CN108484838A - A kind of super collapse protective poly-carboxylic acid series high-performance dehydragent and preparation method thereof - Google Patents
A kind of super collapse protective poly-carboxylic acid series high-performance dehydragent and preparation method thereof Download PDFInfo
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- CN108484838A CN108484838A CN201810234888.3A CN201810234888A CN108484838A CN 108484838 A CN108484838 A CN 108484838A CN 201810234888 A CN201810234888 A CN 201810234888A CN 108484838 A CN108484838 A CN 108484838A
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- Prior art keywords
- carboxylic acid
- acid series
- series high
- esters
- collapse protective
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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
-
- 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
- C04B24/2641—Polyacrylates; Polymethacrylates
-
- 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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- 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)
- Curing Cements, Concrete, And Artificial Stone (AREA)
Abstract
The invention belongs to building material technical fields, and in particular to a kind of super collapse protective poly-carboxylic acid series high-performance dehydragent and preparation method thereof.The characteristics of being hydrolyzed in alkaline environment using esters, introduces different ester groups on poly carboxylic acid series water reducer molecule.Using methyl allyl polyoxyethylene ether as polymeric monomer, it is to polymerize minor comonomer, initiator and chain-transferring agent as reaction condition with acids, esters, synthesizes super collapse protective poly-carboxylic acid series high-performance dehydragent.A kind of this super collapse protective poly-carboxylic acid series high-performance dehydragent has function of slump protection good, and synthesis mode is more flexible with raw material, the wider array of feature of application range.
Description
Technical field
The invention belongs to building material technical fields, and in particular to a kind of super collapse protective poly-carboxylic acid series high-performance dehydragent and its
Preparation method.
Background technology
With economic and science and technology development, building trade also with continuous development, get over by the requirement in engineering for concrete
Come higher, the demand to additive is also increasing, and wherein water-reducing agent has become the indispensable part of modern concrete.
As the third generation product in water-reducing agent, poly carboxylic acid series water reducer is low with volume always, water-reducing rate is high, molecule designability is good
The characteristics of favored by all kinds of engineerings, have become one of the ideal additive for preparing concrete of new generation at present.But with
The raising of poly carboxylic acid series water reducer water-reducing rate, mixing water amount is fewer and fewer, concrete mixing after a while, meeting
It is higher to there is viscosity, the serious phenomenon of slump-loss, therefore multi-party scholar is for super collapse protective poly-carboxylic acid series high-performance diminishing
Agent is made that research.
About the mechanism of action of super collapse protective poly-carboxylic acid series high-performance dehydragent, there are mainly four types of types at present：Carboxy protective
Type, cross-linking type dissolve control type, amphoteric.
The mechanism of action of carboxy protective type is to introduce ester group, acid anhydrides and amide etc. in poly carboxylic acid series water reducer molecule instead
Answering property group can occur hydrolysis in concrete alkaline environment using them and slowly release functional groups carboxyl
The water-reducing agent due to cement granules aquation, absorption and reduction is continuously replenished in feature, to improve point of poly carboxylic acid series water reducer
Holding capacity is dissipated, that is, the guarantor for improving water-reducing agent is collapsed ability.
Invention content
The purpose of the present invention is to provide a kind of function of slump protection is good, synthesis mode is more flexible with raw material, application range
Wider array of super collapse protective poly-carboxylic acid series high-performance dehydragent and preparation method thereof.
Super collapse protective poly-carboxylic acid series high-performance dehydragent proposed by the present invention is big single with methyl allyl polyoxyethylene ether
Body is polymerization minor comonomer with acids, esters, using oxidation component and reduction components as initiator, using chain-transferring agent and water as instead
The raw material, the weight ratio of each component substance is answered to be：
Methyl allyl polyoxyethylene ether 100
Acids 3.0-7.0
Esters 15.0-22.0
Reduction components 0.15-0.25
Oxidation component 1.0-1.50
Chain-transferring agent 0.35-0.50
Water 180-200.
The preferable weight ratio of each component is：
Methyl allyl polyoxyethylene ether 100
Acids 3.4-3.7
Esters 20.2-20.8
Reduction components 0.18-0.20
Oxidation component 1.22-1.30
Chain-transferring agent 0.43-0.46
Water 180-190.
In the present invention, the methyl allyl polyoxyethylene ether is any during molecular weight is 600 to 4000.
In the present invention, the acids is acrylic acid.
In the present invention, the esters are any in methyl acrylate or hydroxypropyl acrylate.
In the present invention, the reduction components are vitamin C, and the oxidation component is hydrogen peroxide.
In the present invention, the chain-transferring agent is any in thioacetic acid or mercaptopropionic acid.
The preparation method of slump-retaining polycarboxylic acid type water reducing agent proposed by the present invention, is as follows：
(1) methyl allyl polyoxyethylene ether is soluble in water；
(2) exist in reduction components, oxidation component and chain-transferring agent, to step（1）In products therefrom be added dropwise acids,
Free radicals copolymerization reaction occurs for the mixed liquor of esters to get required product.
In the copolyreaction of the present invention, polymeric monomer methyl allyl polyoxyethylene ether is by the way of being added at one time, oxygen
Change component before polymerization using being added at one time by the way of, reduction components and chain-transferring agent and water composition solution mixture, acids,
Esters and water compositing monomer solution mixture, after stirring evenly, are fed intake by the way of being at the uniform velocity added dropwise.
In the present invention, step（2）Middle copolyreaction temperature is 40-50 DEG C, and the monomer solution of acids, esters and water composition is mixed
It is 2-4 hour to close object time for adding, what the solution mixture that reduction components and chain-transferring agent form was formed compared with acids, esters and water
Monomer solution mixture time for adding extends 0.5 hour, and keeps the temperature 1-2 hours after being added dropwise to complete to improve conversion ratio.
The beneficial effects of the present invention are：The present invention has selected carboxy protective type being synthesized as the application mechanism of synthesis
It is middle to introduce ester group using esters so that finished product has good function of slump protection, while having certain flexibility, energy in synthesis
Adapt to wider array of application range.
Specific implementation mode
It is further illustrated the present invention below by embodiment.
Embodiment 1, a kind of super slump-retaining polycarboxylic acid type water reducing agent, weight ratio are：Methyl allyl polyoxyethylene ether
100, acrylic acid 3.60, hydroxypropyl acrylate 20.58, vitamin C 0.18, hydrogen peroxide 1.22, thioacetic acid 0.43, water 183.
45 DEG C of reaction temperature, the monomer solution mixture time for adding of acids, esters and water composition 3 hours, soaking time 1.5 hours,
It is configured to the poly carboxylic acid series water reducer of solid content 40%, products obtained therefrom is denoted as A.Concrete test result such as table 1.
Embodiment 2, a kind of super slump-retaining polycarboxylic acid type water reducing agent, weight ratio are：Methyl allyl polyoxyethylene ether
100, acrylic acid 7.0, methyl acrylate 15.0, vitamin C 0.15, hydrogen peroxide 1.0, thioacetic acid 0.50, water 180.Reaction
40 DEG C of temperature, the monomer solution mixture time for adding of acids, esters and water composition 2 hours, soaking time 1 hour is configured to
The poly carboxylic acid series water reducer of solid content 40%, products obtained therefrom are denoted as B.Concrete test result such as table 1.
Embodiment 3, a kind of super slump-retaining polycarboxylic acid type water reducing agent, weight ratio are：Methyl allyl polyoxyethylene ether
100, acrylic acid 3.0, hydroxypropyl acrylate 22.0, vitamin C 0.25, hydrogen peroxide 1.50, mercaptopropionic acid 0.35, water 200.Instead
Temperature 50 C, the monomer solution mixture time for adding of acids, esters and water composition 4 hours, soaking time 2 hours is answered to prepare
At the poly carboxylic acid series water reducer of solid content 38.5%, products obtained therefrom is denoted as C.Concrete experiments result such as table 1.
Embodiment 4, a kind of super slump-retaining polycarboxylic acid type water reducing agent, weight ratio are：Methyl allyl polyoxyethylene ether 100, third
Olefin(e) acid 4.80, hydroxypropyl acrylate 18.20, vitamin C 0.18, hydrogen peroxide 1.22, thioacetic acid 0.43, water 183.Reaction temperature
45 DEG C of degree, the monomer solution mixture time for adding of acids, esters and water composition 3 hours, soaking time 1 hour are configured to solid
The poly carboxylic acid series water reducer of content 40%, products obtained therefrom are denoted as D.Concrete experiments result such as table 1.
1 concrete experiments result of table
Claims (7)
1. a kind of super collapse protective poly-carboxylic acid series high-performance dehydragent, it is characterised in that esters are added and carry out poly carboxylic acid series water reducer conjunction
At using methyl allyl polyoxyethylene ether as polymeric monomer, using acids, esters as synthesis material, with oxidation component and reduction components
For initiator, using chain-transferring agent and water as reaction raw materials, the weight ratio of each component substance is：
Methyl allyl polyoxyethylene ether 100
Acids 3.0-7.0
Esters 15.0-22.0
Reduction components 0.15-0.25
Oxidation component 1.0-1.50
Chain-transferring agent 0.35-0.50
Water 180-200.
2. a kind of super collapse protective poly-carboxylic acid series high-performance dehydragent according to claim 1, it is characterised in that methallyl
Base polyoxyethylene ether is the methyl allyl polyoxyethylene ether that molecular weight is 600-4000.
3. a kind of super collapse protective poly-carboxylic acid series high-performance dehydragent according to claim 1, it is characterised in that acids third
Olefin(e) acid.
4. a kind of super collapse protective poly-carboxylic acid series high-performance dehydragent according to claim 1, it is characterised in that esters third
It is any in e pioic acid methyl ester or hydroxypropyl acrylate.
5. a kind of super collapse protective poly-carboxylic acid series high-performance dehydragent according to claim 1, it is characterised in that reduction components
For vitamin C, oxidation component is hydrogen peroxide.
6. a kind of a kind of preparation method of super collapse protective poly-carboxylic acid series high-performance dehydragent as described in claim 1, feature
It is to be as follows：
(1) methyl allyl polyoxyethylene ether is soluble in water；
(2) exist in reduction components, oxidation component and chain-transferring agent, to step（1）Acids, ester are added dropwise in products therefrom
Free radicals copolymerization reaction occurs for the mixed liquor of class to get required product.
7. a kind of preparation method of super collapse protective poly-carboxylic acid series high-performance dehydragent according to claim 6, feature exist
In step（2）Described in copolyreaction temperature be 40-50 DEG C, acids, esters and water composition monomer solution mixture be added dropwise when
Between be 2-4 hour, the monomer solution that the solution mixture of reduction components and chain-transferring agent composition is formed compared with acids, esters and water mixes
It closes object time for adding and extends 0.5 hour, and 1-2 hours are kept the temperature after being added dropwise to complete.
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| CN201810234888.3A CN108484838A (en) | 2018-03-21 | 2018-03-21 | A kind of super collapse protective poly-carboxylic acid series high-performance dehydragent and preparation method thereof |
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| CN201810234888.3A CN108484838A (en) | 2018-03-21 | 2018-03-21 | A kind of super collapse protective poly-carboxylic acid series high-performance dehydragent and preparation method thereof |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109437647A (en) * | 2018-11-07 | 2019-03-08 | 湖南先锋建材有限公司 | Enhance the high-efficiency water-reducing agent of poly-carboxylic acid and preparation method thereof of adaptability |
| CN109879628A (en) * | 2019-02-25 | 2019-06-14 | 谢新昇 | A kind of water-resistant type building mortar plasticizer and preparation method thereof |
| CN109970385A (en) * | 2019-04-23 | 2019-07-05 | 刘翠芬 | One kind is super to protect the concrete water-reducing agent that collapses |
| CN110818857A (en) * | 2019-11-21 | 2020-02-21 | 四川宇砼建材有限公司 | High slump loss resistant polycarboxylate superplasticizer and preparation method thereof |
| CN113072667A (en) * | 2020-01-06 | 2021-07-06 | 江苏苏博特新材料股份有限公司 | Preparation method and application of novel polycarboxylate superplasticizer |
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| CN102504126A (en) * | 2011-11-03 | 2012-06-20 | 山西合盛邦砼建材有限公司 | Slump loss resistant type gather carboxylate water-reducing agent and preparation method thereof |
| CN104261720A (en) * | 2014-09-22 | 2015-01-07 | 厦门天润锦龙建材有限公司 | Ether polycarboxylate superplasticizer and preparation method thereof |
| CN105601837A (en) * | 2015-11-26 | 2016-05-25 | 重庆建研科之杰新材料有限公司 | Polycarboxylate superplasticizer and preparation method thereof |
| CN106977129A (en) * | 2017-04-10 | 2017-07-25 | 河北润砼新材料科技有限公司 | Anti- mud collapse protective poly-carboxylic acid high efficiency water reducing agent and preparation method thereof |
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Patent Citations (4)
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109437647A (en) * | 2018-11-07 | 2019-03-08 | 湖南先锋建材有限公司 | Enhance the high-efficiency water-reducing agent of poly-carboxylic acid and preparation method thereof of adaptability |
| CN109437647B (en) * | 2018-11-07 | 2021-04-23 | 湖南先锋建材有限公司 | Polycarboxylic acid high-efficiency water reducing agent with enhanced adaptability and preparation method thereof |
| CN109879628A (en) * | 2019-02-25 | 2019-06-14 | 谢新昇 | A kind of water-resistant type building mortar plasticizer and preparation method thereof |
| CN109970385A (en) * | 2019-04-23 | 2019-07-05 | 刘翠芬 | One kind is super to protect the concrete water-reducing agent that collapses |
| CN110818857A (en) * | 2019-11-21 | 2020-02-21 | 四川宇砼建材有限公司 | High slump loss resistant polycarboxylate superplasticizer and preparation method thereof |
| CN113072667A (en) * | 2020-01-06 | 2021-07-06 | 江苏苏博特新材料股份有限公司 | Preparation method and application of novel polycarboxylate superplasticizer |
| CN113072667B (en) * | 2020-01-06 | 2023-01-03 | 江苏苏博特新材料股份有限公司 | Preparation method and application of polycarboxylate superplasticizer |
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Application publication date: 20180904 |