CN101531483A - Method for preparing ether ester copolymer high-efficiency water reducer - Google Patents
Method for preparing ether ester copolymer high-efficiency water reducer Download PDFInfo
- Publication number
- CN101531483A CN101531483A CN200810092566A CN200810092566A CN101531483A CN 101531483 A CN101531483 A CN 101531483A CN 200810092566 A CN200810092566 A CN 200810092566A CN 200810092566 A CN200810092566 A CN 200810092566A CN 101531483 A CN101531483 A CN 101531483A
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- China
- Prior art keywords
- water reducer
- ester copolymer
- efficiency water
- reaction
- ether
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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
- C04B24/28—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- C04B24/32—Polyethers, e.g. alkylphenol polyglycolether
-
- 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)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Organic Chemistry (AREA)
- Curing Cements, Concrete, And Artificial Stone (AREA)
- Polyethers (AREA)
Abstract
The invention discloses a method for preparing an ether ester copolymer high-efficiency water reducer; methyl polyethenoxy ether, methyl methacrylate, polyethylene glycol and the like are taken as raw materials and go through ester condensation reaction, addition reaction and neutralization reaction to prepare the ether ester copolymer high-efficiency water reducer; and the preparation method is simple and the reaction conditions are easy to control. The weight percentages of the raw materials are as follows: 9 percent to 19 percent of methyl polyethenoxy ether, 45 percent to 60 percent of methyl methacrylate, 30 percent to 40 percent of polyethylene glycol; the technology of the preparation method is simple, the reaction is stable, the reaction condition is mild and the technological process is easy to control. The obtained ether ester copolymer high-efficiency water reducer has the advantages of high water reduction rate, good fluidity, high slump retaining ability, good plasticizing effect, low retardation, low shrinkage, high reinforcement and the like, thus meeting the technical requirements and construction requirements of modern high-performance concrete.
Description
Technical field
The present invention relates to a kind of preparation method of water reducer, more specifically to a kind of method for preparing ether ester copolymer high-efficiency water reducer.
Background technology
High efficiency water reducing agent is one of staple product of building material mainstay industry.What present domestic research was more is poly carboxylic acid series water reducer, it is the concrete admixture of new generation after traditional naphthalene system, amido sulfoacid series, melamine system water reducer, its Molecular Structure Design is to introduce strong polar group carboxyl, sulfonic group, polyoxyethylene thiazolinyl etc. on molecular backbone chain or side chain, makes molecule have comb shaped structure.Mainly contain with the maleic anhydride and be the different polyoxyethylene groups of main chain grafting (EO) or polyoxypropylene base (PO) side chain and be main chain grafting (EO) or (PO) side chain two big classes with the methacrylic acid.Bring into play high dispersing property though there is the bibliographical information high-efficiency water-reducing agent of poly-carboxylic acid to have low-dosage, more water reducer can reach domestic such research of 35-50% sees and is in advanced development, really forms product seldom.Most of high-efficiency water-reducing agent of poly-carboxylic acid generally＜30%.And deficiencies such as the synthesis technique than class water reducer is generally comparatively loaded down with trivial details, and the radical polymerization quality product is understable still exist.Therefore the preparation method of ether ester copolymer high-efficiency water reducer excellent property who develops the simple and preparation of a kind of technology is imperative.
Summary of the invention
The object of the present invention is to provide a kind of preparation method of ether ester copolymer high-efficiency water reducer.This preparation method's technology is simple, the water-reducing rate of the water reducer that makes be higher than how be, the water-reducing rate of water reducer such as melamine, thionamic acid, lipid acid and poly carboxylic acid.
Technical solution of the present invention is as follows:
The preparation method of ether ester copolymer high-efficiency water reducer of the present invention comprises the following steps:
A). methyl methacrylate, polyoxyethylene glycol are put into reactor by weight, be diluted with water to 30% concentration, under 83 ± 3 ℃ temperature, reacted 4.5 ± 0.5 hours, finish the ester reaction of contracting, generate β-carbonyl acid esters; B). to A) add the 10-20% of raw material methyl Soxylat A 25-7 total amount in the product, temperature is controlled at 65 ± 5 ℃, stir, drip benzoyl peroxide then at leisure so that addition reaction to take place, speed is dripped in control, make it to drip off in 2 ± 0.3 hours, and then control reaction temperature is in 85 ± 0.5 ℃ of scopes, reacted 4 ± 0.2 hours, and formed the macromolecular compound that contains groups such as ether-ether with certain molecular weight;
C). at B) in after addition reaction finishes, add alkali again and neutralize, stir, the pH value that makes material is 8 ± 0.5, both ether ester copolymer high-efficiency water reducer;
Composition of raw materials (being more excellent proportioning in the weight ratio, bracket) is:
Methyl Soxylat A 25-7 9-19% (15%);
Methyl methacrylate 45-60% (55%);
Polyoxyethylene glycol 30-40% (30%);
The stupid formyl 2-4% of peroxidation (3%);
Sodium hydroxide (or potassium hydroxide) 5-8% (6%).
The invention has the beneficial effects as follows:
This preparation method's technology is simple, and stable reaction, mild condition, technological process are easy to control.The ether ester copolymer high-efficiency water reducer that makes have high water reducing rate, good fluidity, high protect collapse, plasticizing effect is good, low slow setting, the low contraction and advantages such as high enhancing.Be fit to concrete technical requirements of modern high performance and construction requirement.
Embodiment
Embodiment 1
A). methyl methacrylate, polyoxyethylene glycol are put into reactor by weight 2:1.2, be diluted with water to 30% concentration, reaction is 4.5 hours under 80 ℃ temperature, finishes the ester reaction of contracting, generation β-carbonyl acid esters;
B). to A) add 15% of raw material methyl Soxylat A 25-7 total amount in the product, temperature is controlled at 65 ℃, stir, drip benzoyl peroxide 55g then at leisure so that addition reaction to take place, speed is dripped in control, make it to drip off in 2 hours, and then control reaction temperature is in 85 ℃ of scopes, reacted 4 hours, and formed the macromolecular compound that contains groups such as ether-ether with certain molecular weight;
C). at B) in after addition reaction finishes, add alkali again and neutralize, stir, the pH value that makes material is 8 ± 0.5, both ether ester copolymer high-efficiency water reducer;
Embodiment 2
A) methyl methacrylate, polyoxyethylene glycol are put into reactor by weight 2:1, be diluted with water to 30% concentration, reaction is 4 hours under 83 ℃ temperature, finishes the ester reaction of contracting, generation β-carbonyl acid esters;
B). to A) add 18% of raw material methyl Soxylat A 25-7 total amount in the product, temperature is controlled at 60 ℃, stir, drip benzoyl peroxide 50g then at leisure so that addition reaction to take place, speed is dripped in control, make it to drip off in 2 hours, and then control reaction temperature is in 75 ℃ of scopes, reacted 4.5 hours, and formed the macromolecular compound that contains groups such as ether-ether with certain molecular weight;
C). at B) in after addition reaction finishes, add alkali again and neutralize, stir, the pH value that makes material is 8 ± 0.5, both ether ester copolymer high-efficiency water reducer;
Embodiment 3
A). methyl methacrylate, polyoxyethylene glycol are put into reactor by weight 2:1.5, be diluted with water to 30% concentration, reaction is 4.5 hours under 85 ℃ temperature, finishes the ester reaction of contracting, generation β-carbonyl acid esters;
B). to A) add 20% of raw material methyl Soxylat A 25-7 total amount in the product, temperature is controlled at 65 ℃, stir, drip benzoyl peroxide 45g then at leisure so that addition reaction to take place, speed is dripped in control, make it to drip off in 2 hours, and then control reaction temperature is in 80 ℃ of scopes, reacted 5 hours, and formed the macromolecular compound that contains groups such as ether-ether with certain molecular weight;
C). at B) in after addition reaction finishes, add alkali again and neutralize, stir, the pH value that makes material is 8 ± 0.5, both ether ester copolymer high-efficiency water reducer.
Claims (2)
1. a method for preparing ether ester copolymer high-efficiency water reducer is characterized in that comprising the following steps:
A). methyl methacrylate, polyoxyethylene glycol are put into reactor by weight, be diluted with water to 30% concentration, under 83 ± 3 ℃ temperature, reacted 4.5 ± 0.5 hours, finish the ester reaction of contracting, generate β-carbonyl acid esters;
B). to A) add the 10-20% of raw material methyl Soxylat A 25-7 total amount in the product, temperature is controlled at 65 ± 5 ℃, stir, drip benzoyl peroxide then at leisure so that addition reaction to take place, speed is dripped in control, make it to drip off in 2 ± 0.3 hours, and then control reaction temperature is in 85 ± 0.5 ℃ of scopes, reacted 4 ± 0.2 hours, and formed the macromolecular compound that contains groups such as ether-ether with certain molecular weight;
C). at B) in after addition reaction finishes, add alkali again and neutralize, stir, the pH value that makes material is 8 ± 0.5, both ether ester copolymer high-efficiency water reducer;
Composition of raw materials (weight ratio) is:
Methyl Soxylat A 25-7 9-19%;
Methyl methacrylate 45-60%;
Polyoxyethylene glycol 30-40%;
The stupid formyl 2-4% of peroxidation;
Sodium hydroxide (or potassium hydroxide) 5-8%.
2. method for preparing ether ester copolymer high-efficiency water reducer according to claim 1 is characterized in that composition of raw materials (weight ratio) is:
Methyl Soxylat A 25-7 15%;
Methyl methacrylate 55%;
Polyoxyethylene glycol 30%;
The stupid formyl 3% of peroxidation;
Sodium hydroxide (or potassium hydroxide) 6%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200810092566A CN101531483A (en) | 2008-04-18 | 2008-04-18 | Method for preparing ether ester copolymer high-efficiency water reducer |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200810092566A CN101531483A (en) | 2008-04-18 | 2008-04-18 | Method for preparing ether ester copolymer high-efficiency water reducer |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN101531483A true CN101531483A (en) | 2009-09-16 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN200810092566A Pending CN101531483A (en) | 2008-04-18 | 2008-04-18 | Method for preparing ether ester copolymer high-efficiency water reducer |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN101531483A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102372457A (en) * | 2010-08-24 | 2012-03-14 | 上海台界化工有限公司 | Water reducing agent for concrete |
| WO2013001473A1 (en) * | 2011-06-30 | 2013-01-03 | Jaime Grau Genesias | Additive for producing permeable concrete |
| CN105949409A (en) * | 2016-04-29 | 2016-09-21 | 华侨大学 | Polycarboxylate-series concrete water reducing agent containing chitosan, and preparation method thereof |
-
2008
- 2008-04-18 CN CN200810092566A patent/CN101531483A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102372457A (en) * | 2010-08-24 | 2012-03-14 | 上海台界化工有限公司 | Water reducing agent for concrete |
| WO2013001473A1 (en) * | 2011-06-30 | 2013-01-03 | Jaime Grau Genesias | Additive for producing permeable concrete |
| CN105949409A (en) * | 2016-04-29 | 2016-09-21 | 华侨大学 | Polycarboxylate-series concrete water reducing agent containing chitosan, and preparation method thereof |
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| C02 | Deemed withdrawal of patent application after publication (patent law 2001) | ||
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Application publication date: 20090916 |