CN109053973A - A kind of dropwise addition synthesis technology of polycarboxylate water-reducer - Google Patents
A kind of dropwise addition synthesis technology of polycarboxylate water-reducer Download PDFInfo
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- CN109053973A CN109053973A CN201810755453.3A CN201810755453A CN109053973A CN 109053973 A CN109053973 A CN 109053973A CN 201810755453 A CN201810755453 A CN 201810755453A CN 109053973 A CN109053973 A CN 109053973A
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- Prior art keywords
- parts
- acid
- polycarboxylate water
- dropwise addition
- reducer
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- 239000003638 chemical reducing agent Substances 0.000 title claims abstract description 40
- 229920005646 polycarboxylate Polymers 0.000 title claims abstract description 31
- 238000005516 engineering process Methods 0.000 title claims abstract description 20
- 230000015572 biosynthetic process Effects 0.000 title claims abstract description 19
- 238000003786 synthesis reaction Methods 0.000 title claims abstract description 19
- 239000000463 material Substances 0.000 claims abstract description 121
- 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 24
- UFWIBTONFRDIAS-UHFFFAOYSA-N Naphthalene Chemical compound C1=CC=CC2=CC=CC=C21 UFWIBTONFRDIAS-UHFFFAOYSA-N 0.000 claims abstract description 24
- 239000002994 raw material Substances 0.000 claims abstract description 24
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 17
- AEQDJSLRWYMAQI-UHFFFAOYSA-N 2,3,9,10-tetramethoxy-6,8,13,13a-tetrahydro-5H-isoquinolino[2,1-b]isoquinoline Chemical compound C1CN2CC(C(=C(OC)C=C3)OC)=C3CC2C2=C1C=C(OC)C(OC)=C2 AEQDJSLRWYMAQI-UHFFFAOYSA-N 0.000 claims abstract description 12
- CERQOIWHTDAKMF-UHFFFAOYSA-N Methacrylic acid Chemical compound CC(=C)C(O)=O CERQOIWHTDAKMF-UHFFFAOYSA-N 0.000 claims abstract description 12
- DWAQJAXMDSEUJJ-UHFFFAOYSA-M Sodium bisulfite Chemical compound [Na+].OS([O-])=O DWAQJAXMDSEUJJ-UHFFFAOYSA-M 0.000 claims abstract description 12
- QROGIFZRVHSFLM-QHHAFSJGSA-N [(e)-prop-1-enyl]benzene Chemical compound C\C=C\C1=CC=CC=C1 QROGIFZRVHSFLM-QHHAFSJGSA-N 0.000 claims abstract description 12
- KXDAEFPNCMNJSK-UHFFFAOYSA-N benzene carboxamide Natural products NC(=O)C1=CC=CC=C1 KXDAEFPNCMNJSK-UHFFFAOYSA-N 0.000 claims abstract description 12
- ZIUHHBKFKCYYJD-UHFFFAOYSA-N n,n'-methylenebisacrylamide Chemical compound C=CC(=O)NCNC(=O)C=C ZIUHHBKFKCYYJD-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000000176 sodium gluconate Substances 0.000 claims abstract description 12
- 229940005574 sodium gluconate Drugs 0.000 claims abstract description 12
- 235000012207 sodium gluconate Nutrition 0.000 claims abstract description 12
- 229940079827 sodium hydrogen sulfite Drugs 0.000 claims abstract description 12
- 235000010267 sodium hydrogen sulphite Nutrition 0.000 claims abstract description 12
- OFOBLEOULBTSOW-UHFFFAOYSA-N Propanedioic acid Natural products OC(=O)CC(O)=O OFOBLEOULBTSOW-UHFFFAOYSA-N 0.000 claims abstract description 11
- 235000010323 ascorbic acid Nutrition 0.000 claims abstract description 11
- 239000011668 ascorbic acid Substances 0.000 claims abstract description 11
- 229960005070 ascorbic acid Drugs 0.000 claims abstract description 11
- VZCYOOQTPOCHFL-UPHRSURJSA-N maleic acid Chemical compound OC(=O)\C=C/C(O)=O VZCYOOQTPOCHFL-UPHRSURJSA-N 0.000 claims abstract description 11
- 239000011976 maleic acid Substances 0.000 claims abstract description 11
- 229920006324 polyoxymethylene Polymers 0.000 claims abstract description 11
- VZCYOOQTPOCHFL-UHFFFAOYSA-N trans-butenedioic acid Natural products OC(=O)C=CC(O)=O VZCYOOQTPOCHFL-UHFFFAOYSA-N 0.000 claims abstract description 11
- 238000006243 chemical reaction Methods 0.000 claims abstract description 10
- YXYZMHGSOKYZAF-UHFFFAOYSA-M [Cl-].C(C(=C)C)(=O)OCC[N+](C(C)(C)C)(C)C Chemical compound [Cl-].C(C(=C)C)(=O)OCC[N+](C(C)(C)C)(C)C YXYZMHGSOKYZAF-UHFFFAOYSA-M 0.000 claims abstract description 9
- HRZFUMHJMZEROT-UHFFFAOYSA-L sodium disulfite Chemical compound [Na+].[Na+].[O-]S(=O)S([O-])(=O)=O HRZFUMHJMZEROT-UHFFFAOYSA-L 0.000 claims abstract description 9
- 229940001584 sodium metabisulfite Drugs 0.000 claims abstract description 9
- 235000010262 sodium metabisulphite Nutrition 0.000 claims abstract description 9
- GNSFRPWPOGYVLO-UHFFFAOYSA-N 3-hydroxypropyl 2-methylprop-2-enoate Chemical compound CC(=C)C(=O)OCCCO GNSFRPWPOGYVLO-UHFFFAOYSA-N 0.000 claims abstract description 6
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 28
- 229920000056 polyoxyethylene ether Polymers 0.000 claims description 18
- 229940051841 polyoxyethylene ether Drugs 0.000 claims description 18
- 238000009417 prefabrication Methods 0.000 claims description 14
- 239000000203 mixture Substances 0.000 claims description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 11
- 239000003999 initiator Substances 0.000 claims description 10
- 239000002253 acid Substances 0.000 claims description 8
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 8
- 230000032683 aging Effects 0.000 claims description 7
- 238000004090 dissolution Methods 0.000 claims description 7
- 239000007788 liquid Substances 0.000 claims description 7
- 238000003756 stirring Methods 0.000 claims description 7
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 6
- VQTUBCCKSQIDNK-UHFFFAOYSA-N Isobutene Chemical compound CC(C)=C VQTUBCCKSQIDNK-UHFFFAOYSA-N 0.000 claims description 6
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims description 6
- 239000005864 Sulphur Substances 0.000 claims description 6
- PHTQWCKDNZKARW-UHFFFAOYSA-N isoamylol Chemical compound CC(C)CCO PHTQWCKDNZKARW-UHFFFAOYSA-N 0.000 claims description 6
- CHQMHPLRPQMAMX-UHFFFAOYSA-L sodium persulfate Chemical compound [Na+].[Na+].[O-]S(=O)(=O)OOS([O-])(=O)=O CHQMHPLRPQMAMX-UHFFFAOYSA-L 0.000 claims description 6
- 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
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 claims description 4
- QZPSOSOOLFHYRR-UHFFFAOYSA-N 3-hydroxypropyl prop-2-enoate Chemical compound OCCCOC(=O)C=C QZPSOSOOLFHYRR-UHFFFAOYSA-N 0.000 claims description 3
- DKIDEFUBRARXTE-UHFFFAOYSA-N 3-mercaptopropanoic acid Chemical compound OC(=O)CCS DKIDEFUBRARXTE-UHFFFAOYSA-N 0.000 claims description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 3
- DNJIEGIFACGWOD-UHFFFAOYSA-N ethyl mercaptane Natural products CCS DNJIEGIFACGWOD-UHFFFAOYSA-N 0.000 claims description 3
- USHAGKDGDHPEEY-UHFFFAOYSA-L potassium persulfate Chemical compound [K+].[K+].[O-]S(=O)(=O)OOS([O-])(=O)=O USHAGKDGDHPEEY-UHFFFAOYSA-L 0.000 claims description 3
- 235000019394 potassium persulphate Nutrition 0.000 claims description 3
- DGVVWUTYPXICAM-UHFFFAOYSA-N β‐Mercaptoethanol Chemical compound OCCS DGVVWUTYPXICAM-UHFFFAOYSA-N 0.000 claims description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims description 2
- 229910001870 ammonium persulfate Inorganic materials 0.000 claims description 2
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims 2
- 239000004698 Polyethylene Substances 0.000 claims 1
- AJXBTRZGLDTSST-UHFFFAOYSA-N amino 2-methylprop-2-enoate Chemical compound CC(=C)C(=O)ON AJXBTRZGLDTSST-UHFFFAOYSA-N 0.000 claims 1
- WCASXYBKJHWFMY-UHFFFAOYSA-N crotyl alcohol Chemical compound CC=CCO WCASXYBKJHWFMY-UHFFFAOYSA-N 0.000 claims 1
- 125000002485 formyl group Chemical class [H]C(*)=O 0.000 claims 1
- 238000012546 transfer Methods 0.000 claims 1
- FZGRPBJBMUNMQH-UHFFFAOYSA-N trimethyl-$l^{3}-chlorane Chemical compound CCl(C)C FZGRPBJBMUNMQH-UHFFFAOYSA-N 0.000 claims 1
- 238000007796 conventional method Methods 0.000 abstract description 3
- 230000000977 initiatory effect Effects 0.000 abstract description 3
- 230000033116 oxidation-reduction process Effects 0.000 abstract description 3
- 150000003254 radicals Chemical class 0.000 abstract description 3
- 239000004567 concrete Substances 0.000 description 13
- 239000003921 oil Substances 0.000 description 8
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 description 4
- 239000002689 soil Substances 0.000 description 4
- 229920002818 (Hydroxyethyl)methacrylate Polymers 0.000 description 3
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 3
- WOBHKFSMXKNTIM-UHFFFAOYSA-N Hydroxyethyl methacrylate Chemical compound CC(=C)C(=O)OCCO WOBHKFSMXKNTIM-UHFFFAOYSA-N 0.000 description 3
- 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 description 3
- QOSMNYMQXIVWKY-UHFFFAOYSA-N Propyl levulinate Chemical compound CCCOC(=O)CCC(C)=O QOSMNYMQXIVWKY-UHFFFAOYSA-N 0.000 description 3
- -1 acrylyl Chemical group 0.000 description 3
- 239000004568 cement Substances 0.000 description 3
- WBZKQQHYRPRKNJ-UHFFFAOYSA-N disulfurous acid Chemical compound OS(=O)S(O)(=O)=O WBZKQQHYRPRKNJ-UHFFFAOYSA-N 0.000 description 3
- 229910052739 hydrogen Inorganic materials 0.000 description 3
- 239000001257 hydrogen Substances 0.000 description 3
- 229910052708 sodium Inorganic materials 0.000 description 3
- 239000011734 sodium Substances 0.000 description 3
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 2
- 150000001336 alkenes Chemical class 0.000 description 2
- 239000002956 ash Substances 0.000 description 2
- 230000015271 coagulation Effects 0.000 description 2
- 238000005345 coagulation Methods 0.000 description 2
- 239000004744 fabric Substances 0.000 description 2
- JRZJOMJEPLMPRA-UHFFFAOYSA-N olefin Natural products CCCCCCCC=C JRZJOMJEPLMPRA-UHFFFAOYSA-N 0.000 description 2
- 239000010703 silicon Substances 0.000 description 2
- 229910052710 silicon Inorganic materials 0.000 description 2
- 239000002893 slag Substances 0.000 description 2
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 description 1
- ZZZCUOFIHGPKAK-UHFFFAOYSA-N D-erythro-ascorbic acid Natural products OCC1OC(=O)C(O)=C1O ZZZCUOFIHGPKAK-UHFFFAOYSA-N 0.000 description 1
- 229930003268 Vitamin C Natural products 0.000 description 1
- 235000019270 ammonium chloride Nutrition 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000004566 building material Substances 0.000 description 1
- 239000010883 coal ash Substances 0.000 description 1
- 230000006835 compression Effects 0.000 description 1
- 238000007906 compression Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 239000010881 fly ash Substances 0.000 description 1
- 229920000578 graft copolymer Polymers 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 239000004574 high-performance concrete Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000000034 method Methods 0.000 description 1
- 239000000178 monomer Substances 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 230000000379 polymerizing effect Effects 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 125000003396 thiol group Chemical class [H]S* 0.000 description 1
- 235000019154 vitamin C Nutrition 0.000 description 1
- 239000011718 vitamin C 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
- 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
- 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
- C08F220/34—Esters containing nitrogen, e.g. N,N-dimethylaminoethyl (meth)acrylate
-
- 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
- C08F220/52—Amides or imides
- C08F220/54—Amides, e.g. N,N-dimethylacrylamide or N-isopropylacrylamide
- C08F220/56—Acrylamide; Methacrylamide
-
- 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
- C08F222/00—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 carboxyl radical and containing at least one other carboxyl radical in the molecule; Salts, anhydrides, esters, amides, imides, or nitriles thereof
- C08F222/02—Acids; Metal salts or ammonium salts thereof, e.g. maleic acid or itaconic acid
-
- 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
- C08F222/00—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 carboxyl radical and containing at least one other carboxyl radical in the molecule; Salts, anhydrides, esters, amides, imides, or nitriles thereof
- C08F222/36—Amides or imides
- C08F222/38—Amides
-
- 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
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Separation Of Suspended Particles By Flocculating Agents (AREA)
- Detergent Compositions (AREA)
- Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)
Abstract
The invention discloses a kind of dropwise addition synthesis technologies of polycarboxylate water-reducer, specific step is as follows: configuration A material is spare, and the A material includes: methacrylic acid, maleic acid, MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride, propenyl benzene amide, bisacrylamide, hydroxy propyl methacrylate according to the raw material of parts by weight；It is spare to configure B material, the B material includes: sodium hydrogensulfite, sodium metabisulfite, sulfydryl class chain-transferring agent, polyformaldehyde, sodium gluconate, ascorbic acid, naphtalene oil according to the raw material of parts by weight.The time for adding that A, B expect in the present invention extends 1 hour than conventional method time for adding, carry out the reaction of product sufficiently, the homogeneity that free radical supplies in main initiation system to ensure oxidationreduction, to guarantee that the fluctuation range of more stability contorting water-reducing agent product water-reducing rate is capable of in the centralization of water-reducing agent molecular weight distribution, the water-reducing rate of product is reduced.
Description
Technical field
The present invention relates to water-reducing agent technical field, the dropwise addition synthesis technology of specifically a kind of polycarboxylate water-reducer.
Background technique
Currently, polycarboxylate water-reducer because have water-reducing rate is high, protect collapse ability is strong, volume is controllable, molecule structure change from
By spending the features such as big, range of applicability is wide, production process is environment friendly and pollution-free, product safety, so that polycarboxylate water-reducer is as the
Three generations's high-performance water reducing agent represents, and when being applied to concrete batching, can significantly improve the workability of concrete, reduce mix
The dosage of water changes the setting time of concrete, overcomes the problems, such as that concrete slump loss is too fast, enhances the resistance to compression of concrete
Intensity.In addition, because it is difunctional with electrostatic repulsion and steric hindrance, to not only to cement granules with excellent dispersion function
It can, moreover it is possible to slag powders, coal ash, silicon ash etc. be adsorbed and be dispersed, so that it is secondary to promote the industry such as slag, flyash, silicon ash
The application of product, and then dosage of the cement in concrete is reduced, every cube of concrete is relative to water when using other water-reducing agents
Mud can reduce 15%~30% or so.This means that a project can save the cement of a few kiloton, is economizing on resources and protecting
Important function has been played in terms of retaining ring border, has agreed with the developing goal of green building material.Based on above-mentioned advantage, polycarboxylate water-reducer is wide
It is general to be applied to the fields such as municipal administration, railway, highway, harbour, bridge, water power, it has made and having dashed forward for the development of China's high performance concrete
It contributes out.
Polycarboxylate water-reducer is the water-soluble cross-linked graft polymers that two or more monomer one-step polymerizations are formed, polymerizing condition
Requirement it is more special.
Summary of the invention
A kind of dropwise addition for the polycarboxylate water-reducer that the purpose of the present invention is to provide viscosity is higher, reduces water-reducing rate synthesizes work
Skill, to solve the problems mentioned in the above background technology.
To achieve the above object, the invention provides the following technical scheme:
A kind of dropwise addition synthesis technology of polycarboxylate water-reducer, the specific steps are as follows:
(1) configuration A material is spare, and the A material includes: 20-40 parts of methacrylic acid, maleic two according to the raw material of parts by weight
15-20 parts sour, 3-5 parts of MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride, 3-5 parts of propenyl benzene amide, 2-4 parts of bisacrylamide,
10-15 parts of hydroxy propyl methacrylate；
(2) configuration B material is spare, and the B material includes: 1-3 parts of sodium hydrogensulfite, pyrosulfurous acid hydrogen according to the raw material of parts by weight
2-4 parts of sodium, 0.5-1 parts of sulfydryl class chain-transferring agent, 2-4 parts of polyformaldehyde, 0.5-1 parts of sodium gluconate, ascorbic acid 0.8-1.2
Part, 1-2 parts of naphtalene oil；
(3) by the bottom material of 40-60 parts of unsaturated polyoxyethylene ether and 70-90 parts of water composition, investment reaction at 20-40 DEG C
In kettle；
(4) concentrated sulfuric acid is added or concentrated hydrochloric acid accelerates bottom material dissolution, the solution that mass percent is 55-65% is made, wherein
The mass percent that the concentrated sulfuric acid or concentrated hydrochloric acid account for bottom material is 0.5-1%, after bottom material is completely dissolved, puts into 3-5 parts of initiators, stirring
3-5min；
(5) the good B material of configured in advance is then at the uniform velocity added dropwise, is spaced after 5-10min and A material is at the uniform velocity added dropwise again, the A material accounts for bottom
Expect that the 10-15% of quality, B expect to account for the 8-12% of bottom material quality；
(6) the A material and B material drip off in 2-4h, and aging 1-1.5h is kept the temperature after dripping off, and rear 30% liquid alkaline that is added makes it
PH value reaches 5-7, obtains prefabrication；
(7) operation is dried to the prefabrication, obtains the high concentration polycarboxylate water-reducer.
As a further solution of the present invention:
A material includes: 25-35 parts of methacrylic acid, maleic acid 16- according to the raw material of parts by weight in the step (1)
19 parts, 3.5-4.5 parts of MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride, 3.5-4.5 parts of propenyl benzene amide, bisacrylamide 2.5-
3.5 parts, 11-14 parts of hydroxy propyl methacrylate.
As a further solution of the present invention:
A material includes: 30 parts of methacrylic acid, 18 parts of maleic acid, first according to the raw material of parts by weight in the step (1)
4 parts of base acrylyl oxy-ethyl-trimethyl salmiac, 4 parts of propenyl benzene amide, 3 parts of bisacrylamide, hydroxy propyl methacrylate 12
Part.
As a further solution of the present invention:
B material includes: 1.5-2.5 parts of sodium hydrogensulfite, sodium metabisulfite according to the raw material of parts by weight in the step (2)
2.5-3.5 parts, 0.6-0.9 parts of sulfydryl class chain-transferring agent, 2.5-3.5 parts of polyformaldehyde, 0.6-0.9 parts of sodium gluconate, Vitamin C
It is 0.9-1.1 parts sour, 1.2-1.8 parts of naphtalene oil.
As a further solution of the present invention:
B material includes: 2 parts of sodium hydrogensulfite, 3 parts of sodium metabisulfite, mercapto according to the raw material of parts by weight in the step (2)
0.8 part of base class chain-transferring agent, 3 parts of polyformaldehyde, 0.8 part of sodium gluconate, 1 part of ascorbic acid, 1.5 parts of naphtalene oil.
As a further solution of the present invention:
The unsaturated polyoxyethylene ether is isoamyl alcohol polyoxyethylene ether, isobutene alcohol polyoxyethylene ether or methyl alkene
The combination of one or more of propyl alcohol polyoxyethylene ether, molecular weight 1000-3000.
As a further solution of the present invention:
The initiator be selected from one or both of ammonium persulfate, potassium peroxydisulfate, sodium peroxydisulfate or hydrogen peroxide with
On combination.
As a further solution of the present invention:
The sulfydryl class chain-transferring agent is one or more of thioacetic acid, mercaptopropionic acid, mercaptoethanol composition.
As further scheme of the invention:
The sulfydryl class chain-transferring agent is thioacetic acid.
Compared with prior art, the beneficial effects of the present invention are:
The time for adding that A, B expect in the present invention extends 1 hour than conventional method time for adding, makes the reaction of product in this way
It sufficiently carries out, the homogeneity of free radical supply in the main initiation system to ensure oxidationreduction, to guarantee water-reducing agent molecular weight point
The fluctuation range of more stability contorting water-reducing agent product water-reducing rate is capable of in cloth centralization, is reduced the water-reducing rate of product, is added to mixed
Concrete product is wrapped more preferable after solidifying soil, increases the mobility of concrete, and the viscosity of concrete product is higher, improves coagulation
The intensity of soil extends to protect and collapse the time.
Specific embodiment
The technical solution of the patent is explained in further detail With reference to embodiment.
Embodiment 1
A kind of dropwise addition synthesis technology of polycarboxylate water-reducer, the specific steps are as follows:
(1) configuration A material is spare, and the A material includes: 20 parts of methacrylic acid, maleic acid according to the raw material of parts by weight
15 parts, 3 parts of MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride, 3 parts of propenyl benzene amide, 2 parts of bisacrylamide, hydroxyethyl methacrylate
10 parts of propyl ester；
(2) configuration B material is spare, and the B material includes: 1 part of sodium hydrogensulfite, sodium metabisulfite according to the raw material of parts by weight
2 parts, 0.5 part of sulfydryl class chain-transferring agent, 2 parts of polyformaldehyde, 0.5 part of sodium gluconate, 0.8 part of ascorbic acid, 1 part of naphtalene oil；
(3) bottom material of 40 parts of unsaturated polyoxyethylene ether and 70 parts of water composition is put into reaction kettle at 20 DEG C；
(4) concentrated sulfuric acid is added or concentrated hydrochloric acid accelerates bottom material dissolution, the solution that mass percent is 55% is made, wherein dense sulphur
The mass percent that acid or concentrated hydrochloric acid account for bottom material is 0.5%, after bottom material is completely dissolved, and puts into 3 parts of initiators, stirs 3min；
(5) the good B material of configured in advance is then at the uniform velocity added dropwise, is spaced after 5min and A material is at the uniform velocity added dropwise again, the A material accounts for bottom material
10%, the B material of quality accounts for the 8% of bottom material quality；
(6) the A material and B material drip off in 2h, and aging 1h is kept the temperature after dripping off, and rear 30% liquid alkaline that is added reaches its pH value
To 5, prefabrication is obtained；
(7) operation is dried to the prefabrication, obtains the high concentration polycarboxylate water-reducer.
Embodiment 2
A kind of dropwise addition synthesis technology of polycarboxylate water-reducer, the specific steps are as follows:
(1) configuration A material is spare, and the A material includes: 25 parts of methacrylic acid, maleic acid according to the raw material of parts by weight
16 parts, 3.5 parts of MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride, 3.5 parts of propenyl benzene amide, 2.5 parts of bisacrylamide, methyl-prop
11 parts of olefin(e) acid hydroxypropyl acrylate；
(2) configuration B material is spare, and the B material includes: 1.5 parts of sodium hydrogensulfite, pyrosulfurous acid hydrogen according to the raw material of parts by weight
2.5 parts of sodium, 0.6 part of sulfydryl class chain-transferring agent, 2.5 parts of polyformaldehyde, 0.6 part of sodium gluconate, 0.9 part of ascorbic acid, naphtalene oil 1.2
Part；
(3) bottom material of 45 parts of unsaturated polyoxyethylene ether and 75 parts of water composition is put into reaction kettle at 25 DEG C；
(4) concentrated sulfuric acid is added or concentrated hydrochloric acid accelerates bottom material dissolution, the solution that mass percent is 58% is made, wherein dense sulphur
The mass percent that acid or concentrated hydrochloric acid account for bottom material is 0.6%, after bottom material is completely dissolved, puts into 3.5 parts of initiators, stirs
3.5min；
(5) the good B material of configured in advance is then at the uniform velocity added dropwise, is spaced after 6min and A material is at the uniform velocity added dropwise again, the A material accounts for bottom material
11%, the B material of quality accounts for the 9% of bottom material quality；
(6) the A material and B material drip off in 2.5h, and aging 1.1h is kept the temperature after dripping off, and rear 30% liquid alkaline that is added makes its pH
Value reaches 5.5, obtains prefabrication；
(7) operation is dried to the prefabrication, obtains the high concentration polycarboxylate water-reducer.
Embodiment 3
A kind of dropwise addition synthesis technology of polycarboxylate water-reducer, the specific steps are as follows:
(1) configuration A material is spare, and the A material includes: 30 parts of methacrylic acid, maleic acid according to the raw material of parts by weight
18 parts, 4 parts of MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride, 4 parts of propenyl benzene amide, 3 parts of bisacrylamide, hydroxyethyl methacrylate
12 parts of propyl ester；
(2) configuration B material is spare, and the B material includes: 2 parts of sodium hydrogensulfite, sodium metabisulfite according to the raw material of parts by weight
3 parts, 0.8 part of sulfydryl class chain-transferring agent, 3 parts of polyformaldehyde, 0.8 part of sodium gluconate, 1 part of ascorbic acid, 1.5 parts of naphtalene oil；
(3) bottom material of 50 parts of unsaturated polyoxyethylene ether and 80 parts of water composition is put into reaction kettle at 30 DEG C；
(4) concentrated sulfuric acid is added or concentrated hydrochloric acid accelerates bottom material dissolution, the solution that mass percent is 60% is made, wherein dense sulphur
The mass percent that acid or concentrated hydrochloric acid account for bottom material is 0.8%, after bottom material is completely dissolved, and puts into 4 parts of initiators, stirs 4min；
(5) the good B material of configured in advance is then at the uniform velocity added dropwise, is spaced after 8min and A material is at the uniform velocity added dropwise again, the A material accounts for bottom material
12%, the B material of quality accounts for the 10% of bottom material quality；
(6) the A material and B material drip off in 3h, and aging 1.2h is kept the temperature after dripping off, and rear 30% liquid alkaline that is added makes its pH value
Reach 6, obtains prefabrication；
(7) operation is dried to the prefabrication, obtains the high concentration polycarboxylate water-reducer.
Embodiment 4
A kind of dropwise addition synthesis technology of polycarboxylate water-reducer, the specific steps are as follows:
(1) configuration A material is spare, and the A material includes: 35 parts of methacrylic acid, maleic acid according to the raw material of parts by weight
19 parts, 4.5 parts of MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride, 4.5 parts of propenyl benzene amide, 3.5 parts of bisacrylamide, methyl-prop
14 parts of olefin(e) acid hydroxypropyl acrylate；
(2) configuration B material is spare, and the B material includes: 2.5 parts of sodium hydrogensulfite, pyrosulfurous acid hydrogen according to the raw material of parts by weight
3.5 parts of sodium, 0.9 part of sulfydryl class chain-transferring agent, 3.5 parts of polyformaldehyde, 0.9 part of sodium gluconate, 1.1 parts of ascorbic acid, naphtalene oil 1.8
Part；
(3) bottom material of 55 parts of unsaturated polyoxyethylene ether and 85 parts of water composition is put into reaction kettle at 35 DEG C；
(4) concentrated sulfuric acid is added or concentrated hydrochloric acid accelerates bottom material dissolution, the solution that mass percent is 62% is made, wherein dense sulphur
The mass percent that acid or concentrated hydrochloric acid account for bottom material is 0.9%, after bottom material is completely dissolved, puts into 4.5 parts of initiators, stirs
4.5min；
(5) the good B material of configured in advance is then at the uniform velocity added dropwise, is spaced after 9min and A material is at the uniform velocity added dropwise again, the A material accounts for bottom material
14%, the B material of quality accounts for the 11% of bottom material quality；
(6) the A material and B material drip off in 3.5h, and aging 1.4h is kept the temperature after dripping off, and rear 30% liquid alkaline that is added makes its pH
Value reaches 6.5, obtains prefabrication；
(7) operation is dried to the prefabrication, obtains the high concentration polycarboxylate water-reducer.
Embodiment 5
A kind of dropwise addition synthesis technology of polycarboxylate water-reducer, the specific steps are as follows:
(1) configuration A material is spare, and the A material includes: 40 parts of methacrylic acid, maleic acid according to the raw material of parts by weight
20 parts, 5 parts of MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride, 5 parts of propenyl benzene amide, 4 parts of bisacrylamide, hydroxyethyl methacrylate
15 parts of propyl ester；
(2) configuration B material is spare, and the B material includes: 3 parts of sodium hydrogensulfite, sodium metabisulfite according to the raw material of parts by weight
4 parts, 1 part of sulfydryl class chain-transferring agent, 4 parts of polyformaldehyde, 1 part of sodium gluconate, 1.2 parts of ascorbic acid, 2 parts of naphtalene oil；
(3) bottom material of 60 parts of unsaturated polyoxyethylene ether and 90 parts of water composition is put into reaction kettle at 40 DEG C；
(4) concentrated sulfuric acid is added or concentrated hydrochloric acid accelerates bottom material dissolution, the solution that mass percent is 65% is made, wherein dense sulphur
The mass percent that acid or concentrated hydrochloric acid account for bottom material is 1%, after bottom material is completely dissolved, and puts into 5 parts of initiators, stirs 5min；
(5) the good B material of configured in advance is then at the uniform velocity added dropwise, is spaced after 10min and A material is at the uniform velocity added dropwise again, the A material accounts for bottom material
15%, the B material of quality accounts for the 12% of bottom material quality；
(6) the A material and B material drip off in 4h, and aging 1.5h is kept the temperature after dripping off, and rear 30% liquid alkaline that is added makes its pH value
Reach 7, obtains prefabrication；
(7) operation is dried to the prefabrication, obtains the high concentration polycarboxylate water-reducer.
The unsaturated polyoxyethylene ether is isoamyl alcohol polyoxyethylene ether, isobutene alcohol polyoxyethylene ether or methyl alkene
The combination of one or more of propyl alcohol polyoxyethylene ether, molecular weight 1000-3000.The initiator is selected from over cure
The combination of one or more of sour ammonium, potassium peroxydisulfate, sodium peroxydisulfate or hydrogen peroxide.The sulfydryl class chain-transferring agent is
One or more of thioacetic acid, mercaptopropionic acid, mercaptoethanol composition.
The time for adding that A, B expect in the present invention extends 1 hour than conventional method time for adding, makes the reaction of product in this way
It sufficiently carries out, the homogeneity of free radical supply in the main initiation system to ensure oxidationreduction, to guarantee water-reducing agent molecular weight point
The fluctuation range of more stability contorting water-reducing agent product water-reducing rate is capable of in cloth centralization, is reduced the water-reducing rate of product, is added to mixed
Concrete product is wrapped more preferable after solidifying soil, increases the mobility of concrete, and the viscosity of concrete product is higher, improves coagulation
The intensity of soil extends to protect and collapse the time.
The preferred embodiment of the patent is described in detail above, but this patent is not limited to above-mentioned embodiment party
Formula within the knowledge of one of ordinary skill in the art can also be under the premise of not departing from this patent objective
Various changes can be made.
Claims (9)
1. a kind of dropwise addition synthesis technology of polycarboxylate water-reducer, which is characterized in that specific step is as follows:
(1) configuration A material is spare, and the A material includes: 20-40 parts of methacrylic acid, maleic acid according to the raw material of parts by weight
15-20 parts, 3-5 parts of MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride, 3-5 parts of propenyl benzene amide, 2-4 parts of bisacrylamide, first
10-15 parts of base hydroxypropyl acrylate；
(2) configuration B material is spare, and the B material includes: 1-3 parts of sodium hydrogensulfite, sodium metabisulfite 2- according to the raw material of parts by weight
4 parts, 0.5-1 parts of sulfydryl class chain-transferring agent, 2-4 parts of polyformaldehyde, 0.5-1 parts of sodium gluconate, 0.8-1.2 parts of ascorbic acid, naphthalene
It is 1-2 parts oily；
(3) bottom material of 40-60 parts of unsaturated polyoxyethylene ether and 70-90 parts of water composition is put into reaction kettle at 20-40 DEG C
In；
(4) concentrated sulfuric acid is added or concentrated hydrochloric acid accelerates bottom material dissolution, the solution that mass percent is 55-65% is made, wherein dense sulphur
The mass percent that acid or concentrated hydrochloric acid account for bottom material is 0.5-1%, after bottom material is completely dissolved, puts into 3-5 parts of initiators, stirs 3-
5min；
(5) the good B material of configured in advance is then at the uniform velocity added dropwise, is spaced after 5-10min and A material is at the uniform velocity added dropwise again, the A material accounts for bottom material matter
The 10-15% of amount, B expect to account for the 8-12% of bottom material quality；
(6) the A material and B material drip off in 2-4h, and aging 1-1.5h is kept the temperature after dripping off, and rear 30% liquid alkaline that is added makes its pH value
Reach 5-7, obtains prefabrication；
(7) operation is dried to the prefabrication, obtains the high concentration polycarboxylate water-reducer.
2. the dropwise addition synthesis technology of polycarboxylate water-reducer according to claim 1, which is characterized in that A in the step (1)
Material includes: 25-35 parts of methacrylic acid, 16-19 parts of maleic acid, methylacryoyloxyethyl three according to the raw material of parts by weight
3.5-4.5 parts of ammonio methacrylate, 3.5-4.5 parts of propenyl benzene amide, 2.5-3.5 parts of bisacrylamide, hydroxy propyl methacrylate
11-14 parts.
3. the dropwise addition synthesis technology of polycarboxylate water-reducer according to claim 2, which is characterized in that A in the step (1)
Material includes: 30 parts of methacrylic acid, 18 parts of maleic acid, methylacryoyloxyethyl trimethyl chlorine according to the raw material of parts by weight
Change 4 parts of ammonium, 4 parts of propenyl benzene amide, 3 parts of bisacrylamide, 12 parts of hydroxy propyl methacrylate.
4. the dropwise addition synthesis technology of polycarboxylate water-reducer according to claim 1, which is characterized in that B in the step (2)
Material includes: 1.5-2.5 parts of sodium hydrogensulfite, 2.5-3.5 parts of sodium metabisulfite, sulfydryl class chain tra nsfer according to the raw material of parts by weight
0.6-0.9 parts of agent, 2.5-3.5 parts of polyformaldehyde, 0.6-0.9 parts of sodium gluconate, 0.9-1.1 parts of ascorbic acid, naphtalene oil 1.2-1.8
Part.
5. the dropwise addition synthesis technology of polycarboxylate water-reducer according to claim 4, which is characterized in that B in the step (2)
Material includes: 2 parts of sodium hydrogensulfite, 3 parts of sodium metabisulfite, 0.8 part of sulfydryl class chain-transferring agent, poly- first according to the raw material of parts by weight
3 parts of aldehyde, 0.8 part of sodium gluconate, 1 part of ascorbic acid, 1.5 parts of naphtalene oil.
6. the dropwise addition synthesis technology of polycarboxylate water-reducer according to claim 1, which is characterized in that the unsaturation is poly-
Ethylene oxide ether is one of isoamyl alcohol polyoxyethylene ether, isobutene alcohol polyoxyethylene ether or methyl allyl alcohol polyoxyethylene ether
Or two or more combinations, molecular weight 1000-3000.
7. the dropwise addition synthesis technology of polycarboxylate water-reducer according to claim 1, which is characterized in that the initiator choosing
From the combination of one or more of ammonium persulfate, potassium peroxydisulfate, sodium peroxydisulfate or hydrogen peroxide.
8. the dropwise addition synthesis technology of polycarboxylate water-reducer according to claim 1, which is characterized in that the sulfydryl class chain turns
Shifting agent is one or more of thioacetic acid, mercaptopropionic acid, mercaptoethanol composition.
9. the dropwise addition synthesis technology of polycarboxylate water-reducer according to claim 8, which is characterized in that the sulfydryl class chain turns
Shifting agent is thioacetic acid.
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| CN117682891A (en) * | 2023-11-29 | 2024-03-12 | 天津市建筑材料科学研究院有限公司 | A kind of composite grinding aid for low-carbon and low-heat cement clinker and its preparation method |
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Application publication date: 20181221 |