CN111533482A - Ultra-high-efficiency slump-retaining type polycarboxylate superplasticizer for improving high-temperature resistance of concrete - Google Patents

Ultra-high-efficiency slump-retaining type polycarboxylate superplasticizer for improving high-temperature resistance of concrete Download PDF

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CN111533482A
CN111533482A CN202010389777.7A CN202010389777A CN111533482A CN 111533482 A CN111533482 A CN 111533482A CN 202010389777 A CN202010389777 A CN 202010389777A CN 111533482 A CN111533482 A CN 111533482A
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周明
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    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B40/00Processes, in general, for influencing or modifying the properties of mortars, concrete or artificial stone compositions, e.g. their setting or hardening ability
    • C04B40/0028Aspects relating to the mixing step of the mortar preparation
    • C04B40/0039Premixtures of ingredients
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
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    • C08F283/00Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G
    • C08F283/06Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G on to polyethers, polyoxymethylenes or polyacetals
    • C08F283/065Macromolecular 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
    • FMECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25DREFRIGERATORS; COLD ROOMS; ICE-BOXES; COOLING OR FREEZING APPARATUS NOT OTHERWISE PROVIDED FOR
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    • F25D1/02Devices using naturally cold air or cold water using naturally cold water, e.g. household tap water
    • FMECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25DREFRIGERATORS; COLD ROOMS; ICE-BOXES; COOLING OR FREEZING APPARATUS NOT OTHERWISE PROVIDED FOR
    • F25D17/00Arrangements for circulating cooling fluids; Arrangements for circulating gas, e.g. air, within refrigerated spaces
    • F25D17/02Arrangements for circulating cooling fluids; Arrangements for circulating gas, e.g. air, within refrigerated spaces for circulating liquids, e.g. brine
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    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2103/00Function or property of ingredients for mortars, concrete or artificial stone
    • C04B2103/30Water reducers, plasticisers, air-entrainers, flow improvers
    • C04B2103/302Water reducers

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Abstract

The invention belongs to the technical field of concrete production and processing, and particularly relates to an ultra-high-efficiency slump-retaining polycarboxylic acid water reducing agent for improving the high-temperature resistance of concrete; the composition is prepared from the following raw materials in parts by weight: acrylic acid, sodium methacrylate, deionized water, isobutylene alcohol polyoxyethylene ether, a trigger, sodium bisulfate, polyethylene glycol, p-toluenesulfonic acid, a high-temperature resistant mixture and sodium tripolyphosphate; wherein the high-temperature resistant mixture consists of the following raw materials in parts by weight: silica mixture, calcium oxide mixture, ferric oxide mixture, chlorate mixture; after the silicon dioxide mixture, the calcium oxide mixture, the ferric oxide mixture and the chlorate mixture are added into the raw materials, the water reducing agent can effectively increase the heat-resisting effect of the concrete after the concrete is added, reduce the influence of high temperature on the concrete structure and improve the strength of the concrete at high temperature.

Description

Ultra-high-efficiency slump-retaining type polycarboxylate superplasticizer for improving high-temperature resistance of concrete
Technical Field
The invention belongs to the technical field of concrete production and processing, and particularly relates to an ultra-high-efficiency slump-retaining polycarboxylic acid water reducer for improving the high-temperature resistance of concrete.
Background
Concrete admixture, referred to as admixture for short, is a substance for improving the performance of concrete which is added before or during the mixing process of mixing the concrete; the admixture can effectively improve the performance of concrete and has good economic benefit, is widely applied in many countries, and is more and more emphasized in engineering, so that the admixture becomes an indispensable material in the concrete; the water reducing agent is the most important additive in concrete, and can reduce the water consumption for mixing and improve the strength of the concrete under the condition of unchanged concrete workability and cement consumption; or the cement consumption is saved under the condition of unchanged workability and strength.
Some technical solutions related to water reducing agents also appear in the prior art, such as a polycarboxylic acid type water reducing agent disclosed in a chinese patent with application number 2018103900908, which comprises the following components in percentage by weight: 14-21 parts of unsaturated polyoxyethylene ether, 2.8-3.5 parts of a slow-release high-efficiency water reducing agent, 3.8-12.5 parts of sodium dodecyl sulfate, 5.5-8.5 parts of acrylic acid, 5-10 parts of a crosslinking monomer, 11-26 parts of diethanol monoisopropanolamine, 8-20 parts of sodium gluconate, 1.6-3.0 parts of maleic anhydride, 8-16 parts of mercaptopropionic acid, 1-2 parts of N-dimethylcyclohexylamine, 3.5-7.5 parts of carboxylic ester, 7-9 parts of sodium methallyl sulfonate, 8-13 parts of sodium hypophosphite, 3-5 parts of an initiator and 6-12 parts of a preservative; the water reducing agent provided by the production method of the high-performance water reducing agent can reduce the water amount added in the concrete construction process, is beneficial to shortening the solidification time of the concrete and improving the strength of the concrete; however, the technical scheme does not solve the problem of poor heat resistance of concrete, the heat-resistant effect of the concrete on the existing market is poor, and the surface structure of the concrete is loosened and collapsed under long-time heating or exposure to the sun, so that the overall strength and the service life of the concrete structure are influenced.
Disclosure of Invention
In order to make up the defects of the prior art, the concrete in the existing market has poor heat-resistant effect, and the surface structure of the concrete is loosened and collapsed after being heated for a long time or exposed to the sun, so that the overall strength and the service life of the concrete structure are influenced; the invention provides an ultra-high efficiency slump retaining type polycarboxylate superplasticizer for improving the high temperature resistance of concrete.
The technical scheme adopted by the invention for solving the technical problems is as follows: the invention relates to an ultra-high-efficiency slump retaining type polycarboxylate superplasticizer for improving high temperature resistance of concrete, which is prepared from the following raw materials in parts by weight:
Figure BDA0002485350060000021
preferably, the high-temperature resistant mixture consists of the following raw materials in parts by weight:
Figure BDA0002485350060000022
after the silicon dioxide mixture, the calcium oxide mixture, the ferric oxide mixture and the chlorate mixture are added into the raw materials, the water reducing agent can effectively increase the heat-resisting effect of the concrete after the concrete is added, so that the concrete can ensure small decomposition rate and small expansion rate at high temperature, the influence of high temperature on the concrete structure is reduced, and the strength of the concrete at high temperature is improved.
Preferably, the trigger is ammonium persulfate or potassium persulfate, and the trigger needs to be heated and stirred to be uniform before being added.
Preferably, the preparation method of the ultra-high-efficiency slump-retaining type polycarboxylate superplasticizer for improving the high-temperature resistance of concrete comprises the following steps:
s1: weighing various raw materials, and determining the preparation proportion among acrylic acid, sodium methacrylate, deionized water, isobutylene alcohol polyoxyethylene ether, a trigger, sodium bisulfate, polyethylene glycol, p-toluenesulfonic acid, a high-temperature resistant mixture and sodium tripolyphosphate;
s2: sequentially pouring acrylic acid, sodium methacrylate, deionized water and isobutylene alcohol polyoxyethylene ether into a mixing container, heating the mixing container to ensure that the temperature in the mixing container reaches 45-50 ℃, continuously stirring the raw materials in the mixing container in the adding process, inserting a cooling device into the mixing container for cooling after uniformly stirring, and till the temperature in the mixing container is restored to the room temperature;
s3: continuously adding sodium bisulfate, polyethylene glycol, p-toluenesulfonic acid, the high-temperature-resistant mixture and sodium tripolyphosphate into the mixing container, heating the mixing container again until the temperature in the mixing container reaches 70-80 ℃, continuously stirring and mixing the raw materials in the mixing container in the heating process, stopping heating after uniformly stirring, and reinserting the cooling device into the mixing container for cooling until the temperature in the mixing container is recovered to room temperature;
s4; and continuously adding a trigger into the mixing container, and carrying out reduced pressure treatment on the mixing container to ensure that the pressure in the mixing container is 1.5-1.8MPa, continuously stirring the mixing container at the moment, gradually reducing the pressure of the mixing container after uniform stirring until the pressure is restored to normal temperature and normal pressure, and then completing the preparation of the water reducer.
Preferably, when the mixing vessel is cooled, the mixing vessel is always stirred, and the cooling rate of the raw material is increased.
Preferably, the cooling device comprises a first plate, a cold flow pipe, a second plate, a collecting tank, a water changing tank, a cooling tank and a water pump; the cold flow pipe is arranged on the side wall of the bottom end of the first plate; the collecting box is arranged on the side wall of the top end of the first plate and is communicated with the cold flow pipe; the second plate is arranged on the side wall of the top end of the collecting box; the cooling box is arranged on the side wall of the top end of the second plate, and a heat dissipation unit is arranged in the cooling box; the water pump is arranged on the side wall of the top end of the second plate; the water changing tank is arranged on the side wall of the top end of the second plate between the cooling tank and the water pump and is respectively communicated with the collecting tank and the water pump through water pipes; the heat dissipation unit comprises a material storage bag, a nozzle and a heat dissipation fin; the storage bag is arranged on the side wall of the cooling box, and dimethylamine is filled in the storage bag; the nozzle is arranged on the inner side wall of the cooling box and is communicated with the material storage bag; the cooling fins are arranged in the cooling box through the struts, so that the water pipes are wound on the cooling fins; the cooling effect on the mixing container is enhanced through the matching of the first plate, the cold flow pipe, the second plate, the collecting tank, the water changing tank, the cooling tank and the water pump; when the cooling device works, when the mixing container needs to be cooled, the cooling device is inserted into the mixing container, the water pump is electrified at the moment, so that cooling liquid in the water changing tank flows into the collecting tank through the water pump and then flows into the cold flow pipe through the collecting tank, the temperature on the surface of the cold flow pipe is reduced, the temperature difference between the cold flow pipe and the raw material is increased, heat in the raw material is absorbed through the cold flow pipe and is transferred into the cooling liquid through the cold flow pipe, the temperature of the cooling liquid is increased after the cooling liquid absorbs the heat and continuously flows into the collecting tank along the cold flow pipe, the cooling liquid passes through the cooling tank through the water pipe, dimethylamine in the storage bag is sprayed into the water pipe through the nozzle at the moment, the cooling effect on the water pipe is realized, the temperature of the cooling liquid in the water pipe is reduced, and meanwhile, because the water pipe is wound on the radiating fins, the heat of the cooling liquid in, and accelerate the cooling effect of cooling liquid in the water pipe through the fin, the cooling liquid flows back to in the water change box through the water pipe after the cooling to continue to be flowed by the suction of water pump suction, thereby realized the circulative cooling effect to in the mixing vessel, accelerated the cooling of raw materials in the mixing vessel, avoided reducing the radiating rate of raw materials under the effect of high temperature resistant mixture, thereby further improve the preparation efficiency of water-reducing agent.
Preferably, an elastic filter screen is arranged on the side wall of the water changing tank; the elastic piece is arranged on the elastic filter screen; the connecting rods are symmetrically arranged on the side wall of the elastic sheet; the top end of the connecting rod is hinged with a push plate; the heat transfer effect between the upper layer cooling liquid and the lower layer cooling liquid in the water exchange tank is enhanced through the matching of the elastic filter screen, the connecting rod and the push plate; when the device works, the cold flow pipe absorbs heat in raw materials, the heat is transferred to cooling liquid through the cold flow pipe, the temperature of the cooling liquid rises after the cooling liquid absorbs the heat, the cooling liquid continuously flows into the collecting tank along the cold flow pipe and passes through the cooling tank through the water pipe, dimethylamine in the storage bag is sprayed into the water pipe through the nozzle at the moment, the cooling effect on the water pipe is realized, the temperature of the cooling liquid in the water pipe is reduced, meanwhile, the heat of the cooling liquid in the water pipe is transferred to the radiating fins through heat conduction due to the fact that the water pipe is wound on the radiating fins, the cooling effect of the cooling liquid in the water pipe is accelerated through the radiating fins, the cooling liquid flows back into the water changing tank through the water pipe after being cooled, the elastic filter screen vibrates under the action of water flow, the elastic pieces are driven to fluctuate back and forth in the vibration process of the elastic filter screen, and the push, the lower coolant liquid of drive water change box bottom temperature forms the layer phenomenon of trading between the higher coolant liquid of water change box top temperature with trading, and the reinforcing trades the equilibrium of the coolant liquid temperature in the water box, guarantees that the coolant liquid can form sufficient temperature difference through between cold flow pipe and the raw materials when passing through the cold flow pipe to further strengthen the cooling effect to the raw materials.
Preferably, the side wall of the cooling box close to the radiating fin is provided with a flow guide column; the outer side of the flow guide column is provided with a conical groove, so that the groove part of the flow guide column corresponds to the area between the radiating fins; the during operation, absorb the heat in the raw materials through the cold flow pipe, and through cold flow pipe with heat transfer to coolant liquid in, the coolant liquid is temperature rise after absorbing the heat, and continue to flow to the header along the cold flow pipe, and the lead-through pipe passes through the cooler bin, dimethylamine in the storage bag spouts to the water pipe in through the nozzle this moment, realize the cooling effect to the water pipe, reduce the temperature of cooling liquid in the water pipe, through nozzle spun dimethylamine behind the water pipe surface, to striking with the groove of water conservancy diversion post, and flow back with the direction of perpendicular to water conservancy diversion post recess lateral wall, carry out secondary cooling effect to the water pipe, thereby strengthen the cooling effect to the coolant liquid, improve the utilization ratio to dimethylamine simultaneously.
The invention has the following beneficial effects:
1. according to the ultra-high-efficiency slump-retaining polycarboxylic acid water reducing agent for improving the high-temperature resistance of the concrete, after the silicon dioxide mixture, the calcium oxide mixture, the ferric oxide mixture and the chlorate mixture are added into the raw materials, the heat-resistant effect of the concrete can be effectively improved after the water reducing agent is added into the concrete, the decomposition rate and the expansion rate of the concrete at high temperature can be ensured to be small, so that the influence of high temperature on the concrete structure is reduced, and the strength of the concrete at high temperature is improved.
2. According to the ultra-high-efficiency slump retaining type polycarboxylate water reducer for improving the high-temperature resistance of concrete, the cooling effect on a mixing container is enhanced through the matching of the first plate, the cold flow pipe, the second plate, the collecting tank, the water changing tank, the cooling tank and the water pump, the circulating cooling effect in the mixing container is realized, the cooling of raw materials in the mixing container is accelerated, the reduction of the heat dissipation rate of the raw materials under the action of a high-temperature resistant mixture is avoided, and the preparation efficiency of the water reducer is further improved.
Drawings
The invention will be further explained with reference to the drawings.
FIG. 1 is a flow chart of a preparation method of the ultra-high-efficiency slump-retaining type polycarboxylate superplasticizer for improving the high-temperature resistance of concrete in the invention;
FIG. 2 is a perspective view of the cooling device of the present invention;
FIG. 3 is a schematic view of the structure of the change water tank of the present invention;
FIG. 4 is a schematic view of the structure of the cooling tank of the present invention;
in the figure: the plate cooling system comprises a first plate 1, a cold flow pipe 2, a second plate 3, a collecting box 4, a water changing box 5, an elastic filter screen 51, an elastic sheet 52, a connecting rod 53, a push plate 54, a cooling box 6, a guide column 61, a water pump 7, a heat dissipation unit 8, a storage bag 81, a nozzle 82 and a cooling fin 83.
Detailed Description
In order to make the technical means, the creation characteristics, the achievement purposes and the effects of the invention easy to understand, the invention is further described with the specific embodiments.
Example 1
An ultra-high efficiency slump retaining type polycarboxylate superplasticizer for improving high temperature resistance of concrete is composed of the following raw materials in parts by weight: 7 parts of acrylic acid, 6 parts of sodium methacrylate, 40 parts of deionized water, 23 parts of isobutylene alcohol polyoxyethylene ether, 17 parts of a trigger, 7 parts of sodium bisulfate, 50 parts of polyethylene glycol, 3 parts of p-toluenesulfonic acid, 20 parts of a high-temperature resistant mixture and 6 parts of sodium tripolyphosphate; wherein the high-temperature resistant mixture consists of the following raw materials in parts by weight: 7 parts of silicon dioxide mixture, 7 parts of calcium oxide mixture, 7 parts of ferric oxide mixture and 7 parts of chlorate mixture.
Adding the prepared water reducing agent into concrete for full mixing, and building a three-dimensional model with the length, width and height of one meter by using the concrete; and heating the three-dimensional model at 800 ℃ for 3h, cooling the three-dimensional model at room temperature for 4h after heating, and measuring the expansion rate, residual temperature and decomposition rate of the three-dimensional model.
Example 2
An ultra-high efficiency slump retaining type polycarboxylate superplasticizer for improving high temperature resistance of concrete is composed of the following raw materials in parts by weight: 7 parts of acrylic acid, 6 parts of sodium methacrylate, 40 parts of deionized water, 23 parts of isobutylene alcohol polyoxyethylene ether, 17 parts of a trigger, 7 parts of sodium bisulfate, 50 parts of polyethylene glycol, 3 parts of p-toluenesulfonic acid, 30 parts of a high-temperature resistant mixture and 6 parts of sodium tripolyphosphate; wherein the high-temperature resistant mixture consists of the following raw materials in parts by weight: 7 parts of silicon dioxide mixture, 7 parts of calcium oxide mixture, 7 parts of ferric oxide mixture and 7 parts of chlorate mixture.
Adding the prepared water reducing agent into concrete for full mixing, and building a three-dimensional model with the length, width and height of one meter by using the concrete; and heating the three-dimensional model at 800 ℃ for 3h, cooling the three-dimensional model at room temperature for 4h after heating, and measuring the expansion rate, residual temperature and decomposition rate of the three-dimensional model.
Example 3
An ultra-high efficiency slump retaining type polycarboxylate superplasticizer for improving high temperature resistance of concrete is composed of the following raw materials in parts by weight: 7 parts of acrylic acid, 6 parts of sodium methacrylate, 40 parts of deionized water, 23 parts of isobutylene alcohol polyoxyethylene ether, 17 parts of a trigger, 7 parts of sodium bisulfate, 50 parts of polyethylene glycol, 3 parts of p-toluenesulfonic acid, 40 parts of a high-temperature resistant mixture and 6 parts of sodium tripolyphosphate; wherein the high-temperature resistant mixture consists of the following raw materials in parts by weight: 7 parts of silicon dioxide mixture, 7 parts of calcium oxide mixture, 7 parts of ferric oxide mixture and 7 parts of chlorate mixture.
Adding the prepared water reducing agent into concrete for full mixing, and building a three-dimensional model with the length, width and height of one meter by using the concrete; and heating the three-dimensional model at 800 ℃ for 3h, cooling the three-dimensional model at room temperature for 4h after heating, and measuring the expansion rate, residual temperature and decomposition rate of the three-dimensional model.
The use effect of the obtained ultra-high efficiency slump retaining type polycarboxylate superplasticizer for improving the high temperature resistance of concrete is shown in table 1.
TABLE 1
Expansion ratio of three-dimensional model Residual temperature of three-dimensional model Decomposition rate of stereo model
Example 1 104.8% 230℃ 3.2%
Example 2 102.5% 160℃ 2.5%
Example 3 101.2% 80℃ 1.8%
Through the embodiments 1-3, it can be seen that after the silicon dioxide mixture, the calcium oxide mixture, the ferric oxide mixture and the chlorate mixture are added into the raw materials, the heat-resistant effect of the concrete can be effectively increased after the water reducing agent is added into the concrete, so that the concrete can ensure that the decomposition rate and the expansion rate are small at high temperature, the influence of the high temperature on the concrete structure is reduced, and the strength of the concrete at the high temperature is improved.
As shown in FIGS. 1 to 4, the preparation method of the ultra-high-efficiency slump-retaining type polycarboxylate superplasticizer for improving the high temperature resistance of concrete comprises the following steps:
s1: weighing various raw materials, and determining the preparation proportion among acrylic acid, sodium methacrylate, deionized water, isobutylene alcohol polyoxyethylene ether, a trigger, sodium bisulfate, polyethylene glycol, p-toluenesulfonic acid, a high-temperature resistant mixture and sodium tripolyphosphate;
s2: sequentially pouring acrylic acid, sodium methacrylate, deionized water and isobutylene alcohol polyoxyethylene ether into a mixing container, heating the mixing container to ensure that the temperature in the mixing container reaches 45-50 ℃, continuously stirring the raw materials in the mixing container in the adding process, inserting a cooling device into the mixing container for cooling after uniformly stirring, and till the temperature in the mixing container is restored to the room temperature;
s3: continuously adding sodium bisulfate, polyethylene glycol, p-toluenesulfonic acid, the high-temperature-resistant mixture and sodium tripolyphosphate into the mixing container, heating the mixing container again until the temperature in the mixing container reaches 70-80 ℃, continuously stirring and mixing the raw materials in the mixing container in the heating process, stopping heating after uniformly stirring, and reinserting the cooling device into the mixing container for cooling until the temperature in the mixing container is recovered to room temperature;
s4; and continuously adding a trigger into the mixing container, and carrying out reduced pressure treatment on the mixing container to ensure that the pressure in the mixing container is 1.5-1.8MPa, continuously stirring the mixing container at the moment, gradually reducing the pressure of the mixing container after uniform stirring until the pressure is restored to normal temperature and normal pressure, and then completing the preparation of the water reducer.
In one embodiment of the present invention, the cooling rate of the raw material is increased by always stirring the mixing container when the mixing container is cooled.
The cooling device comprises a first plate 1, a cold flow pipe 2, a second plate 3, a collecting tank 4, a water changing tank 5, a cooling tank 6 and a water pump 7; the cold flow pipe 2 is arranged on the side wall of the bottom end of the first plate 1; the collecting box 4 is arranged on the side wall of the top end of the first plate 1 and is communicated with the cold flow pipe 2; the second plate 3 is arranged on the side wall of the top end of the collecting box 4; the cooling box 6 is arranged on the side wall of the top end of the second plate 3, and a heat dissipation unit 8 is arranged in the cooling box 6; the water pump 7 is arranged on the side wall of the top end of the second plate 3; the water changing tank 5 is arranged on the side wall of the top end of the second plate 3 between the cooling tank 6 and the water pump 7, and the water changing tank 5 is respectively communicated with the collecting tank 4 and the water pump 7 through water pipes; the heat dissipation unit 8 includes a storage pocket 81, a nozzle 82, and a heat dissipation fin 83; the storage bag 81 is arranged on the side wall of the cooling box 6, and dimethylamine is filled in the storage bag 81; the nozzle 82 is arranged on the inner side wall of the cooling box 6 and is communicated with the material storage bag 81; the cooling fins 83 are installed in the cooling box 6 through pillars so that the water pipes are wound around the cooling fins 83; the cooling effect on the mixing container is enhanced through the matching of the first plate 1, the cold flow pipe 2, the second plate 3, the collecting box 4, the water changing box 5, the cooling box 6 and the water pump 7; when the cooling device works, when the mixing container needs to be cooled, the cooling device is inserted into the mixing container, the water pump 7 is powered on at the moment, so that cooling liquid in the water changing tank 5 flows into the collecting tank 4 through the water pump 7 and then flows into the cold flow pipe 2 through the collecting tank 4, the temperature of the surface of the cold flow pipe 2 is reduced, the temperature difference between the cold flow pipe 2 and the raw material is increased, heat in the raw material is absorbed through the cold flow pipe 2, the heat is transferred into the cooling liquid through the cold flow pipe 2, the temperature of the cooling liquid rises after absorbing the heat and continuously flows into the collecting tank 4 along the cold flow pipe 2, the cooling liquid passes through the cooling tank 6 through the water pipe, dimethylamine in the material storing bag 81 is sprayed into the water pipe through the nozzle 82 at the moment, the cooling effect on the water pipe is achieved, the temperature of the cooling liquid in the water pipe is reduced, meanwhile, because the water pipe is wound on the radiating fins 83, the heat of the cooling liquid in the, and the cooling effect of the cooling liquid in the water pipe is accelerated through the cooling fins 83, the cooling liquid flows back to the water change tank 5 through the water pipe after being cooled, and continues to be sucked out by the water pump 7 to flow, so that the circulating cooling effect in the mixing container is realized, the cooling of the raw materials in the mixing container is accelerated, the reduction of the heat dissipation rate of the raw materials under the action of the high-temperature-resistant mixture is avoided, and the preparation efficiency of the water reducing agent is further improved.
As an embodiment of the present invention, an elastic filter screen 51 is disposed on a side wall of the water change box 5; the elastic filter screen 51 is provided with an elastic sheet 52; the connecting rods 53 are symmetrically arranged on the side wall of the elastic sheet 52; the top end of the connecting rod 53 is hinged with a push plate 54; the heat transfer effect between the upper layer cooling liquid and the lower layer cooling liquid in the water change tank 5 is enhanced through the matching of the elastic filter screen 51, the connecting rod 53 and the push plate 54; when the device works, the cold flow pipe 2 absorbs heat in raw materials, the heat is transferred to cooling liquid through the cold flow pipe 2, the temperature of the cooling liquid rises after absorbing the heat, the cooling liquid continuously flows into the collecting box 4 along the cold flow pipe 2 and passes through the cooling box 6 through a water pipe, dimethylamine in the storage bag 81 is sprayed into the water pipe through the nozzle 82 at the moment, the cooling effect on the water pipe is realized, the temperature of the cooling liquid in the water pipe is reduced, meanwhile, the water pipe is wound on the radiating fin 83, the heat of the cooling liquid in the water pipe is transferred to the radiating fin 83 through heat conduction, the cooling effect of the cooling liquid in the water pipe is accelerated through the radiating fin 83, the cooling liquid flows back into the water changing box 5 through the water pipe after being cooled, the elastic filter screen 51 vibrates under the action of water flow, the elastic sheet 52 is driven to fluctuate back and forth in the vibration process of the elastic filter screen 51, and the push plate 54 is driven by the connecting rod, the lower coolant liquid of 5 bottom temperatures of drive water changing box forms the layer phenomenon with changing between the higher coolant liquid of 5 top temperatures of water changing box, and the equilibrium of the coolant liquid temperature in the 5 reinforcing water changing box guarantees that the coolant liquid can form sufficient temperature difference through cold flow pipe 2 and between the raw materials when 2 is managed in the cold flow to further strengthen the cooling effect to the raw materials.
As an embodiment of the present invention, the cooling box 6 is provided with a guide post 61 on a side wall near the fin 83; a conical groove is formed on the outer side of the guide column 61, so that the groove part of the guide column 61 corresponds to the area between the radiating fins 83; the during operation, absorb the heat in the raw materials through cold flow pipe 2, and through cold flow pipe 2 with heat transfer to the coolant liquid in, the coolant liquid is temperature rise after absorbing the heat, and continue to flow to the header tank 4 along cold flow pipe 2 in, and lead to pipe through cooler bin 6, dimethylamine in the storage bag 81 spouts to the water pipe in through nozzle 82 this moment, realize the cooling effect to the water pipe, reduce the temperature of coolant liquid in the water pipe, through nozzle 82 spun dimethylamine behind water pipe surface, to striking with the groove of water conservancy diversion post 61, and flow back with the direction of perpendicular to water conservancy diversion post 61 recess lateral wall, carry out secondary cooling effect to the water pipe, thereby strengthen the cooling effect to the coolant liquid, improve the utilization ratio to dimethylamine simultaneously.
When the cooling device works, when the mixing container needs to be cooled, the cooling device is inserted into the mixing container, the water pump 7 is powered on at the moment, so that cooling liquid in the water changing tank 5 flows into the collecting tank 4 through the water pump 7 and then flows into the cold flow pipe 2 through the collecting tank 4, the temperature of the surface of the cold flow pipe 2 is reduced, the temperature difference between the cold flow pipe 2 and the raw material is increased, heat in the raw material is absorbed through the cold flow pipe 2, the heat is transferred into the cooling liquid through the cold flow pipe 2, the temperature of the cooling liquid rises after absorbing the heat and continuously flows into the collecting tank 4 along the cold flow pipe 2, the cooling liquid passes through the cooling tank 6 through the water pipe, dimethylamine in the material storing bag 81 is sprayed into the water pipe through the nozzle 82 at the moment, the cooling effect on the water pipe is achieved, the temperature of the cooling liquid in the water pipe is reduced, meanwhile, because the water pipe is wound on the radiating fins 83, the heat of the cooling liquid in the, the cooling effect of the cooling liquid in the water pipe is accelerated through the cooling fins 83, the cooling liquid flows back into the water change tank 5 through the water pipe after being cooled and is continuously sucked out by the water pump 7 to flow, so that the circulating cooling effect in the mixing container is realized, the cooling of the raw materials in the mixing container is accelerated, the reduction of the heat dissipation rate of the raw materials under the action of a high-temperature-resistant mixture is avoided, and the preparation efficiency of the water reducing agent is further improved; the heat in the raw materials is absorbed by the cold flow pipe 2, the heat is transferred to the cooling liquid by the cold flow pipe 2, the temperature of the cooling liquid rises after absorbing the heat, the cooling liquid continuously flows into the collecting tank 4 along the cold flow pipe 2 and passes through the cooling tank 6 by a water pipe, dimethylamine in the storage bag 81 is sprayed into the water pipe by the nozzle 82 at the moment, the cooling effect on the water pipe is realized, the temperature of the cooling liquid in the water pipe is reduced, meanwhile, the heat of the cooling liquid in the water pipe is transferred to the radiating fin 83 by heat conduction because the water pipe is wound on the radiating fin 83, the cooling effect of the cooling liquid in the water pipe is accelerated by the radiating fin 83, the cooling liquid flows back into the water changing tank 5 by the water pipe after being cooled, the elastic filter screen 51 vibrates under the action of the water flow, the elastic sheet 52 is driven to fluctuate back and forth in the vibration process of the elastic filter screen 51, and the push plate 54 is, the cooling liquid with lower temperature at the bottom of the water changing box 5 is driven to form a layer changing phenomenon with the cooling liquid with higher temperature at the top of the water changing box 5, so that the balance of the temperature of the cooling liquid in the water changing box 5 is enhanced, and the cooling liquid can form enough temperature difference with the raw material through the cold flow pipe 2 when passing through the cold flow pipe 2, thereby further enhancing the cooling effect on the raw material; absorb the heat in the raw materials through cold flow tube 2, and through cold flow tube 2 with heat transfer to the coolant liquid in, the coolant liquid is temperature rise after absorbing the heat, and continue to flow to the collection flow box 4 along cold flow tube 2 in, and the lead to pipe passes through cooler bin 6, dimethylamine in the storage bag 81 spouts to the water pipe in through nozzle 82 this moment, realize the cooling effect to the water pipe, reduce the temperature of cooling liquid in the water pipe, through nozzle 82 spun dimethylamine behind the water pipe surface, to striking with the groove of guide post 61, and flow back with the direction of perpendicular to guide post 61 recess lateral wall, carry out secondary cooling effect to the water pipe, thereby strengthen the cooling effect to the coolant liquid, improve the utilization ratio to dimethylamine simultaneously.
The foregoing illustrates and describes the principles, general features, and advantages of the present invention. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, which are described in the specification and illustrated only to illustrate the principle of the present invention, but that various changes and modifications may be made therein without departing from the spirit and scope of the present invention, which fall within the scope of the invention as claimed. The scope of the invention is defined by the appended claims and equivalents thereof.

Claims (8)

1. An ultra-high efficiency slump retaining type polycarboxylate superplasticizer for improving high temperature resistance of concrete is characterized in that: the composition is prepared from the following raw materials in parts by weight:
Figure FDA0002485350050000011
2. the ultra-high efficiency slump retaining type polycarboxylate superplasticizer for improving the high temperature resistance of concrete according to claim 1, is characterized in that: the high-temperature-resistant mixture is composed of the following raw materials in parts by weight:
Figure FDA0002485350050000012
3. the ultra-high efficiency slump retaining type polycarboxylate superplasticizer for improving the high temperature resistance of concrete according to claim 1, is characterized in that: the trigger is ammonium persulfate or potassium persulfate, and before the trigger is added, the trigger needs to be heated and stirred uniformly.
4. The ultra-high efficiency slump retaining type polycarboxylate superplasticizer for improving the high temperature resistance of concrete according to claim 1, is characterized in that: the preparation method of the ultra-high-efficiency slump retaining type polycarboxylate superplasticizer for improving the high temperature resistance of concrete comprises the following steps:
s1: weighing various raw materials, and determining the preparation proportion among acrylic acid, sodium methacrylate, deionized water, isobutylene alcohol polyoxyethylene ether, a trigger, sodium bisulfate, polyethylene glycol, p-toluenesulfonic acid, a high-temperature resistant mixture and sodium tripolyphosphate;
s2: sequentially pouring acrylic acid, sodium methacrylate, deionized water and isobutylene alcohol polyoxyethylene ether into a mixing container, heating the mixing container to ensure that the temperature in the mixing container reaches 45-50 ℃, continuously stirring the raw materials in the mixing container in the adding process, inserting a cooling device into the mixing container for cooling after uniformly stirring, and till the temperature in the mixing container is restored to the room temperature;
s3: continuously adding sodium bisulfate, polyethylene glycol, p-toluenesulfonic acid, the high-temperature-resistant mixture and sodium tripolyphosphate into the mixing container, heating the mixing container again until the temperature in the mixing container reaches 70-80 ℃, continuously stirring and mixing the raw materials in the mixing container in the heating process, stopping heating after uniformly stirring, and reinserting the cooling device into the mixing container for cooling until the temperature in the mixing container is recovered to room temperature;
s4; and continuously adding a trigger into the mixing container, and carrying out reduced pressure treatment on the mixing container to ensure that the pressure in the mixing container is 1.5-1.8MPa, continuously stirring the mixing container at the moment, gradually reducing the pressure of the mixing container after uniform stirring until the pressure is restored to normal temperature and normal pressure, and then completing the preparation of the water reducer.
5. The ultra-high efficiency slump retaining type polycarboxylate superplasticizer for improving high temperature resistance of concrete according to claim 4, is characterized in that: when the mixing container is cooled, the mixing container is always stirred, and the cooling speed of the raw materials is increased.
6. The ultra-high efficiency slump retaining type polycarboxylate superplasticizer for improving high temperature resistance of concrete according to claim 4, is characterized in that: the cooling device comprises a first plate (1), a cold flow pipe (2), a second plate (3), a collecting tank (4), a water changing tank (5), a cooling tank (6) and a water pump (7); the cold flow pipe (2) is arranged on the side wall of the bottom end of the first plate (1); the collecting box (4) is arranged on the side wall of the top end of the first plate (1) and is communicated with the cold flow pipe (2); the second plate (3) is arranged on the side wall of the top end of the collecting box (4); the cooling box (6) is arranged on the side wall of the top end of the second plate (3), and a heat dissipation unit (8) is arranged in the cooling box (6); the water pump (7) is arranged on the side wall of the top end of the second plate (3); the water changing tank (5) is arranged on the side wall of the top end of the second plate (3) between the cooling tank (6) and the water pump (7), and the water changing tank (5) is respectively communicated with the collecting tank (4) and the water pump (7) through water pipes; the heat dissipation unit (8) comprises a storage bag (81), a nozzle (82) and a heat dissipation fin (83); the storage bag (81) is arranged on the side wall of the cooling box (6), and dimethylamine is filled in the storage bag (81); the nozzle (82) is arranged on the inner side wall of the cooling box (6) and is communicated with the material storage bag (81); the radiating fins (83) are arranged in the cooling box (6) through the struts, so that the water pipes are wound on the radiating fins (83); the cooling effect on the mixing container is enhanced through the matching of the first plate (1), the cold flow pipe (2), the second plate (3), the collecting tank (4), the water changing tank (5), the cooling tank (6) and the water pump (7).
7. The ultra-high efficiency slump retaining type polycarboxylate superplasticizer for improving high temperature resistance of concrete according to claim 6, is characterized in that: an elastic filter screen (51) is arranged on the side wall of the water changing tank (5); the elastic filter screen (51) is provided with an elastic sheet (52); the side wall of the elastic sheet (52) is symmetrically provided with connecting rods (53); the top end of the connecting rod (53) is hinged with a push plate (54); the heat transfer effect between the upper layer cooling liquid and the lower layer cooling liquid in the water change tank (5) is enhanced through the matching of the elastic filter screen (51), the connecting rod (53) and the push plate (54).
8. The ultra-high efficiency slump retaining type polycarboxylate superplasticizer for improving high temperature resistance of concrete according to claim 6, is characterized in that: the side wall of the cooling box (6) close to the radiating fins (83) is provided with a flow guide column (61); the outer side of the flow guide column (61) is provided with a conical groove, so that the groove part of the flow guide column (61) corresponds to the area between the radiating fins (83).
CN202010389777.7A 2020-05-11 2020-05-11 Ultra-high-efficiency slump-retaining type polycarboxylate superplasticizer for improving high-temperature resistance of concrete Pending CN111533482A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112815623A (en) * 2021-01-11 2021-05-18 南京浩轩化工科技有限公司 Concrete high efficiency water reducing agent preparation processing system

Citations (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103833940A (en) * 2013-12-26 2014-06-04 四川石达化学股份有限公司 Polycarboxylate superplasticizer containing phosphine and preparation method thereof
CN104016615A (en) * 2014-06-13 2014-09-03 石家庄市长安育才建材有限公司 Slow release type efficient polycarboxylic acid water reducer and preparation method thereof
CN104497228A (en) * 2014-11-25 2015-04-08 四川吉龙化学建材有限公司 Method for mixing polyester-ether macromonomers for preparation of polycarboxylic acid water reducer
CN105037648A (en) * 2015-08-25 2015-11-11 科之杰新材料集团有限公司 Slump-retaining water-reducing polycarboxylic acid water reducing agent and low-temperature quick preparation method thereof
CN105367720A (en) * 2015-11-25 2016-03-02 科之杰新材料集团有限公司 Water-reducing slump-retaining type polycarboxylic acid water reducing agent and preparing method thereof
CN106082759A (en) * 2016-06-21 2016-11-09 河南省交通科学技术研究院有限公司 A kind of high-thin arch dam polycarboxylate composite water reducing agent and preparation method thereof
CN106478896A (en) * 2016-10-31 2017-03-08 科之杰新材料集团有限公司 A kind of preparation method of comprehensive polycarboxylate water-reducer
CN106839508A (en) * 2015-12-06 2017-06-13 天津市欧汇科技有限公司 A kind of cooling device of efficiently low failure
CN206823218U (en) * 2017-06-26 2018-01-02 谱尼测试集团江苏有限公司 A kind of capable of self-circulating type condensing unit of condensate liquid
CN108716867A (en) * 2018-06-19 2018-10-30 成都翼添科技有限公司 A kind of cooling device in liquid drug production process
CN109337024A (en) * 2018-10-24 2019-02-15 浙江建研科之杰新材料有限公司 A kind of preparation method of slow-setting polycarboxylic acid water reducing agent

Patent Citations (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103833940A (en) * 2013-12-26 2014-06-04 四川石达化学股份有限公司 Polycarboxylate superplasticizer containing phosphine and preparation method thereof
CN104016615A (en) * 2014-06-13 2014-09-03 石家庄市长安育才建材有限公司 Slow release type efficient polycarboxylic acid water reducer and preparation method thereof
CN104497228A (en) * 2014-11-25 2015-04-08 四川吉龙化学建材有限公司 Method for mixing polyester-ether macromonomers for preparation of polycarboxylic acid water reducer
CN105037648A (en) * 2015-08-25 2015-11-11 科之杰新材料集团有限公司 Slump-retaining water-reducing polycarboxylic acid water reducing agent and low-temperature quick preparation method thereof
CN105367720A (en) * 2015-11-25 2016-03-02 科之杰新材料集团有限公司 Water-reducing slump-retaining type polycarboxylic acid water reducing agent and preparing method thereof
CN106839508A (en) * 2015-12-06 2017-06-13 天津市欧汇科技有限公司 A kind of cooling device of efficiently low failure
CN106082759A (en) * 2016-06-21 2016-11-09 河南省交通科学技术研究院有限公司 A kind of high-thin arch dam polycarboxylate composite water reducing agent and preparation method thereof
CN106478896A (en) * 2016-10-31 2017-03-08 科之杰新材料集团有限公司 A kind of preparation method of comprehensive polycarboxylate water-reducer
CN206823218U (en) * 2017-06-26 2018-01-02 谱尼测试集团江苏有限公司 A kind of capable of self-circulating type condensing unit of condensate liquid
CN108716867A (en) * 2018-06-19 2018-10-30 成都翼添科技有限公司 A kind of cooling device in liquid drug production process
CN109337024A (en) * 2018-10-24 2019-02-15 浙江建研科之杰新材料有限公司 A kind of preparation method of slow-setting polycarboxylic acid water reducing agent

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112815623A (en) * 2021-01-11 2021-05-18 南京浩轩化工科技有限公司 Concrete high efficiency water reducing agent preparation processing system
CN112815623B (en) * 2021-01-11 2022-11-01 合肥元旭环保新型材料有限公司 Concrete high efficiency water reducing agent preparation processing system

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