阅读说明：本技术 一种高分散性陶瓷减水剂及其制备方法 (High-dispersity ceramic water reducing agent and preparation method thereof ) 是由 陈艳林 王俊玮 赵娜 黄康 柯凯 于 2021-02-01 设计创作，主要内容包括：本发明提供了一种高分散性陶瓷减水剂及其制备方法,包括如下操作步骤：将150-240份分散型聚合物和210-290份分散保持型聚合物复配,再加水至总份数为1000份,即得到所需的高分散性陶瓷减水剂溶液。本发明通过将两种不同作用的聚合物复配使用,来调节陶瓷的分散性与强度等指标。在陶瓷中加入这种减水剂,改善陶瓷材料的分散性能,降低陶瓷材料的用水量并保证陶瓷坯体的强度,增强陶瓷性能。(The invention provides a high-dispersity ceramic water reducing agent and a preparation method thereof, wherein the preparation method comprises the following operation steps: and (3) compounding 150-240 parts of dispersion type polymer and 210-290 parts of dispersion maintaining type polymer, and adding water to reach the total part of 1000 parts to obtain the required high-dispersibility ceramic water reducer solution. The invention adjusts the indexes of the ceramic such as the dispersibility, the strength and the like by compounding two polymers with different functions. The water reducing agent is added into the ceramic, so that the dispersion performance of the ceramic material is improved, the water consumption of the ceramic material is reduced, the strength of a ceramic blank is ensured, and the ceramic performance is enhanced.)

1. The high-dispersity ceramic water reducing agent is characterized by comprising the following components: 150 portions of dispersion type polymer, 290 portions of dispersion keeping type polymer, 210 portions of dispersion keeping type polymer and the balance of water, and the total mass portion is 1000 portions.

2. The high-dispersibility ceramic water-reducing agent according to claim 1, characterized in that: the dispersion polymer is prepared by the following steps:

the method comprises the following steps: adding 30.7-33.9 parts of 4-methoxybut-2-en-1-ol and 0.6-1.2 parts of lithium aluminum hydride into a high-pressure reaction kettle provided with a stirrer and a thermometer, performing nitrogen replacement for 3 times, then starting vacuumizing to gauge pressure of-0.055 MPa, then heating to 120 ℃, starting dehydration for 0.5 hour, measuring the oxygen content, introducing 62.1-65.7 parts of ethylene oxide and 240.7-245.4 parts of propylene oxide into the reaction kettle at a constant speed after the oxygen content is qualified, controlling the pressure to be less than 0.5MPa, keeping the temperature of 120 ℃ after all the cyclic monomers are introduced into the reaction kettle, aging to negative pressure, cooling and discharging to obtain a polyether monomer;

step two: adding the prepared polyether monomer into a four-neck flask with a stirring rod, heating to 60 ℃ by adopting a water bath, preparing solution A from 1.8-4.1 parts of di-tert-butyl peroxide, 0.7-1.3 parts of thioglycolic acid and 60 parts of water, preparing solution B from 38.9-43.6 parts of diethyl acrylate, 3-5 parts of 4-methoxybut-2-en-1-ol, 3.7-6.3 parts of sodium formaldehyde sulfoxylate and 120 parts of water, simultaneously dropwise adding A, B solution, dropwise adding the solution A for 2.5 hours, dropwise adding the solution B for 2 hours, preserving heat for 1 hour after the addition of the solution A is finished, and adding 7.2-12.3 parts of triethanolamine at one time and supplementing water until the total mass is 1000 parts to obtain the dispersion polymer.

3. The high dispersibility ceramic water reducing agent according to claim 2, wherein said dispersion polymer is further prepared by the steps of:

the method comprises the following steps: adding 31.6 parts of 4-methoxybut-2-en-1-ol and 1.2 parts of lithium aluminum hydride into a high-pressure reaction kettle provided with a stirrer and a thermometer, performing nitrogen replacement for 3 times, vacuumizing to gauge pressure of-0.055 MPa, heating to 120 ℃, dehydrating for 0.5 hour, measuring the oxygen content, introducing 63.7 parts of ethylene oxide and 242.4 parts of propylene oxide into the reaction kettle at constant speed after the oxygen content is qualified, controlling the pressure to be less than 0.5MPa, introducing all cyclic monomers into the reaction kettle, keeping the temperature of 120 ℃, aging to negative pressure, cooling and discharging to obtain a polyether monomer;

step two: adding the prepared polyether monomer into a four-neck flask with a stirring rod, heating to 60 ℃ by adopting a water bath, preparing solution A from 3.3 parts of di-tert-butyl peroxide, 0.9 part of thioglycolic acid and 60 parts of water, preparing solution B from 40.2 parts of diethyl acrylate, 5 parts of 4-methoxybut-2-en-1-ol, 4.3 parts of sodium formaldehyde sulfoxylate and 120 parts of water, dropwise adding A, B simultaneously, dropwise adding the solution A for 2.5 hours, dropwise adding the solution B for 2 hours, preserving heat for 1 hour after the dropwise adding of the solution A is finished, and adding 12.3 parts of triethanolamine at one time and supplementing water until the total mass is 1000 parts to obtain the dispersion type polymer.

4. The high-dispersibility ceramic water-reducing agent according to claim 1, characterized in that: the dispersion retaining polymer is prepared by the steps of:

the method comprises the following steps: adding 20.3-25.7 parts of 3-allyloxy-1, 2-propylene glycol and 0.6-1.2 parts of lithium aluminum hydride into a high-pressure reaction kettle provided with a stirrer and a thermometer, performing nitrogen replacement for 3 times, then starting vacuumizing to gauge pressure of-0.085 MPa, then heating to 120 ℃, starting dehydration for 1-2 hours, measuring the oxygen content, cooling to 115 ℃ after the oxygen content is qualified, then introducing 60.1-64.2 parts of ethylene oxide and 240.3-246.7 parts of propylene oxide into the reaction kettle at a constant speed, controlling the pressure to be less than 0.4MPa, introducing all cyclic monomers into the reaction kettle, keeping the temperature of 120 ℃ for aging to negative pressure, cooling and discharging to obtain a polyether monomer;

step two: adding the prepared polyether monomer into a four-neck flask with a stirring rod, heating to 65 ℃ by adopting a water bath, preparing solution A from 1.7-3.9 parts of di-tert-butyl peroxide, 0.6-1.3 parts of thioglycolic acid and 60 parts of water, preparing solution B from 42.8-49.1 parts of acrylic acid, 0.5-1.4 parts of 3-allyloxy-1, 2-propylene glycol, 2.6-5.8 parts of sodium formaldehyde sulfoxylate and 120 parts of water, simultaneously dropwise adding A, B solution, dropwise adding the solution A for 2.5 hours, dropwise adding the solution B for 2 hours, preserving heat for 1 hour after the addition of the solution A is finished, and adding 7.2-9.3 parts of triethanolamine at one time and supplementing water until the total mass is 1000 parts to obtain the dispersion-maintenance polymer.

5. The high dispersibility ceramic water reducing agent according to claim 4, wherein: further the dispersion retaining polymer is prepared by the steps of:

the method comprises the following steps: adding 22.6 parts of 3-allyloxy-1, 2-propylene glycol and 1.2 parts of lithium aluminum hydride into a high-pressure reaction kettle provided with a stirrer and a thermometer, performing nitrogen replacement for 3 times, vacuumizing to gauge pressure of-0.085 MPa, heating to 120 ℃, dehydrating for 1-2 hours, measuring the oxygen content, cooling to 115 ℃ after the oxygen content is qualified, introducing 63.7 parts of ethylene oxide and 242.4 parts of propylene oxide into the reaction kettle at a constant speed, controlling the pressure to be less than 0.4MPa, introducing all cyclic monomers into the reaction kettle, keeping the temperature of 120 ℃ for aging to negative pressure, cooling and discharging to obtain a polyether monomer;

step two: adding the prepared polyether monomer into a four-neck flask with a stirring rod, heating to 65 ℃ by adopting a water bath, preparing solution A from 3.3 parts of di-tert-butyl peroxide, 0.9 part of thioglycolic acid and 60 parts of water, preparing solution B from 46.2 parts of acrylic acid, 0.8 part of 3-allyloxy-1, 2-propylene glycol, 4.3 parts of sodium formaldehyde sulfoxylate and 120 parts of water, dropwise adding A, B solution at the same time, dropwise adding the solution A for 2.5 hours, dropwise adding the solution B for 2 hours, preserving heat for 1 hour after the dropwise adding of the solution A is finished, and adding 8.3 parts of triethanolamine at one time and supplementing water until the total mass is 1000 parts to obtain the dispersion-retaining polymer.

6. The preparation method of the high-dispersibility ceramic water reducing agent as claimed in any one of claims 1 to 6, characterized by comprising the following steps: and (3) compounding 150-240 parts of dispersion type polymer and 210-290 parts of dispersion maintaining type polymer, and adding water to reach the total part of 1000 parts to obtain the required high-dispersibility ceramic water reducer solution.

Technical Field

The invention belongs to the technical field of high-dispersity ceramic water reducing agents, relates to a dispersion mechanism of the high-dispersity ceramic water reducing agent, and particularly relates to a high-dispersity ceramic water reducing agent and a preparation method thereof.

Background

The dispersing agent is a surfactant which can quickly wet the surface of solid particles and can increase the energy between solid particles to a high enough level, can effectively improve the particle wettability, suspension stability and slurry rheological property of a slurry sample under the condition of low moisture content, and enables the slurry to have proper viscosity so as to achieve the purposes of saving energy and reducing consumption. The excellent dispersing agent plays several roles of wetting, grinding aid, dilution and stabilization simultaneously in the preparation process of ceramic slurry, and plays an important role in improving the performance of ceramic products and reducing the manufacturing cost.

The patent application with the application number of 201711338641.8 discloses a high-dispersion dispersing agent for inorganic particles, which comprises the following raw materials in parts by weight: 5-20 parts of polyethylene diamine, 20-40 parts of acrylate, 2-10 parts of initiator, 2-10 parts of chain transfer agent and 45-100 parts of solvent. The invention provides a high-dispersion dispersing agent for inorganic particles, which can greatly improve the dispersion degree of solid particles in an inorganic particle dispersion system and improve the stability of the dispersion system.

The patent application with publication number CN111627699A discloses a manufacturing process of high-dispersity inner electrode paste for MLCC, and the invention discloses a manufacturing process of high-dispersity inner electrode paste for MLCC. Step three, stirring and mixing the metal paste prepared in the step one and the ceramic slurry prepared in the step two, and then carrying out high-pressure homogenization treatment by using a high-pressure nano fluid homogenizer; and step four, filtering the slurry prepared in the step three by using a filter press under positive pressure to obtain a slurry finished product. The manufacturing process is simple, the production cost is low, and no impurity is doped. The slurry prepared by the process has the characteristics of uniform dispersion of metal particles, good slurry flow R mobility, good storage stability and the like, and is beneficial to thinning of the thickness of the electrode layer.

The patent application with the publication number of CN1762816A discloses a preparation method of high-dispersity a-Al2O3 nano powder, and the invention provides a method for synthesizing a-Al203 nano powder. It uses intermediate product AI (OH)3 of alumina factory as raw material, adds phase-change additive, seed crystal and dispersing agent, grinds in high-purity alumina grinding medium, then carries on roasting, dispersing, processing and centrifugal separation, gets a-AI2O, nano powder with high dispersibility. The invention has the characteristics of cheap raw materials, low roasting temperature, simple method and low production cost. The obtained a-Al2O3 nano powder has high purity, and the content of Al2O3 is more than 99 percent; the product has controllable granularity and good dispersibility, the grain size of the powder is less than 40nm, and the secondary particle size is less than 200 nm. The a-Al2O3 nano powder prepared by the method has excellent performance and can be widely applied to fields of metallurgy, ceramics, electronics and the like. The invention can obviously reduce the preparation cost of the a-Al203 nano powder.

The ceramic water reducing agent provided by the above patents and the prior art has poor adsorption performance between water reducing agent molecules and ceramic particles, poor dispersibility of ceramic slurry caused by poor adsorption performance between the water reducing agent molecules and the ceramic particles, low action rate in actual use, large required mixing amount and high cost. Different from the patents, the invention prepares the high-dispersity ceramic water reducing agent. According to the invention, 2 polymers are compounded for use, so that the high-dispersity ceramic water reducing agent can improve the binding force among ceramic particles and reduce the surface tension among media when the ceramic dispersing performance is improved, and the effects of increasing the strength, increasing the dispersion and the like are achieved.

Disclosure of Invention

Aiming at the problems in the prior art, the invention discloses a high-dispersity porcelain water reducing agent. The indexes of the ceramic such as dispersibility, strength and the like are adjusted by compounding two polymers with different functions. The water reducing agent is added into the ceramic, so that the dispersion performance of the ceramic material is improved, the water consumption of the ceramic material is reduced, the strength of a ceramic blank is ensured, and the ceramic performance is enhanced.

The technical scheme adopted for solving the problems in the prior art is as follows:

the high-dispersity ceramic water reducing agent is characterized by comprising the following components: 150 portions of dispersion type polymer, 290 portions of dispersion keeping type polymer, 210 portions of dispersion keeping type polymer and the balance of water, and the total mass portion is 1000 portions.

The dispersion polymer is prepared by the following steps:

the method comprises the following steps: adding 30.7-33.9 parts of 4-methoxybut-2-en-1-ol and 0.6-1.2 parts of lithium aluminum hydride into a high-pressure reaction kettle provided with a stirrer and a thermometer, performing nitrogen replacement for 3 times, then starting vacuumizing to gauge pressure of-0.055 MPa, then heating to 120 ℃, starting dehydration for 0.5 hour, measuring the oxygen content, introducing 62.1-65.7 parts of ethylene oxide and 240.7-245.4 parts of propylene oxide into the reaction kettle at a constant speed after the oxygen content is qualified, controlling the pressure to be less than 0.5MPa, keeping the temperature of 120 ℃ after all the cyclic monomers are introduced into the reaction kettle, aging to negative pressure, cooling and discharging to obtain the polyether monomer.

Step two: adding the prepared polyether monomer into a four-neck flask with a stirring rod, and heating to 60 ℃ by adopting water bath. Preparing solution A from 1.8-4.1 parts of di-tert-butyl peroxide, 0.7-1.3 parts of thioglycolic acid and 60 parts of water, preparing solution B from 38.9-43.6 parts of diethyl acrylate, 3-5 parts of 4-methoxybut-2-en-1-ol, 3.7-6.3 parts of sodium formaldehyde sulfoxylate and 120 parts of water, and simultaneously dropwise adding A, B solution, wherein the solution A is dropwise added for 2.5 hours, and the solution B is dropwise added for 2 hours. And (3) after the liquid A is dripped, preserving the heat for 1 hour, adding 7.2-12.3 parts of triethanolamine at one time, and supplementing water until the total mass is 1000 parts, thus obtaining the dispersion type polymer.

Preferably the dispersed polymer is prepared by the steps of:

the method comprises the following steps: adding 31.6 parts of 4-methoxybut-2-en-1-ol and 1.2 parts of lithium aluminum hydride into a high-pressure reaction kettle provided with a stirrer and a thermometer, performing nitrogen replacement for 3 times, vacuumizing to gauge pressure of-0.055 MPa, heating to 120 ℃, dehydrating for 0.5 hour, measuring the oxygen content, introducing 63.7 parts of ethylene oxide and 242.4 parts of propylene oxide into the reaction kettle at constant speed after the oxygen content is qualified, controlling the pressure to be less than 0.5MPa, introducing all cyclic monomers into the reaction kettle, keeping the temperature of 120 ℃, aging to negative pressure, cooling and discharging to obtain the polyether monomer.

Step two: adding the prepared polyether monomer into a four-neck flask with a stirring rod, and heating to 60 ℃ by adopting water bath. 3.3 parts of di-tert-butyl peroxide, 0.9 part of thioglycolic acid and 60 parts of water are prepared into solution A, 40.2 parts of diethyl acrylate, 5 parts of 4-methoxybut-2-en-1-ol, 4.3 parts of sodium formaldehyde sulfoxylate and 120 parts of water are prepared into solution B, and A, B solution is simultaneously added dropwise, wherein the solution A is added dropwise for 2.5 hours, and the solution B is added dropwise for 2 hours. And (3) after the liquid A is dripped, preserving the heat for 1 hour, adding 12.3 parts of triethanolamine at one time and supplementing water until the total mass is 1000 parts, thus obtaining the dispersed polymer.

The dispersion retaining polymer is prepared by the steps of:

the method comprises the following steps: adding 20.3-25.7 parts of 3-allyloxy-1, 2-propylene glycol and 0.6-1.2 parts of lithium aluminum hydride into a high-pressure reaction kettle provided with a stirrer and a thermometer, performing nitrogen replacement for 3 times, vacuumizing to gauge pressure of-0.085 MPa, heating to 120 ℃, dehydrating for 1-2 hours, measuring the oxygen content, and cooling to 115 ℃ after the oxygen content is qualified. And then introducing a uniform mixture of 60.1-64.2 parts of ethylene oxide and 240.3-246.7 parts of propylene oxide into the reaction kettle at a constant speed, controlling the pressure to be less than 0.4MPa, keeping the temperature of 120 ℃ after all the cyclic monomers are introduced into the reaction kettle, aging to a negative pressure, cooling and discharging to obtain the polyether monomer.

Step two: adding the prepared polyether monomer into a four-neck flask with a stirring rod, and heating to 65 ℃ by adopting water bath. Preparing solution A from 1.7-3.9 parts of di-tert-butyl peroxide, 0.6-1.3 parts of thioglycolic acid and 60 parts of water, preparing solution B from 42.8-49.1 parts of acrylic acid, 0.5-1.4 parts of 3-allyloxy-1, 2-propylene glycol, 2.6-5.8 parts of sodium formaldehyde sulfoxylate and 120 parts of water, and simultaneously dropwise adding A, B solution, wherein the solution A is dropwise added for 2.5 hours, and the solution B is dropwise added for 2 hours. And (3) after the liquid A is dripped, preserving the heat for 1 hour, adding 7.2-9.3 parts of triethanolamine at one time, and supplementing water until the total mass is 1000 parts, thus obtaining the dispersion-retention polymer.

Preferably, the dispersion-retaining polymer is prepared by the steps of:

the method comprises the following steps: adding 22.6 parts of 3-allyloxy-1, 2-propylene glycol and 1.2 parts of lithium aluminum hydride into a high-pressure reaction kettle provided with a stirrer and a thermometer, performing nitrogen replacement for 3 times, vacuumizing to gauge pressure of-0.085 MPa, heating to 120 ℃, dehydrating for 1-2 hours, measuring the oxygen content, and cooling to 115 ℃ after the oxygen content is qualified. And then introducing 63.7 parts of ethylene oxide and 242.4 parts of propylene oxide into the reaction kettle at a constant speed, controlling the pressure to be less than 0.4MPa, introducing all the cyclic monomers into the reaction kettle, keeping the temperature of 120 ℃, aging to a negative pressure, cooling and discharging to obtain the polyether monomer.

Step two: adding the prepared polyether monomer into a four-neck flask with a stirring rod, and heating to 65 ℃ by adopting water bath. 3.3 parts of di-tert-butyl peroxide, 0.9 part of thioglycolic acid and 60 parts of water are prepared into solution A, 46.2 parts of acrylic acid, 0.8 part of 3-allyloxy-1, 2-propylene glycol, 4.3 parts of sodium formaldehyde sulfoxylate and 120 parts of water are prepared into solution B, and A, B solution is added dropwise, wherein the solution A is added dropwise for 2.5 hours, and the solution B is added dropwise for 2 hours. And (3) after the liquid A is dripped, preserving the heat for 1 hour, adding 8.3 parts of triethanolamine at one time and supplementing water until the total mass is 1000 parts, thus obtaining the dispersion-retention polymer.

The preparation method of the high-dispersity ceramic water reducing agent is characterized by comprising the following operation steps of: and (3) compounding 150-240 parts of dispersion type polymer and 210-290 parts of dispersion maintaining type polymer, and adding water to reach the total part of 1000 parts to obtain the required high-dispersibility ceramic water reducer solution.

The invention has the following advantages:

1. the dispersing agent is prepared by compounding a dispersion polymer and a dispersion maintaining polymer, and the preparation method is simple and is convenient for large-scale use.

2. The dispersion type polymer of the invention adopts styrenated phenol as a raw material, the styrenated phenol has 2 double bonds and can be crosslinked during polymerization, so that polymer molecules form a network structure, the steric hindrance effect is strong and the dispersion effect is good when the styrenated phenol is adsorbed on ceramic particles, and meanwhile, the polymer can fill gaps in the ceramic molecules, disperse stress and improve the toughness of a dispersing agent material, so that the polymer can also have a certain reinforcing effect when acting in the interior of ceramic.

3. The raw material of the dispersion-maintaining polymer used in the invention is ethylene oxide, the density of ether bonds on a long-chain branch chain of the dispersion-maintaining polymer is higher, the dispersion-maintaining polymer has good hydrophilicity and strong water retention capacity, and can provide good wettability in a ceramic filler.

Detailed Description

The technical scheme of the invention is further specifically described by the following embodiments.

Example 1

The high-dispersity ceramic water reducing agent and the preparation method thereof are characterized in that the preparation process comprises the following operation steps: and compounding 165 parts of dispersion type polymer and 255 parts of dispersion maintaining type polymer, and adding water to the total parts of 1000 to obtain the required high-dispersibility ceramic water reducer.

The dispersion polymer is prepared by the following steps:

the method comprises the following steps: adding 31.6 parts of 4-methoxybut-2-en-1-ol and 1.2 parts of lithium aluminum hydride into a high-pressure reaction kettle provided with a stirrer and a thermometer, performing nitrogen replacement for 3 times, vacuumizing to gauge pressure of-0.055 MPa, heating to 120 ℃, dehydrating for 0.5 hour, measuring the oxygen content, introducing 63.7 parts of ethylene oxide and 242.4 parts of propylene oxide into the reaction kettle at constant speed after the oxygen content is qualified, controlling the pressure to be less than 0.5MPa, introducing all cyclic monomers into the reaction kettle, keeping the temperature of 120 ℃, aging to negative pressure, cooling and discharging to obtain the polyether monomer.

Step two: adding the prepared polyether monomer into a four-neck flask with a stirring rod, and heating to 60 ℃ by adopting water bath. 3.3 parts of di-tert-butyl peroxide, 0.9 part of thioglycolic acid and 60 parts of water are prepared into solution A, 40.2 parts of diethyl acrylate, 5 parts of 4-methoxybut-2-en-1-ol, 4.3 parts of sodium formaldehyde sulfoxylate and 120 parts of water are prepared into solution B, and A, B solution is simultaneously added dropwise, wherein the solution A is added dropwise for 2.5 hours, and the solution B is added dropwise for 2 hours. And (3) after the liquid A is dripped, preserving the heat for 1 hour, adding 12.3 parts of triethanolamine at one time and supplementing water until the total mass is 1000 parts, thus obtaining the dispersed polymer.

The dispersion retaining polymer is prepared by the steps of:

the method comprises the following steps: 22.6 parts of 3-allyloxy-1, 2-propylene glycol and 1.2 parts of lithium aluminum hydride are added into a high-pressure reaction kettle provided with a stirrer and a thermometer, after 3 times of nitrogen replacement, vacuumizing is started to gauge pressure of-0.085 MPa, then the temperature is increased to 120 ℃, dehydration is started for 1h, the oxygen content is measured, and after the oxygen content is qualified, the temperature is reduced to 115 ℃. And then introducing 63.7 parts of ethylene oxide and 242.4 parts of propylene oxide into the reaction kettle at a constant speed, controlling the pressure to be less than 0.4MPa, introducing all the cyclic monomers into the reaction kettle, keeping the temperature of 120 ℃, aging to a negative pressure, cooling and discharging to obtain the polyether monomer.

Step two: adding the prepared polyether monomer into a four-neck flask with a stirring rod, and heating to 65 ℃ by adopting water bath. 3.3 parts of di-tert-butyl peroxide, 0.9 part of thioglycolic acid and 60 parts of water are prepared into solution A, 46.2 parts of acrylic acid, 0.8 part of 3-allyloxy-1, 2-propylene glycol, 4.3 parts of sodium formaldehyde sulfoxylate and 120 parts of water are prepared into solution B, and A, B solution is added dropwise, wherein the solution A is added dropwise for 2.5 hours, and the solution B is added dropwise for 2 hours. And (3) after the liquid A is dripped, preserving the heat for 1 hour, adding 8.3 parts of triethanolamine at one time and supplementing water until the total mass is 1000 parts, thus obtaining the dispersion-retention polymer.

Example 2

The high-dispersity ceramic water reducing agent and the preparation method thereof are characterized in that the preparation process comprises the following operation steps: 183 parts of dispersion type polymer and 257 parts of dispersion maintaining type polymer are compounded, and water is added until the total parts are 1000 parts, so that the required high-dispersibility ceramic water reducing agent is obtained.

The dispersion polymer is prepared by the following steps:

the method comprises the following steps: adding 31.6 parts of 4-methoxybut-2-en-1-ol and 1.2 parts of lithium aluminum hydride into a high-pressure reaction kettle provided with a stirrer and a thermometer, performing nitrogen replacement for 3 times, vacuumizing to gauge pressure of-0.055 MPa, heating to 120 ℃, dehydrating for 0.5 hour, measuring the oxygen content, introducing 63.7 parts of ethylene oxide and 242.4 parts of propylene oxide into the reaction kettle at constant speed after the oxygen content is qualified, controlling the pressure to be less than 0.5MPa, introducing all cyclic monomers into the reaction kettle, keeping the temperature of 120 ℃, aging to negative pressure, cooling and discharging to obtain the polyether monomer.

Step two: adding the prepared polyether monomer into a four-neck flask with a stirring rod, and heating to 60 ℃ by adopting water bath. 3.3 parts of di-tert-butyl peroxide, 0.9 part of thioglycolic acid and 60 parts of water are prepared into solution A, 40.2 parts of diethyl acrylate, 5 parts of 4-methoxybut-2-en-1-ol, 4.3 parts of sodium formaldehyde sulfoxylate and 120 parts of water are prepared into solution B, and A, B solution is simultaneously added dropwise, wherein the solution A is added dropwise for 2.5 hours, and the solution B is added dropwise for 2 hours. And (3) after the liquid A is dripped, preserving the heat for 1 hour, adding 12.3 parts of triethanolamine at one time and supplementing water until the total mass is 1000 parts, thus obtaining the dispersed polymer.

The dispersion retaining polymer is prepared by the steps of:

the method comprises the following steps: 22.6 parts of 3-allyloxy-1, 2-propylene glycol and 1.2 parts of lithium aluminum hydride are added into a high-pressure reaction kettle provided with a stirrer and a thermometer, after 3 times of nitrogen replacement, vacuumizing is started to gauge pressure of-0.085 MPa, then the temperature is increased to 120 ℃, dehydration is started for 1h, the oxygen content is measured, and after the oxygen content is qualified, the temperature is reduced to 115 ℃. And then introducing 63.7 parts of ethylene oxide and 242.4 parts of propylene oxide into the reaction kettle at a constant speed, controlling the pressure to be less than 0.4MPa, introducing all the cyclic monomers into the reaction kettle, keeping the temperature of 120 ℃, aging to a negative pressure, cooling and discharging to obtain the polyether monomer.

Step two: adding the prepared polyether monomer into a four-neck flask with a stirring rod, and heating to 65 ℃ by adopting water bath. 3.3 parts of di-tert-butyl peroxide, 0.9 part of thioglycolic acid and 60 parts of water are prepared into solution A, 46.2 parts of acrylic acid, 0.8 part of 3-allyloxy-1, 2-propylene glycol, 4.3 parts of sodium formaldehyde sulfoxylate and 120 parts of water are prepared into solution B, and A, B solution is added dropwise, wherein the solution A is added dropwise for 2.5 hours, and the solution B is added dropwise for 2 hours. And (3) after the liquid A is dripped, preserving the heat for 1 hour, adding 8.3 parts of triethanolamine at one time and supplementing water until the total mass is 1000 parts, thus obtaining the dispersion-retention polymer.

Example 3

The high-dispersity ceramic water reducing agent and the preparation method thereof are characterized in that the preparation process comprises the following operation steps: and compounding 194 parts of dispersion type polymer and 210 parts of dispersion maintaining type polymer, and adding water to the total parts of 1000 to obtain the required high-dispersibility ceramic water reducer.

The dispersion polymer is prepared by the following steps:

the method comprises the following steps: adding 31.6 parts of 4-methoxybut-2-en-1-ol and 1.2 parts of lithium aluminum hydride into a high-pressure reaction kettle provided with a stirrer and a thermometer, performing nitrogen replacement for 3 times, vacuumizing to gauge pressure of-0.055 MPa, heating to 120 ℃, dehydrating for 0.5 hour, measuring the oxygen content, introducing 63.7 parts of ethylene oxide and 242.4 parts of propylene oxide into the reaction kettle at constant speed after the oxygen content is qualified, controlling the pressure to be less than 0.5MPa, introducing all cyclic monomers into the reaction kettle, keeping the temperature of 120 ℃, aging to negative pressure, cooling and discharging to obtain the polyether monomer.

Step two: adding the prepared polyether monomer into a four-neck flask with a stirring rod, and heating to 60 ℃ by adopting water bath. 3.3 parts of di-tert-butyl peroxide, 0.9 part of thioglycolic acid and 60 parts of water are prepared into solution A, 40.2 parts of diethyl acrylate, 5 parts of 4-methoxybut-2-en-1-ol, 4.3 parts of sodium formaldehyde sulfoxylate and 120 parts of water are prepared into solution B, and A, B solution is simultaneously added dropwise, wherein the solution A is added dropwise for 2.5 hours, and the solution B is added dropwise for 2 hours. And (3) after the liquid A is dripped, preserving the heat for 1 hour, adding 12.3 parts of triethanolamine at one time and supplementing water until the total mass is 1000 parts, thus obtaining the dispersed polymer.

The dispersion retaining polymer is prepared by the steps of:

the method comprises the following steps: 22.6 parts of 3-allyloxy-1, 2-propylene glycol and 1.2 parts of lithium aluminum hydride are added into a high-pressure reaction kettle provided with a stirrer and a thermometer, after 3 times of nitrogen replacement, vacuumizing is started to gauge pressure of-0.085 MPa, then the temperature is increased to 120 ℃, dehydration is started for 1h, the oxygen content is measured, and after the oxygen content is qualified, the temperature is reduced to 115 ℃. And then introducing 63.7 parts of ethylene oxide and 242.4 parts of propylene oxide into the reaction kettle at a constant speed, controlling the pressure to be less than 0.4MPa, introducing all the cyclic monomers into the reaction kettle, keeping the temperature of 120 ℃, aging to a negative pressure, cooling and discharging to obtain the polyether monomer.

Step two: adding the prepared polyether monomer into a four-neck flask with a stirring rod, and heating to 65 ℃ by adopting water bath. 3.3 parts of di-tert-butyl peroxide, 0.9 part of thioglycolic acid and 60 parts of water are prepared into solution A, 46.2 parts of acrylic acid, 0.8 part of 3-allyloxy-1, 2-propylene glycol, 4.3 parts of sodium formaldehyde sulfoxylate and 120 parts of water are prepared into solution B, and A, B solution is added dropwise, wherein the solution A is added dropwise for 2.5 hours, and the solution B is added dropwise for 2 hours. And (3) after the liquid A is dripped, preserving the heat for 1 hour, adding 8.3 parts of triethanolamine at one time and supplementing water until the total mass is 1000 parts, thus obtaining the dispersion-retention polymer.

Example 4

The high-dispersity ceramic water reducing agent and the preparation method thereof are characterized in that the preparation process comprises the following operation steps: and (3) compounding 162 parts of a dispersion type polymer and 226 parts of a dispersion maintaining type polymer, and adding water until the total parts are 1000 parts to obtain the required high-dispersibility ceramic water reducing agent.

The dispersion polymer is prepared by the following steps:

the method comprises the following steps: adding 31.6 parts of 4-methoxybut-2-en-1-ol and 1.2 parts of lithium aluminum hydride into a high-pressure reaction kettle provided with a stirrer and a thermometer, performing nitrogen replacement for 3 times, vacuumizing to gauge pressure of-0.055 MPa, heating to 120 ℃, dehydrating for 0.5 hour, measuring the oxygen content, introducing 63.7 parts of ethylene oxide and 242.4 parts of propylene oxide into the reaction kettle at constant speed after the oxygen content is qualified, controlling the pressure to be less than 0.5MPa, introducing all cyclic monomers into the reaction kettle, keeping the temperature of 120 ℃, aging to negative pressure, cooling and discharging to obtain the polyether monomer.

Step two: adding the prepared polyether monomer into a four-neck flask with a stirring rod, and heating to 60 ℃ by adopting water bath. 3.3 parts of di-tert-butyl peroxide, 0.9 part of thioglycolic acid and 60 parts of water are prepared into solution A, 40.2 parts of diethyl acrylate, 5 parts of 4-methoxybut-2-en-1-ol, 4.3 parts of sodium formaldehyde sulfoxylate and 120 parts of water are prepared into solution B, and A, B solution is simultaneously added dropwise, wherein the solution A is added dropwise for 2.5 hours, and the solution B is added dropwise for 2 hours. And (3) after the liquid A is dripped, preserving the heat for 1 hour, adding 12.3 parts of triethanolamine at one time and supplementing water until the total mass is 1000 parts, thus obtaining the dispersed polymer.

The dispersion retaining polymer is prepared by the steps of:

the method comprises the following steps: 22.6 parts of 3-allyloxy-1, 2-propylene glycol and 1.2 parts of lithium aluminum hydride are added into a high-pressure reaction kettle provided with a stirrer and a thermometer, after 3 times of nitrogen replacement, vacuumizing is started to gauge pressure of-0.085 MPa, then the temperature is increased to 120 ℃, dehydration is started for 1h, the oxygen content is measured, and after the oxygen content is qualified, the temperature is reduced to 115 ℃. And then introducing 63.7 parts of ethylene oxide and 242.4 parts of propylene oxide into the reaction kettle at a constant speed, controlling the pressure to be less than 0.4MPa, introducing all the cyclic monomers into the reaction kettle, keeping the temperature of 120 ℃, aging to a negative pressure, cooling and discharging to obtain the polyether monomer.

Step two: adding the prepared polyether monomer into a four-neck flask with a stirring rod, and heating to 65 ℃ by adopting water bath. 3.3 parts of di-tert-butyl peroxide, 0.9 part of thioglycolic acid and 60 parts of water are prepared into solution A, 46.2 parts of acrylic acid, 0.8 part of 3-allyloxy-1, 2-propylene glycol, 4.3 parts of sodium formaldehyde sulfoxylate and 120 parts of water are prepared into solution B, and A, B solution is added dropwise, wherein the solution A is added dropwise for 2.5 hours, and the solution B is added dropwise for 2 hours. And (3) after the liquid A is dripped, preserving the heat for 1 hour, adding 8.3 parts of triethanolamine at one time and supplementing water until the total mass is 1000 parts, thus obtaining the dispersion-retention polymer.

Example 5

The high-dispersity ceramic water reducing agent and the preparation method thereof are characterized in that the preparation process comprises the following operation steps: 177 parts of dispersion type polymer and 233 parts of dispersion maintaining type polymer are compounded, and water is added until the total parts is 1000 parts, so that the required high-dispersibility ceramic water reducing agent is obtained.

The dispersion polymer is prepared by the following steps:

the method comprises the following steps: adding 31.6 parts of 4-methoxybut-2-en-1-ol and 1.2 parts of lithium aluminum hydride into a high-pressure reaction kettle provided with a stirrer and a thermometer, performing nitrogen replacement for 3 times, vacuumizing to gauge pressure of-0.055 MPa, heating to 120 ℃, dehydrating for 0.5 hour, measuring the oxygen content, introducing 63.7 parts of ethylene oxide and 242.4 parts of propylene oxide into the reaction kettle at constant speed after the oxygen content is qualified, controlling the pressure to be less than 0.5MPa, introducing all cyclic monomers into the reaction kettle, keeping the temperature of 120 ℃, aging to negative pressure, cooling and discharging to obtain the polyether monomer.

Step two: adding the prepared polyether monomer into a four-neck flask with a stirring rod, and heating to 60 ℃ by adopting water bath. 3.3 parts of di-tert-butyl peroxide, 0.9 part of thioglycolic acid and 60 parts of water are prepared into solution A, 40.2 parts of diethyl acrylate, 5 parts of 4-methoxybut-2-en-1-ol, 4.3 parts of sodium formaldehyde sulfoxylate and 120 parts of water are prepared into solution B, and A, B solution is simultaneously added dropwise, wherein the solution A is added dropwise for 2.5 hours, and the solution B is added dropwise for 2 hours. And (3) after the liquid A is dripped, preserving the heat for 1 hour, adding 12.3 parts of triethanolamine at one time and supplementing water until the total mass is 1000 parts, thus obtaining the dispersed polymer.

The dispersion retaining polymer is prepared by the steps of:

the method comprises the following steps: 22.6 parts of 3-allyloxy-1, 2-propylene glycol and 1.2 parts of lithium aluminum hydride are added into a high-pressure reaction kettle provided with a stirrer and a thermometer, after 3 times of nitrogen replacement, vacuumizing is started to gauge pressure of-0.085 MPa, then the temperature is increased to 120 ℃, dehydration is started for 1h, the oxygen content is measured, and after the oxygen content is qualified, the temperature is reduced to 115 ℃. And then introducing 63.7 parts of ethylene oxide and 242.4 parts of propylene oxide into the reaction kettle at a constant speed, controlling the pressure to be less than 0.4MPa, introducing all the cyclic monomers into the reaction kettle, keeping the temperature of 120 ℃, aging to a negative pressure, cooling and discharging to obtain the polyether monomer.

Step two: adding the prepared polyether monomer into a four-neck flask with a stirring rod, and heating to 65 ℃ by adopting water bath. 3.3 parts of di-tert-butyl peroxide, 0.9 part of thioglycolic acid and 60 parts of water are prepared into solution A, 46.2 parts of acrylic acid, 0.8 part of 3-allyloxy-1, 2-propylene glycol, 4.3 parts of sodium formaldehyde sulfoxylate and 120 parts of water are prepared into solution B, and A, B solution is added dropwise, wherein the solution A is added dropwise for 2.5 hours, and the solution B is added dropwise for 2 hours. And (3) after the liquid A is dripped, preserving the heat for 1 hour, adding 8.3 parts of triethanolamine at one time and supplementing water until the total mass is 1000 parts, thus obtaining the dispersion-retention polymer.

Example 6

The high-dispersity ceramic water reducing agent and the preparation method thereof are characterized in that the preparation process comprises the following operation steps: and compounding 159 parts of dispersion type polymer and 272 parts of dispersion maintaining type polymer, and adding water to the total parts of 1000 parts to obtain the required high-dispersibility ceramic water reducer.

The dispersion polymer is prepared by the following steps:

the method comprises the following steps: adding 31.6 parts of 4-methoxybut-2-en-1-ol and 1.2 parts of lithium aluminum hydride into a high-pressure reaction kettle provided with a stirrer and a thermometer, performing nitrogen replacement for 3 times, vacuumizing to gauge pressure of-0.055 MPa, heating to 120 ℃, dehydrating for 0.5 hour, measuring the oxygen content, introducing 63.7 parts of ethylene oxide and 242.4 parts of propylene oxide into the reaction kettle at constant speed after the oxygen content is qualified, controlling the pressure to be less than 0.5MPa, introducing all cyclic monomers into the reaction kettle, keeping the temperature of 120 ℃, aging to negative pressure, cooling and discharging to obtain the polyether monomer.

Step two: adding the prepared polyether monomer into a four-neck flask with a stirring rod, and heating to 60 ℃ by adopting water bath. 3.3 parts of di-tert-butyl peroxide, 0.9 part of thioglycolic acid and 60 parts of water are prepared into solution A, 40.2 parts of diethyl acrylate, 5 parts of 4-methoxybut-2-en-1-ol, 4.3 parts of sodium formaldehyde sulfoxylate and 120 parts of water are prepared into solution B, and A, B solution is simultaneously added dropwise, wherein the solution A is added dropwise for 2.5 hours, and the solution B is added dropwise for 2 hours. And (3) after the liquid A is dripped, preserving the heat for 1 hour, adding 12.3 parts of triethanolamine at one time and supplementing water until the total mass is 1000 parts, thus obtaining the dispersed polymer.

The dispersion retaining polymer is prepared by the steps of:

the method comprises the following steps: 22.6 parts of 3-allyloxy-1, 2-propylene glycol and 1.2 parts of lithium aluminum hydride are added into a high-pressure reaction kettle provided with a stirrer and a thermometer, after 3 times of nitrogen replacement, vacuumizing is started to gauge pressure of-0.085 MPa, then the temperature is increased to 120 ℃, dehydration is started for 1h, the oxygen content is measured, and after the oxygen content is qualified, the temperature is reduced to 115 ℃. And then introducing 63.7 parts of ethylene oxide and 242.4 parts of propylene oxide into the reaction kettle at a constant speed, controlling the pressure to be less than 0.4MPa, introducing all the cyclic monomers into the reaction kettle, keeping the temperature of 120 ℃, aging to a negative pressure, cooling and discharging to obtain the polyether monomer.

Step two: adding the prepared polyether monomer into a four-neck flask with a stirring rod, and heating to 65 ℃ by adopting water bath. 3.3 parts of di-tert-butyl peroxide, 0.9 part of thioglycolic acid and 60 parts of water are prepared into solution A, 46.2 parts of acrylic acid, 0.8 part of 3-allyloxy-1, 2-propylene glycol, 4.3 parts of sodium formaldehyde sulfoxylate and 120 parts of water are prepared into solution B, and A, B solution is added dropwise, wherein the solution A is added dropwise for 2.5 hours, and the solution B is added dropwise for 2 hours. And (3) after the liquid A is dripped, preserving the heat for 1 hour, adding 8.3 parts of triethanolamine at one time and supplementing water until the total mass is 1000 parts, thus obtaining the dispersion-retention polymer.

TABLE 1 compositional parameters of inventive examples 1-6

Ceramic slurry samples prepared from examples 1 to 6 of the present invention and a hoisin frezf 414 ceramic water reducing agent were tested for their properties to obtain the following table (viscosity was measured using a rotational viscometer, and zeta potential of ceramic slurry was measured using a BLD-B type surface potential particle size analyzer):

TABLE 2

As can be seen from the above table, the ceramic water reducing agents of the embodiments 1 to 6 of the present invention can well disperse ceramic slurry particles, reduce system viscosity, ensure that the ceramic slurry has a higher zeta potential, and maintain slurry stability.

The protective scope of the present invention is not limited to the above-described embodiments, and it is apparent that various modifications and variations can be made to the present invention by those skilled in the art without departing from the scope and spirit of the present invention. It is intended that the present invention cover the modifications and variations of this invention provided they come within the scope of the appended claims and their equivalents.