CN113512154B - Method for synthesizing solid polycarboxylate superplasticizer - Google Patents
Method for synthesizing solid polycarboxylate superplasticizer Download PDFInfo
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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
- 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
- C08F2/00—Processes of polymerisation
- C08F2/38—Polymerisation using regulators, e.g. chain terminating agents, e.g. telomerisation
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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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- Ceramic Engineering (AREA)
- Materials Engineering (AREA)
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- Polymerisation Methods In General (AREA)
- Curing Cements, Concrete, And Artificial Stone (AREA)
- Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)
Abstract
A method for synthesizing a solid polycarboxylic acid water reducer uses prenyl polyoxyethylene ether macromonomer and acrylic acid as main raw materials for preparing the solid polycarboxylic acid water reducer, and two solubilizers (dimethyl maleate and dimethyl itaconate) are added in the preparation process of the water reducer, so that the obtained water reducer can optimize the dispersion performance of the solid polycarboxylic acid water reducer, improve the net slurry fluidity of cement and reduce the loss with time. And under the specific proportioning of the solubilizer, the water reducing agent system can play a role in synergy, so that the dispersibility of the water reducing agent system is greatly improved.
Description
Technical Field
The invention relates to the field of water reducer manufacturing, and particularly relates to a method for synthesizing a solid polycarboxylic acid water reducer.
Background
The water reducing agent is also called as plasticizer or cement dispersant, and is named because the water consumption of fresh concrete can be obviously reduced when the water reducing agent is used. The concrete is doped with a proper amount of water reducing agent, so that the water consumption is reduced, the water-cement ratio is obviously reduced, and the effects of improving the strength, frost resistance, impermeability and a series of physical and mechanical properties are achieved under the condition of keeping the workability of fresh concrete the same.
The water reducing agent is mostly a surfactant, wherein the polycarboxylate water reducing agent is a surfactant with a molecular structure of carboxyl-containing graft copolymer, the molecular structure is in a comb shape and is mainly obtained by copolymerizing unsaturated monomers under the action of an initiator, a main chain is formed by polymerizing carboxyl-containing active monomers, a side chain is formed by grafting and copolymerizing functional group-containing active monomers and the main chain, and the polycarboxylate water reducing agent has high water reducing rate and enables concrete stirrers to have good fluidity. The net paste fluidity of cement can measure the diffusion capacity of the water reducing agent to the cement paste, and when the net paste fluidity is high, the net paste fluidity usually means that the cement loss with time is low. Based on this, how to improve the net slurry fluidity is a subject worth long-term research.
Disclosure of Invention
Aiming at the problems in the prior art, the invention aims to provide a method for synthesizing a solid polycarboxylic acid water reducing agent, and the solid polycarboxylic acid water reducing agent prepared by the method can improve the net slurry fluidity of cement and reduce the loss with time.
The method for synthesizing the solid polycarboxylic acid water reducing agent is characterized by comprising the following steps of:
adding an isopentenol polyoxyethylene ether macromonomer (IPEG) with the monomer mole number of 2-4mol into a reaction kettle, heating to 60-68 ℃, and starting stirring;
adding 1-2mol of Acrylic Acid (AA), mercaptopropionic acid and a solubilizer into a dripping tank, and stirring and mixing uniformly to obtain a dripping liquid;
after the IPEG macromonomer is completely melted, 0.3-0.4% of initiator by mass of IPEG is added into a reaction kettle, the dropping liquid is dripped by a constant flow pump after the initiator is dissolved, the total dripping time is 4.0h, the initiator is respectively replenished when the dripping liquid is dripped for 2.0h and 3.0h, and the mass of the initiator replenished every time is 0.2% of the IPEG;
after the dripping is finished, the heat preservation and aging reaction is carried out for 1 to 1.5 hours, and the solid polycarboxylic acid water reducing agent can be obtained after the natural cooling and hardening through crushing and grinding.
Further, the mass of the mercaptopropionic acid is 0.6% of the mass of the IPEG.
Further, the solubilizer is a mixture of dimethyl maleate and dimethyl itaconate.
Further, the initiator is one or more of azobisisobutyronitrile, persulfate and azobisisobutyronitrile.
Further, the mass content of the solubilizer in the dropping liquid is 0.4-0.8% of the IPEG.
Further, the mass content of the solubilizer in the dropping liquid is 0.6 percent of the IPEG.
Further, the dosage ratio of the dimethyl maleate to the dimethyl itaconate in the dropping liquid is 1: 3.
The invention takes the prenyl polyoxyethylene ether macromonomer and the acrylic acid as main raw materials for preparing the solid polycarboxylate water reducer, and two solubilizers (dimethyl maleate and dimethyl itaconate) are added in the preparation process of the water reducer, so that the obtained water reducer can optimize the dispersion performance of the solid polycarboxylate water reducer, improve the net slurry fluidity of cement and reduce the time loss. And under the specific proportioning of the solubilizer, the water reducing agent system can play a role in synergy, so that the dispersibility of the water reducing agent system is greatly improved.
Detailed Description
The technical effects of the present invention are demonstrated below by specific examples, but the embodiments of the present invention are not limited thereto.
Example 1
A method for synthesizing a solid polycarboxylic acid water reducing agent comprises the following steps:
adding an isopentenol polyoxyethylene ether macromonomer (IPEG) with the monomer mole number of 4mol into a reaction kettle, heating to 68 ℃, and starting stirring;
adding 1mol of Acrylic Acid (AA), mercaptopropionic acid (0.6 percent of IPEG in mass) and solubilizer (dimethyl maleate and dimethyl itaconate) into a dropwise adding tank, and stirring and mixing uniformly to obtain a dropwise adding liquid;
after the IPEG macromonomer is completely melted, 0.4% of initiator Azobisisobutyronitrile (AIBN) with the mass of IPEG is added into a reaction kettle, the dropping liquid is dripped by a constant flow pump after the initiator is dissolved, the total dripping time is 4.0h, the initiator is respectively replenished when the dropping liquid is dripped for 2.0h and 3.0h, and the mass of the initiator replenished each time is 0.2% of the IPEG;
after the dripping is finished, the heat preservation and aging reaction is carried out for 1h, and the solid polycarboxylic acid water reducing agent can be obtained after the natural cooling and hardening through crushing and grinding.
The mass content of the solubilizer in the dropping liquid prepared by the preparation method is 0.6 percent of IPEG, and the two solubilizers, namely dimethyl maleate and dimethyl itaconate, are distributed in equal proportion.
Example 2
A method for synthesizing a solid polycarboxylic acid water reducing agent comprises the following steps:
adding an isopentenol polyoxyethylene ether macromonomer (IPEG) with the monomer mole number of 4mol into a reaction kettle, heating to 68 ℃, and starting stirring;
adding 1mol of Acrylic Acid (AA), mercaptopropionic acid (0.6 percent of IPEG in mass) and solubilizer (dimethyl maleate and dimethyl itaconate) into a dropwise adding tank, and stirring and mixing uniformly to obtain a dropwise adding liquid;
after the IPEG macromonomer is completely melted, 0.4% of initiator Azobisisobutyronitrile (AIBN) with the mass of IPEG is added into a reaction kettle, the dropping liquid is dripped by a constant flow pump after the initiator is dissolved, the total dripping time is 4.0h, the initiator is respectively replenished when the dropping liquid is dripped for 2.0h and 3.0h, and the mass of the initiator replenished each time is 0.2% of the IPEG;
after the dripping is finished, the heat preservation and aging reaction is carried out for 1h, and the solid polycarboxylic acid water reducing agent can be obtained after the natural cooling and hardening through crushing and grinding.
The mass content of the solubilizer in the dropping liquid prepared by the preparation method is 0.4 percent of IPEG, and the two solubilizers, namely dimethyl maleate and dimethyl itaconate, are distributed in equal proportion.
Example 3
A method for synthesizing a solid polycarboxylic acid water reducing agent comprises the following steps:
adding an isopentenol polyoxyethylene ether macromonomer (IPEG) with the monomer mole number of 4mol into a reaction kettle, heating to 68 ℃, and starting stirring;
adding 1mol of Acrylic Acid (AA), mercaptopropionic acid (0.6 percent of IPEG in mass) and solubilizer (dimethyl maleate and dimethyl itaconate) into a dropwise adding tank, and stirring and mixing uniformly to obtain a dropwise adding liquid;
after the IPEG macromonomer is completely melted, 0.4% of initiator Azobisisobutyronitrile (AIBN) with the mass of IPEG is added into a reaction kettle, the dropping liquid is dripped by a constant flow pump after the initiator is dissolved, the total dripping time is 4.0h, the initiator is respectively replenished when the dropping liquid is dripped for 2.0h and 3.0h, and the mass of the initiator replenished each time is 0.2% of the IPEG;
after the dripping is finished, the heat preservation and aging reaction is carried out for 1h, and the solid polycarboxylic acid water reducing agent can be obtained after the natural cooling and hardening through crushing and grinding.
The mass content of the solubilizer in the dropping liquid prepared by the preparation method is 0.6 percent of IPEG, and the dosage ratio of dimethyl maleate and dimethyl itaconate of the two solubilizers is 1: 3.
Example 4
A method for synthesizing a solid polycarboxylic acid water reducing agent comprises the following steps:
adding an isopentenol polyoxyethylene ether macromonomer (IPEG) with the monomer mole number of 4mol into a reaction kettle, heating to 68 ℃, and starting stirring;
adding 1mol of Acrylic Acid (AA), mercaptopropionic acid (0.6 percent of IPEG in mass) and solubilizer (dimethyl maleate and dimethyl itaconate) into a dropwise adding tank, and stirring and mixing uniformly to obtain a dropwise adding liquid;
after the IPEG macromonomer is completely melted, 0.4% of initiator Azobisisobutyronitrile (AIBN) with the mass of IPEG is added into a reaction kettle, the dropping liquid is dripped by a constant flow pump after the initiator is dissolved, the total dripping time is 4.0h, the initiator is respectively replenished when the dropping liquid is dripped for 2.0h and 3.0h, and the mass of the initiator replenished each time is 0.2% of the IPEG;
after the dripping is finished, the heat preservation and aging reaction is carried out for 1h, and the solid polycarboxylic acid water reducing agent can be obtained after the natural cooling and hardening through crushing and grinding.
The mass content of the solubilizer in the dropping liquid prepared by the preparation method is 0.6 percent of IPEG, and the dosage ratio of dimethyl maleate and dimethyl itaconate of the two solubilizers is 3: 1.
Example 5
A method for synthesizing a solid polycarboxylic acid water reducing agent comprises the following steps:
adding an isopentenol polyoxyethylene ether macromonomer (IPEG) with the monomer mole number of 4mol into a reaction kettle, heating to 68 ℃, and starting stirring;
adding 1mol of Acrylic Acid (AA), mercaptopropionic acid (0.6 percent of IPEG in mass) and solubilizer (dimethyl maleate and dimethyl itaconate) into a dropwise adding tank, and stirring and mixing uniformly to obtain a dropwise adding liquid;
after the IPEG macromonomer is completely melted, 0.4% of initiator Azobisisobutyronitrile (AIBN) with the mass of IPEG is added into a reaction kettle, the dropping liquid is dripped by a constant flow pump after the initiator is dissolved, the total dripping time is 4.0h, the initiator is respectively replenished when the dropping liquid is dripped for 2.0h and 3.0h, and the mass of the initiator replenished each time is 0.2% of the IPEG;
after the dripping is finished, the heat preservation and aging reaction is carried out for 1h, and the solid polycarboxylic acid water reducing agent can be obtained after the natural cooling and hardening through crushing and grinding.
The mass content of the solubilizer in the dropping liquid prepared by the preparation method is 0.8 percent of IPEG, and the dosage ratio of dimethyl maleate and dimethyl itaconate of the two solubilizers is 1: 1.
Hereinafter, we evaluate the dispersion performance of the solid polycarboxylate superplasticizer by the cement paste fluidity, and the test method is performed according to GB/T8077-. The water-gel ratio is 0.29, the solid content of the water reducer sample to be measured is diluted to 8 percent in order to reduce the weighing error, and the solid content of the water reducer is 0.15 percent. Examples 1-5 correspond to A-E and use the solid polycarboxylate superplasticizer prepared without the addition of a solubilizer as a blank control (corresponding to Z). The results of the experiment are shown in table 1:
TABLE 1 dispersancy Properties of solid polycarboxylic acid Water-reducing Agents
As can be seen from Table 1, the dispersion properties of the solid polycarboxylic acid water reducing agent can be greatly optimized after the two solubilizers of the invention are added, the net slurry fluidity is improved, and the loss with time is reduced. Surprisingly, in a number of experiments, the inventors surprisingly found that the net slurry fluidity of example 3 was much higher than that of the other examples, which may be synergistic effect at a specific ratio of dimethyl maleate to dimethyl itaconate, and further conducted the following experiments in order to verify the effect.
Comparative example 1
A method for synthesizing a solid polycarboxylic acid water reducing agent comprises the following steps:
adding an isopentenol polyoxyethylene ether macromonomer (IPEG) with the monomer mole number of 4mol into a reaction kettle, heating to 68 ℃, and starting stirring;
adding 1mol of Acrylic Acid (AA), mercaptopropionic acid (0.6 percent of IPEG in mass) and a solubilizer (dimethyl maleate) into a dropping tank, and stirring and mixing uniformly to obtain a dropping liquid;
after the IPEG macromonomer is completely melted, 0.4% of initiator Azobisisobutyronitrile (AIBN) with the mass of IPEG is added into a reaction kettle, the dropping liquid is dripped by a constant flow pump after the initiator is dissolved, the total dripping time is 4.0h, the initiator is respectively replenished when the dropping liquid is dripped for 2.0h and 3.0h, and the mass of the initiator replenished each time is 0.2% of the IPEG;
after the dripping is finished, the heat preservation and aging reaction is carried out for 1h, and the solid polycarboxylic acid water reducing agent can be obtained after the natural cooling and hardening through crushing and grinding.
The mass content of the solubilizer in the dropping liquid prepared by the preparation method is 0.6 percent of the IPEG.
Comparative example 2
A method for synthesizing a solid polycarboxylic acid water reducing agent comprises the following steps:
adding an isopentenol polyoxyethylene ether macromonomer (IPEG) with the monomer mole number of 4mol into a reaction kettle, heating to 68 ℃, and starting stirring;
adding 1mol of Acrylic Acid (AA), mercaptopropionic acid (0.6 percent of IPEG in mass) and solubilizer (dimethyl itaconate) into a dropwise adding tank, and stirring and mixing uniformly to obtain dropwise added liquid;
after the IPEG macromonomer is completely melted, 0.4% of initiator Azobisisobutyronitrile (AIBN) with the mass of IPEG is added into a reaction kettle, the dropping liquid is dripped by a constant flow pump after the initiator is dissolved, the total dripping time is 4.0h, the initiator is respectively replenished when the dropping liquid is dripped for 2.0h and 3.0h, and the mass of the initiator replenished each time is 0.2% of the IPEG;
after the dripping is finished, the heat preservation and aging reaction is carried out for 1h, and the solid polycarboxylic acid water reducing agent can be obtained after the natural cooling and hardening through crushing and grinding.
The mass content of the solubilizer in the dropping liquid prepared by the preparation method is 0.6 percent of the IPEG.
Comparative example 3
A method for synthesizing a solid polycarboxylic acid water reducing agent comprises the following steps:
adding an isopentenol polyoxyethylene ether macromonomer (IPEG) with the monomer mole number of 4mol into a reaction kettle, heating to 68 ℃, and starting stirring;
adding 1mol of Acrylic Acid (AA), mercaptopropionic acid (0.6 percent of IPEG in mass) and a solubilizer (dimethyl maleate) into a dropping tank, and stirring and mixing uniformly to obtain a dropping liquid;
after the IPEG macromonomer is completely melted, 0.4% of initiator Azobisisobutyronitrile (AIBN) with the mass of IPEG is added into a reaction kettle, the dropping liquid is dripped by a constant flow pump after the initiator is dissolved, the total dripping time is 4.0h, the initiator is respectively replenished when the dropping liquid is dripped for 2.0h and 3.0h, and the mass of the initiator replenished each time is 0.2% of the IPEG;
after the dripping is finished, the heat preservation and aging reaction is carried out for 1h, and the solid polycarboxylic acid water reducing agent can be obtained after the natural cooling and hardening through crushing and grinding.
The mass content of the solubilizer in the dropping liquid prepared by the preparation method is 0.15 percent of the IPEG.
Comparative example 4
A method for synthesizing a solid polycarboxylic acid water reducing agent comprises the following steps:
adding an isopentenol polyoxyethylene ether macromonomer (IPEG) with the monomer mole number of 4mol into a reaction kettle, heating to 68 ℃, and starting stirring;
adding 1mol of Acrylic Acid (AA), mercaptopropionic acid (0.6 percent of IPEG in mass) and solubilizer (dimethyl itaconate) into a dropwise adding tank, and stirring and mixing uniformly to obtain dropwise added liquid;
after the IPEG macromonomer is completely melted, 0.4% of initiator Azobisisobutyronitrile (AIBN) with the mass of IPEG is added into a reaction kettle, the dropping liquid is dripped by a constant flow pump after the initiator is dissolved, the total dripping time is 4.0h, the initiator is respectively replenished when the dropping liquid is dripped for 2.0h and 3.0h, and the mass of the initiator replenished each time is 0.2% of the IPEG;
after the dripping is finished, the heat preservation and aging reaction is carried out for 1h, and the solid polycarboxylic acid water reducing agent can be obtained after the natural cooling and hardening through crushing and grinding.
The mass content of the solubilizer in the dropping liquid prepared by the preparation method is 0.45 percent of the IPEG.
The experimental data for comparative examples 1-4 are shown in table 2:
TABLE 2 Dispersion Performance of solid polycarboxylic acid water-reducing agent
The above description is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, several modifications and variations can be made without departing from the technical principle of the present invention, and these modifications and variations should also be regarded as the protection scope of the present invention.
Claims (4)
1. The method for synthesizing the solid polycarboxylic acid water reducing agent is characterized by comprising the following steps of:
adding an isopentenol polyoxyethylene ether macromonomer (IPEG) with the monomer mole number of 2-4mol into a reaction kettle, heating to 60-68 ℃, and starting stirring;
adding 1-2mol of Acrylic Acid (AA), mercaptopropionic acid and a solubilizer into a dripping tank, and stirring and mixing uniformly to obtain a dripping liquid;
after the IPEG macromonomer is completely melted, 0.3-0.4% of initiator by mass of IPEG is added into a reaction kettle, the dropping liquid is dripped by a constant flow pump after the initiator is dissolved, the total dripping time is 4.0h, the initiator is respectively replenished when the dripping liquid is dripped for 2.0h and 3.0h, and the mass of the initiator replenished every time is 0.2% of the IPEG;
after the dripping is finished, carrying out heat preservation and aging reaction for 1-1.5h, naturally cooling and hardening, and then crushing and grinding to obtain the solid polycarboxylic acid water reducing agent;
the mass content of the solubilizer in the dropping liquid is 0.4-0.8% of the IPEG, the solubilizer is a mixture of dimethyl maleate and dimethyl itaconate, and the dosage ratio of the dimethyl maleate to the dimethyl itaconate is 1: 3.
2. A method as claimed in claim 1, characterized by: the mass of the mercaptopropionic acid is 0.6 percent of the mass of the IPEG.
3. The method of claim 1, wherein the initiator is one or more of azobisisobutyronitrile, persulfate, and azobisisobutyronitrile.
4. The process according to claim 1, wherein the mass content of solubilizer in the instillation is 0.6% of IPEG.
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