CN104177557A - Low-temperature preparation method of high-adaptability ether polycarboxylic acid water reducer - Google Patents
Low-temperature preparation method of high-adaptability ether polycarboxylic acid water reducer Download PDFInfo
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- CN104177557A CN104177557A CN201410417642.1A CN201410417642A CN104177557A CN 104177557 A CN104177557 A CN 104177557A CN 201410417642 A CN201410417642 A CN 201410417642A CN 104177557 A CN104177557 A CN 104177557A
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- Prior art keywords
- adaptability
- polycarboxylic acid
- acid
- sodium
- low temperature
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 44
- 239000003638 chemical reducing agent Substances 0.000 title claims abstract description 35
- 239000002253 acid Substances 0.000 title claims abstract description 22
- 238000002360 preparation method Methods 0.000 title claims abstract description 20
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 title claims abstract description 10
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 21
- 238000006243 chemical reaction Methods 0.000 claims abstract description 20
- 239000000243 solution Substances 0.000 claims abstract description 20
- 239000011259 mixed solution Substances 0.000 claims abstract description 16
- 238000003756 stirring Methods 0.000 claims abstract description 7
- 150000003009 phosphonic acids Chemical class 0.000 claims abstract description 6
- 150000001732 carboxylic acid derivatives Chemical class 0.000 claims abstract description 5
- 239000012986 chain transfer agent Substances 0.000 claims abstract description 5
- 150000002170 ethers Chemical class 0.000 claims description 17
- -1 polyoxy Vinyl Ethers Polymers 0.000 claims description 12
- 229920005646 polycarboxylate Polymers 0.000 claims description 10
- 229920000056 polyoxyethylene ether Polymers 0.000 claims description 9
- 239000003795 chemical substances by application Substances 0.000 claims description 8
- 230000002829 reductive effect Effects 0.000 claims description 8
- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical compound [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 claims description 7
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 6
- NIXOWILDQLNWCW-UHFFFAOYSA-N Acrylic acid Chemical compound OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims description 6
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 6
- KFSLWBXXFJQRDL-UHFFFAOYSA-N Peracetic acid Chemical compound CC(=O)OO KFSLWBXXFJQRDL-UHFFFAOYSA-N 0.000 claims description 6
- ABLZXFCXXLZCGV-UHFFFAOYSA-N Phosphorous acid Chemical compound OP(O)=O ABLZXFCXXLZCGV-UHFFFAOYSA-N 0.000 claims description 6
- 229940051841 polyoxyethylene ether Drugs 0.000 claims description 6
- LCPVQAHEFVXVKT-UHFFFAOYSA-N 2-(2,4-difluorophenoxy)pyridin-3-amine Chemical compound NC1=CC=CN=C1OC1=CC=C(F)C=C1F LCPVQAHEFVXVKT-UHFFFAOYSA-N 0.000 claims description 5
- 125000003903 2-propenyl group Chemical group [H]C([*])([H])C([H])=C([H])[H] 0.000 claims description 5
- BAPJBEWLBFYGME-UHFFFAOYSA-N Methyl acrylate Chemical compound COC(=O)C=C BAPJBEWLBFYGME-UHFFFAOYSA-N 0.000 claims description 5
- KLSBASGQHCAVHQ-UHFFFAOYSA-L disodium;2-hydroxy-2-sulfinatoacetate Chemical compound [Na+].[Na+].[O-]C(=O)C(O)S([O-])=O KLSBASGQHCAVHQ-UHFFFAOYSA-L 0.000 claims description 5
- CHQMHPLRPQMAMX-UHFFFAOYSA-L sodium persulfate Substances [Na+].[Na+].[O-]S(=O)(=O)OOS([O-])(=O)=O CHQMHPLRPQMAMX-UHFFFAOYSA-L 0.000 claims description 5
- 239000000872 buffer Substances 0.000 claims description 4
- 239000003153 chemical reaction reagent Substances 0.000 claims description 4
- 235000019800 disodium phosphate Nutrition 0.000 claims description 4
- OPGYRRGJRBEUFK-UHFFFAOYSA-L disodium;diacetate Chemical compound [Na+].[Na+].CC([O-])=O.CC([O-])=O OPGYRRGJRBEUFK-UHFFFAOYSA-L 0.000 claims description 4
- LVHBHZANLOWSRM-UHFFFAOYSA-N itaconic acid Chemical compound OC(=O)CC(=C)C(O)=O LVHBHZANLOWSRM-UHFFFAOYSA-N 0.000 claims description 4
- 235000017557 sodium bicarbonate Nutrition 0.000 claims description 4
- 150000003460 sulfonic acids Chemical class 0.000 claims description 4
- HVCNQTCZNBPWBV-UHFFFAOYSA-N 2-hydroxy-2-sulfinoacetic acid Chemical compound OC(=O)C(O)S(O)=O HVCNQTCZNBPWBV-UHFFFAOYSA-N 0.000 claims description 3
- OMIGHNLMNHATMP-UHFFFAOYSA-N 2-hydroxyethyl prop-2-enoate Chemical compound OCCOC(=O)C=C OMIGHNLMNHATMP-UHFFFAOYSA-N 0.000 claims description 3
- YHQXBTXEYZIYOV-UHFFFAOYSA-N 3-methylbut-1-ene Chemical group CC(C)C=C YHQXBTXEYZIYOV-UHFFFAOYSA-N 0.000 claims description 3
- HMBNQNDUEFFFNZ-UHFFFAOYSA-N 4-ethenoxybutan-1-ol Chemical compound OCCCCOC=C HMBNQNDUEFFFNZ-UHFFFAOYSA-N 0.000 claims description 3
- 239000004160 Ammonium persulphate Substances 0.000 claims description 3
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 claims description 3
- JPAOMENBKRZQDR-UHFFFAOYSA-N CC=CC.[Na] Chemical compound CC=CC.[Na] JPAOMENBKRZQDR-UHFFFAOYSA-N 0.000 claims description 3
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 claims description 3
- 235000019395 ammonium persulphate Nutrition 0.000 claims description 3
- 125000000118 dimethyl group Chemical group [H]C([H])([H])* 0.000 claims description 3
- 125000005395 methacrylic acid group Chemical group 0.000 claims description 3
- 125000004805 propylene group Chemical group [H]C([H])([H])C([H])([*:1])C([H])([H])[*:2] 0.000 claims description 3
- XWGJFPHUCFXLBL-UHFFFAOYSA-M rongalite Chemical compound [Na+].OCS([O-])=O XWGJFPHUCFXLBL-UHFFFAOYSA-M 0.000 claims description 3
- 229910000030 sodium bicarbonate Inorganic materials 0.000 claims description 3
- GEHJYWRUCIMESM-UHFFFAOYSA-L sodium sulfite Chemical compound [Na+].[Na+].[O-]S([O-])=O GEHJYWRUCIMESM-UHFFFAOYSA-L 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
- BDHFUVZGWQCTTF-UHFFFAOYSA-M sulfonate Chemical compound [O-]S(=O)=O BDHFUVZGWQCTTF-UHFFFAOYSA-M 0.000 claims description 3
- 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 2
- DKIDEFUBRARXTE-UHFFFAOYSA-N 3-mercaptopropanoic acid Chemical compound OC(=O)CCS DKIDEFUBRARXTE-UHFFFAOYSA-N 0.000 claims description 2
- JIGUQPWFLRLWPJ-UHFFFAOYSA-N Ethyl acrylate Chemical compound CCOC(=O)C=C JIGUQPWFLRLWPJ-UHFFFAOYSA-N 0.000 claims description 2
- 239000004159 Potassium persulphate Substances 0.000 claims description 2
- LXCYSACZTOKNNS-UHFFFAOYSA-N diethoxy(oxo)phosphanium Chemical compound CCO[P+](=O)OCC LXCYSACZTOKNNS-UHFFFAOYSA-N 0.000 claims description 2
- BNIILDVGGAEEIG-UHFFFAOYSA-L disodium hydrogen phosphate Chemical compound [Na+].[Na+].OP([O-])([O-])=O BNIILDVGGAEEIG-UHFFFAOYSA-L 0.000 claims description 2
- 229910000397 disodium phosphate Inorganic materials 0.000 claims description 2
- HPGPEWYJWRWDTP-UHFFFAOYSA-N lithium peroxide Chemical compound [Li+].[Li+].[O-][O-] HPGPEWYJWRWDTP-UHFFFAOYSA-N 0.000 claims description 2
- PNJWIWWMYCMZRO-UHFFFAOYSA-N pent‐4‐en‐2‐one Natural products CC(=O)CC=C PNJWIWWMYCMZRO-UHFFFAOYSA-N 0.000 claims description 2
- USHAGKDGDHPEEY-UHFFFAOYSA-L potassium persulfate Chemical compound [K+].[K+].[O-]S(=O)(=O)OOS([O-])(=O)=O USHAGKDGDHPEEY-UHFFFAOYSA-L 0.000 claims description 2
- 235000019394 potassium persulphate Nutrition 0.000 claims description 2
- PFUVRDFDKPNGAV-UHFFFAOYSA-N sodium peroxide Chemical compound [Na+].[Na+].[O-][O-] PFUVRDFDKPNGAV-UHFFFAOYSA-N 0.000 claims description 2
- 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 2
- 238000000034 method Methods 0.000 abstract description 7
- 230000001105 regulatory effect Effects 0.000 abstract description 6
- 238000006116 polymerization reaction Methods 0.000 abstract description 2
- 239000006172 buffering agent Substances 0.000 abstract 1
- 230000002708 enhancing effect Effects 0.000 abstract 1
- 238000006386 neutralization reaction Methods 0.000 abstract 1
- 239000007800 oxidant agent Substances 0.000 abstract 1
- 125000001273 sulfonato group Chemical class [O-]S(*)(=O)=O 0.000 abstract 1
- 239000004568 cement Substances 0.000 description 13
- 239000004567 concrete Substances 0.000 description 8
- 239000000178 monomer Substances 0.000 description 6
- 239000000463 material Substances 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 3
- 239000004575 stone Substances 0.000 description 3
- 150000007513 acids Chemical class 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 238000010276 construction Methods 0.000 description 2
- 238000007334 copolymerization reaction Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 150000003254 radicals Chemical class 0.000 description 2
- 238000007670 refining Methods 0.000 description 2
- 239000004576 sand Substances 0.000 description 2
- 229920003171 Poly (ethylene oxide) Polymers 0.000 description 1
- 125000002843 carboxylic acid group Chemical group 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 125000004185 ester group Chemical group 0.000 description 1
- JEIPFZHSYJVQDO-UHFFFAOYSA-N ferric oxide Chemical compound O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000004574 high-performance concrete Substances 0.000 description 1
- 239000003999 initiator Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000007086 side reaction Methods 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 125000002769 thiazolinyl group Chemical group 0.000 description 1
- 230000009466 transformation Effects 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
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/10—Esters
- C08F220/20—Esters of polyhydric alcohols or phenols, e.g. 2-hydroxyethyl (meth)acrylate or glycerol mono-(meth)acrylate
-
- 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
- C04B24/16—Sulfur-containing compounds
-
- 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
-
- 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
- C08F2/00—Processes of polymerisation
- C08F2/38—Polymerisation using regulators, e.g. chain terminating agents, e.g. telomerisation
-
- 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
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/04—Acids; Metal salts or ammonium salts thereof
- C08F220/06—Acrylic acid; Methacrylic acid; Metal salts or ammonium salts thereof
-
- 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
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/10—Esters
- C08F220/12—Esters of monohydric alcohols or phenols
- C08F220/14—Methyl esters, e.g. methyl (meth)acrylate
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- 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
- C08F228/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a bond to sulfur or by a heterocyclic ring containing sulfur
- C08F228/02—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a bond to sulfur or by a heterocyclic ring containing sulfur by a bond to sulfur
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- 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
- C08F230/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and containing phosphorus, selenium, tellurium or a metal
- C08F230/02—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and containing phosphorus, selenium, tellurium or a metal containing phosphorus
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- 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
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- 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
- C08F4/00—Polymerisation catalysts
- C08F4/40—Redox systems
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- Polymers & Plastics (AREA)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a low-temperature preparation method of a high-adaptability ether polycarboxylic acid water reducer, which comprises the following steps: preparing unsaturated carboxylic acid, unsaturated sulfonate, unsaturated phosphonic acid, a chain-transfer agent and water into a mixed solution A; preparing a reducer a and water into a mixed solution B; adding unsaturated polyethenoxy ether a buffering agent and water into a reaction kettle; regulating the reaction temperature to 10-40 DEG C, adding an oxidizer at one time, and dissolving by stirring; dropwisely adding the mixed solution A and mixed solution B simultaneously; after finishing drowse addition, adding 0-0.5 part of reducer b at one time, and continuing reaction for 1-2 hours; and finally, adding 10-20 parts of 30 wt% sodium hydroxide solution for neutralization, thereby obtaining the polycarboxylic acid water reducer. The method is simple, and the prepared water reducer can have high dispersibility by low doping amount. The low-temperature high-efficiency reducer is introduced to implement low-temperature polymerization of the polycarboxylic acid, thereby enhancing the conversion rate of the product.
Description
Technical field
The invention belongs to the technical field of material of construction, relate in particular to a kind of low temperature preparation method of high-adaptability ethers polycarboxylic acid water reducing agent.
Background technology
Along with the future development of concrete to high performance and multifunction, require concrete to there is high workability, high strength, high-durability, and can meet in many application in particular cases.Have super dispersing property polycarboxylate water-reducer oneself become indispensable component in high performance concrete.
Polycarboxylate water-reducer is in preparation process, can according to molecular designing pass in principle free radical copolymerization by the synthetic predetermined structure of polymerizable structural unit the water reducer with performance, conventionally by containing some monomers with unsaturated group such as carboxylic acid group, sulfonic group, ester group and polyoxyethylene thiazolinyl, by free radicals copolymerization reaction, synthesize.In the molecule cohesive process of polymkeric substance, different monomers, to condense together at random or regularly, makes molecule have comb-type structure, the structures shape that it is special its high-performance.
Because the application of concrete admixture relates to the problem of admixture self and cement, sand material, although the water-reducing property of polycarboxylate water-reducer excellence is extensively approved by industry at present, but wherein the adaptability about gelling material such as admixture and cement has still become an important difficult problem in current concrete construction process, its main manifestations is the problems such as bad adaptability, the adaptability problem that improves polycarboxylate water-reducer, particularly ethers polycarboxylic acid water reducing agent is extremely urgent; And, along with the attention of country to energy-conserving and environment-protective industry, reduce the common recognition that the consumption of the energy has been become to the whole society, therefore develop low temperature polymerization technique very helpful for the energy-saving and emission-reduction of concrete admixture.
Summary of the invention
Technical problem to be solved by this invention is to provide a kind of high-adaptability ethers polycarboxylic acid water reducing agent and low temperature preparation method thereof, it can overcome the problem and shortage existing in prior art and production, employing, without thermal source technique, can synthesize the high-performance water reducing agent with low-dosage, high water reducing rate, low slump loss.
For solving the problems of the technologies described above, technical solution of the present invention is:
A low temperature preparation method for high-adaptability ethers polycarboxylic acid water reducing agent, comprises the following steps:
1), in mass parts, 5-20 part unsaturated carboxylic acid, 0-5 part unsaturated sulfonic acid salt (preferably 2-5 part), the unsaturated phosphonic acids of 0.5-3 part, 0-2 part chain-transfer agent (preferably 0.6-2 part) and 30 parts of water are configured to mixed solution A;
2) 0.1-1.0 part reductive agent a and 30 parts of water are configured to mixing solutions B.
3) 100 parts of unsaturated polyoxy Vinyl Ethers, 1-3 part buffer reagent and 50 parts of water are joined in reactor;
4) regulating temperature of reaction is 10-40 ℃, and disposable 0.1-3 part oxygenant that adds stirs and makes its dissolving.Drip respectively mixed solution A and mixing solutions B, time for adding is 2-4h simultaneously;
5), after dropping finishes, the disposable 0-0.5 part reductive agent b (preferably 0.3-0.5 part) that adds, continues reaction 1-2 hour; Finally add the sodium hydroxide solution that 10-20 part mass concentration is 30% to neutralize, obtain described polycarboxylate water-reducer.
Described unsaturated carboxylic acid is one or both in vinylformic acid, methyl acrylate, ethyl propenoate, vinylformic acid hydroxyl methyl esters, Hydroxyethyl acrylate, methylene-succinic acid.
Described unsaturated sulfonic acid salt is a kind of in sodium vinyl sulfonate, sodium allyl sulfonate, methylpropene sodium sulfonate, Sodium styrene sulfonate.
Described unsaturated phosphonic acids is a kind of in isopropylene and phosphonic acid, 2-acrylamide-2-methyl-propyl phosphonic acids, Dimethyl ally phosphite, allyl group diethyl phosphonate.
Described chain-transfer agent is a kind of in 2-Thiovanic acid, 3-thiohydracrylic acid.
Described reductive agent a is one or both in 2-hydroxyl-2-sulfino acetic acid, 2-hydroxyl-2-sulfino acetic acid disodium salt, 2-hydroxyl-2-sulfonic group acetic acid, 2-hydroxyl-2-sulfonic group acetic acid disodium salt.
Described unsaturated polyoxy Vinyl Ether is a kind of in allyl polyethenoxy base ether, methacrylic polyoxyethylene ether, isopentene group polyoxyethylene ether, 4-hydroxy butyl vinyl ether polyoxyethylene ether.
Described buffer reagent is a kind of in Sodium phosphate dibasic, sodium bicarbonate.
Described oxygenant is a kind of in hydrogen peroxide, sodium peroxide, lithium peroxide, Sodium Persulfate, Potassium Persulphate, ammonium persulphate, Sodium persulfate, peroxide potassium borate, peracetic acid.
Described reductive agent b is a kind of of rongalite, xitix, S-WAT.
Adopt after such scheme, the present invention has following effectively effect:
1, preparation method of the present invention adopts the redox system initiator system of low-activation energy, has improved reactive behavior, reduces the generation of side reaction, makes the transformation efficiency of product high, can reach 99% left and right.
2, preparation method of the present invention is polymerizable at normal temperatures, is easy to suitability for industrialized production, and technique is simple, does not need heating in production, is a kind of technique of environmental protection.
3. preparation method of the present invention adopts by introducing carboxylate radical, sulfonate radical, phosphonate groups, has improved the dispersed and dispersed hold facility of product, and the adaptability to gelling material.
Embodiment
Below in conjunction with specific embodiment, the invention will be further described.Following umber all refers to mass fraction.
Embodiment 1
In mass parts, 5 parts of vinylformic acid, 5 parts of sodium allyl sulfonates, 3 parts of isopropylene and phosphonic acids and 30 parts of water are configured to mixed solution A; 0.9 part of 2-hydroxyl-2-sulfino acetic acid, 0.1 part of 2-hydroxyl-2-sulfonic group acetic acid disodium salt and 30 parts of water are configured to mixing solutions B.100 parts of allyl polyethenoxy base ethers, 2 parts of Sodium phosphate dibasics and 50 parts of water are joined in reactor; Regulating temperature of reaction is 40 ℃, disposablely adds 1 part of hydrogen peroxide, stirs and makes its dissolving.Drip respectively mixed solution A and mixing solutions B, time for adding is 2h simultaneously; After dropping finishes, continue reaction 1 hour; Finally add the sodium hydroxide solution that 10 parts of mass concentrations are 30% to neutralize, obtain described polycarboxylate water-reducer, monomer conversion 98.9%.
Embodiment 2
In mass parts, 7 parts of vinylformic acid, 2 parts of methyl acrylates, 2 parts of sodium vinyl sulfonates, 0.5 part of 2-acrylamide-2-methyl-propyl phosphonic acids, 0.6 part of 2-Thiovanic acid and 30 parts of water are configured to mixed solution A; 0.4 part of 2-hydroxyl-2-sulfino acetic acid disodium salt and 30 parts of water are configured to mixing solutions B.100 parts of methacrylic polyoxyethylene ethers, 1 part of sodium bicarbonate and 50 parts of water are joined in reactor; Regulating temperature of reaction is 15 ℃, disposablely adds 0.4 part of Sodium Persulfate, stirs and makes its dissolving.Drip respectively mixed solution A and mixing solutions B, time for adding is 4h simultaneously; After dropping finishes, can disposablely add 0.5 part of rongalite, continue reaction 2 hours; Finally add the sodium hydroxide solution that 12 parts of mass concentrations are 30% to neutralize, obtain described polycarboxylate water-reducer, monomer conversion 99.5%.
Embodiment 3
In mass parts, 10 parts of vinylformic acid, 2 parts of vinylformic acid hydroxyl methyl esters, 1 part of methylpropene sodium sulfonate, 1 part of Dimethyl ally phosphite, 2 parts of 2-Thiovanic acids and 30 parts of water are configured to mixed solution A; 0.1 part of 2-hydroxyl-2-sulfino acetic acid disodium salt, 0.1 part of 2-hydroxyl-2-sulfonic group acetic acid disodium salt and 30 parts of water are configured to mixing solutions B.100 parts of 4-hydroxy butyl vinyl ether polyoxyethylene ethers, 3 parts of Sodium phosphate dibasics and 50 parts of water are joined in reactor; Regulating temperature of reaction is 10 ℃, disposablely adds 3 parts of peracetic acid, stirs and makes its dissolving.Drip respectively mixed solution A and mixing solutions B, time for adding is 3h simultaneously; After dropping finishes, can disposablely add 0.3 part of xitix, continue reaction 1 hour; Finally add the sodium hydroxide solution that 15 parts of mass concentrations are 30% to neutralize, obtain described polycarboxylate water-reducer, monomer conversion 98.7%.
Embodiment 4
In mass parts, 2 parts of vinylformic acid, 18 parts of Hydroxyethyl acrylates, 2 parts of allyl group diethyl phosphonates, 1.2 parts of 3-thiohydracrylic acids and 30 parts of water are configured to mixed solution A; 0.1 part of 2-hydroxyl-2-sulfino acetic acid disodium salt and 30 parts of water are configured to mixing solutions B.100 parts of isopentene group polyoxyethylene ethers, 3 parts of sodium bicarbonates and 50 parts of water are joined in reactor; Regulating temperature of reaction is 25 ℃, disposablely adds 0.1 part of ammonium persulphate, stirs and makes its dissolving.Drip respectively mixed solution A and mixing solutions B, time for adding is 3h simultaneously; After dropping finishes, can disposablely add 0.4 part of S-WAT, continue reaction 1 hour; Finally add the sodium hydroxide solution that 20 parts of mass concentrations are 30% to neutralize, obtain described polycarboxylate water-reducer, monomer conversion 99.2%.
By synthetic sample and the comparative example (commercially available ethers polycarboxylic acid water reducing agent) obtaining of embodiment 1-4, adopt standard cement, China Resources cement PO.42.5, refining stone cement PO.42.5, Fujian good fortune cement PO.42.5, volume is pressed cement quality 0.2%, according to GB 8076-2008 < < concrete admixture > >, survey its concrete water-reducing ratio.Concrete mix is: cement 360kg/m
3, sand 803kg/m
3, stone 982kg/m
3, the slump is controlled at 210 ± 10mm, and acquired results is as shown in the table.
| Adopt cement | Comparative example | Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 |
| ? | Water-reducing rate | Water-reducing rate | Water-reducing rate | Water-reducing rate | Water-reducing rate |
| Standard cement | 29.5％ | 30.1％ | 32.8％ | 33.4％ | 31.5％ |
| China Resources cement | 29.8％ | 30.4％ | 32.3％ | 33.5％ | 32.3％ |
| Refining stone cement | 28.4％ | 30.5％ | 33.0％ | 33.2％ | 31.2％ |
| Fujian good fortune cement | 26.3％ | 29.9％ | 32.6％ | 32.9％ | 31.5％ |
The above, be only preferred embodiment of the present invention, not technical scope of the present invention is imposed any restrictions, thus variation or the modification in every case according to claim of the present invention and specification sheets, done, within all should belonging to the scope that patent of the present invention contains.
Claims (10)
1. a low temperature preparation method for high-adaptability ethers polycarboxylic acid water reducing agent, is characterized in that comprising the following steps:
1), in mass parts, 5-20 part unsaturated carboxylic acid, 0-5 part unsaturated sulfonic acid salt, the unsaturated phosphonic acids of 0.5-3 part, 0-2 part chain-transfer agent and 30 parts of water are configured to mixed solution A;
2) 0.1-1.0 part reductive agent a and 30 parts of water are configured to mixing solutions B;
3) 100 parts of unsaturated polyoxy Vinyl Ethers, 1-3 part buffer reagent and 50 parts of water are joined in reactor; Adjusting temperature of reaction is 10-40 ℃, and disposable 0.1-3 part oxygenant that adds stirs and makes its dissolving;
4) drip respectively mixed solution A and mixing solutions B, time for adding is 2-4h simultaneously;
5), after dropping finishes, disposable 0-0.5 part reductive agent b that adds, continues reaction 1-2 hour; Finally add the sodium hydroxide solution that 10-20 part mass concentration is 30% to neutralize, obtain described polycarboxylate water-reducer.
2. the low temperature preparation method of a kind of high-adaptability ethers polycarboxylic acid water reducing agent according to claim 1, is characterized in that: described unsaturated carboxylic acid is one or both in vinylformic acid, methyl acrylate, ethyl propenoate, vinylformic acid hydroxyl methyl esters, Hydroxyethyl acrylate or methylene-succinic acid.
3. the low temperature preparation method of a kind of high-adaptability ethers polycarboxylic acid water reducing agent according to claim 1, is characterized in that: described unsaturated sulfonic acid salt is a kind of in sodium vinyl sulfonate, sodium allyl sulfonate, methylpropene sodium sulfonate or Sodium styrene sulfonate.
4. the low temperature preparation method of a kind of high-adaptability ethers polycarboxylic acid water reducing agent according to claim 1, is characterized in that: described unsaturated phosphonic acids is a kind of in isopropylene and phosphonic acid, 2-acrylamide-2-methyl-propyl phosphonic acids, Dimethyl ally phosphite or allyl group diethyl phosphonate.
5. the low temperature preparation method of a kind of high-adaptability ethers polycarboxylic acid water reducing agent according to claim 1, is characterized in that: described chain-transfer agent is a kind of in 2-Thiovanic acid or 3-thiohydracrylic acid.
6. the low temperature preparation method of a kind of high-adaptability ethers polycarboxylic acid water reducing agent according to claim 1, is characterized in that: described reductive agent a is one or both in 2-hydroxyl-2-sulfino acetic acid, 2-hydroxyl-2-sulfino acetic acid disodium salt, 2-hydroxyl-2-sulfonic group acetic acid or 2-hydroxyl-2-sulfonic group acetic acid disodium salt.
7. the low temperature preparation method of a kind of high-adaptability ethers polycarboxylic acid water reducing agent according to claim 1, is characterized in that: described unsaturated polyoxy Vinyl Ether is a kind of in allyl polyethenoxy base ether, methacrylic polyoxyethylene ether, isopentene group polyoxyethylene ether or 4-hydroxy butyl vinyl ether polyoxyethylene ether.
8. the low temperature preparation method of a kind of high-adaptability ethers polycarboxylic acid water reducing agent according to claim 1, is characterized in that: described buffer reagent is a kind of in Sodium phosphate dibasic or sodium bicarbonate.
9. the low temperature preparation method of a kind of high-adaptability ethers polycarboxylic acid water reducing agent according to claim 1, is characterized in that: described oxygenant is a kind of in hydrogen peroxide, sodium peroxide, lithium peroxide, Sodium Persulfate, Potassium Persulphate, ammonium persulphate, Sodium persulfate, peroxide potassium borate or peracetic acid.
10. the low temperature preparation method of a kind of high-adaptability ethers polycarboxylic acid water reducing agent according to claim 1, is characterized in that: described reductive agent b is a kind of of rongalite, xitix or S-WAT.
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| CN201410417642.1A CN104177557B (en) | 2014-08-22 | 2014-08-22 | A kind of low temperature preparation method of high-adaptability ethers polycarboxylic acid water reducing agent |
| PCT/CN2015/081810 WO2016026346A1 (en) | 2014-08-22 | 2015-06-18 | Low-temperature method for preparing high-adaptability ether polycarboxylic acid water reducer |
| PH12015502804A PH12015502804A1 (en) | 2014-08-22 | 2015-12-17 | Method for preparing high-adaptable ether polycarboxylate superplasticizer at low temperature |
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| Publication number | Publication date |
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| CN104177557B (en) | 2017-09-15 |
| PH12015502804A1 (en) | 2016-03-21 |
| WO2016026346A1 (en) | 2016-02-25 |
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