CN107056994B - A kind of preparation method of Mobyneb polycarboxylate water-reducer - Google Patents
A kind of preparation method of Mobyneb polycarboxylate water-reducer Download PDFInfo
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- CN107056994B CN107056994B CN201710056584.8A CN201710056584A CN107056994B CN 107056994 B CN107056994 B CN 107056994B CN 201710056584 A CN201710056584 A CN 201710056584A CN 107056994 B CN107056994 B CN 107056994B
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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
- 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)
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- Health & Medical Sciences (AREA)
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- Polymers & Plastics (AREA)
- Curing Cements, Concrete, And Artificial Stone (AREA)
Abstract
The invention discloses a kind of preparation method of Mobyneb polycarboxylate water-reducer, 180 mass parts of isopentene group polyoxyethylene ether, 10 mass parts of fumaric acid are added in the water of 120 mass parts first for this method, are added oxidant, are stirred to obtain homogeneous solution；Then 7 mass parts of acrylic acid, hydroxy-ethyl acrylate 20-25 mass parts, acrylamido methylpropane sulfonic acid 1-2 mass parts, acrylamide 1-2 mass parts are added in 20 mass parts water, obtain 1# solution；1 mass parts of reducing agent and 0.8 mass parts of chain-transferring agent are added in 50 mass parts water, 2# solution is obtained；1# solution and 2# solution are successively added dropwise in gained homogeneous solution；Aging 1 hour at 40 DEG C supplements remaining water, stirs 0.5 hour, obtain Mobyneb polycarboxylate water-reducer；Mobyneb polycarboxylate water-reducer prepared by the present invention is adaptable extensively, protects function admirable of collapsing, can be improved the characteristics of concrete strength.
Description
Technical field
The invention belongs to building material industry concrete admixture fields, and in particular to arrive a kind of Mobyneb polycarboxylate water-reducer
Preparation method.
Background technique
Basic raw material of the concrete as a state fundamental construction, is widely used in civil engineering, and dosage is huge,
It is the indispensable goods and materials of the national economic development.
High performance concrete is the concrete with high-durability, high workability and high volume stability.In process for preparation
Using high-quality raw material, water-cement ratio is usually lower, in addition to cement, aggregate and water, adds outside ground mineral admixture and high-performance
Add agent, not only greatly improves the performance of normal concrete, and be formulated using Modern New concrete new technology, applicability
Good, intensity height, durability are high.Water-reducing agent can be effectively improved the working performance of concrete and improve durability.
Water-reducing agent experienced lignosulfonates, naphthalenesulfonate formaldehyde condensation compound/condensate of melamine and formaldehyde and gather
Three developing stage of carboxylic acid high-performance water reducing agent
High performance water reducing agent of polyocarboxy acid is the important additive of concrete, is the key technology for guaranteeing concrete high-performance.
Traditional water-reducing agent only has single performance, such as high collapse-preventing type, early-strength.
Patent CN102976655A discloses a kind of invention of collapse-preventing type polycarboxylic acid super-plasticizer, with a variety of ester type compounds
Collapsing property is protected to it carrying out research and show that extraordinary guarantor is collapsed effect, which, which studies emphatically, protects collapsing property not to the intensity of concrete
It is studied.
Patent CN103951796A discloses a kind of invention of Early-strength polycarboxylate superplasticizer modified with triethanolamine, uses
Triethanolamine reacts generation acrylic acid triethanolamine ester with acrylic acid in advance can guarantee concrete strength under higher water-reducing rate
It increased.But the patent does not introduce guarantor's performance of collapsing.
Summary of the invention
The purpose of the present invention is be to provide a kind of system of Mobyneb polycarboxylate water-reducer in view of the deficiencies of the prior art
Preparation Method, Mobyneb polycarboxylate water-reducer prepared by the present invention is adaptable extensively, protects function admirable of collapsing, can be improved coagulation
The characteristics of native intensity.
The purpose of the present invention is achieved through the following technical solutions: a kind of preparation of Mobyneb polycarboxylate water-reducer
Method, comprising the following steps:
(1), raw material: 180 mass parts of isopentene group polyoxyethylene ether, 10 mass parts of fumaric acid, 7 mass of acrylic acid is chosen
Part, hydroxy-ethyl acrylate 20-25 mass parts, acrylamido methylpropane sulfonic acid 1-2 mass parts, acrylamide 1-2 mass parts, oxidation
1.5 mass parts of agent, 1 mass parts of reducing agent, 0.8 mass parts of chain-transferring agent, 5 mass parts of sodium hydroxide, water 338.7-349.2 mass
Part；
(2), isopentene group polyoxyethylene ether, fumaric acid are added in the water of 120 mass parts, stirring and dissolving adds oxygen
Agent stirs to get homogeneous solution；
(3), 20 mass parts water are added in acrylic acid, hydroxy-ethyl acrylate, acrylamido methylpropane sulfonic acid, acrylamide
In, obtain 1# solution；Reducing agent and chain-transferring agent are added in 50 mass parts water, 2# solution is obtained；It is uniformly molten in step 2 gained
In liquid, 1# solution and 2# solution are successively added dropwise at 30 DEG C；Wherein, 1# solution is added dropwise 3 hours, and 2# solution is added dropwise 3.5 hours；
(4) aging 1 hour, the water of supplement 148.7-159.2 mass parts are stirred 0.5 hour, are obtained at 40 DEG C after dripping
To Mobyneb polycarboxylate water-reducer.
The beneficial effects of the present invention are:
1, the present invention has high water reducing rate under specific graft ratio, can effectively improve hydrated cementitious degree.
2, the present invention in cement alkaline environment, hydroxy-ethyl acrylate can slow release, have certain collapsing property of guarantor.
3, present invention introduces amide groups can enhance concrete strength, is adapted to a variety of concrete.
Specific embodiment
The present invention provides a kind of preparation method of Mobyneb polycarboxylate water-reducer, comprising the following steps:
1, choose raw material: 180 mass parts of isopentene group polyoxyethylene ether, 10 mass parts of fumaric acid, 7 mass parts of acrylic acid,
Hydroxy-ethyl acrylate 20-25 mass parts, acrylamido methylpropane sulfonic acid 1-2 mass parts, acrylamide 1-2 mass parts, oxidant
1.5 mass parts, 1 mass parts of reducing agent, 0.8 mass parts of chain-transferring agent, 5 mass parts of sodium hydroxide, water 338.7-349.2 mass
Part.
2, isopentene group polyoxyethylene ether, fumaric acid are added in the water of 120 mass parts, stirring and dissolving adds oxidation
Agent stirs to get homogeneous solution.
3, acrylic acid, hydroxy-ethyl acrylate, acrylamido methylpropane sulfonic acid, acrylamide are added in 20 mass parts water,
Obtain 1# solution；Reducing agent and chain-transferring agent are added in 50 mass parts water, 2# solution is obtained；In step 2 gained homogeneous solution
In, 1# solution and 2# solution are successively added dropwise at 30 DEG C；Wherein, 1# solution is added dropwise 3 hours, and 3.5 hours are added dropwise in 2# solution
4, aging 1 hour, the water of supplement 148.7-159.2 mass parts stir half an hour, obtain at 40 DEG C after dripping
Mobyneb polycarboxylate water-reducer.
It is the hydrogen peroxide of 28wt% that the oxidant, which selects concentration,.The reducing agent is L-AA (Vc).Oxidant
It can produce free radical as redox system with reducing agent, cause monomer polymerization.
The chain-transferring agent is that 1 mixing forms by mercaptopropionic acid and methyl propane sulfonic acid sodium in molar ratio.Can effectively it make
Radical transfer occurs for propagating radical, adjusts molecular size range.
The isopentene group polyoxyethylene ether is TPEG-2400.It is free-radical polymerized with fumaric acid and acrylic acid progress,
Polycarboxylate water-reducer is as branch.
Fumaric acid is in polycarboxylate water-reducer as main chain.
Hydroxy-ethyl acrylate: slow release is hydrolyzed in cement alkaline environment using ester group, plays the role of guarantor and collapses.
Acrylamido methylpropane sulfonic acid, acrylamide: the intensity of concrete is improved using its amide group.
The present invention obtains graft ratio by many experiments, to reach optimal water-reducing rate, acrylic acid hydroxyl second is utilized
Ester slow release in cement alkalinity is collapsed effect with reaching guarantor, while introducing amide group and sulfonic acid group improves the strong of concrete
Degree.
The present invention prepares high-performance Mobyneb polycarboxylate water-reducer, which is to have connecing for specific graft ratio
Graft copolymer, so that graft copolymer as much as possible is distributed in the interface of cement and water, produces under synthetic method of the present invention
Raw stronger electrostatic repulsion effect and steric effect, initial stage can be in concrete slow releases.Finally greatly improve concrete
Initial flow degree, while it is good to protect performance of collapsing, and the water-reducing agent is after the concrete has set, improves the intensity of concrete.This hair
It is bright that key contributions are made that concrete admixture material manufacturing technology from molecular configuration and chemical engineering research, it is industrial production
Provide new approaches.Concrete can be improved as concrete admixture by high-performance polycarboxylic acids water reducing agent prepared by this method
Initial flow degree, loss of slump is small, the intensity after capable of increasing concrete coagulation.
Embodiment 1-4
The proportion of embodiment 1-4 according to the form below 1 is drawn materials, and prepares 4 Mobyneb polycarboxylic acids diminishings according to step 1-3 of the present invention
Agent.
Table 1: specific implementation material mixture ratio unit/g
| Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 | |
| TPEG-2400 | 180 | 180 | 180 | 180 |
| Fumaric acid | 10 | 10 | 10 | 10 |
| Acrylic acid | 7 | 7 | 7 | 7 |
| Hydrogen peroxide | 1.5 | 1.5 | 1.5 | 1.5 |
| Hydroxy-ethyl acrylate | 20 | 25 | 25 | 25 |
| Acrylamido methylpropane sulfonic acid | 2 | 2 | 1 | 2 |
| Acrylamide | 1 | 1 | 1 | 2 |
| Vitamin C | 1 | 1 | 1 | 1 |
| Chain-transferring agent | 0.8 | 0.8 | 0.8 | 0.8 |
| Sodium hydroxide | 5 | 5 | 5 | 5 |
Embodiment 5
1-4 of the embodiment of the present invention Mobyneb polycarboxylate water-reducer prepared and contrast sample are subjected to pulp flowage
Degree test, it is 40% or so that solid content is obtained after the Mobyneb polycarboxylate water-reducer moisturizing of 1-4 of embodiment of the present invention preparation
Transparency liquid.Contrast sample is the early strength water-reducing agent that commercially available solid content is 40%.
Referring to GB/T8077-2000, cement 300g, amount of water 87g, volume 0.6g, detailed test data are shown in Table 2:
Table 2: paste flowing degree test
As can be seen from Table 2, polycarboxylate water-reducer of the invention compared with low-dosage, has preferable adaptability, initial stage
Embodiment 4 can adapt to various cement and have preferably protect effect of collapsing.
Embodiment 6
Strength of cement mortar test: cement is conch cement, according to GB/T17671-1999 " strength of cement mortar inspection party
Method " operation, wherein cement 450g, normal sand 1350g, water consumption 180g, water-reducing agent volume 1.5g.Detailed test data are shown in Table 3:
Table 3: strength of cement mortar
| Water-reducing rate | 1d intensity/% | 3d intensity/% | 7d intensity/% | 30d intensity/% | |
| Embodiment 1 | 35 | 200 | 185 | 162 | 140 |
| Embodiment 2 | 33.5 | 196 | 183 | 160 | 140 |
| Embodiment 3 | 36 | 195 | 178 | 162 | 135 |
| Embodiment 4 | 35.5 | 210 | 188 | 175 | 143 |
| Contrast sample | 33 | 190 | 170 | 150 | 130 |
Seen from table 3, embodiment 1-4 is above commercially available early strength water-reducing agent intensity.
Not only there is well adapting to property, but also have it can be found that embodiment 4, has comprehensive performance best by application implementation
Guarantor is collapsed effect, moreover it is possible to enhance the intensity of concrete.
Claims (5)
1. a kind of preparation method of Mobyneb polycarboxylate water-reducer, which comprises the following steps:
(1) raw material: 180 mass parts of isopentene group polyoxyethylene ether, 10 mass parts of fumaric acid, 7 mass parts of acrylic acid, propylene is chosen
Sour hydroxyl ethyl ester 20-25 mass parts, acrylamido methylpropane sulfonic acid 1-2 mass parts, acrylamide 1-2 mass parts, 1.5 matter of oxidant
Measure part, 1 mass parts of reducing agent, 0.8 mass parts of chain-transferring agent, 5 mass parts of sodium hydroxide, water 338.7-349.2 mass parts；
(2) isopentene group polyoxyethylene ether, fumaric acid being added in the water of 120 mass parts, stirring and dissolving adds oxidant,
Stir to get homogeneous solution；
(3) acrylic acid, hydroxy-ethyl acrylate, acrylamido methylpropane sulfonic acid, acrylamide are added in 20 mass parts water, are obtained
1# solution；Reducing agent and chain-transferring agent are added in 50 mass parts water, 2# solution is obtained；In step 2 gained homogeneous solution,
1# solution and 2# solution are successively added dropwise at 30 DEG C；Wherein, 1# solution is added dropwise 3 hours, and 2# solution is added dropwise 3.5 hours；
(4) aging 1 hour, the water of supplement 148.7-159.2 mass parts are stirred 0.5 hour, are obtained more at 40 DEG C after dripping
Functional polycarboxylate superplasticizer.
2. the preparation method of Mobyneb polycarboxylate water-reducer according to claim 1, which is characterized in that the oxidant choosing
The hydrogen peroxide for being 28wt% with concentration, the reducing agent are L-AA (Vc)；Oxidizing and Reducing Agents is as redox
System generates free radicals, and causes monomer polymerization.
3. the preparation method of Mobyneb polycarboxylate water-reducer according to claim 1, which is characterized in that the chain-transferring agent
In molar ratio it is that 1 mixing forms by mercaptopropionic acid and methyl propane sulfonic acid sodium, propagating radical can be effectively made to occur freely
Group-transfer adjusts molecular size range.
4. the preparation method of Mobyneb polycarboxylate water-reducer according to claim 1, which is characterized in that the isopentene group
Polyoxyethylene ether is TPEG-2400, it is free-radical polymerized with fumaric acid and acrylic acid progress, in polycarboxylate water-reducer as branch
Chain.
5. the preparation method of Mobyneb polycarboxylate water-reducer according to claim 1, which is characterized in that the fumaric acid exists
Polycarboxylate water-reducer is as main chain.
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| CN104356314A (en) * | 2014-10-21 | 2015-02-18 | 福建建工建材科技开发有限公司 | Normal-temperature synthetizing method for slow release type polycarboxylate water-reducer and product produced by same |
| CN104628969A (en) * | 2015-01-30 | 2015-05-20 | 江苏奥莱特新材料有限公司 | Preparation method of slow-release solid polycarboxylic acid water reducing agent |
| CN105271885A (en) * | 2015-09-24 | 2016-01-27 | 四川恒泽建材有限公司 | Mud resistance and slump loss resistance type high-performance polycarboxylic acid water reducer and preparation method thereof |
| CN105669911A (en) * | 2016-01-14 | 2016-06-15 | 厦门路桥翔通建材科技有限公司 | Concrete water-retention anti-segregation agent and preparation method thereof |
| CN105776933A (en) * | 2014-12-22 | 2016-07-20 | 上海东大化学有限公司 | Mud-resisting type polycarboxylate-type water reducer and preparation method and use method thereof |
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104356314A (en) * | 2014-10-21 | 2015-02-18 | 福建建工建材科技开发有限公司 | Normal-temperature synthetizing method for slow release type polycarboxylate water-reducer and product produced by same |
| CN105776933A (en) * | 2014-12-22 | 2016-07-20 | 上海东大化学有限公司 | Mud-resisting type polycarboxylate-type water reducer and preparation method and use method thereof |
| CN104628969A (en) * | 2015-01-30 | 2015-05-20 | 江苏奥莱特新材料有限公司 | Preparation method of slow-release solid polycarboxylic acid water reducing agent |
| CN105271885A (en) * | 2015-09-24 | 2016-01-27 | 四川恒泽建材有限公司 | Mud resistance and slump loss resistance type high-performance polycarboxylic acid water reducer and preparation method thereof |
| CN105669911A (en) * | 2016-01-14 | 2016-06-15 | 厦门路桥翔通建材科技有限公司 | Concrete water-retention anti-segregation agent and preparation method thereof |
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