CN105837738B - A kind of anti-mud agent of polycarboxylic-acid cation and its preparation method and application - Google Patents
A kind of anti-mud agent of polycarboxylic-acid cation and its preparation method and application Download PDFInfo
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- CN105837738B CN105837738B CN201610136882.3A CN201610136882A CN105837738B CN 105837738 B CN105837738 B CN 105837738B CN 201610136882 A CN201610136882 A CN 201610136882A CN 105837738 B CN105837738 B CN 105837738B
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- polycarboxylic
- mud agent
- acid cation
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- 239000002253 acid Substances 0.000 title claims abstract description 50
- 239000003795 chemical substances by application Substances 0.000 title claims abstract description 48
- 150000001768 cations Chemical class 0.000 title claims abstract description 38
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- 239000003638 chemical reducing agent Substances 0.000 claims abstract description 20
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims abstract description 19
- 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 18
- JPAOMENBKRZQDR-UHFFFAOYSA-N CC=CC.[Na] Chemical compound CC=CC.[Na] JPAOMENBKRZQDR-UHFFFAOYSA-N 0.000 claims abstract description 18
- BDHFUVZGWQCTTF-UHFFFAOYSA-M sulfonate Chemical compound [O-]S(=O)=O BDHFUVZGWQCTTF-UHFFFAOYSA-M 0.000 claims abstract description 18
- GNSFRPWPOGYVLO-UHFFFAOYSA-N 3-hydroxypropyl 2-methylprop-2-enoate Chemical compound CC(=C)C(=O)OCCCO GNSFRPWPOGYVLO-UHFFFAOYSA-N 0.000 claims abstract description 16
- 229920005646 polycarboxylate Polymers 0.000 claims abstract description 7
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 61
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 46
- 239000007788 liquid Substances 0.000 claims description 37
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 32
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 32
- 239000008367 deionised water Substances 0.000 claims description 25
- 229910021641 deionized water Inorganic materials 0.000 claims description 25
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical group [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 claims description 24
- 235000011121 sodium hydroxide Nutrition 0.000 claims description 23
- 239000000243 solution Substances 0.000 claims description 19
- UEEJHVSXFDXPFK-UHFFFAOYSA-N N-dimethylaminoethanol Chemical compound CN(C)CCO UEEJHVSXFDXPFK-UHFFFAOYSA-N 0.000 claims description 16
- FPYJFEHAWHCUMM-UHFFFAOYSA-N maleic anhydride Chemical compound O=C1OC(=O)C=C1 FPYJFEHAWHCUMM-UHFFFAOYSA-N 0.000 claims description 16
- FDRCDNZGSXJAFP-UHFFFAOYSA-M sodium chloroacetate Chemical compound [Na+].[O-]C(=O)CCl FDRCDNZGSXJAFP-UHFFFAOYSA-M 0.000 claims description 15
- 229910001870 ammonium persulfate Inorganic materials 0.000 claims description 12
- 238000013329 compounding Methods 0.000 claims description 9
- 239000002994 raw material Substances 0.000 claims description 9
- 239000007864 aqueous solution Substances 0.000 claims description 8
- 238000006243 chemical reaction Methods 0.000 claims description 7
- JRKICGRDRMAZLK-UHFFFAOYSA-L peroxydisulfate Chemical compound [O-]S(=O)(=O)OOS([O-])(=O)=O JRKICGRDRMAZLK-UHFFFAOYSA-L 0.000 claims description 7
- 238000003756 stirring Methods 0.000 claims description 7
- 238000010792 warming Methods 0.000 claims description 7
- 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
- 229920002818 (Hydroxyethyl)methacrylate Polymers 0.000 claims 2
- WOBHKFSMXKNTIM-UHFFFAOYSA-N Hydroxyethyl methacrylate Chemical compound CC(=C)C(=O)OCCO WOBHKFSMXKNTIM-UHFFFAOYSA-N 0.000 claims 2
- QOSMNYMQXIVWKY-UHFFFAOYSA-N Propyl levulinate Chemical compound CCCOC(=O)CCC(C)=O QOSMNYMQXIVWKY-UHFFFAOYSA-N 0.000 claims 2
- 239000004567 concrete Substances 0.000 abstract description 16
- 239000000178 monomer Substances 0.000 abstract description 9
- 239000004927 clay Substances 0.000 abstract description 6
- 230000000694 effects Effects 0.000 abstract description 5
- 238000002474 experimental method Methods 0.000 abstract description 5
- 230000010148 water-pollination Effects 0.000 abstract description 4
- 239000000654 additive Substances 0.000 abstract description 3
- 239000006185 dispersion Substances 0.000 abstract description 3
- 230000002401 inhibitory effect Effects 0.000 abstract description 2
- 238000004519 manufacturing process Methods 0.000 abstract description 2
- 229920000642 polymer Polymers 0.000 abstract description 2
- 238000001179 sorption measurement Methods 0.000 abstract description 2
- 150000007513 acids Chemical class 0.000 description 10
- 238000000034 method Methods 0.000 description 6
- 238000012360 testing method Methods 0.000 description 6
- 229960002887 deanol Drugs 0.000 description 5
- 239000012972 dimethylethanolamine Substances 0.000 description 5
- 239000003643 water by type Substances 0.000 description 5
- 239000004576 sand Substances 0.000 description 4
- 239000004568 cement Substances 0.000 description 3
- 238000010998 test method Methods 0.000 description 3
- 239000002202 Polyethylene glycol Substances 0.000 description 2
- 239000004566 building material Substances 0.000 description 2
- 150000001732 carboxylic acid derivatives Chemical class 0.000 description 2
- GUJOJGAPFQRJSV-UHFFFAOYSA-N dialuminum;dioxosilane;oxygen(2-);hydrate Chemical compound O.[O-2].[O-2].[O-2].[Al+3].[Al+3].O=[Si]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O GUJOJGAPFQRJSV-UHFFFAOYSA-N 0.000 description 2
- 230000003467 diminishing effect Effects 0.000 description 2
- 150000002148 esters Chemical class 0.000 description 2
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 229910052901 montmorillonite Inorganic materials 0.000 description 2
- 239000004570 mortar (masonry) Substances 0.000 description 2
- 229920001223 polyethylene glycol Polymers 0.000 description 2
- 239000002002 slurry Substances 0.000 description 2
- 239000002689 soil Substances 0.000 description 2
- XNWFRZJHXBZDAG-UHFFFAOYSA-N 2-METHOXYETHANOL Chemical compound COCCO XNWFRZJHXBZDAG-UHFFFAOYSA-N 0.000 description 1
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
- CERQOIWHTDAKMF-UHFFFAOYSA-N Methacrylic acid Chemical compound CC(=C)C(O)=O CERQOIWHTDAKMF-UHFFFAOYSA-N 0.000 description 1
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 1
- VMHLLURERBWHNL-UHFFFAOYSA-M Sodium acetate Chemical compound [Na+].CC([O-])=O VMHLLURERBWHNL-UHFFFAOYSA-M 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000000460 chlorine Substances 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 230000032050 esterification Effects 0.000 description 1
- 238000005886 esterification reaction Methods 0.000 description 1
- NLVXSWCKKBEXTG-UHFFFAOYSA-M ethenesulfonate Chemical compound [O-]S(=O)(=O)C=C NLVXSWCKKBEXTG-UHFFFAOYSA-M 0.000 description 1
- 125000000816 ethylene group Chemical class [H]C([H])([*:1])C([H])([H])[*:2] 0.000 description 1
- 239000011396 hydraulic cement Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 229920000151 polyglycol Polymers 0.000 description 1
- 239000010695 polyglycol Substances 0.000 description 1
- 239000011591 potassium Substances 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- XAEFZNCEHLXOMS-UHFFFAOYSA-M potassium benzoate Chemical compound [K+].[O-]C(=O)C1=CC=CC=C1 XAEFZNCEHLXOMS-UHFFFAOYSA-M 0.000 description 1
- 238000010526 radical polymerization reaction Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000001632 sodium acetate Substances 0.000 description 1
- 235000017281 sodium acetate Nutrition 0.000 description 1
- 239000003583 soil stabilizing agent Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 150000005846 sugar alcohols Polymers 0.000 description 1
- 229920002554 vinyl polymer Polymers 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
- C08F220/26—Esters containing oxygen in addition to the carboxy oxygen
- C08F220/28—Esters containing oxygen in addition to the carboxy oxygen containing no aromatic rings in the alcohol moiety
-
- 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
- C04B24/161—Macromolecular compounds comprising sulfonate or sulfate groups
- C04B24/163—Macromolecular compounds comprising sulfonate or sulfate groups obtained by reactions only involving carbon-to-carbon unsaturated bonds
-
- 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
- C04B2103/0068—Ingredients with a function or property not provided for elsewhere in C04B2103/00
-
- 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
- C08F220/26—Esters containing oxygen in addition to the carboxy oxygen
- C08F220/28—Esters containing oxygen in addition to the carboxy oxygen containing no aromatic rings in the alcohol moiety
- C08F220/281—Esters containing oxygen in addition to the carboxy oxygen containing no aromatic rings in the alcohol moiety and containing only one oxygen, e.g. furfuryl (meth)acrylate or 2-methoxyethyl (meth)acrylate
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Organic Chemistry (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)
Abstract
The invention discloses anti-mud agent of a kind of polycarboxylic-acid cation and its preparation method and application, it is related to technical field of concrete additives, the present invention replaces the preferable side chain monomer of hydrophily using the poor hydroxy propyl methacrylate of hydrophily, a kind of monomer with partial cation electric charge is synthesized, using acrylic acid and methylpropene sodium sulfonate as Anion-adsorption monomer, molecular weight polymers have been synthesized by Raolical polymerizable.It the experiment proved that, in aggregate clay content under the same conditions, the dispersion effect of polycarboxylate water-reducer added with the anti-mud agent of the present invention is remarkably reinforced, improve concrete initial fluidity, reduce slump-loss, concrete crushing strength improves 1.5~3MPa, there is good inhibiting effect, suitable industrial mass production to clay content.
Description
Technical field
The present invention relates to technical field of concrete additives, and in particular to a kind of anti-mud agent of polycarboxylic-acid cation and its system
Preparation Method and application.
Background technology
The third generation water-reducing agent of building material industry is the high-performance water reducing agent using polycarboxylic acids as representative, high with its high diminishing
The favor protected the excellent properties to collapse and good environmental protection characteristic and make it enjoy building material industry.Polycarboxylate water-reducer is in concreter
While extensive use is obtained in journey, the defects of some are obvious is also exposed, the soil particularly contained in sandstone makes polycarboxylic acids
The performance of based water reducer is greatly affected, and causes that concrete fluidity is poor, and slump-loss is big.In recent years, with natural sand
Exhaustion, Machine-made Sand or second-rate natural sand instead, plus various aggregates clay content occupy height do not drop, to polycarboxylic-acid
Water-reducing agent performance produces a very large impact, and causes that concrete fluidity is poor, and slump-loss is big.Under such circumstances, it is necessary to grind
Send out water-reducing agent new, or research and develop some anti-mud additives and existing poly carboxylic acid series water reducer compounding use, to eliminate or subtract
The negative effect that weak cement content height produces poly carboxylic acid series water reducer, while improve the working performance of concrete.
At present, the existing report in terms of anti-mud agent on a small quantity.Patent CN102617811A proposes a kind of two sex ethylenes
The preparation method of based polyalcohol agent on crack resistance of concrete mud agent.Its preparation method is：Using methacrylic acid and poly glycol monomethyl ether into
Row esterification prepares polyethylene glycol monomethyl ethermethacrylic acid esters, then again by polyethylene glycol monomethyl ethermethacrylic acid esters,
Acrylic monomer, cationic vinyl monomer and vinyl sulfonate monomers are made by free radical polymerization.Patent
CN102775088A proposes a kind of resistance chamotte mould cement water reducing agent and preparation method, by by quaternary soil stabilizer,
Inorganic potassium salt, organophosphor antisludging agent and polycarboxylic acids water reducing agent compositional use.Both anti-mud agent are adapted to just for specific soil
Face is not wide.
The content of the invention
It is an object of the invention to provide anti-mud agent of a kind of polycarboxylic-acid cation and preparation method thereof.
In order to achieve the above object, the present invention is achieved by the following technical programs：
A kind of anti-mud agent of polycarboxylic-acid cation, is made of the raw material of following parts by weight：40~60 parts of maleic anhydride,
N, 40~90 parts of N dimethyl monoethanolamine, 30~50 parts of sodium chloroacetate, 30~50 parts of acrylic acid, hydroxy propyl methacrylate 50~
70 parts, 10~20 parts of methylpropene sodium sulfonate, 1.5~4 parts of persulfate, 30% 1~3 part of hydrogen peroxide, acetone 140~200
Part, 2~5 parts of VC, 32% 40~80 parts of sodium hydrate aqueous solution, appropriate deionized water.
Preferably, it is made of the raw material of following parts by weight：49 parts of maleic anhydride, N, 45 parts of N dimethyl monoethanolamine, chlorine
47 parts of sodium acetate, 36 parts of acrylic acid, 65 parts of hydroxy propyl methacrylate, 11.2 parts of methylpropene sodium sulfonate, persulfate 2.1
Part, 30% 2.2 parts of hydrogen peroxide, 150 parts of acetone, 2.2 parts of VC, 32% 40~80 parts of sodium hydrate aqueous solution, deionized water
In right amount.
Preferably, the persulfate is ammonium persulfate or potassium peroxydisulfate.
Preferably, the VC is pharmaceutical grade.
The preparation method of the anti-mud agent of polycarboxylic-acid cation, comprises the following steps：
1) by maleic anhydride dissolving in acetone, at the uniform velocity it is added dropwise N, N dimethyl monoethanolamine controls the time for adding to be
15-20min, keeps 5h in the range of 10-20 DEG C of constant temperature, is then heated to 65 DEG C and boils off acetone, cools down；
2) to adding appropriate amount of deionized water in step 1), system pH is adjusted to 9 with sodium hydroxide solution, while stirring
Sodium chloroacetate is added, 5h is reacted under the conditions of 25-40 DEG C；
3) hydroxy propyl methacrylate, acrylic acid, VC and methylpropene sodium sulfonate are dissolved in suitable deionized water,
It is uniformly mixed, as A liquid, separately takes ammonium persulfate, hydrogen peroxide to be dissolved in appropriate amount of deionized water, is uniformly mixed, as B liquid；
4) temperature of reaction system of step 2) is risen into 30-60 DEG C, while a dropping step 3) in A liquid and B liquid, control A
In 2-3h, B liquid time for adding is warming up to 60-80 DEG C and keeps 2-3h in 2-3.5h liquid time for adding after all dripping off；
5) system pH is adjusted to 9 with sodium hydroxide solution, you can obtain finished product.
The application of the anti-mud agent of polycarboxylic-acid cation, is the poly- carboxylic that the anti-mud agent of polycarboxylic-acid cation is replaced to 5%-20%
Sour water-reducing agent, carries out compounding use.
Beneficial effect of the present invention：The present invention replaces hydrophily preferable using the poor hydroxy propyl methacrylate of hydrophily
Side chain monomer, has synthesized a kind of monomer with partial cation electric charge, using acrylic acid and methylpropene sodium sulfonate as cloudy
Ionic adsorption monomer, molecular weight polymers have been synthesized by Raolical polymerizable.It the experiment proved that, it is identical in aggregate clay content
Under conditions of, the dispersion effect of the polycarboxylate water-reducer added with the anti-mud agent of the present invention is remarkably reinforced, and improves concrete initial flow
Dynamic property, reduces slump-loss, and concrete crushing strength improves 1.5~3MPa, has good inhibiting effect to clay content, suitably
Industrial mass production.
Embodiment
To make the purpose, technical scheme and advantage of the embodiment of the present invention clearer, below in conjunction with the embodiment of the present invention,
Technical solution in the embodiment of the present invention is clearly and completely described, it is clear that described embodiment is the present invention one
Divide embodiment, instead of all the embodiments.Based on the embodiments of the present invention, those of ordinary skill in the art are not making
All other embodiments obtained under the premise of creative work, belong to the scope of protection of the invention.
Embodiment 1：
A kind of anti-mud agent of polycarboxylic-acid cation, is made of the raw material of following parts by weight：49 parts of maleic anhydride, N, N
45 parts of dimethylethanolamine, 47 parts of sodium chloroacetate, 36 parts of acrylic acid, 65 parts of hydroxy propyl methacrylate, methylpropene sodium sulfonate
11.2 parts, 2.1 parts of ammonium persulfate, 30% 2.2 parts of hydrogen peroxide, 150 parts of acetone, 2.2 parts of VC, 32% sodium hydroxide it is water-soluble
50 parts of liquid, appropriate deionized water.
The preparation method of the anti-mud agent of polycarboxylic-acid cation, comprises the following steps：
1) by maleic anhydride dissolving in acetone, at the uniform velocity it is added dropwise N, N dimethyl monoethanolamine controls the time for adding to be
20min, keeps 5h in the range of 10 DEG C of constant temperature, is then heated to 65 DEG C and boils off acetone, cools down；
2) to adding 200 parts of deionized waters in step 1), system pH is adjusted to 9 with sodium hydroxide solution, stirring it is same
When add sodium chloroacetate, react 5h under the conditions of 30 DEG C；
3) hydroxy propyl methacrylate, acrylic acid, VC and methylpropene sodium sulfonate are dissolved in 100 parts of deionized water
In, it is uniformly mixed, as A liquid, separately takes ammonium persulfate, hydrogen peroxide to be dissolved in 120 parts of deionized waters, is uniformly mixed, as B liquid；
4) temperature of reaction system of step 2) is risen into 50 DEG C, while a dropping step 3) in A liquid and B liquid, control A drops
In 3h between added-time, B liquid time for adding is warming up to 80 DEG C and keeps 2h in 3.5h after all dripping off；
5) system pH is adjusted to 9 with sodium hydroxide solution, you can obtain finished product.
The application of the anti-mud agent of polycarboxylic-acid cation, is to subtract the anti-mud agent of polycarboxylic-acid cation instead of 9% polycarboxylic acids
Aqua, carries out compounding use.
Embodiment 2：
A kind of anti-mud agent of polycarboxylic-acid cation, is made of the raw material of following parts by weight：49 parts of maleic anhydride, N, N
90 parts of dimethylethanolamine, 50 parts of sodium chloroacetate, 40 parts of acrylic acid, 60 parts of hydroxy propyl methacrylate, methylpropene sodium sulfonate
14 parts, 3.1 parts of ammonium persulfate, 30% 1.2 parts of hydrogen peroxide, 150 parts of acetone, 2 parts of VC, 32% sodium hydrate aqueous solution 55
Part, appropriate deionized water.
The preparation method of the anti-mud agent of polycarboxylic-acid cation, comprises the following steps：
1) by maleic anhydride dissolving in acetone, at the uniform velocity it is added dropwise N, N dimethyl monoethanolamine controls the time for adding to be
20min, keeps 5h in the range of 10 DEG C of constant temperature, is then heated to 65 DEG C and boils off acetone, cools down；
2) to adding 200 parts of deionized waters in step 1), system pH is adjusted to 9 with sodium hydroxide solution, stirring it is same
When add sodium chloroacetate, react 5h under the conditions of 30 DEG C；
3) hydroxy propyl methacrylate, acrylic acid, VC and methylpropene sodium sulfonate are dissolved in 100 parts of deionized waters,
It is uniformly mixed, as A liquid, separately takes ammonium persulfate, hydrogen peroxide to be dissolved in 120 parts of deionized waters, is uniformly mixed, as B liquid；
4) temperature of reaction system of step 2) is risen into 50 DEG C, while a dropping step 3) in A liquid and B liquid, control A drops
In 2h between added-time, B liquid time for adding is warming up to 80 DEG C and keeps 3h in 2.5h after all dripping off；
5) system pH is adjusted to 9 with sodium hydroxide solution, you can obtain finished product.
The application of the anti-mud agent of polycarboxylic-acid cation, is to subtract the anti-mud agent of polycarboxylic-acid cation instead of 15% polycarboxylic acids
Aqua, carries out compounding use.
Embodiment 3：
A kind of anti-mud agent of polycarboxylic-acid cation, is made of the raw material of following parts by weight：60 parts of maleic anhydride, N, N
50 parts of dimethylethanolamine, 50 parts of sodium chloroacetate, 40 parts of acrylic acid, 70 parts of hydroxy propyl methacrylate, methylpropene sodium sulfonate
10 parts, 3.5 parts of potassium peroxydisulfate, 30% 2 parts of hydrogen peroxide, 200 parts of acetone, 2 parts of VC, 32% 56 parts of sodium hydrate aqueous solution,
Appropriate deionized water.
The preparation method of the anti-mud agent of polycarboxylic-acid cation, comprises the following steps：
1) by maleic anhydride dissolving in acetone, at the uniform velocity it is added dropwise N, N dimethyl monoethanolamine controls the time for adding to be
15min, keeps 5h in the range of 15 DEG C of constant temperature, is then heated to 65 DEG C and boils off acetone, cools down；
2) to adding appropriate amount of deionized water in step 1), system pH is adjusted to 9 with sodium hydroxide solution, while stirring
Sodium chloroacetate is added, reacts 5h under the conditions of 35 DEG C；
3) hydroxy propyl methacrylate, acrylic acid, VC and methylpropene sodium sulfonate are dissolved in suitable deionized water,
It is uniformly mixed, as A liquid, separately takes ammonium persulfate, hydrogen peroxide to be dissolved in appropriate amount of deionized water, is uniformly mixed, as B liquid；
4) temperature of reaction system of step 2) is risen into 60 DEG C, while a dropping step 3) in A liquid and B liquid, control A drops
In 2.5h between added-time, B liquid time for adding is warming up to 80 DEG C and keeps 2.5h in 2.5h after all dripping off；
5) system pH is adjusted to 9 with sodium hydroxide solution, you can obtain finished product.
The application of the anti-mud agent of polycarboxylic-acid cation, is to subtract the anti-mud agent of polycarboxylic-acid cation instead of 20% polycarboxylic acids
Aqua, carries out compounding use.
Embodiment 4：
A kind of anti-mud agent of polycarboxylic-acid cation, is made of the raw material of following parts by weight：40 parts of maleic anhydride, N, N
90 parts of dimethylethanolamine, 30 parts of sodium chloroacetate, 50 parts of acrylic acid, 50 parts of hydroxy propyl methacrylate, methylpropene sodium sulfonate
15 parts, 1.5 parts of persulfate potassium, 30% 3 parts of hydrogen peroxide, 140 parts of acetone, 3.5 parts of VC, 32% sodium hydrate aqueous solution
70 parts, appropriate deionized water.
The preparation method of the anti-mud agent of polycarboxylic-acid cation, comprises the following steps：
1) by maleic anhydride dissolving in acetone, at the uniform velocity it is added dropwise N, N dimethyl monoethanolamine controls the time for adding to be
20min, keeps 5h in the range of 20 DEG C of constant temperature, is then heated to 65 DEG C and boils off acetone, cools down；
2) to adding appropriate amount of deionized water in step 1), system pH is adjusted to 9 with sodium hydroxide solution, while stirring
Sodium chloroacetate is added, reacts 5h under the conditions of 30 DEG C；
3) hydroxy propyl methacrylate, acrylic acid, VC and methylpropene sodium sulfonate are dissolved in suitable deionized water,
It is uniformly mixed, as A liquid, separately takes ammonium persulfate, hydrogen peroxide to be dissolved in appropriate amount of deionized water, is uniformly mixed, as B liquid；
4) temperature of reaction system of step 2) is risen into 40 DEG C, while a dropping step 3) in A liquid and B liquid, control A drops
In 3h between added-time, B liquid time for adding is warming up to 60 DEG C and keeps 3h in 3.5h after all dripping off；
5) system pH is adjusted to 9 with sodium hydroxide solution, you can obtain finished product.
The application of the anti-mud agent of polycarboxylic-acid cation, is to subtract the anti-mud agent of polycarboxylic-acid cation instead of 5% polycarboxylic acids
Aqua, carries out compounding use.
Embodiment 5：
A kind of anti-mud agent of polycarboxylic-acid cation, is made of the raw material of following parts by weight：55 parts of maleic anhydride, N, N
70 parts of dimethylethanolamine, 45 parts of sodium chloroacetate, 40 parts of acrylic acid, 65 parts of hydroxy propyl methacrylate, methylpropene sodium sulfonate
14 parts, 2.5 parts of ammonium persulfate, 30% 2.5 parts of hydrogen peroxide, 160 parts of acetone, 3 parts of VC, 32% sodium hydrate aqueous solution 60
Part, appropriate deionized water.
The preparation method of the anti-mud agent of polycarboxylic-acid cation, comprises the following steps：
1) by maleic anhydride dissolving in acetone, at the uniform velocity it is added dropwise N, N dimethyl monoethanolamine controls the time for adding to be
15min, keeps 5h in the range of 15 DEG C of constant temperature, is then heated to 65 DEG C and boils off acetone, cools down；
2) to adding appropriate amount of deionized water in step 1), system pH is adjusted to 9 with sodium hydroxide solution, while stirring
Sodium chloroacetate is added, reacts 5h under the conditions of 40 DEG C；
3) hydroxy propyl methacrylate, acrylic acid, VC and methylpropene sodium sulfonate are dissolved in appropriate amount of deionized water, mixed
Close uniformly, as A liquid, separately take ammonium persulfate, hydrogen peroxide to be dissolved in appropriate amount of deionized water, be uniformly mixed, as B liquid；
4) temperature of reaction system of step 2) is risen into 55 DEG C, while a dropping step 3) in A liquid and B liquid, control A drops
In 2h between added-time, B liquid time for adding is warming up to 70 DEG C and keeps 2.5h in 3h after all dripping off；
5) system pH is adjusted to 9 with sodium hydroxide solution, you can obtain finished product.
The application of the anti-mud agent of polycarboxylic-acid cation, is to subtract the anti-mud agent of polycarboxylic-acid cation instead of 20% polycarboxylic acids
Aqua, carries out compounding use.
Case study on implementation：
The anti-mud agent of polycarboxylic-acid cation prepared by Example 1 and Example 2 of the present invention and polycarboxylic acids water reducing agent compositional,
The compounding water-reducing agent with anti-mud effect is obtained, and detects its performance parameter, the net slurry test of implementation result experiment is according to national standard GB/
T 8077-2012《Concrete admixture uniformity test method》Carry out, mixed in montmorillonite, substitute the cement of corrresponding quality.Sand
Slurry test is according to national standard GB/T 19671-1999《Test method for strength of hydraulic cement mortar》Carry out, testing concrete performance is with reference to state
Mark GB/T 50080-2002《Standard for test methods of properties of ordinary concrete mixture》Carry out.
Anti- mud agent made from embodiment 1 is replaced to 9% and 15% polycarboxylate water-reducer, numbering respectively No. 1,2 respectively
Number, by anti-mud agent made from embodiment 2 respectively replace 9% and 15% polycarboxylate water-reducer, numbering be respectively No. 3 and No. 4, reality
It is as follows to test result：
1st, paste flowing degree is tested
Table 1
2nd, additional montmorillonite water-reducing agent Mortar'S Flowability experiment
Table 2
3rd, concrete experiments
Concrete mix is as follows：
Table 3
Test result is as follows：
Table 4
Above test result indicates that, in aggregate clay content under the same conditions, the compositional liquor diminishing of anti-mud agent and polycarboxylic acids
Agent, its dispersion effect are substantially better than common polycarboxylate water-reducer, and concrete slump keeps also preferable.
It should be noted that herein, relational terms such as first and second and the like are used merely to a reality
Body or operation are distinguished with another entity or operation, are deposited without necessarily requiring or implying between these entities or operation
In any this actual relation or order.Moreover, term " comprising ", "comprising" or its any other variant are intended to
Non-exclusive inclusion, so that process, method, article or equipment including a series of elements not only will including those
Element, but also including other elements that are not explicitly listed, or further include as this process, method, article or equipment
Intrinsic key element.In the absence of more restrictions, the key element limited by sentence "including a ...", it is not excluded that
Also there are other identical element in process, method, article or equipment including the key element.
The above embodiments are merely illustrative of the technical solutions of the present invention, rather than its limitations；Although with reference to the foregoing embodiments
The present invention is described in detail, it will be understood by those of ordinary skill in the art that：It still can be to foregoing each implementation
Technical solution described in example is modified, or carries out equivalent substitution to which part technical characteristic；And these modification or
Replace, the essence of appropriate technical solution is departed from the spirit and scope of various embodiments of the present invention technical solution.
Claims (6)
1. a kind of anti-mud agent of polycarboxylic-acid cation, it is characterised in that be made of the raw material of following parts by weight：Maleic anhydride
40~60 parts, N, 40~90 parts of N dimethyl monoethanolamine, 30~50 parts of sodium chloroacetate, 30~50 parts of acrylic acid, hydroxyethyl methacrylate
50~70 parts of propyl ester, 10~20 parts of methylpropene sodium sulfonate, 1.5~4 parts of persulfate, 30% 1~3 part of hydrogen peroxide, acetone
140~200 parts, 2~5 parts of VC, 32% 40~80 parts of sodium hydrate aqueous solution, appropriate deionized water.
2. the anti-mud agent of polycarboxylic-acid cation as claimed in claim 1, it is characterised in that by the raw material system of following parts by weight
Into：49 parts of maleic anhydride, N, 45 parts of N dimethyl monoethanolamine, 47 parts of sodium chloroacetate, 36 parts of acrylic acid, hydroxyethyl methacrylate
65 parts of propyl ester, 11.2 parts of methylpropene sodium sulfonate, 2.1 parts of persulfate, 30% 2.2 parts of hydrogen peroxide, 150 parts of acetone, VC
2.2 parts, 32% 40~80 parts of sodium hydrate aqueous solution, appropriate deionized water.
3. the anti-mud agent of polycarboxylic-acid cation as claimed in claim 2, it is characterised in that the persulfate is ammonium persulfate
Or potassium peroxydisulfate.
4. the anti-mud agent of polycarboxylic-acid cation as claimed in claim 2, it is characterised in that the VC is pharmaceutical grade.
5. the preparation method of the anti-mud agent of polycarboxylic-acid cation as described in claim 1-4 is any, it is characterised in that including with
Lower step：
1) by maleic anhydride dissolving in acetone, N is at the uniform velocity added dropwise, N dimethyl monoethanolamine, it is 15- to control time for adding
20min, keeps 5h in the range of 10-20 DEG C of constant temperature, is then heated to 65 DEG C and boils off acetone, cools down；
2) to adding appropriate amount of deionized water in step 1), system pH is adjusted to 9 with sodium hydroxide solution, stirring while adds
Sodium chloroacetate, reacts 5h under the conditions of 25-40 DEG C；
3) hydroxy propyl methacrylate, acrylic acid, VC and methylpropene sodium sulfonate are dissolved in suitable deionized water, mixed
Uniformly, as A liquid, separately take ammonium persulfate, hydrogen peroxide to be dissolved in appropriate amount of deionized water, be uniformly mixed, as B liquid；
4) temperature of reaction system of step 2) is risen into 30-60 DEG C, while a dropping step 3) in A liquid and B liquid, control A drops
In 2-3h between added-time, B liquid time for adding is warming up to 60-80 DEG C and keeps 2-3h in 2-3.5h after all dripping off；
5) system pH is adjusted to 9 with sodium hydroxide solution, you can obtain finished product.
6. the application of the anti-mud agent of polycarboxylic-acid cation as claimed in claim 1, it is characterised in that be by polycarboxylic-acid sun from
The anti-mud agent of son replaces the polycarboxylate water-reducer of 5%-20%, carries out compounding use.
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| CN106478896B (en) * | 2016-10-31 | 2019-07-19 | 科之杰新材料集团有限公司 | A kind of preparation method of comprehensive polycarboxylate water-reducer |
| CN109575260B (en) * | 2018-11-30 | 2021-12-14 | 中建西部建设股份有限公司 | Quaternary ammonium salt type concrete anti-mud agent and preparation method thereof |
| CN110845663A (en) * | 2019-12-06 | 2020-02-28 | 佛山市华轩新材料有限公司 | Concrete anti-mud agent |
| CN112960935A (en) * | 2021-02-25 | 2021-06-15 | 贵州天威建材科技有限责任公司 | Special mud-resistant sacrificial agent for polycarboxylic acid water reducer and preparation method thereof |
| CN116553857B (en) * | 2023-05-15 | 2024-07-16 | 山东恒丰天利新材料科技有限公司 | Small molecule anti-mud agent |
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| CN102617811A (en) * | 2012-03-21 | 2012-08-01 | 陕西科技大学 | Preparation method of amphiprotic vinyl polymer concrete mud-resistant agent |
| CN102775088A (en) * | 2012-07-24 | 2012-11-14 | 苏州鼎恩建材科技有限公司 | Damped water reducing agent and preparation method for concrete |
| CN104177543A (en) * | 2014-08-18 | 2014-12-03 | 武汉格瑞林葛店混凝土外加剂有限公司 | Concrete anti-mud agent and preparation method thereof |
| CN105085822A (en) * | 2015-08-07 | 2015-11-25 | 科之杰新材料集团有限公司 | Sludge-proof type polycarboxylate water-reducer and normal temperature preparing method thereof |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102617811A (en) * | 2012-03-21 | 2012-08-01 | 陕西科技大学 | Preparation method of amphiprotic vinyl polymer concrete mud-resistant agent |
| CN102775088A (en) * | 2012-07-24 | 2012-11-14 | 苏州鼎恩建材科技有限公司 | Damped water reducing agent and preparation method for concrete |
| CN104177543A (en) * | 2014-08-18 | 2014-12-03 | 武汉格瑞林葛店混凝土外加剂有限公司 | Concrete anti-mud agent and preparation method thereof |
| CN105085822A (en) * | 2015-08-07 | 2015-11-25 | 科之杰新材料集团有限公司 | Sludge-proof type polycarboxylate water-reducer and normal temperature preparing method thereof |
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