CN111018397A - High slump loss resistant type polycarboxylic acid high-performance water reducing agent and preparation method thereof - Google Patents
High slump loss resistant type polycarboxylic acid high-performance water reducing agent and preparation method thereof Download PDFInfo
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- CN111018397A CN111018397A CN201911211109.9A CN201911211109A CN111018397A CN 111018397 A CN111018397 A CN 111018397A CN 201911211109 A CN201911211109 A CN 201911211109A CN 111018397 A CN111018397 A CN 111018397A
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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
- C04B40/00—Processes, in general, for influencing or modifying the properties of mortars, concrete or artificial stone compositions, e.g. their setting or hardening ability
- C04B40/0028—Aspects relating to the mixing step of the mortar preparation
- C04B40/0039—Premixtures of ingredients
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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
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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
- 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)
- Organic Chemistry (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Curing Cements, Concrete, And Artificial Stone (AREA)
Abstract
The invention relates to a high slump retaining type polycarboxylic acid high-performance water reducing agent and a preparation method thereof, wherein the high slump retaining type polycarboxylic acid high-performance water reducing agent is prepared by processing the following raw materials in parts by weight: 400 parts of methallyl alcohol polyoxyethylene ether 380 organic glass, 3.5-4.5 parts of hydrogen peroxide, 2-2.5 parts of mercaptopropionic acid, 0.5-1.0 part of vitamin C, 35-40 parts of acrylic acid, 15-18 parts of caustic soda flakes, 10-20 parts of 1-ethyl- (3-dimethylaminopropyl) carbodiimide hydrochloride, 5-8 parts of dimethylacetamide and 340 parts of water 300 organic glass. In the formula of the water reducing agent, a certain amount of the auxiliary agent is added, so that the dispersibility can be improved, the organic reaction can be promoted, the reaction efficiency can be accelerated, particularly, whether the 1-ethyl- (3-dimethylaminopropyl) carbodiimide hydrochloride and the dimethylacetamide are combined or not has great influence on the reaction efficiency and the water reducing effect, and the combined use amount of the two auxiliary agents is particularly sensitive and can not achieve the ideal effect if the two auxiliary agents are slightly more or less in practice. The water reducing agent prepared by the formula has high water reducing rate and good slump retaining property.
Description
Technical Field
The invention relates to a high slump loss resistant type polycarboxylic acid high-performance water reducing agent and a preparation method thereof, belonging to the technical field of water reducing agent processing.
Background
The water reducing agent is a concrete admixture capable of reducing the water consumption for mixing under the condition of maintaining the slump constant of concrete basically. Most of them are anionic surfactants, such as lignosulfonate and naphthalene sulfonate formaldehyde polymer. After the concrete mixture is added, the dispersion effect on cement particles is achieved, the workability of the concrete mixture can be improved, the unit water consumption is reduced, and the fluidity of the concrete mixture is improved; or the unit cement consumption is reduced, and the cement is saved.
With the increasing requirements on the durability and strength of concrete buildings in engineering construction and application, the requirement is to develop a water reducing agent with higher performance, and the existing high-efficiency water reducing agents comprise naphthalene high-efficiency water reducing agents, melamine high-efficiency water reducing agents, sulfamate water reducing agents, aliphatic water reducing agents and the like, and because the water reducing rate is low, the slump loss resistance is poor, obvious retardation is easy to cause, and the factors such as high alkali content and the like are difficult to meet the technology and requirements of modern concrete. The present invention aims to solve this technical problem.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides a high slump loss resistant polycarboxylic acid high-performance water reducing agent and a preparation method thereof.
The technical scheme adopted by the invention for solving the technical problems is as follows:
a high slump retaining type polycarboxylic acid high-performance water reducing agent is prepared by processing the following raw materials in parts by weight:
400 parts of methallyl alcohol polyoxyethylene ether 380 organic glass, 3.5-4.5 parts of hydrogen peroxide, 2-2.5 parts of mercaptopropionic acid, 0.5-1.0 part of vitamin C, 35-40 parts of acrylic acid, 15-18 parts of caustic soda flakes, 10-20 parts of 1-ethyl- (3-dimethylaminopropyl) carbodiimide hydrochloride, 5-8 parts of dimethylacetamide and 340 parts of water 300 organic glass.
In the formula of the water reducing agent, a certain amount of the auxiliary agent is added, so that the dispersibility can be improved, the organic reaction can be promoted, the reaction efficiency can be accelerated, particularly, whether the 1-ethyl- (3-dimethylaminopropyl) carbodiimide hydrochloride and the dimethylacetamide are combined or not has great influence on the reaction efficiency and the water reducing effect, and the combined use amount of the two auxiliary agents is particularly sensitive and can not achieve the ideal effect if the two auxiliary agents are slightly more or less in practice.
Preferably, the food is processed by the following raw materials in parts by weight:
390 parts of methallyl alcohol polyoxyethylene ether, 3.75 parts of hydrogen peroxide, 2.125 parts of mercaptopropionic acid, 0.875 part of vitamin C, 38.5 parts of acrylic acid, 16.5 parts of caustic soda flakes, 15 parts of 1-ethyl- (3-dimethylaminopropyl) carbodiimide hydrochloride, 6 parts of dimethylacetamide and 325 parts of water.
A preparation method of a high slump retaining type polycarboxylic acid high-performance water reducing agent comprises the following steps:
step S1, adding methallyl alcohol polyoxyethylene ether and part of water with the formula amount into a reaction kettle, and heating to 40 +/-2 ℃ for later use;
step S2: adding hydrogen peroxide into the material obtained in the step S1, and reacting for a period of time;
step S3: preparing mercaptopropionic acid and vitamin C into a material A, preparing acrylic acid into a material B, preparing 1-ethyl- (3-dimethylaminopropyl) carbodiimide hydrochloride and dimethylacetamide into a material C, respectively dripping A, B, C materials into the material system obtained in the step S2 by using the balance of water, reacting for 1-2 hours under heat preservation, and neutralizing the solution by using the tablet base with the formula amount.
Preferably, in step S1, the amount of water is not less than 70% of the total formula amount.
Preferably, in step S2, the reaction temperature is 40-45 ℃ and the reaction time is 0.5-1 h.
Preferably, in step S3, the material a is dripped off within 2.5h, the material B is dripped off within 2h, and the material C is dripped off within 2 h.
The invention has the beneficial effects that: in the formula of the water reducing agent, a certain amount of the auxiliary agent is added, so that the dispersibility can be improved, the organic reaction can be promoted, the reaction efficiency can be accelerated, particularly, whether the 1-ethyl- (3-dimethylaminopropyl) carbodiimide hydrochloride and the dimethylacetamide are combined or not has great influence on the reaction efficiency and the water reducing effect, and the combined use amount of the two auxiliary agents is particularly sensitive and can not achieve the ideal effect if the two auxiliary agents are slightly more or less in practice.
The water reducing agent prepared by the formula has high water reducing rate and good slump retaining property.
Detailed Description
The technical solution of the present invention will be further specifically described below by way of specific examples.
Example 1:
a high slump retaining type polycarboxylic acid high-performance water reducing agent is prepared by processing the following raw materials in parts by weight:
380 parts of methallyl alcohol polyoxyethylene ether, 3.5 parts of hydrogen peroxide, 2 parts of mercaptopropionic acid, 0.5 part of vitamin C, 35 parts of acrylic acid, 15 parts of caustic soda flakes, 10 parts of 1-ethyl- (3-dimethylaminopropyl) carbodiimide hydrochloride, 5 parts of dimethylacetamide and 300 parts of water
The method of preparation of example 1, the method steps are as follows:
step S1, adding methallyl alcohol polyoxyethylene ether and part of water with the formula amount into a reaction kettle, and heating to 40 +/-2 ℃ for later use;
step S2: adding hydrogen peroxide into the material obtained in the step S1, and reacting for a period of time;
step S3: preparing mercaptopropionic acid and vitamin C into a material A, preparing acrylic acid into a material B, preparing 1-ethyl- (3-dimethylaminopropyl) carbodiimide hydrochloride and dimethylacetamide into a material C, respectively dripping A, B, C materials into the material system obtained in the step S2 by using the balance of water, reacting for 1-2 hours under heat preservation, and neutralizing the solution by using the tablet base with the formula amount.
Specifically, in step S1, the amount of water is not less than 70% of the total formula amount, in step S2, the reaction temperature is 40 ℃, the reaction time is 1h, in step S3, the material A is dripped out within 2.5h, the material B is dripped out within 2h, and the material C is dripped out within 2 h.
Example 2:
a high slump retaining type polycarboxylic acid high-performance water reducing agent is prepared by processing the following raw materials in parts by weight:
400 parts of methallyl alcohol polyoxyethylene ether, 4.5 parts of hydrogen peroxide, 2.5 parts of mercaptopropionic acid, 1.0 part of vitamin C, 40 parts of acrylic acid, 18 parts of caustic soda flakes, 20 parts of 1-ethyl- (3-dimethylaminopropyl) carbodiimide hydrochloride, 8 parts of dimethylacetamide and 340 parts of water.
The method of preparation of example 2, the method steps are as follows:
step S1, adding methallyl alcohol polyoxyethylene ether and part of water with the formula amount into a reaction kettle, and heating to 40 +/-2 ℃ for later use;
step S2: adding hydrogen peroxide into the material obtained in the step S1, and reacting for a period of time;
step S3: preparing mercaptopropionic acid and vitamin C into a material A, preparing acrylic acid into a material B, preparing 1-ethyl- (3-dimethylaminopropyl) carbodiimide hydrochloride and dimethylacetamide into a material C, respectively dripping A, B, C materials into the material system obtained in the step S2 by using the balance of water, reacting for 1-2 hours under heat preservation, and neutralizing the solution by using the tablet base with the formula amount.
Specifically, in step S1, the amount of water is not less than 70% of the total formula amount, in step S2, the reaction temperature is 45 ℃, the reaction time is 0.5h, in step S3, the material A is dripped out within 2.5h, the material B is dripped out within 2h, and the material C is dripped out within 2 h.
Example 3:
a high slump retaining type polycarboxylic acid high-performance water reducing agent is prepared by processing the following raw materials in parts by weight:
390 parts of methallyl alcohol polyoxyethylene ether, 3.75 parts of hydrogen peroxide, 2.125 parts of mercaptopropionic acid, 0.875 part of vitamin C, 38.5 parts of acrylic acid, 16.5 parts of caustic soda flakes, 15 parts of 1-ethyl- (3-dimethylaminopropyl) carbodiimide hydrochloride, 6 parts of dimethylacetamide and 325 parts of water.
The method of preparation of example 3, the method steps are as follows:
step S1, adding methallyl alcohol polyoxyethylene ether and part of water with the formula amount into a reaction kettle, and heating to 40 +/-2 ℃ for later use;
step S2: adding hydrogen peroxide into the material obtained in the step S1, and reacting for a period of time;
step S3: preparing mercaptopropionic acid and vitamin C into a material A, preparing acrylic acid into a material B, preparing 1-ethyl- (3-dimethylaminopropyl) carbodiimide hydrochloride and dimethylacetamide into a material C, respectively dripping A, B, C materials into the material system obtained in the step S2 by using the balance of water, reacting for 1-2 hours under heat preservation, and neutralizing the solution by using the tablet base with the formula amount.
Specifically, in step S1, the amount of water is not less than 70% of the total formula amount, in step S2, the reaction temperature is 42 ℃, the reaction time is 0.75h, in step S3, the material A is dripped out within 2.5h, the material B is dripped out within 2h, and the material C is dripped out within 2 h.
Comparative example 1:
a high slump retaining type polycarboxylic acid high-performance water reducing agent is prepared by processing the following raw materials in parts by weight:
390 parts of methallyl alcohol polyoxyethylene ether, 3.75 parts of hydrogen peroxide, 2.125 parts of mercaptopropionic acid, 0.875 part of vitamin C, 38.5 parts of acrylic acid, 16.5 parts of caustic soda flakes and 325 parts of water.
The preparation method of comparative example 1, comprising the following steps:
step S1, adding methallyl alcohol polyoxyethylene ether and part of water with the formula amount into a reaction kettle, and heating to 40 +/-2 ℃ for later use;
step S2: adding hydrogen peroxide into the material obtained in the step S1, and reacting for a period of time;
step S3: preparing mercaptopropionic acid and vitamin C into a material A, preparing acrylic acid into a material B, respectively dripping A, B materials into the material system obtained in the step S2 by using the balance of water, carrying out heat preservation reaction for 1-2 hours, and neutralizing the solution by using the flake caustic soda with the formula amount.
Specifically, in step S1, the amount of water is not less than 70% of the total formula amount, in step S2, the reaction temperature is 42 ℃, the reaction time is 0.75h, in step S3, the material A is dripped out within 2.5h, and the material B is dripped out within 2 h.
Comparative example 2:
a high slump retaining type polycarboxylic acid high-performance water reducing agent is prepared by processing the following raw materials in parts by weight:
390 parts of methallyl alcohol polyoxyethylene ether, 3.75 parts of hydrogen peroxide, 2.125 parts of mercaptopropionic acid, 0.875 part of vitamin C, 38.5 parts of acrylic acid, 16.5 parts of caustic soda flakes, 15 parts of 1-ethyl- (3-dimethylaminopropyl) carbodiimide hydrochloride and 325 parts of water.
The preparation method of comparative example 2, which comprises the following steps:
step S1, adding methallyl alcohol polyoxyethylene ether and part of water with the formula amount into a reaction kettle, and heating to 40 +/-2 ℃ for later use;
step S2: adding hydrogen peroxide into the material obtained in the step S1, and reacting for a period of time;
step S3: preparing mercaptopropionic acid and vitamin C into a material A, preparing acrylic acid into a material B, preparing 1-ethyl- (3-dimethylaminopropyl) carbodiimide hydrochloride into a material C, respectively dripping A, B, C materials into the material system obtained in the step S2 by using the balance of water, reacting for 1-2 hours under heat preservation, and neutralizing the solution by using the flake caustic soda with the formula amount.
Specifically, in step S1, the amount of water is not less than 70% of the total formula amount, in step S2, the reaction temperature is 42 ℃, the reaction time is 0.75h, in step S3, the material A is dripped out within 2.5h, the material B is dripped out within 2h, and the material C is dripped out within 2 h.
Comparative example 3:
a high slump retaining type polycarboxylic acid high-performance water reducing agent is prepared by processing the following raw materials in parts by weight:
390 parts of methallyl alcohol polyoxyethylene ether, 3.75 parts of hydrogen peroxide, 2.125 parts of mercaptopropionic acid, 0.875 part of vitamin C, 38.5 parts of acrylic acid, 16.5 parts of caustic soda flakes, 6 parts of dimethylacetamide and 325 parts of water.
The preparation method of comparative example 3, comprising the following steps:
step S1, adding methallyl alcohol polyoxyethylene ether and part of water with the formula amount into a reaction kettle, and heating to 40 +/-2 ℃ for later use;
step S2: adding hydrogen peroxide into the material obtained in the step S1, and reacting for a period of time;
step S3: preparing mercaptopropionic acid and vitamin C into a material A, preparing acrylic acid into a material B, preparing dimethylacetamide into a material C, respectively dropwise adding A, B, C into the material system obtained in the step S2 by using the balance of water, reacting for 1-2 hours under heat preservation, and neutralizing the solution by using the tablet alkali in a formula amount.
Specifically, in step S1, the amount of water is not less than 70% of the total formula amount, in step S2, the reaction temperature is 42 ℃, the reaction time is 0.75h, in step S3, the material A is dripped out within 2.5h, the material B is dripped out within 2h, and the material C is dripped out within 2 h.
The reducing agents of examples 1 to 3 and comparative examples 1 to 3 were used in concrete formulations with an addition of 0.5%, and the standard performance indexes of concrete doped with a water reducing agent were as follows:
subject: six groups of 42.5 ordinary silica cement are taken as experimental objects, and the 42.5 ordinary silica cement in each group is 1m3Is matched with 3m3The sand and stone are divided into 10 square cement boards with the thickness of 10 cm.
The experimental method comprises the following steps: the performance of the water reducing agent of the examples and the water reducing agent of the comparative example (the addition amount is 0.5%) is tested according to a water reducing rate test, a gas content test, a setting time test, a compressive strength ratio and a shrinkage ratio; the test time was 30 days. The average values of comparative examples 1 to 3 are as follows:
the average value of the test data of the water reducing agent of the embodiments 1 to 3 is as follows:
the test results show that the cement board prepared from the water reducer is superior to the cement board prepared from the water reducer of the comparative example. The water reducer can embody the characteristics of high slump loss resistance, high water reducing rate and short setting time.
The above-described embodiments are only preferred embodiments of the present invention, and are not intended to limit the present invention in any way, and other variations and modifications may be made without departing from the spirit of the invention as set forth in the claims.
Claims (6)
1. A high slump loss resistant type polycarboxylic acid high-performance water reducing agent is characterized by being prepared by processing the following raw materials in parts by weight:
400 parts of methallyl alcohol polyoxyethylene ether 380 organic glass, 3.5-4.5 parts of hydrogen peroxide, 2-2.5 parts of mercaptopropionic acid, 0.5-1.0 part of vitamin C, 35-40 parts of acrylic acid, 15-18 parts of caustic soda flakes, 10-20 parts of 1-ethyl- (3-dimethylaminopropyl) carbodiimide hydrochloride, 5-8 parts of dimethylacetamide and 340 parts of water 300 organic glass.
2. The high slump retaining type polycarboxylic acid high-performance water reducing agent of claim 1, which is prepared by processing the following raw materials in parts by weight:
390 parts of methallyl alcohol polyoxyethylene ether, 3.75 parts of hydrogen peroxide, 2.125 parts of mercaptopropionic acid, 0.875 part of vitamin C, 38.5 parts of acrylic acid, 16.5 parts of caustic soda flakes, 15 parts of 1-ethyl- (3-dimethylaminopropyl) carbodiimide hydrochloride, 6 parts of dimethylacetamide and 325 parts of water.
3. A preparation method of the high slump retaining type polycarboxylic acid high-performance water reducing agent disclosed by claim 1 or 2 is characterized by comprising the following steps:
step S1, adding methallyl alcohol polyoxyethylene ether and part of water with the formula amount into a reaction kettle, and heating to 40 +/-2 ℃ for later use;
step S2: adding hydrogen peroxide into the material obtained in the step S1, and reacting for a period of time;
step S3: preparing mercaptopropionic acid and vitamin C into a material A, preparing acrylic acid into a material B, preparing 1-ethyl- (3-dimethylaminopropyl) carbodiimide hydrochloride and dimethylacetamide into a material C, respectively dripping A, B, C materials into the material system obtained in the step S2 by using the balance of water, reacting for 1-2 hours under heat preservation, and neutralizing the solution by using the tablet base with the formula amount.
4. The preparation method of the high slump retaining type polycarboxylic acid high-performance water reducing agent according to claim 3, wherein in the step S1, the amount of water is not less than 70% of the total formula amount.
5. The preparation method of the high slump retaining type polycarboxylic acid high-performance water reducing agent according to claim 3, characterized in that in step S2, the reaction temperature is 40-45 ℃ and the reaction time is 0.5-1 h.
6. The preparation method of the high slump retaining type polycarboxylic acid high performance water reducing agent according to claim 3, wherein in step S3, the material A is dripped out within 2.5h, the material B is dripped out within 2h, and the material C is dripped out within 2 h.
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