CN113956407B - Modified polyether macromonomer and preparation method and use method thereof - Google Patents
Modified polyether macromonomer and preparation method and use method thereof Download PDFInfo
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- CN113956407B CN113956407B CN202111314480.5A CN202111314480A CN113956407B CN 113956407 B CN113956407 B CN 113956407B CN 202111314480 A CN202111314480 A CN 202111314480A CN 113956407 B CN113956407 B CN 113956407B
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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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- Polymers & Plastics (AREA)
- Polyethers (AREA)
- Curing Cements, Concrete, And Artificial Stone (AREA)
Abstract
The invention discloses a modified polyether macromonomer as well as a preparation method and a use method thereof, belonging to the technical field of water reducing agents, wherein the modified polyether macromonomer is composed of the following components in parts by weight: 100 parts of polyether macromonomer, 0.1-0.3 part of tributyl phosphate, 0.1-0.3 part of polydimethylsiloxane, 0-0.2 part of polyoxyethylene polyoxypropylene pentaerythritol ether, 0.01-0.05 part of polyoxyethylene polyoxypropylene alcohol amine ether, 0.01-0.05 part of polyoxyethylene polyoxypropylene glycerol ether, 0.05-0.25 part of sodium dodecyl sulfate, 0.05-0.25 part of triterpenoid saponin, 0-1 part of fumaric acid, 0-1 part of itaconic acid and 1-2 parts of citric acid. Solves the technical problems of large gas content, reduced strength, poor durability and the like in the concrete after the polycarboxylate superplasticizer is used.
Description
Technical Field
The invention belongs to the technical field of water reducing agents, and particularly relates to a modified polyether macromonomer, and a preparation method and a use method thereof.
Background
With the rapid development of the building industry, the effect of the polycarboxylic acid high-performance water reducing agent in engineering application is more and more prominent. Compared with traditional high-efficiency water reducing agents such as naphthalene water reducing agents, the polycarboxylic acid high-performance water reducing agent has a plurality of unique technical performance advantages: the mixing amount is low, the water reducing rate is high, the slump retaining effect is good, the prepared concrete has small shrinkage, and the volume stability and the durability of the concrete are favorably improved; and the production and use processes are environment-friendly and pollution-free, and the additive belongs to a green additive. Meanwhile, the raw materials of concrete are almost exhausted, and the machine-made sand concrete is more and more, but the cohesiveness of the machine-made sand concrete is poor due to poor machine-made sand particle type and poor gradation, so that the fluidity and the durability of the concrete are influenced. At the present stage, the macromonomer used for the polycarboxylate superplasticizer mainly comprises methyl allyl polyoxyethylene ether, isopentenyl polyoxyethylene ether, ethylene glycol vinyl polyoxyethylene ether, diethylene glycol vinyl polyoxyethylene ether and 4-hydroxybutyl vinyl polyoxyethylene ether, a polyether macromonomer product in the market is prepared by ring-opening polymerization of a corresponding initiator and ethylene oxide under the action of an alkaline catalyst, and the polyether macromonomer structurally contains long polyethylene glycol side chains and has hydrophilicity and air entraining property, but the introduced bubbles are different in size, so that certain troubles are caused for synthesis and application.
Therefore, there is a need in the art to improve the performance of polyether macromonomer so as to solve the problems of high air content, reduced strength, poor durability and the like in concrete after the polycarboxylate superplasticizer is used.
Disclosure of Invention
Aiming at the defect of air entraining of polyether macromonomer in the prior art, the invention provides the modified polyether macromonomer and the preparation method and the use method thereof.
The technical scheme adopted by the invention for solving the technical problem is as follows: a modified polyether macromonomer is composed of the following components in parts by weight: 100 parts of polyether macromonomer, 0.1-0.3 part of tributyl phosphate, 0.1-0.3 part of polydimethylsiloxane, 0-0.2 part of polyoxyethylene polyoxypropylene pentaerythritol ether, 0.01-0.05 part of polyoxyethylene polyoxypropylene alcohol amine ether, 0.01-0.05 part of polyoxyethylene polyoxypropylene glycerol ether, 0.05-0.25 part of sodium dodecyl sulfate, 0.05-0.25 part of triterpenoid saponin, 0-1 part of fumaric acid, 0-1 part of itaconic acid and 1-2 parts of citric acid.
Preferably, the weight part ratio of each component is as follows: 100 parts of polyether macromonomer, 0.15-0.25 part of tributyl phosphate, 0.15-0.25 part of polydimethylsiloxane, 0.05-0.15 part of polyoxyethylene polyoxypropylene pentaerythritol ether, 0.02-0.04 part of polyoxyethylene polyoxypropylene alcohol amine ether, 0.02-0.04 part of polyoxyethylene polyoxypropylene glycerol ether, 0.10-0.20 part of sodium dodecyl sulfate, 0.10-0.20 part of triterpenoid saponin, 0.25-0.75 part of fumaric acid, 0.25-0.75 part of itaconic acid and 1.25-1.75 parts of citric acid.
Preferably, the polyether macromonomer comprises any one or more of methyl allyl polyoxyethylene ether, isopentenyl polyoxyethylene ether, ethylene glycol vinyl polyoxyethylene ether, diethylene glycol vinyl polyoxyethylene ether and 4-hydroxybutyl vinyl polyoxyethylene ether, and the number average molecular weight of the polyether macromonomer is 2400-6000.
A method of preparing a modified polyether macromonomer, comprising: adding 0.1-0.3 part of tributyl phosphate, 0.1-0.3 part of polydimethylsiloxane, 0-0.2 part of polyoxyethylene polyoxypropylene pentaerythritol ether, 0.01-0.05 part of polyoxyethylene polyoxypropylene alcohol amine ether, 0.01-0.05 part of polyoxyethylene polyoxypropylene glycerol ether, 0.05-0.25 part of sodium dodecyl sulfate, 0.05-0.25 part of triterpenoid saponin, 0-1 part of fumaric acid, 0-1 part of itaconic acid and 1-2 parts of citric acid into 100 parts of polyether macromonomer at the temperature of 60-100 ℃ under the stirring state, and uniformly stirring to obtain the modified polyether macromonomer with the pH value of 3.5-4.5.
Preferably, in order to improve the performance effect of the modified polyether macromonomer, the stirring time for uniformly stirring the modified polyether macromonomer is 20-60 min.
Preferably, the effect is better when the stirring time required for uniformly stirring the modified monomer is 30-50 min.
Preferably, the preparation temperature of the modified monomer is preferably 70-90 ℃ which is good.
In the preferred embodiment, the preparation method can be carried out without protection of inert atmosphere, so that the production cost can be reduced in the actual production process, and the preparation method is suitable for comprehensive popularization and application.
The use method of the modified polyether macromonomer comprises the steps of carrying out polymerization reaction on the prepared modified monomer and acrylic acid under the action of an initiator, a reducing agent and a chain transfer agent to obtain a polycarboxylic acid water reducing agent; the polycarboxylic acid water reducing agent is prepared by polymerizing the following components in parts by weight: 400-450 parts of modified macromonomer, 50-60 parts of acrylic acid, 8-12 parts of hydrogen peroxide, 1.5-2 parts of vitamin C, 1.8-2.2 parts of mercaptopropionic acid, 5-10 parts of sodium hydroxide and 450 parts of deionized water; wherein the polymerization temperature is 5-45 ℃ and the polymerization time is 1-5 hours.
In the modified polyether macromonomer provided by the invention, defoaming components such as tributyl phosphate, polydimethylsiloxane, polyoxyethylene polyoxypropylene pentaerythritol ether, polyoxyethylene polyoxypropylene alcohol amine ether, polyoxyethylene polyoxypropylene glycerol ether and the like are introduced, so that uneven bubbles introduced into the polyether macromonomer are reduced, the hardened concrete has no harmful holes, and the compressive strength and the anti-carbonization effect of the hardened concrete are improved; air entraining components such as sodium dodecyl sulfate, triterpenoid saponin and the like are introduced, so that a proper amount of small bubbles can be introduced into the synthesized water reducing agent in the application of the concrete, the workability of the concrete is improved, the concrete has good construction performance, and the shrinkage of the concrete is improved. Simultaneously, fumaric acid and itaconic acid are adopted to further modify the polyether macromonomer, and both the fumaric acid and the itaconic acid contain double bonds and carboxyl groups, so that the polymerization activity of the polyether macromonomer can be improved, the polymerization degree can be improved, and the water reducing and slump retaining effects of the water reducing agent can be improved; the citric acid structure contains polycarboxyl, so that the citric acid structure can play a role in retarding in concrete and improve the slump retaining effect of the concrete.
The invention has the beneficial effects that:
(1) The modified polyether macromonomer breaks through the performance of the existing monomer, the synthesized water reducing agent has good economic benefit, and the water reducing agent prepared from the modified polyether macromonomer has good adaptability, high water reducing rate, good slump retaining effect, good air entraining effect, small shrinkage, high strength and improved carbonization resistance.
(2) The modified monomer simultaneously introduces defoaming and air entraining components, so that the defoaming and air entraining effects of the modified monomer are improved; double bonds and carboxyl groups are introduced at the same time, so that the polymerization activity of the monomers is improved, and the water reducing and slump retaining effects of the product are ensured; improve the workability and durability of concrete.
(3) The modified monomer can be widely applied to synthesis of various water reducing agents.
Detailed Description
The present invention will be further described with reference to the following examples.
Example 1
A preparation method of a modified polyether macromonomer comprises the following steps: 0.1 part of tributyl phosphate, 0.3 part of polydimethylsiloxane, 0.05 part of polyoxyethylene polyoxypropylene alcohol ether, 0.01 part of polyoxyethylene polyoxypropylene glycerol ether, 0.1 part of sodium dodecyl sulfonate, 0.2 part of triterpenoid saponin, 0.5 part of fumaric acid, 0.5 part of itaconic acid and 1 part of citric acid are added into a polymerization reaction kettle into which a polyether macromonomer is added under stirring at 80 ℃, and the obtained modified polyether macromonomer is stirred for 30min until uniform mixing, wherein the pH value of the obtained modified polyether macromonomer is 4.0.
The prepared modified polyether macromonomer is subjected to polymerization reaction to prepare the polycarboxylic acid water reducing agent which is applied to C30 concrete, wherein the formula of the C30 concrete is shown in Table 1: concrete tests are carried out according to GB 8076-2008 concrete admixture and GB/T50082-2009 test method standard for long-term performance and durability of common concrete.
TABLE 1
Through detection, 1.8kg of polycarboxylic acid water reducing agent synthesized by adding the modified polyether macromonomer 1 into C30 concrete, the initial expansion degree of the concrete is 550mm, the 120min expansion degree is 500mm, the initial gas content is 4.5%, the 120min gas content is 4.0%, the 28d shrinkage ratio is 98%, the 28d compressive strength is 37MPa, and the 28d carbonization depth is 1.9mm.
Examples 2 to 5
Modified polyether macromonomers were prepared according to the procedure and procedure of example 1, following the formulation and operating parameters of table 1.
TABLE 2
The modified polyether macromonomer obtained in the above examples 1 to 5 was used to prepare a polycarboxylic acid water reducing agent by a conventional synthesis process in the art, and the polycarboxylic acid water reducing agent was applied to the above concrete with C30 mix proportion to test the properties thereof, as shown in Table 3 below.
Wherein comparative example 1 is a polycarboxylic acid water reducer prepared by adopting methyl allyl polyoxyethylene ether with a commercial data molecular weight of 2400 according to a conventional synthesis process in the field, and comparative example 2 is a polycarboxylic acid water reducer prepared by adopting isopentenyl polyoxyethylene ether with a commercial data molecular weight of 2400 according to a conventional synthesis process in the field.
The performance test results of the modified polyether macromonomer synthesized into the polycarboxylic acid water reducer obtained in examples 1 to 5 are shown in Table 3. As can be seen from Table 3, in C30 concrete, the polycarboxylic acid water reducer synthesized by the modified polyether macromonomer has an initial expansion degree of 550-600mm, an expansion degree of 120min still reaches 500-550 mm, an initial gas content of 4.3-4.5%, a gas content of 4.0-4.2% in 120min, a 28d shrinkage ratio of 98-102%, a 28d compressive strength of 37-42MPa and a 28d carbonization depth of 1.5-1.9 mm. The modified polyether macromonomer prepared by the invention has good use effect in C30 concrete, and is superior to the polyether macromonomer sold in the market.
The above embodiments are only for illustrating the invention and are not to be construed as limiting the invention, and those skilled in the art can make various changes and modifications without departing from the spirit and scope of the invention, therefore, all equivalent technical solutions also belong to the scope of the invention, and the scope of the invention is defined by the claims.
The above embodiments are only for illustrating the invention and are not to be construed as limiting the invention, and those skilled in the art can make various changes and modifications without departing from the spirit and scope of the invention, therefore, all equivalent technical solutions also belong to the scope of the invention, and the scope of the invention is defined by the claims.
Claims (8)
1. The modified polyether macromonomer is characterized by comprising the following components in parts by weight: 100 parts of a polyether macromonomer, 0.1 to 0.3 part of tributyl phosphate, 0.1 to 0.3 part of polydimethylsiloxane, 0 to 0.2 part of polyoxyethylene polyoxypropylene pentaerythritol ether, 0.01 to 0.05 part of polyoxyethylene polyoxypropylene alcohol amine ether, 0.01 to 0.05 part of polyoxyethylene polyoxypropylene glycerol ether, 0.05 to 0.25 part of sodium dodecyl sulfate, 0.05 to 0.25 part of triterpenoid saponin, 0 to 1 part of fumaric acid, 0 to 1 part of itaconic acid and 1 to 2 parts of citric acid.
2. The modified polyether macromonomer of claim 1, wherein the weight portion ratio of each component is as follows: 100 parts of polyether macromonomer, 0.15 to 0.25 part of tributyl phosphate, 0.15 to 0.25 part of polydimethylsiloxane, 0.05 to 0.15 part of polyoxyethylene polyoxypropylene pentaerythritol ether, 0.02 to 0.04 part of polyoxyethylene polyoxypropylene alcohol amine ether, 0.02 to 0.04 part of polyoxyethylene polyoxypropylene glycerol ether, 0.10 to 0.20 part of sodium dodecyl sulfonate, 0.10 to 0.20 part of triterpene saponin, 0.25 to 0.75 part of fumaric acid, 0.25 to 0.75 part of itaconic acid and 1.25 to 1.75 parts of citric acid.
3. The modified polyether macromonomer of claim 1 or 2, wherein the polyether macromonomer comprises one or more of methallyl polyoxyethylene ether, isopentenyl polyoxyethylene ether, ethylene glycol ethylene polyoxyethylene ether, diethylene glycol ethylene polyoxyethylene ether, and 4-hydroxybutyl ethylene polyoxyethylene ether.
4. The modified polyether macromonomer according to claim 3, wherein the polyether macromonomer has a number average molecular weight of 2400 to 6000.
5. A preparation method of a modified polyether macromonomer comprises the following steps: adding 0.1 to 0.3 part of tributyl phosphate, 0.1 to 0.3 part of polydimethylsiloxane, 0 to 0.2 part of polyoxyethylene polyoxypropylene pentaerythritol ether, 0.01 to 0.05 part of polyoxyethylene polyoxypropylene alcohol amine ether, 0.01 to 0.05 part of polyoxyethylene polyoxypropylene glycerol ether, 0.05 to 0.25 part of sodium dodecyl sulfate, 0.05 to 0.25 part of triterpenoid saponin, 0 to 1 part of fumaric acid, 0 to 1 part of itaconic acid and 1 to 2 parts of citric acid into 100 parts of the polyether macromonomer under the condition of stirring at the preparation temperature of 60 to 100 ℃, and uniformly stirring to obtain the modified polyether macromonomer with the pH value of 3.5 to 4.5.
6. The method for preparing the modified polyether macromonomer according to claim 5, wherein the preparation temperature is 70 to 90 ℃.
7. A use method of a modified polyether macromonomer is characterized in that the modified polyether macromonomer prepared by the preparation method of the modified polyether macromonomer in claim 5 or 6 and acrylic acid are subjected to polymerization reaction under the action of an initiator, a reducing agent and a chain transfer agent to prepare the polycarboxylic acid water reducing agent.
8. A preparation method of a polycarboxylic water reducer is characterized by comprising the following steps of polymerizing 400 to 450 parts by weight of a modified polyether macromonomer prepared by the preparation method of the modified polyether macromonomer according to claim 5 or 6, 50 to 60 parts by weight of acrylic acid, 8 to 12 parts by weight of hydrogen peroxide, 1.5 to 2 parts by weight of vitamin C, 1.8 to 2.2 parts by weight of mercaptopropionic acid, 5 to 10 parts by weight of sodium hydroxide and 450 parts by weight of deionized water; wherein the polymerization temperature is 5 to 45 ℃, and the polymerization time is 1 to 5 hours.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2000203910A (en) * | 1998-11-09 | 2000-07-25 | Denki Kagaku Kogyo Kk | Polycarboxylic acid type water-reducing agent and concrete composition using the same |
| CN103626419A (en) * | 2012-08-23 | 2014-03-12 | 上海东大化学有限公司 | Polycarboxylate water reducer prepared by taking novel polyether as raw material, and preparation and application method thereof |
| CN113527592A (en) * | 2021-07-30 | 2021-10-22 | 连云港石化有限公司 | Polycarboxylic acid water reducer for gypsum-based self-leveling mortar and preparation method and use method thereof |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2000203910A (en) * | 1998-11-09 | 2000-07-25 | Denki Kagaku Kogyo Kk | Polycarboxylic acid type water-reducing agent and concrete composition using the same |
| CN103626419A (en) * | 2012-08-23 | 2014-03-12 | 上海东大化学有限公司 | Polycarboxylate water reducer prepared by taking novel polyether as raw material, and preparation and application method thereof |
| CN113527592A (en) * | 2021-07-30 | 2021-10-22 | 连云港石化有限公司 | Polycarboxylic acid water reducer for gypsum-based self-leveling mortar and preparation method and use method thereof |
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