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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- 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
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- 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
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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
- 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
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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
- 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
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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
- 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
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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
- 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
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- 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
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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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- 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
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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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