylene ether.
In above-mentioned preparation method, the unsaturated sulfonic acid salt is by sodium vinyl sulfonate, acrylic sodium sulfonate, metering system sulphur
One or more of sour sodium, sodium styrene sulfonate, 2- acrylamide-2-methyl propane sulfonic composition；Preferred mass is than for 1:1's
The composition of acrylic sodium sulfonate and methylpropene sodium sulfonate.
In above-mentioned preparation method, phenyl carboxylic acid's function monomer is by methylacryoyloxyethyl trimellitic anhydride, methyl
One or more of acrylyl oxy-ethyl phthalic monoester, equal benzene dianhydride dimethacrylate hydroxyl ethyl ester composition；It is preferred that
The larger equal benzene dianhydride dimethacrylate hydroxyl ethyl ester with certain space steric hindrance of molecular weight.
In above-mentioned preparation method, the phosphate function monomer is by methylacryoyloxyethyl phosphate, Ethylene Glycol Methyl
One or both of acrylate phosphate composition；Preferred mass is than the methylacryoyloxyethyl phosphate and second for 2:1
The composition of glycol methacrylate phosphate.
In above-mentioned preparation method, the chain-transferring agent is by thioacetic acid, mercaptopropionic acid, mercaptoethanol, mercaprol
One or more composition；Composition of the preferred mass than thioacetic acid and mercaptopropionic acid for 1:2.
In above-mentioned preparation method, the neutralizer by sodium hydroxide, potassium hydroxide, sodium carbonate, sodium bicarbonate, potassium carbonate,
One or more of sodium methoxide, sodium ethoxide, ethanol amine, diethanol amine, triethanolamine, triisopropanolamine composition；Preferred mass
Than the composition of sodium methoxide and triisopropanolamine for 1:1.
In above-mentioned preparation method, the hydrogen peroxide is that mass percent is 27.5% industrial grade hydrogen peroxide.
In the step 3) of above-mentioned preparation method, the solution A time for adding is preferably 3h.
In the step 4) of above-mentioned preparation method, the curing time is preferably 2.5h.
The beneficial effects of the present invention are:
1, use 3000 molecular weight polyethers as raw material, obtain longer side chain, longer side chain can promote main chain longer
Promote to form thicker hydrated sheath, diminishing agent molecule is made to play good dispersibility.In the higher hydrated environment of clay content, side
Chain is longer to allow side chain not lose whole steric hindrance effects into adsorbate interlayer, and side chain is longer and side chain
Density is smaller, causes when having side chain to be adsorbed on clay interlayer, and the side chain into interlayer can be because of approach axis and interlayer
Detent is caused in direction there are differential seat angle, makes adsorbate that can not further influence entire diminishing agent molecule.Long side chain, downside chain are close
The structure of degree can also reduce diminishing agent molecule in adjacent domain and by clay particle while adsorb the probabilities of a large amount of side chains.Introduce benzene
Yl carboxylic acid function monomer, enhancing steric hindrance effect, and phenyl ring can be contradicted in lamellar clay end face, and side chain is prevented to enter argillic horizon
Between.
2, side chain is longer to bring side chain degree of disturbing larger to make up, and causes two cement granules because of the intermolecular mutual sky of water-reducing agent
Between steric hindrance it is unobvious and too close to the problem of, prepare longer main chain and peracid ether than design, obtain be higher than it is general poly-
The carboxyl density of carboxylic acid water reducer is using the powerful electrostatic repulsion of high carboxyl density bring by two intermolecular length of water-reducing agent
Side chain intersection, the repulsion of commissure state contradict state to chain end of drawing money on credit, this conflict state can preferably play diminishing agent molecule
Steric hindrance effect；In addition, the carboxyl density design point of the diminishing agent molecule is the 1.5-2 of normality water-reducing agent carboxyl density
Times, match sulfonic group, the strong anchoring group of phosphate, adsorption capacity and suction of the enhancing diminishing agent molecule to positively charged cement granules
Attached probability.
Specific embodiment
For the ease of those of ordinary skill in the art understand and implement the present invention, below by embodiment to the present invention make into
The detailed description of one step, it should be appreciated that embodiment described herein is merely to illustrate and explain the present invention, and is not used to limit
The fixed present invention.
Losec 702 is specially the isoamyl alcohol polyoxyethylene ether of 3000 molecular weight, and Losec 703 is specially 3000 molecular weight
Methyl allyl polyoxyethylene ether joins the methyl allyl polyoxyethylene ether that deep WR6251 is specially 3000 molecular weight.
Embodiment 1
A kind of anti-chamotte mould polycarboxylate water-reducer of 3000 molecular weight polyethers, is mainly prepared from the following components: 3000 points
Son amount polyether macromonomer, hydrogen peroxide, acrylic acid, unsaturated sulfonic acid salt, ascorbic acid, phenyl carboxylic acid's function monomer, phosphate function
It can monomer, chain-transferring agent, neutralizer and water；1000 parts of gross mass, final product quality score is 40% after preparation, and preparation method includes
Following steps:
1) by 335 parts of Losecs, 702,5 parts of methylacryoyloxyethyl phthalic monoesters, 5.5 parts of Ethylene Glycol Methyls third
Olefin(e) acid ester phosphate and 220 parts of water are added in reaction kettle, and agitating and heating waits for its dissolution；
2) temperature in the kettle is measured, control temperature is at 46 DEG C, and after temperature is stablized, being added at one time 0.8 part of mass percent is
27.5% industrial grade hydrogen peroxide；
3) after 5min, start that solution B is added dropwise, start that solution A is added dropwise after solution B is added dropwise, in 10min；Solution A drop
It is 2 hours between added-time, solution B time for adding is 2.5 hours；Solution B is 1:2's by 0.35 part of ascorbic acid, 0.6 part of mass ratio
The composition of thioacetic acid and mercaptopropionic acid, 80 parts of water compositions, solution A is by 40 parts of acrylic acid, 1.5 parts of acrylic sodium sulfonates and 70
Part water composition；
4) it after completion of dropwise addition, keeps temperature constant, cures 1 hour, when reaction solution temperature is lower than 30 DEG C, be slowly added to
12 parts of sodium carbonate, moisturizing to 1000 parts to get mass fraction be 40% the anti-chamotte mould polycarboxylic acids diminishing of 3000 molecular weight polyethers
Agent.
Embodiment 2
A kind of anti-chamotte mould polycarboxylate water-reducer of 3000 molecular weight polyethers, is mainly prepared from the following components: 3000 points
Son amount polyether macromonomer, hydrogen peroxide, acrylic acid, unsaturated sulfonic acid salt, ascorbic acid, phenyl carboxylic acid's function monomer, phosphate function
It can monomer, chain-transferring agent, neutralizer and water；1000 parts of gross mass, final product quality score is 40% after preparation, and preparation method includes
Following steps:
1) by 342 parts 703,2 parts of Losec equal benzene dianhydride dimethacrylate hydroxyl ethyl esters, 5.3 parts of methylacryoyloxyethyls
Phosphate and 210 parts of water are added in reaction kettle, and agitating and heating waits for its dissolution；
2) temperature in the kettle is measured, control temperature is at 47 DEG C, and after temperature is stablized, being added at one time 0.9 part of mass percent is
27.5% industrial grade hydrogen peroxide；
3) after 5min, start that solution B is added dropwise, start that solution A is added dropwise after solution B is added dropwise, in 10min；Solution A drop
It is 2.5 hours between added-time, solution B time for adding is 3 hours；Solution B is by 0.5 part of ascorbic acid, 0.35 part of thioacetic acid and 95
Part water composition, solution A are made of 39 parts of acrylic acid, 4 parts of sodium vinyl sulfonates and 66 parts of water；
4) it after completion of dropwise addition, keeps temperature constant, cures 1.5 hours, when reaction solution temperature is lower than 30 DEG C, slowly add
Enter 7 parts of ethanol amines, moisturizing to 1000 parts be 40% to get mass fraction the anti-chamotte mould polycarboxylic acids diminishing of 3000 molecular weight polyethers
Agent.
Embodiment 3
A kind of anti-chamotte mould polycarboxylate water-reducer of 3000 molecular weight polyethers, is mainly prepared from the following components: 3000 points
Son amount polyether macromonomer, hydrogen peroxide, acrylic acid, unsaturated sulfonic acid salt, ascorbic acid, phenyl carboxylic acid's function monomer, phosphate function
It can monomer, chain-transferring agent, neutralizer and water；1000 parts of gross mass, final product quality score is 40% after preparation, and preparation method includes
Following steps:
1) by 340 parts of deep WR6251 of connection, 6 parts of methylacryoyloxyethyl trimellitic anhydrides, 4 parts of mass ratio 2:1 methyl
The composition of acrylyl oxy-ethyl phosphate and glycolmethacrylate phosphate, 200 parts of water are added in reaction kettle, are stirred
Heating is mixed to its dissolution；
2) temperature in the kettle is measured, control temperature is at 48 DEG C, and after temperature is stablized, being added at one time 1 part of mass percent is
27.5% industrial grade hydrogen peroxide；
3) after 5min, start that solution B is added dropwise, start that solution A is added dropwise after solution B is added dropwise, in 10min；Solution A drop
It is 3 hours between added-time, solution B time for adding is 3.5 hours；Solution B is by 0.34 part of ascorbic acid, 0.4 part of mercaptoethanol and 86
Part water composition, solution A are made of 37 parts of acrylic acid, 3.8 parts of 2- acrylamide-2-methyl propane sulfonics and 58 parts of water；
4) it after completion of dropwise addition, keeps temperature constant, cures 1.8 hours, when reaction solution temperature is lower than 30 DEG C, slowly add
Enter 9 parts of potassium hydroxide, moisturizing subtracts to the anti-chamotte mould polycarboxylic acids of 3000 molecular weight polyethers that 1000 parts are 40% to get mass fraction
Aqua.
Embodiment 4
A kind of anti-chamotte mould polycarboxylate water-reducer of 3000 molecular weight polyethers, is mainly prepared from the following components: 3000 points
Son amount polyether macromonomer, hydrogen peroxide, acrylic acid, unsaturated sulfonic acid salt, ascorbic acid, phenyl carboxylic acid's function monomer, phosphate function
It can monomer, chain-transferring agent, neutralizer and water；1000 parts of gross mass, final product quality score is 40% after preparation, and preparation method includes
Following steps:
1) by the methylacryoyloxyethyl phthalic monoester and equal benzene of 343 parts of Losecs, 703,5.5 parts of mass ratio 1:1
The methylacryoyloxyethyl phosphate and ethylene glycol first of the composition of dianhydride dimethacrylate hydroxyl ethyl ester, 2 parts of mass ratio 1:1
The composition of base acrylate phosphate, 190 parts of water are added in reaction kettle, and agitating and heating waits for its dissolution；
2) temperature in the kettle is measured, control temperature is at 50 DEG C, and after temperature is stablized, being added at one time 1.1 parts of mass percents is
27.5% industrial grade hydrogen peroxide；
3) after 5min, start that solution B is added dropwise, start that solution A is added dropwise after solution B is added dropwise, in 10min；Solution A drop
It is 3.5 hours between added-time, solution B time for adding is 4 hours；Solution B is by 0.45 part of ascorbic acid, 0.45 part of mercaprol and 98
Part water composition, solution A are made of 36 parts of acrylic acid, 2 parts of sodium styrene sulfonate and 56 parts of water；
4) it after completion of dropwise addition, keeps temperature constant, cures 2 hours, when reaction solution temperature is lower than 30 DEG C, be slowly added to
11 parts of ethanol amines, moisturizing to 1000 parts to get mass fraction be 40% the anti-chamotte mould polycarboxylic acids diminishing of 3000 molecular weight polyethers
Agent.
Embodiment 5
A kind of anti-chamotte mould polycarboxylate water-reducer of 3000 molecular weight polyethers, is mainly prepared from the following components: 3000 points
Son amount polyether macromonomer, hydrogen peroxide, acrylic acid, unsaturated sulfonic acid salt, ascorbic acid, phenyl carboxylic acid's function monomer, phosphate function
It can monomer, chain-transferring agent, neutralizer and water；1000 parts of gross mass, final product quality score is 40% after preparation, and preparation method includes
Following steps:
1) by the methylacryoyloxyethyl trimellitic anhydride and equal benzene two of 350 parts of deep WR6251 of connection, 4 parts of mass ratio 2:1
The methylacryoyloxyethyl phosphate and Ethylene Glycol Methyl of the composition of acid anhydride dimethacrylate hydroxyl ethyl ester, 3 parts of mass ratio 1:2
The composition of acrylate phosphate, 185 parts of water are added in reaction kettle, and agitating and heating waits for its dissolution；
2) temperature in the kettle is measured, control temperature is at 50 DEG C, and after temperature is stablized, being added at one time 1.3 parts of mass percents is
27.5% industrial grade hydrogen peroxide；
3) after 5min, start that solution B is added dropwise, start that solution A, solution A drop is added dropwise after solution B is added dropwise, in 10min
It is 4 hours between added-time, solution B time for adding is 4.5 hours；Solution B is by 0.5 part of ascorbic acid, 0.55 part of mercaptopropionic acid and 85
Part water composition, solution A are made of 34 parts of acrylic acid, 2 parts of methylpropene sodium sulfonates and 60 parts of water；
4) it after completion of dropwise addition, keeps temperature constant, cures 2.8 hours, when reaction solution temperature is lower than 30 DEG C, slowly add
Enter the sodium methoxide and triisopropanolamine of 6 parts of mass ratio 1:1, moisturizing to 1000 parts be 40% to get mass fraction 3000 molecules
Measure the anti-chamotte mould polycarboxylate water-reducer of polyethers.
Embodiment 6
A kind of anti-chamotte mould polycarboxylate water-reducer of 3000 molecular weight polyethers, is mainly prepared from the following components: 3000 points
Son amount polyether macromonomer, hydrogen peroxide, acrylic acid, unsaturated sulfonic acid salt, ascorbic acid, phenyl carboxylic acid's function monomer, phosphate function
It can monomer, chain-transferring agent, neutralizer and water；1000 parts of gross mass, final product quality score is 40% after preparation, and preparation method includes
Following steps:
1) by the methylacryoyloxyethyl trimellitic anhydride and methacryl of 345 parts of Losecs, 702,7 parts of mass ratio 1:1
The methylacryoyloxyethyl phosphate and ethylene glycol first of the composition of oxygen ethyl phthalic monoester, 1.5 parts of mass ratio 2:3
The composition of base acrylate phosphate, 180 parts of water are added in reaction kettle, and agitating and heating waits for its dissolution；
2) temperature in the kettle is measured, control temperature is at 52 DEG C, and after temperature is stablized, being added at one time 1.5 parts of mass percents is
27.5% industrial grade hydrogen peroxide；
3) after 5min, start that solution B is added dropwise, start that solution A is added dropwise after solution B is added dropwise, in 10min；Solution A drop
It is 4.5 hours between added-time, solution B time for adding is 5 hours；Solution B is by 0.55 part of ascorbic acid, the mercapto of 0.3 part of mass ratio 1:1
The composition of guanidine-acetic acid and mercaprol, 100 parts of water composition, solution A is by 33 parts of acrylic acid, the acrylic sulphur of 5 parts of mass ratio 1:1
The composition of sour sodium and methylpropene sodium sulfonate, 50 parts of water compositions；
4) it after completion of dropwise addition, keeps temperature constant, cures 3 hours, when reaction solution temperature is lower than 30 DEG C, be slowly added to
8 parts of triethanolamines, moisturizing to 1000 parts to get mass fraction be 40% the anti-chamotte mould polycarboxylic acids diminishing of 3000 molecular weight polyethers
Agent.
Respectively test above-described embodiment 1,2,3,4,5,6 3000 molecular weight polyethers with anti-chamotte mould polycarboxylate water-reducer with it is general
Net slurry initial fluidity, 1h mobility and concrete under logical polycarboxylate water-reducer comparable sodium in different cement is initial
The slump/divergence and through when the slump/divergence.Testing cement used is new 42.5 ordinary portland cement of China, with reference to GB/8076-
2008 " concrete admixture " testing standards.
The different Water-reducing Admixtures To Cements net slurry flow effects of table 1 (new 42.5 ordinary portland cement of China)
| Water-reducing agent type | Initial fluidity/mm | 1h mobility/mm |
| Ordinary water-reducing agent | 240 | 200 |
| Embodiment 1 | 245 | 210 |
| Embodiment 2 | 250 | 220 |
| Embodiment 3 | 240 | 215 |
| Embodiment 4 | 245 | 210 |
| Embodiment 5 | 245 | 220 |
| Embodiment 6 | 255 | 225 |
The different water-reducing agents of table 2 influence (new 42.5 ordinary portland cement of China) to normal concrete mobility
The different water-reducing agents of table 3 influence (new 42.5 ordinary portland cement of China) to the biggish concrete flowability of clay content
| Water-reducing agent type | Initial slump/divergence mm | Through when the slump/divergence mm |
| Ordinary water-reducing agent | 175/370 | 130/350 |
| Embodiment 1 | 215/490 | 190/475 |
| Embodiment 2 | 210/490 | 200/480 |
| Embodiment 3 | 220/500 | 185/475 |
| Embodiment 4 | 225/495 | 190/485 |
| Embodiment 5 | 210/505 | 185/490 |
| Embodiment 6 | 230/485 | 190/480 |
According to above-mentioned cement paste initial fluidity, 1h mobility and concrete initial fluidity and through when mobility ratio
Compared with the anti-chamotte mould polycarboxylate water-reducer embodiment 1,2,3,4,5,6 of 3000 molecular weight polyethers and ordinary water-reducing agent are in experiment, water
The initial fluidity of cement paste, 1h mobility are not much different compared with ordinary water-reducing agent, embodiment 1,2,3,4,5,6 be slightly better than it is general
Logical water-reducing agent.When applied to normal concrete, embodiment 1,2,3,5,6 initial slumps/divergence and through when the slump/extension
It is all better than ordinary water-reducing agent to spend, when being applied to the biggish concrete of clay content, initial slump/divergence of ordinary water-reducing agent and
Through when the slump/divergence have and significantly decline very much, and embodiment 1,2,3,4,5,6 initial slumps/divergence and warp
When the slump/divergence still keep higher level.In conclusion the anti-chamotte mould polycarboxylic acids diminishing of 3000 molecular weight polyether
Agent can show good adaptability in the biggish raw material of clay content, and water-reducing property is not influenced by the quality of raw material.
Claims (8)
1. a kind of anti-chamotte mould polycarboxylate water-reducer preparation method of 3000 molecular weight polyethers, it is characterised in that: the water-reducing agent is main
Be prepared from the following components: 3000 molecular weight polyether polymeric monomers, hydrogen peroxide, acrylic acid, unsaturated sulfonic acid salt, ascorbic acid,
Phenyl carboxylic acid's function monomer, phosphate function monomer, chain-transferring agent, neutralizer and water；1000 parts of gross mass, at quality after preparation
Measure score be 40%, preparation method the following steps are included:
1) by 3000 molecular weight polyether polymeric monomer of 335-350 part, 2-7 parts of phenyl carboxylic acid's function monomers, 1.5-5.5 parts of phosphate function
Energy monomer and 180-220 parts of water are added in reaction kettle, and agitating and heating waits for its dissolution；
2) temperature in the kettle is measured, control temperature after temperature is stablized, is added at one time 0.8-1.5 parts of hydrogen peroxide at 46-52 DEG C；
3) after 5min, successively start that solution B is added dropwise, start that solution A is added dropwise after solution B is added dropwise, in 10min；Solution A drop
It is a hours between added-time, a value is 2-4, and solution B time for adding is a+0.5 hours；Solution B by 0.35-0.55 parts of ascorbic acid,
0.3-0.6 parts of chain-transferring agents and 80-100 parts of water composition, solution A by 33-40 parts of acrylic acid, 1.5-5 portions of unsaturated sulfonic acid salt and
50-70 parts of water compositions；
4) it after completion of dropwise addition, keeps temperature constant, cures 1-3 hours, when reaction solution temperature is lower than 30 DEG C, be slowly added to 6-
12 parts of neutralizers, moisturizing to 1000 parts to get mass fraction be 40% the anti-chamotte mould polycarboxylic acids diminishing of 3000 molecular weight polyethers
Agent.
2. preparation method according to claim 1, it is characterised in that: the 3000 molecular weight polyether polymeric monomer is by 3000 molecules
Allyl polyethenoxy ether, methyl allyl polyoxyethylene ether, isoamyl alcohol polyoxyethylene ether, the vinyl butyl ether polyoxy of amount
One or more of vinethene composition.
3. preparation method according to claim 1, it is characterised in that: the unsaturated sulfonic acid salt is by sodium vinyl sulfonate, third
One or more of sodium olefin sulfonate, methylpropene sodium sulfonate, sodium styrene sulfonate, 2- acrylamide-2-methyl propane sulfonic
Composition.
4. preparation method according to claim 1, it is characterised in that: phenyl carboxylic acid's function monomer is by methacryloxypropyl
Ethyl trimellitic anhydride, methylacryoyloxyethyl phthalic monoester, in equal benzene dianhydride dimethacrylate hydroxyl ethyl ester
One or more composition.
5. preparation method according to claim 1, it is characterised in that: the phosphate function monomer is by methacryloxypropyl second
One or both of base phosphate, glycolmethacrylate phosphate composition.
6. preparation method according to claim 1, it is characterised in that: the chain-transferring agent is by thioacetic acid, mercaptopropionic acid, mercapto
One or more of base ethyl alcohol, mercaprol composition.
7. preparation method according to claim 1, it is characterised in that: the neutralizer is by sodium hydroxide, potassium hydroxide, carbonic acid
One of sodium, sodium bicarbonate, potassium carbonate, sodium methoxide, sodium ethoxide, ethanol amine, diethanol amine, triethanolamine, triisopropanolamine
Or several compositions.
8. preparation method according to claim 1, it is characterised in that: the hydrogen peroxide is that mass percent is 27.5% industry
Grade hydrogen peroxide.
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| CN112812288A (en) * | 2021-02-03 | 2021-05-18 | 湖北工业大学 | Preparation method of nano-alumina dispersant and nano-alumina dispersant |
| CN112940197A (en) * | 2021-02-03 | 2021-06-11 | 湖北工业大学 | Viscosity-reducing and mud-resisting polymer for concrete and preparation method thereof |
| CN112940197B (en) * | 2021-02-03 | 2023-05-16 | 湖北工业大学 | Viscosity-reducing and mud-resisting polymer for concrete and preparation method thereof |
| CN113150219A (en) * | 2021-02-09 | 2021-07-23 | 武汉理工大学 | High-adaptability mud-resistant water reducing agent and preparation method thereof |
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