CN111018387B - Reinforced and toughened polycarboxylic acid water reducer, preparation method and preparation device - Google Patents

Reinforced and toughened polycarboxylic acid water reducer, preparation method and preparation device Download PDF

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CN111018387B
CN111018387B CN201911381051.2A CN201911381051A CN111018387B CN 111018387 B CN111018387 B CN 111018387B CN 201911381051 A CN201911381051 A CN 201911381051A CN 111018387 B CN111018387 B CN 111018387B
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preparation
polycarboxylic acid
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acid water
water reducer
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CN111018387A (en
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卢伟雄
肖山虎
蔡健
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Guangdong Jiansheng High Tech Materials Co ltd
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Guangdong Jiansheng High Tech Materials Co ltd
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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
    • C04B18/00—Use of agglomerated or waste materials or refuse as fillers for mortars, concrete or artificial stone; Treatment of agglomerated or waste materials or refuse, specially adapted to enhance their filling properties in mortars, concrete or artificial stone
    • C04B18/02—Agglomerated materials, e.g. artificial aggregates
    • C04B18/023—Fired or melted materials
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/0053—Details of the reactor
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J4/00—Feed or outlet devices; Feed or outlet control devices
    • B01J4/02—Feed or outlet devices; Feed or outlet control devices for feeding measured, i.e. prescribed quantities of reagents
    • 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
    • C04B40/0046—Premixtures of ingredients characterised by their processing, e.g. sequence of mixing the ingredients when preparing the premixtures
    • 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

Abstract

The invention discloses a reinforced and toughened polycarboxylic acid water reducer, a preparation method and a preparation device, belonging to the technical field of preparation of polycarboxylic acid water reducers, wherein an initiator solution and heat storage porcelain powder are simultaneously added into a polymerization monomer solution at an even speed, so that the initiator solution and the heat storage porcelain powder are kept for the same adding time, the reaction time is saved, all the substances are mixed more fully and uniformly, and the preparation efficiency of the polycarboxylic acid water reducer is improved; when the external temperature rises, the heat storage porcelain powder can absorb a large amount of heat, so that molecular chains in the polycarboxylic acid water reducer cannot absorb enough heat to be decomposed and broken, the original molecular performance is kept, the thermal stability is improved, and the slump retaining performance of the polycarboxylic acid water reducer at high temperature is obviously improved; meanwhile, due to the extremely low water absorption of the heat storage porcelain powder, the HLB (water-oil-degree) value is reduced, the possibility of forming combined water by cement particles and water is reduced, more free water is released, and the viscosity of cement paste is reduced.

Description

Reinforced and toughened polycarboxylic acid water reducer, preparation method and preparation device
Technical Field
The invention relates to the technical field of preparation of polycarboxylic acid water reducing agents, and particularly relates to a reinforced and toughened polycarboxylic acid water reducing agent, a preparation method and a preparation device.
Background
In recent years, the infrastructure of China, such as high-speed rail, highway, airport, dam, municipal engineering and the like, keeps increasing at a high speed, and simultaneously promotes the rapid development of the concrete admixture technology. The development of concrete admixtures can be roughly divided into the following stages: the first stage is a starting stage, and takes common water reducing agent lignin as a representative; in the second stage, a development stage represented by a naphthalene-based high-efficiency water reducing agent emerges various water reducing agents such as melamine, sulfamate-based water reducing agents and aliphatic water reducing agents; the third stage, which is the current stage, is a stage in the high-tech field of concrete admixtures, and takes the polycarboxylic acid high-performance water reducing agent as a main representative.
Compared with other water reducing agents, the polycarboxylic acid water reducing agent has the characteristics of low mixing amount, high water reducing rate, low alkali content, high strength increase, low slump loss, environmental friendliness and the like. Meanwhile, the problems of shortage of naphthalene resources, continuous rising of industrial naphthalene price, long production period of the naphthalene water reducing agent, environmental pollution and the like are increasingly prominent, and the application of the polycarboxylic acid water reducing agent is imperative. It will replace naphthalene series water reducing agent and become the mainstream product.
The main chain of the polycarboxylate water reducing agent molecule is firmly adsorbed on the surface of cement particles, the hydration reaction can be effectively hindered, the plasticity retention property of the polycarboxylate water reducing agent molecule can be improved, the branched chain surrounds the cement particles, and the polycarboxylate water reducing agent has double effects of steric hindrance and electrostatic repulsion, which is completely different from the traditional water reducing agent in the mechanism of dispersing the cement particles through electrostatic repulsion, so that the polycarboxylate water reducing agent has better dispersing capacity and water reducing effect.
However, the existing polycarboxylic acid water reducing agent has strong temperature sensitivity, when the temperature rises, macromolecular chains in the product can move rapidly, chain decomposition and random fracture are easy to occur, the degradation speed of a polymer is accelerated, and the quality of the water reducing agent product is deteriorated, so that the polycarboxylic acid water reducing agent has poor working performance and insufficient slump retention at high temperature.
Disclosure of Invention
1. The technical problem to be solved.
Aiming at the problems in the prior art, the invention aims to provide a reinforced and toughened polycarboxylic acid water reducer, a preparation method and a preparation device, which simultaneously add an initiator solution and heat storage porcelain powder into a polymerization monomer solution at a uniform speed, so that the initiator solution and the heat storage porcelain powder are kept for the same adding time, the reaction time is saved, all the substances are fully and uniformly mixed, and the preparation efficiency of the polycarboxylic acid water reducer is remarkably improved; the heat storage porcelain powder has stable physical and chemical properties, and when the external temperature rises, the added heat storage porcelain powder can absorb a large amount of heat, so that molecular chains in the polycarboxylic acid water reducing agent cannot absorb enough heat to be decomposed and broken, and the original molecular performance of the polycarboxylic acid water reducing agent is maintained, so that the prepared polycarboxylic acid water reducing agent has good thermal stability, and the slump retaining performance of the polycarboxylic acid water reducing agent at high temperature is obviously improved; meanwhile, due to the extremely low water absorption of the heat storage porcelain powder, the HLB (water-oil-degree) value is reduced, the possibility of forming combined water by cement particles and water is reduced when the heat storage porcelain powder is used, and more free water is released, so that the viscosity of cement slurry is reduced, and the slurry can be pumped for a long distance and is convenient to construct.
2. Technical scheme
In order to solve the above problems, the present invention adopts the following technical solutions.
A preparation method of a reinforced and toughened polycarboxylic acid water reducer comprises the following steps:
firstly, weighing 20-30 parts of methacrylic acid, 15-25 parts of acrylic acid, 10-15 parts of ethyl acrylate, 10-15 parts of hydroxyethyl acrylate, 10-15 parts of sodium allylsulfonate, 8-12 parts of methyl methacrylate, 5-10 parts of allyl polyoxyethylene ether, 0.5-1 part of initiator, 3-5 parts of thermal storage ceramic powder and 1-3 parts of molecular weight regulator according to parts by weight;
the second step is that: mixing methacrylic acid, acrylic acid, ethyl acrylate, hydroxyethyl acrylate, sodium allylsulfonate, methyl methacrylate, allyl polyoxyethylene ether, a molecular weight regulator and deionized water to prepare a polymerized monomer solution with the content of 50-60% by mass;
the third step: mixing an initiator and water to prepare an initiator solution with the content of 10-20% by mass;
the fourth step: putting the polymerization monomer solution into a reaction kettle, wherein the reaction temperature is 80-100 ℃, adding the initiator solution into the polymerization monomer solution at a constant speed in a dropwise adding mode, and simultaneously adding the heat storage ceramic powder into the polymerization monomer solution at a constant speed, wherein the reaction time is 3-4 hours; then cooling to 40-50 ℃, adding an alkaline solution to adjust the pH value to 6.5-7.5, and obtaining the final polycarboxylic acid water reducing agent.
According to the invention, the initiator solution and the heat storage ceramic powder are simultaneously added into the polymerization monomer solution at a uniform speed, so that the initiator solution and the heat storage ceramic powder are kept for the same adding time, the reaction time is saved, the substances can be mixed more fully and uniformly, and the preparation efficiency of the polycarboxylic acid water reducer is obviously improved; the heat storage porcelain powder has stable physical and chemical properties, and when the external temperature rises, the added heat storage porcelain powder can absorb a large amount of heat, so that molecular chains in the polycarboxylic acid water reducing agent cannot absorb enough heat to be decomposed and broken, and the original molecular performance of the polycarboxylic acid water reducing agent is maintained, so that the prepared polycarboxylic acid water reducing agent has good thermal stability, and the slump retaining performance of the polycarboxylic acid water reducing agent at high temperature is obviously improved; meanwhile, due to the extremely low water absorption of the heat storage porcelain powder, the HLB (water-oil-degree) value is reduced, the possibility of forming combined water by cement particles and water is reduced when the heat storage porcelain powder is used, and more free water is released, so that the viscosity of cement slurry is reduced, and the slurry can be pumped for a long distance and is convenient to construct.
The utility model provides a preparation facilities of reinforcing and toughening type polycarboxylate water reducing agent, reation kettle includes the reation kettle main part, the upper end fixedly connected with measurement section of thick bamboo of reation kettle main part at preparation polycarboxylate water reducing agent in-process, the reation kettle main part is used for placing polymerization monomer solution, and the measurement section of thick bamboo is arranged in adding initiator solution and heat accumulation porcelain powder at the uniform velocity in the reation kettle main part.
Further, the metering cylinder comprises a cylinder shell, a partition board is fixedly connected to the inner wall of the cylinder shell, the inside of the cylinder shell is divided into a powder groove and a liquid groove through the partition board, when initiator solution and heat storage porcelain powder are added, the initiator solution is placed in the liquid groove, the heat storage porcelain powder is placed in the powder groove, and the initiator solution and the heat storage porcelain powder can be added separately at the same time.
Further, the lower extreme fixedly connected with main siphunculus and the vice siphunculus of barrel shell, main siphunculus communicates with each other with the liquid tank, vice siphunculus communicates with each other with the powder groove, equal fixedly connected with velocity of flow governing valve on main siphunculus and the vice siphunculus lets in the reation kettle main part respectively with initiator solution and heat accumulation porcelain powder through main siphunculus and vice siphunculus, controls the velocity of flow between them through velocity of flow governing valve, makes the interpolation time between them keep unanimous in the at utmost, still can make each material mix ground more fully even when practicing thrift reaction time.
Furthermore, the outer end of the cylinder shell is carved with capacity scales, and the addition amounts of the initiator solution and the heat storage porcelain powder can be strictly controlled.
Further, the shell of the cylinder body is made of transparent acrylic materials, so that the adding conditions of the initiator solution and the heat storage porcelain powder are conveniently observed, and the initiator solution and the heat storage porcelain powder are kept for the same adding time to the maximum extent.
Furthermore, the main through pipe is in a circular pipe shape, and the auxiliary through pipe is in a funnel shape, so that the initiator solution and the heat storage porcelain powder can flow conveniently in different state substances.
The heat storage porcelain powder comprises aluminum oxide, silicon oxide, calcium oxide, magnesium oxide, kaolin, mullite crystals, titanium dioxide and silicon dioxide.
Further, the preparation method of the heat storage ceramic powder comprises the following steps:
s1, weighing 12-16 parts of alumina, 3-5 parts of silicon oxide, 0.2-0.5 part of calcium oxide, 0.2-0.5 part of magnesium oxide, 1-3 parts of kaolin, 1-2 parts of mullite crystal, 2-3 parts of titanium dioxide and 0.5-1 part of silicon dioxide according to parts by weight, and placing the materials into a ball mill for ball milling for 4-6 hours with the ball milling granularity of 0.6-0.8mm to obtain a first mixture;
s2, placing the mixture I in a sodium hydroxide solution with the concentration of 0.5-1mol/L, reacting for 1-2h, and performing primary drying; spray drying the primarily dried material at an inlet temperature of 130-150 ℃ and an outlet temperature of 70-100 ℃ to obtain a mixture II;
s3, placing the mixture II into a vacuum sintering furnace for sintering, wherein the sintering temperature is 1200-1500 ℃, and the sintering time is 8-12 h; then the temperature is reduced to 100-300 ℃, the temperature is kept for 1-3h, and the heat storage ceramic powder is obtained after natural cooling to the normal temperature.
The silicon oxide, the calcium oxide and the silicon dioxide have strong dissolving power to the aluminum oxide at proper high temperature, and a certain amount of aluminosilicate melt can be formed, so that sintering is promoted; the titanium dioxide can be used as a mineralizer, and the main functions of the mineralizer are solid melting with alumina, grain activation and sintering promotion; the added kaolin can improve the plasticity of the materials and is beneficial to the dissolution and sintering of alumina; the mullite crystal has the function of improving the hydrogen fluoride acid erosion resistance of the prepared heat storage ceramic powder and is also beneficial to reducing the firing temperature.
The prepared heat storage ceramic powder has high temperature resistance, corrosion resistance and large heat capacity, has good thermal stability at high temperature, and is not easy to generate physical and chemical deformation or quality change.
Further, the initiator is one or a mixture of ammonium persulfate, potassium persulfate and benzoyl peroxide.
3. Advantageous effects
Compared with the prior art, the invention has the advantages that:
(1) according to the scheme, the initiator solution and the heat storage ceramic powder are simultaneously added into the polymerization monomer solution at a uniform speed, so that the initiator solution and the heat storage ceramic powder are kept for the same adding time, the reaction time is saved, the substances can be mixed more fully and uniformly, and the preparation efficiency of the polycarboxylic acid water reducer is remarkably improved; the heat storage porcelain powder has stable physical and chemical properties, and when the external temperature rises, the added heat storage porcelain powder can absorb a large amount of heat, so that molecular chains in the polycarboxylic acid water reducing agent cannot absorb enough heat to be decomposed and broken, and the original molecular performance of the polycarboxylic acid water reducing agent is maintained, so that the prepared polycarboxylic acid water reducing agent has good thermal stability, and the slump retaining performance of the polycarboxylic acid water reducing agent at high temperature is obviously improved; meanwhile, due to the extremely low water absorption of the heat storage porcelain powder, the HLB (water-oil-degree) value is reduced, the possibility of forming combined water by cement particles and water is reduced when the heat storage porcelain powder is used, and more free water is released, so that the viscosity of cement slurry is reduced, and the slurry can be pumped for a long distance and is convenient to construct.
(2) The reaction kettle comprises a reaction kettle main body, wherein a metering cylinder is fixedly connected to the upper end of the reaction kettle main body, the reaction kettle main body is used for placing a polymerization monomer solution in the process of preparing the polycarboxylic acid water reducing agent, and the metering cylinder is used for adding an initiator solution and heat storage ceramic powder into the reaction kettle main body at a constant speed.
(3) The metering cylinder comprises a cylinder shell, a partition board is fixedly connected to the inner wall of the cylinder shell, the inside of the cylinder shell is divided into a powder groove and a liquid groove through the partition board, when initiator solution and heat storage porcelain powder are added, the initiator solution is placed in the liquid groove, the heat storage porcelain powder is placed in the powder groove, and the initiator solution and the heat storage porcelain powder can be separately added simultaneously.
(4) The lower extreme fixedly connected with main siphunculus and the vice siphunculus of barrel shell, main siphunculus communicates with each other with the liquid tank, vice siphunculus communicates with each other with the powder groove, equal fixedly connected with velocity of flow governing valve on main siphunculus and the vice siphunculus, let initiator solution and heat accumulation porcelain powder respectively in the reation kettle main part through main siphunculus and vice siphunculus, flow rate between them is controlled through the velocity of flow governing valve, make the interpolation time between them keep unanimous to the utmost, still can make each material mix ground more fully even when practicing thrift reaction time.
(5) The outer end of the cylinder shell is carved with capacity scales, and the addition amounts of the initiator solution and the heat storage porcelain powder can be strictly controlled.
(6) The shell of the cylinder body is made of transparent acrylic materials, so that the adding conditions of the initiator solution and the heat storage porcelain powder are conveniently observed, and the initiator solution and the heat storage porcelain powder are kept for the same adding time to the maximum extent.
(7) The main through pipe is in a circular pipe shape, the auxiliary through pipe is in a funnel shape, and the flow of substances in different states of an initiator solution and heat storage ceramic powder is facilitated.
(8) The heat storage ceramic powder comprises alumina, silicon oxide, calcium oxide, magnesium oxide, kaolin, mullite crystals, titanium dioxide and silicon dioxide, and the silicon oxide, the calcium oxide and the silicon dioxide have strong dissolving power to the alumina at proper high temperature and can form a certain amount of aluminosilicate melt, so that sintering is promoted; the titanium dioxide can be used as a mineralizer, and the main function of the titanium dioxide is to be in solid fusion with alumina, activate grains and promote sintering; the added kaolin can improve the plasticity of the materials and is beneficial to the dissolution and sintering of alumina; the mullite crystal has the functions of improving the hydrogen fluoride acid erosion resistance of the prepared heat storage ceramic powder and also is beneficial to reducing the firing temperature; the prepared heat storage ceramic powder has high temperature resistance, corrosion resistance and large heat capacity, has good thermal stability at high temperature, and is not easy to generate physical and chemical deformation or quality change.
Drawings
FIG. 1 is a flow chart of the preparation of the present invention;
FIG. 2 is a front perspective view of a reaction vessel of the present invention;
FIG. 3 is a side perspective view of a reactor of the present invention;
FIG. 4 is a perspective view of a metering drum of the present invention;
FIG. 5 is a schematic front view of a metering drum of the present invention;
FIG. 6 is a flow chart of the preparation of the heat-accumulating porcelain powder of the present invention.
The reference numbers in the figures illustrate:
1 reaction kettle main body, 2 metering cylinders, 21 cylinder shell, 22 partition plates, 23 powder grooves, 24 liquid grooves, 25 main through pipes, 26 auxiliary through pipes, 27 flow rate regulating valves and 28 volume scales.
Detailed Description
The drawings in the embodiments of the invention will be combined; the technical scheme in the embodiment of the invention is clearly and completely described; obviously; the described embodiments are only some of the embodiments of the invention; but not all embodiments, are based on the embodiments of the invention; all other embodiments obtained by a person skilled in the art without making any inventive step; all fall within the scope of protection of the present invention.
In the description of the present invention, it should be noted that the terms "upper", "lower", "inner", "outer", "top/bottom", and the like indicate orientations or positional relationships based on those shown in the drawings, and are only for convenience of description and simplification of description, but do not indicate or imply that the referred device or element must have a specific orientation, be constructed in a specific orientation, and be operated, and thus should not be construed as limiting the present invention. Furthermore, the terms "first" and "second" are used for descriptive purposes only and are not to be construed as indicating or implying relative importance.
In the description of the present invention, it should be noted that, unless otherwise explicitly specified or limited, the terms "mounted," "disposed," "sleeved/connected," "connected," and the like are to be construed broadly, e.g., "connected," which may be fixedly connected, detachably connected, or integrally connected; can be mechanically or electrically connected; they may be connected directly or indirectly through intervening media, or they may be interconnected between two elements. The specific meanings of the above terms in the present invention can be understood in specific cases to those skilled in the art.
Example (b):
referring to fig. 1, a method for preparing a reinforced and toughened polycarboxylic acid water reducer includes the following steps:
weighing 20 parts of methacrylic acid, 15 parts of acrylic acid, 10 parts of ethyl acrylate, 10 parts of hydroxyethyl acrylate, 10 parts of sodium allylsulfonate, 8 parts of methyl methacrylate, 5 parts of allyl polyoxyethylene ether, 0.5 part of initiator, 3 parts of thermal storage ceramic powder and 1 part of molecular weight regulator according to parts by weight;
the second step is that: mixing methacrylic acid, acrylic acid, ethyl acrylate, hydroxyethyl acrylate, sodium allylsulfonate, methyl methacrylate, allyl polyoxyethylene ether, a molecular weight regulator and deionized water to prepare a polymeric monomer solution with the content of 50% by mass;
the third step: mixing an initiator and water to prepare an initiator solution with the content of 10% by mass;
the initiator is one or a mixture of ammonium persulfate, potassium persulfate or benzoyl peroxide.
The fourth step: putting the polymerization monomer solution into a reaction kettle, wherein the reaction temperature is 80 ℃, adding the initiator solution into the polymerization monomer solution at a constant speed in a dropwise adding mode, and simultaneously adding the heat storage porcelain powder into the polymerization monomer solution at a constant speed, wherein the reaction time is 3 hours; then cooling to 40 ℃, adding an alkaline solution to adjust the pH value to 6.5, and obtaining the final polycarboxylic acid water reducing agent.
Referring to fig. 2 and fig. 3, a preparation apparatus of a reinforced and toughened polycarboxylic acid water reducing agent, a reaction kettle includes a reaction kettle main body 1, an upper end of the reaction kettle main body 1 is fixedly connected with a metering cylinder 2, in the process of preparing the polycarboxylic acid water reducing agent, the reaction kettle main body 1 is used for placing a polymerization monomer solution, and the metering cylinder 2 is used for adding an initiator solution and heat storage ceramic powder into the reaction kettle main body 1 at a constant speed.
Referring to fig. 4, the measuring cylinder 2 includes a cylinder housing 21, a partition 22 is fixedly connected to an inner wall of the cylinder housing 21, the interior of the cylinder housing 21 is divided into a powder tank 23 and a liquid tank 24 by the partition 22, when adding the initiator solution and the heat-storage ceramic powder, the initiator solution is placed in the liquid tank 24, and the heat-storage ceramic powder is placed in the powder tank 23, so that the initiator solution and the heat-storage ceramic powder can be added separately at the same time.
Referring to fig. 4, a main pipe 25 and an auxiliary pipe 26 are fixedly connected to the lower end of the cylinder housing 21, the main pipe 25 is communicated with the liquid tank 24, the auxiliary pipe 26 is communicated with the powder tank 23, flow rate regulating valves 27 are fixedly connected to the main pipe 25 and the auxiliary pipe 26, the initiator solution and the heat storage porcelain powder are respectively introduced into the reaction kettle main body 1 through the main pipe 25 and the auxiliary pipe 26, the flow rates of the initiator solution and the heat storage porcelain powder are controlled by the flow rate regulating valves 27, the adding time of the initiator solution and the heat storage porcelain powder is kept consistent to the greatest extent, and the reaction time is saved while the substances are mixed more fully and uniformly.
Referring to fig. 4, the outer end of the cylinder housing 21 is engraved with volume scales 28, which can strictly control the addition amounts of the initiator solution and the thermal storage ceramic powder, and the cylinder housing 21 is made of a transparent acrylic material, so that the addition conditions of the initiator solution and the thermal storage ceramic powder can be conveniently observed, and the same addition time can be maintained for the initiator solution and the thermal storage ceramic powder to the greatest extent.
Referring to fig. 5, the main pipe 25 is in the shape of a circular pipe, and the sub-pipe 26 is in the shape of a funnel, so that the initiator solution and the heat-accumulating porcelain powder can flow in different states.
Referring to fig. 6, the heat-accumulating porcelain powder includes alumina, silica, calcium oxide, magnesium oxide, kaolin, mullite crystal, titanium dioxide and silica.
The preparation method of the heat storage porcelain powder comprises the following steps:
s1, weighing 12 parts of alumina, 3 parts of silicon oxide, 0.2 part of calcium oxide, 0.2 part of magnesium oxide, 1 part of kaolin, 1 part of mullite crystal, 2 parts of titanium dioxide and 0.5 part of silicon dioxide according to parts by weight, and placing the materials in a ball mill for ball milling, wherein the ball milling time is 4 hours, and the ball milling granularity is 0.6mm to obtain a first mixture;
s2, placing the first mixture in a sodium hydroxide solution with the concentration of 0.5mol/L, reacting for 1 hour, and then primarily drying; spray drying the primarily dried material at an inlet temperature of 130 ℃ and an outlet temperature of 70 ℃ to obtain a mixture II;
s3, placing the mixture II into a vacuum sintering furnace for sintering, wherein the sintering temperature is 1200 ℃, and the sintering time is 8 hours; then reducing the temperature to 100 ℃, preserving the heat for 1h, and naturally cooling to the normal temperature to obtain the heat storage ceramic powder.
The silicon oxide, the calcium oxide and the silicon dioxide have strong dissolving power to the aluminum oxide at proper high temperature, and a certain amount of aluminosilicate melt can be formed, so that sintering is promoted; the titanium dioxide can be used as a mineralizer, and the main function of the titanium dioxide is to be in solid fusion with alumina, activate grains and promote sintering; the added kaolin can improve the plasticity of the materials and is beneficial to the dissolution and sintering of alumina; the mullite crystal has the function of improving the hydrogen fluoride acid erosion resistance of the prepared heat storage ceramic powder and is also beneficial to reducing the firing temperature.
The prepared heat storage ceramic powder has high temperature resistance, corrosion resistance and large heat capacity, has good thermal stability at high temperature, and is not easy to generate physical and chemical deformation or quality change.
According to the invention, the initiator solution and the heat storage ceramic powder are simultaneously added into the polymerization monomer solution at a uniform speed, so that the initiator solution and the heat storage ceramic powder are kept for the same adding time, the reaction time is saved, the substances can be mixed more fully and uniformly, and the preparation efficiency of the polycarboxylic acid water reducer is obviously improved; the heat storage porcelain powder has stable physical and chemical properties, and when the external temperature rises, the added heat storage porcelain powder can absorb a large amount of heat, so that molecular chains in the polycarboxylic acid water reducing agent cannot absorb enough heat to be decomposed and broken, and the original molecular performance of the polycarboxylic acid water reducing agent is maintained, so that the prepared polycarboxylic acid water reducing agent has good thermal stability, and the slump retaining performance of the polycarboxylic acid water reducing agent at high temperature is obviously improved; meanwhile, due to the extremely low water absorption of the heat storage porcelain powder, the HLB (water-oil-degree) value is reduced, the possibility of forming combined water by cement particles and water is reduced when the heat storage porcelain powder is used, and more free water is released, so that the viscosity of cement slurry is reduced, and the slurry can be pumped for a long distance and is convenient to construct.
The above; but are merely preferred embodiments of the invention; the scope of the invention is not limited thereto; any person skilled in the art is within the technical scope of the present disclosure; the technical scheme and the improved concept of the invention are equally replaced or changed; are intended to be covered by the scope of the present invention.

Claims (10)

1. A preparation method of a reinforced and toughened polycarboxylic acid water reducer is characterized by comprising the following steps:
firstly, weighing 20-30 parts of methacrylic acid, 15-25 parts of acrylic acid, 10-15 parts of ethyl acrylate, 10-15 parts of hydroxyethyl acrylate, 10-15 parts of sodium allylsulfonate, 8-12 parts of methyl methacrylate, 5-10 parts of allyl polyoxyethylene ether, 0.5-1 part of initiator, 3-5 parts of thermal storage ceramic powder and 1-3 parts of molecular weight regulator according to parts by weight;
the second step is that: mixing methacrylic acid, acrylic acid, ethyl acrylate, hydroxyethyl acrylate, sodium allylsulfonate, methyl methacrylate, allyl polyoxyethylene ether and deionized water to prepare a polymerized monomer solution with the content of 50-60% by mass;
the third step: mixing an initiator and water to prepare an initiator solution with the content of 10-20% by mass;
the fourth step: putting the polymerization monomer solution into a reaction kettle, wherein the reaction temperature is 80-100 ℃, adding the initiator solution into the polymerization monomer solution at a constant speed in a dropwise adding mode, and simultaneously adding the heat storage ceramic powder and the molecular weight regulator into the polymerization monomer solution at a constant speed, wherein the reaction time is 3-4 h; then cooling to 40-50 ℃, adding an alkaline solution to adjust the pH value to 6.5-7.5, and obtaining the final polycarboxylic acid water reducing agent.
2. The preparation device used in the preparation method of the reinforced and toughened polycarboxylic acid water reducer according to claim 1, characterized in that: the reaction kettle comprises a reaction kettle main body (1), and a metering cylinder (2) is fixedly connected to the upper end of the reaction kettle main body (1).
3. The preparation device used in the preparation method of the reinforced and toughened polycarboxylic acid water reducer according to claim 2, characterized in that: the metering cylinder (2) comprises a cylinder shell (21), a partition plate (22) is fixedly connected to the inner wall of the cylinder shell (21), and the inside of the cylinder shell (21) is divided into a powder groove (23) and a liquid groove (24) through the partition plate (22).
4. The preparation device used in the preparation method of the reinforced and toughened polycarboxylic acid water reducer according to claim 3, characterized in that: the lower extreme fixedly connected with main siphunculus (25) and vice siphunculus (26) of barrel shell (21), main siphunculus (25) communicate with each other with liquid groove (24), vice siphunculus (26) communicate with each other with powder groove (23), all fixedly connected with velocity of flow governing valve (27) on main siphunculus (25) and vice siphunculus (26).
5. The preparation device used in the preparation method of the reinforced and toughened polycarboxylic acid water reducer according to claim 3, characterized in that: the outer end of the cylinder shell (21) is carved with a volume scale (28).
6. The preparation device used in the preparation method of the reinforced and toughened polycarboxylic acid water reducer according to claim 4, wherein: the cylinder shell (21) is made of transparent acrylic materials.
7. The preparation device used in the preparation method of the reinforced and toughened polycarboxylic acid water reducer according to claim 4, wherein: the main through pipe (25) is in a circular pipe shape, and the auxiliary through pipe (26) is in a funnel shape.
8. The water reducer obtained by the preparation method of the reinforced and toughened polycarboxylic acid water reducer according to claim 1, which is characterized in that: the heat storage porcelain powder comprises aluminum oxide, silicon oxide, calcium oxide, magnesium oxide, kaolin, mullite crystals, titanium dioxide and silicon dioxide.
9. The water reducer obtained by the preparation method of the reinforced and toughened polycarboxylic acid water reducer according to claim 8, characterized in that: the preparation method of the heat storage ceramic powder comprises the following steps:
s1, weighing 12-16 parts of alumina, 3-5 parts of silicon oxide, 0.2-0.5 part of calcium oxide, 0.2-0.5 part of magnesium oxide, 1-3 parts of kaolin, 1-2 parts of mullite crystal, 2-3 parts of titanium dioxide and 0.5-1 part of silicon dioxide according to parts by weight, and placing the materials into a ball mill for ball milling for 4-6 hours with the ball milling granularity of 0.6-0.8mm to obtain a first mixture;
s2, placing the mixture I in a sodium hydroxide solution with the concentration of 0.5-1mol/L, reacting for 1-2h, and performing primary drying; spray drying the primarily dried material at an inlet temperature of 130-150 ℃ and an outlet temperature of 70-100 ℃ to obtain a mixture II;
s3, placing the mixture II into a vacuum sintering furnace for sintering, wherein the sintering temperature is 1200-1500 ℃, and the sintering time is 8-12 h; then the temperature is reduced to 100-300 ℃, the temperature is kept for 1-3h, and the heat storage ceramic powder is obtained after natural cooling to the normal temperature.
10. The water reducer obtained by the preparation method of the reinforced and toughened polycarboxylic acid water reducer according to claim 1, which is characterized in that: the initiator is one or a mixture of ammonium persulfate, potassium persulfate or benzoyl peroxide.
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