CN109053977A - A kind of collapse protective poly-carboxylic acid water reducing agent and preparation method thereof - Google Patents

A kind of collapse protective poly-carboxylic acid water reducing agent and preparation method thereof Download PDF

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CN109053977A
CN109053977A CN201810836950.6A CN201810836950A CN109053977A CN 109053977 A CN109053977 A CN 109053977A CN 201810836950 A CN201810836950 A CN 201810836950A CN 109053977 A CN109053977 A CN 109053977A
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mixed solution
reducing agent
parts
carboxylic acid
preparation
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杨美跃
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Beijing Baochen Joint Polytron Technologies Inc
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    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08FMACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F293/00Macromolecular compounds obtained by polymerisation on to a macromolecule having groups capable of inducing the formation of new polymer chains bound exclusively at one or both ends of the starting macromolecule
    • C08F293/005Macromolecular compounds obtained by polymerisation on to a macromolecule having groups capable of inducing the formation of new polymer chains bound exclusively at one or both ends of the starting macromolecule using free radical "living" or "controlled" polymerisation, e.g. using a complexing agent
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B24/00Use of organic materials as active ingredients for mortars, concrete or artificial stone, e.g. plasticisers
    • C04B24/24Macromolecular compounds
    • C04B24/26Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
    • C04B24/2688Copolymers containing at least three different monomers
    • C04B24/2694Copolymers containing at least three different monomers containing polyether side chains
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08FMACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F2/00Processes of polymerisation
    • C08F2/38Polymerisation using regulators, e.g. chain terminating agents, e.g. telomerisation
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08FMACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F4/00Polymerisation catalysts
    • C08F4/40Redox systems
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2103/00Function or property of ingredients for mortars, concrete or artificial stone
    • C04B2103/0045Polymers chosen for their physico-chemical characteristics
    • C04B2103/0061Block (co-)polymers
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2103/00Function or property of ingredients for mortars, concrete or artificial stone
    • C04B2103/30Water reducers, plasticisers, air-entrainers, flow improvers
    • C04B2103/302Water reducers

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  • 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)
  • Curing Cements, Concrete, And Artificial Stone (AREA)

Abstract

The invention discloses a kind of collapse protective poly-carboxylic acid water reducing agents and preparation method thereof, the present invention using allyl polyether polymeric monomer, esters of acrylic acid and acrylic monomer as main monomer, using oxidation-reduction agent as initiator, chain-transferring agent is added to carry out copolymerization and pass through the block copolymer of control the acrylic acid synthesizing class and esters of acrylic acid of synthesis technology.The present invention is designed by the structure of block, has been provided simultaneously with diminishing and has been protected the performance collapsed, and the compatibility issue of traditional Compositional type function water-reducing agent and material is avoided, and the guarantor of the polycarboxylate water-reducer synthesized collapses the time for 4-6h.

Description

A kind of collapse protective poly-carboxylic acid water reducing agent and preparation method thereof
Technical field
The present invention relates to a kind of water-reducing agents, and in particular to a kind of collapse protective poly-carboxylic acid water reducing agent and preparation method thereof.
Technical background
Polycarboxylate water-reducer due to the flexible design and change of its molecular structure, make it have low-dosage, high water reducing rate, can The molecular structure of control, it is good dispersed, environmentally protective, adaptable the advantages that, by domestic and international numerous scholars and expert Pay attention to and studies.Polycarboxylate water-reducer begins one's study so far from mid-term the 1980s, is promoted in synthetic technology, properties of product Etc. there has been significant progress, compared with the states such as America and Europe, the country starts late, and grinds since phase late 1990s System, by nearly research of technique in 20 years, the gap of home products and external product increasingly reduces, be widely applied with railway, The key project of the related fieldss such as highway, nuclear power, water conservancy.
Slump-loss is the main problem faced in modern concrete construction, and many scholars at home and abroad are to concrete Slump-loss mechanism and control method are furtherd investigate, and have developed it is some be capable of effectively inhibition of slump-loss it is additional Agent product.The main function of collapse protective poly-carboxylic acid water reducing agent is that concrete mix is enable to keep flowing in a long time Property, to meet the construction needs of modern concrete.Its main design thought is to be crosslinked and introduce response type molecule knot by being formed Structure monomer realizes its function of slump protection.Currently, Molecular Design thinking is in the majority using the latter, directly using esters monomer in alkali Property environment in hydrolysis properties: with the progress of hydrated cementitious, concrete hole solution is in alkalinity, and esters monomer is in alkaline environment It can gradually hydrolyze, the carboxyl that polymer molecule is formed in hydrolytic process will constantly adsorb cement granules, disperse, thus Ensure that concrete there can be good mobility in a long time.
Summary of the invention
In order to solve the above technical problems, the present invention provides a kind of collapse protective poly-carboxylic acid water reducing agent and preparation method thereof, Technique is added dropwise using segmentation in the preparation method, can synthesize the polycarboxylate water-reducer with high-collapse-retentivity.
The technical scheme adopted by the invention is that:
The present invention provides a kind of preparation methods of collapse protective poly-carboxylic acid water reducing agent, method includes the following steps:
(1) in terms of mass parts, by 70-90 parts of allyl polyether polymeric monomer, 10-15 parts of acrylic monomer, chain-transferring agent 0.5-2.0 parts, 1-3 parts of oxidant and 70 parts of water are configured to mixed solution A;By 70-90 parts of allyl polyether polymeric monomer, acrylic acid 15-20 parts of esters monomer, 0.8-1.8 parts of chain-transferring agent, 2-3 parts of oxidant and 70 parts of water are configured to mixed solution B;By reducing agent 0.6-1.0 parts and 60 parts of water, it is configured to mixed solution C;
(2) water is added in a kettle, adjusting reaction temperature is 40-80 DEG C, under agitation, mixed solution is first added dropwise Used time 10-15min is added dropwise in C;Then, while mixed solution A and mixed solution C 110-130min is added dropwise, mixed solution A is added dropwise After the completion, then simultaneously mixed solution B and mixed solution C 110-130min is added dropwise, after mixed solution B is added dropwise to complete, then is added dropwise mixed Close solution C 10-20min.
(3) after completion of dropwise addition, continue insulation reaction 1-2h, sodium hydroxide solution is then added and is neutralized to get described Collapse protective poly-carboxylic acid water reducing agent.
For the present invention with allyl polyether polymeric monomer, acrylic compounds and acrylic ester monomer are main monomer, with oxidationreduction Agent is initiator, and chain-transferring agent is added and carries out copolymerization and the block copolymer of acrylic acid synthesizing class and propylene esters.To synthesis The structure of water-reducing agent is designed, and is designed by the structure of block copolymer, so that the water-reducing agent of preparation is with higher initial Under conditions of fluidity, while ensureing that concrete there can be good mobility in a long time.Resulting polymers molecule Structure is as follows:
Further, in step (2), 20 mass parts of water are added in a kettle.
It needs to further illustrate, allyl polyether polymeric monomer is methoxy polyethylene glycol methacrylate-styrene polymer (methoxyl group Obtained by polyethylene glycol and methacrylated), allyl polyglycol, methacrylic polyoxyethylene ether, isopentene group At least one of polyoxyethylene ether.
Acrylic monomer is at least one of acrylic acid, methacrylic acid, itaconic acid, succinic anhydride.
Acrylic ester monomer be methyl acrylate, methyl methacrylate, hydroxy-ethyl acrylate, hydroxypropyl acrylate, At least one of β-acryloxy propionic, hydroxyethyl methacrylate.
Chain-transferring agent is 2- thioacetic acid, 3- mercaptopropionic acid, mercaptoethanol, methyl propane sulfonic acid sodium, one in ethyl acetate Kind.
Oxidant is hydrogen peroxide, sodium peroxydisulfate, potassium peroxydisulfate, ammonium persulfate, one in benzoyl peroxide Kind.
Reducing agent is one of sodium formaldehyde sulfoxylate, sodium sulfite, ascorbic acid, green vitriol.
The present invention also provides collapse protective poly-carboxylic acid water reducing agents made from above-mentioned preparation method.
The present invention has following effective effect:
(1) preparation method of collapse protective poly-carboxylic acid water reducing agent of the present invention is successively added dropwise using mixed solution A with mixed solution B Dropwise addition technique, can effectively control the structure of polymer.
(2) present invention is designed by the structure of block, has been provided simultaneously with diminishing and has been protected the performance collapsed, has avoided traditional compounding The compatibility issue of type function water-reducing agent and material.
(3) for the present invention with allyl polyether polymeric monomer, acrylic compounds and acrylic ester monomer are main monomer, with oxidation- Reducing agent is initiator, and addition chain-transferring agent carries out copolymerization and the guarantor of the polycarboxylate water-reducer synthesized collapses the time for 4-6h.
Specific embodiment
The invention will be further described combined with specific embodiments below.
In following embodiments, if not otherwise indicated, agents useful for same and material are that conventional commercial can obtain.
Embodiment 1
A kind of preparation method of collapse protective poly-carboxylic acid water reducing agent the following steps are included:
(1) by 80kg isopentene group polyoxyethylene ether, 14.4kg acrylic acid, 1.2kg mercaptoethanol, 1.0kg potassium peroxydisulfate Mixed solution A is configured to 70kg water;By 80kg isopentene group polyoxyethylene ether, 20kg methyl methacrylate, 1.2kg sulfydryl Ethyl alcohol, 3kg potassium peroxydisulfate and 70kg water are configured to mixed solution B;By 0.4kg sodium formaldehyde sulfoxylate, 0.4kg green vitriol and 60kg water is configured to mixed solution C;
(2) 20kg water is added in a kettle, adjusting reaction temperature is 60 DEG C, opens stirring;Mixed solution C is first added dropwise 10min (refers here to that mixed solution C is added dropwise always, the dropwise addition used time is 10min), and mixed solution A is then added dropwise simultaneously and mixes Solution C 120min (referring here to that mixed solution A and mixed solution C are added dropwise always, the dropwise addition used time is 120min) is closed, to mixed After closing solution A completion of dropwise addition, then mixed solution B is added dropwise and mixed solution C 120min (refers here to be added dropwise always molten simultaneously Liquid B and mixed solution C, dropwise addition used time are 120min);After solution B completion of dropwise addition to be mixed, then mixed solution C 10min is added dropwise; Time for adding: mixed solution A 120min, mixed solution B are 120min;Mixed solution C is 260min;
(3) after completion of dropwise addition, the reaction was continued 2h;The sodium hydroxide solution that 45kg mass concentration is 40% is eventually adding to carry out It neutralizes to get the polycarboxylate water-reducer, monomer conversion 99.6% is arrived.
Embodiment 2
A kind of preparation method of collapse protective poly-carboxylic acid water reducing agent the following steps are included:
(1) by 50kg isopentene group polyoxyethylene ether, 40kg methacrylic polyoxyethylene ether, 15kg acrylic acid, 2kg Mercaptoethanol, 3kg Ammonium Persulfate 98.5 and 70kg water are configured to mixed solution A;By 50kg isopentene group polyoxyethylene ether, 40kg methyl Allyl polyethenoxy base ether, 20kg hydroxy-ethyl acrylate, 1.8kg mercaptoethanol, 3kg Ammonium Persulfate 98.5 and 70kg water are configured to mix Close solution B;0.5kg sodium formaldehyde sulfoxylate, 0.5kg green vitriol and 60kg water are configured to mixed solution C;
(2) 20kg water is added in a kettle, adjusting reaction temperature is 40 DEG C, opens stirring;Mixed solution C is first added dropwise 15min (refers here to that mixed solution C is added dropwise always, the dropwise addition used time is 10min), and mixed solution A is then added dropwise simultaneously and mixes Solution C 110min (referring here to that mixed solution A and mixed solution C are added dropwise always, the dropwise addition used time is 110min) is closed, to mixed After closing solution A completion of dropwise addition, then mixed solution B is added dropwise and mixed solution C 130min (refers here to be added dropwise always molten simultaneously Liquid B and mixed solution C, dropwise addition used time are 130min);After solution B completion of dropwise addition to be mixed;Mixed solution C 10min is added dropwise again; Time for adding: mixed solution A 110min, mixed solution B are 130min;Mixed solution C is 265min;
(3) after completion of dropwise addition, the reaction was continued 1h;The sodium hydroxide solution that 45kg mass concentration is 40% is eventually adding to carry out It neutralizes to get the polycarboxylate water-reducer, monomer conversion 99.7% is arrived.
Embodiment 3
A kind of preparation method of collapse protective poly-carboxylic acid water reducing agent the following steps are included:
(1) by 70kg methacrylic polyoxyethylene ether, 10kg acrylic acid, 0.5kg methyl propane sulfonic acid sodium, 1kg over cure Sour potassium and 70kg water are configured to mixed solution A;By 70kg methacrylic polyoxyethylene ether, 15kg β-acryloxy third Acid, 0.8kg methyl propane sulfonic acid sodium, 2kg potassium peroxydisulfate and 70kg water are configured to mixed solution B;By 0.6kg ascorbic acid and 60kg Water is configured to mixed solution C;
(2) 20kg water is added in a kettle, adjusting reaction temperature is 80 DEG C, opens stirring;Mixed solution C is first added dropwise 10min (refers here to that mixed solution C is added dropwise always, the dropwise addition used time is 10min), and mixed solution A is then added dropwise simultaneously and mixes Solution C 130min (referring here to that mixed solution A and mixed solution C are added dropwise always, the dropwise addition used time is 130min) is closed, to mixed After closing solution A completion of dropwise addition, then mixed solution B is added dropwise and mixed solution C 110min (refers here to be added dropwise always molten simultaneously Liquid B and mixed solution C, dropwise addition used time are 110min);After solution B completion of dropwise addition to be mixed;Mixed solution C 20min is added dropwise again; Time for adding: mixed solution A 130min, mixed solution B are 110min;Mixed solution C is 270min;
(3) after completion of dropwise addition, the reaction was continued 2h;The sodium hydroxide solution that 40kg mass concentration is 40% is eventually adding to carry out It neutralizes to get the polycarboxylate water-reducer, monomer conversion 99.7% is arrived.
Comparative example 1
A kind of preparation method of polycarboxylate water-reducer the following steps are included:
(1) by 80kg isopentene group polyoxyethylene ether, 14.4kg acrylic acid, 1.2kg mercaptoethanol, 1.0kg potassium peroxydisulfate Mixed solution A is configured to 70kg water;By 80kg isopentene group polyoxyethylene ether, 20kg methyl methacrylate, 1.2kg sulfydryl Ethyl alcohol, 3kg potassium peroxydisulfate and 70kg water are configured to mixed solution B;By 0.4kg sodium formaldehyde sulfoxylate, 0.4kg green vitriol and 60kg water is configured to mixed solution C;
(2) 20kg water is added in a kettle, adjusting reaction temperature is 60 DEG C, opens stirring;Mixed solution A, B, C is same When be added drop-wise in reaction kettle, time for adding 120min;
(3) after completion of dropwise addition, the reaction was continued 2h;The sodium hydroxide solution that 45kg mass concentration is 40% is eventually adding to carry out It neutralizes to get the polycarboxylate water-reducer is arrived.
Comparative example 2
A kind of preparation method of polycarboxylate water-reducer the following steps are included:
(1) by 80kg isopentene group polyoxyethylene ether, 14.4kg acrylic acid, 1.2kg mercaptoethanol, 1.0kg potassium peroxydisulfate Mixed solution A is configured to as reaction kettle bottom liquid with 70kg water;By 80kg isopentene group polyoxyethylene ether, 20kg methacrylic acid Methyl esters, 1.2kg mercaptoethanol, 3kg potassium peroxydisulfate and 70kg water are configured to mixed solution B;By 0.4kg sodium formaldehyde sulfoxylate, seven water of 0.4kg It closes ferrous sulfate and 30kg water is configured to mixed solution C;
(2) adjusting reaction temperature is 25 DEG C, opens stirring;10min first is added dropwise in mixed solution C, then mixed solution B and Mixed solution C is added dropwise simultaneously, mixed solution B time for adding 120min;After solution B completion of dropwise addition to be mixed, then be added dropwise mixing it is molten Liquid C10min, total time for adding are 140min;
(3) after completion of dropwise addition, the reaction was continued 2h;The sodium hydroxide solution that 45kg mass concentration is 40% is eventually adding to carry out It neutralizes to get the polycarboxylate water-reducer is arrived.
Comparative example 3
A kind of preparation method of polycarboxylate water-reducer the following steps are included:
(1) by 80kg isopentene group polyoxyethylene ether, 14.4kg acrylic acid, 1.2kg mercaptoethanol, 1.0kg potassium peroxydisulfate Mixed solution A is configured to 70kg water;By 80kg isopentene group polyoxyethylene ether, 20kg methyl methacrylate, 1.2kg sulfydryl Ethyl alcohol, 3kg potassium peroxydisulfate and 70kg water are configured to mixed solution B;By 0.4kg sodium formaldehyde sulfoxylate, 0.4kg green vitriol and 30kg water is configured to mixed solution C;
(2) using mixed solution A and mixed solution B as reaction kettle bottom liquid, adjusting reaction temperature is 25 DEG C, opens stirring; Mixed solution C is added drop-wise in reaction kettle, time for adding 120min;
(3) after completion of dropwise addition, the reaction was continued 2h;The sodium hydroxide solution that 45kg mass concentration is 40% is eventually adding to carry out It neutralizes to get the polycarboxylate water-reducer is arrived.
Comparative example 4
A kind of preparation method of high-efficiency water-reducing agent of poly-carboxylic acid the following steps are included:
(1) by 60kg isopentene group polyoxyethylene ether, 10kg acrylic acid, 4kg methyl methacrylate, 1.2kg sulfydryl Ethyl alcohol, potassium peroxydisulfate 3kg and 70kg water are configured to mixed solution A;By 0.175kg sodium formaldehyde sulfoxylate, 0.3kg green vitriol and 30kg water is configured to mixed solution B;
(2) 20kg water is added in reaction kettle;Adjusting reaction temperature is 25 DEG C, opens stirring;B mixed solution is first added dropwise 10min, then A mixed solution and B mixed solution is added dropwise simultaneously, after A mixed solution is added dropwise to complete, B mixed solution continues to be added dropwise 30min, time for adding: A mixed solution is 120min, and B mixed solution is 160min;
(3) after completion of dropwise addition, the reaction was continued 2h;The sodium hydroxide solution that 45kg mass concentration is 40% is eventually adding to carry out It neutralizes to get the high-efficiency water-reducing agent of poly-carboxylic acid is arrived.
The evaluation of water-reducing rate and slump retaining is carried out to polycarboxylate water-reducer made from above-described embodiment 1-3 and comparative example 1-4. Specific method and result are as follows:
1, water-reducing rate is evaluated
Admixtures water-reducing ratio test method is carried out by GB8076-2008 " concrete admixture " standard.Specific experiment method It is as follows:
(1) water consumption: the slump reaches 210 ± 10mm;
(2) reference cement, dosage 360kg/m cement: are used3
(3) stone: 5-10mm accounts for 40%, 10-20mm and accounts for 60%
(4) sand: sand in use
(5) sand coarse aggregate ratio: 43~47%
After mix-design is good, material is poured into and stirs 2min in agitated kettle, turned after taking the dish out of the pot and uniformly carry out slump examination It tests.
Slump detection: dividing two layers and be fitted into cylinder, and every layer plugs and pounds 15 times, plugs and pounds and is carried out by export-oriented center with spiral, and second Layer is inserted into one layer of surface, and the concrete that then will be above cylinder is erased, lift-off slump cone, after then measuring Control Measures for Concrete Slump Height between height and slump cone is the slump.
The calculating of water-reducing rate:
Water-reducing rate=(normal concrete water consumption-is by inspection concrete water amount)/normal concrete water consumption × 100%. Wherein, normal concrete: the concrete of additive is not mixed;By inspection concrete: mixing the concrete of additive.
The test result of water-reducing rate is as shown in table 1.
Table 1
Embodiment Water-reducing rate
Embodiment 1 31.1%
Embodiment 2 32.2%
Embodiment 3 30.5%
Comparative example 1 18.1%
Comparative example 2 17.9%
Comparative example 3 19.8%
Comparative example 4 30.1%
2, slump retaining measures
According to above-mentioned slump detection method, height after the Control Measures for Concrete Slump of 0,30min, 1h, 2h, 4h, 6h is tested respectively Height between degree and slump cone.Test result is as shown in table 2.
Table 2
As shown in Table 1, the present invention is by the block design to water-reducing agent molecular structure, the diminishing of the water-reducing agent synthesized Rate is apparently higher than the water-reducing agent obtained in comparative example with other synthesis technologies, and water-reducing agent produced by the present invention has excellent diminishing Property.As shown in Table 2, the concrete slump for adding water-reducing agent of the present invention collapses significantly less than the concrete for adding comparative example water-reducing agent Degree of falling, water-reducing agent produced by the present invention have superelevation slump retaining.
Cement water reducing agent provided by the present invention and preparation method thereof is described in detail above.It is used herein A specific example illustrates the principle and implementation of the invention, and the above embodiments are only used to help understand originally The method and its core concept of invention.It should be pointed out that for those skilled in the art, not departing from this hair , can be with several improvements and modifications are made to the present invention under the premise of bright principle, these improvement and modification also fall into power of the present invention In the protection scope that benefit requires.

Claims (9)

1. a kind of preparation method of collapse protective poly-carboxylic acid water reducing agent, which is characterized in that method includes the following steps:
(1) in terms of mass parts, by 70-90 parts of allyl polyether polymeric monomer, 10-15 parts of acrylic monomer, chain-transferring agent 0.5- 2.0 parts, 1-3 parts of oxidant and 70 parts of water are configured to mixed solution A;By 70-90 parts of allyl polyether polymeric monomer, esters of acrylic acid 15-20 parts of monomer, 0.8-1.8 parts of chain-transferring agent, 2-3 parts of oxidant and 70 parts of water are configured to mixed solution B;By reducing agent 0.6- 1.0 parts and 60 parts of water, it is configured to mixed solution C;
(2) water is added in a kettle, adjusting reaction temperature is 40-80 DEG C, under agitation, mixed solution C is first added dropwise, and is dripped Add used time 10-15min;Then, while mixed solution A is added dropwise and mixed solution C 110-130min, mixed solution A are added dropwise to complete Afterwards, then simultaneously mixed solution B and mixed solution C 110-130min is added dropwise, after mixed solution B is added dropwise to complete, then be added dropwise mixing it is molten Liquid C 10-20min;
(3) after completion of dropwise addition, continue insulation reaction 1-2h, then addition sodium hydroxide solution is neutralized described to get arriving Collapse protective poly-carboxylic acid water reducing agent.
2. the preparation method of collapse protective poly-carboxylic acid water reducing agent according to claim 1, which is characterized in that in step (2), 20 mass parts of water are added in reaction kettle.
3. the preparation method of collapse protective poly-carboxylic acid water reducing agent according to claim 1, which is characterized in that allyl polyether is big Monomer is methoxy polyethylene glycol methacrylate-styrene polymer, allyl polyglycol, methacrylic polyoxyethylene ether, iso-amylene At least one of base polyoxyethylene ether.
4. the preparation method of collapse protective poly-carboxylic acid water reducing agent according to claim 1, which is characterized in that acrylic monomer For at least one of acrylic acid, methacrylic acid, itaconic acid, succinic anhydride.
5. the preparation method of collapse protective poly-carboxylic acid water reducing agent according to claim 1, which is characterized in that esters of acrylic acid list Body is methyl acrylate, methyl methacrylate, hydroxy-ethyl acrylate, hydroxypropyl acrylate, β-acryloxy propionic, methyl At least one of hydroxy-ethyl acrylate.
6. the preparation method of collapse protective poly-carboxylic acid water reducing agent according to claim 1, which is characterized in that chain-transferring agent 2- One of thioacetic acid, 3- mercaptopropionic acid, mercaptoethanol, methyl propane sulfonic acid sodium, ethyl acetate.
7. the preparation method of collapse protective poly-carboxylic acid water reducing agent according to claim 1, which is characterized in that oxidant is peroxide Change one of hydrogen, sodium peroxydisulfate, potassium peroxydisulfate, ammonium persulfate, benzoyl peroxide.
8. the preparation method of collapse protective poly-carboxylic acid water reducing agent according to claim 1, which is characterized in that reducing agent is white to hang One of block, sodium sulfite, ascorbic acid, green vitriol.
9. collapse protective poly-carboxylic acid water reducing agent made from the described in any item preparation methods of claim 1-8.
CN201810836950.6A 2018-07-26 2018-07-26 A kind of collapse protective poly-carboxylic acid water reducing agent and preparation method thereof Pending CN109053977A (en)

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Publication number Priority date Publication date Assignee Title
CN110922546A (en) * 2019-11-21 2020-03-27 湖北工业大学 Phenyl hydroxyl compound ATRP method modified polycarboxylic acid slump retaining agent and preparation method thereof
TWI779346B (en) * 2020-09-04 2022-10-01 漢鴻實業股份有限公司 Additives that can inhibit the blackening of concrete
CN115521414A (en) * 2022-09-29 2022-12-27 贵州石博士科技股份有限公司 Polycarboxylic slump retaining agent and preparation method and application thereof

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