CN111647115A - Polycarboxylate superplasticizer mother liquor and preparation method thereof, and polycarboxylate superplasticizer and preparation method thereof - Google Patents
Polycarboxylate superplasticizer mother liquor and preparation method thereof, and polycarboxylate superplasticizer and preparation method thereof Download PDFInfo
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- CN111647115A CN111647115A CN202010544583.XA CN202010544583A CN111647115A CN 111647115 A CN111647115 A CN 111647115A CN 202010544583 A CN202010544583 A CN 202010544583A CN 111647115 A CN111647115 A CN 111647115A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F283/00—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G
- C08F283/06—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G on to polyethers, polyoxymethylenes or polyacetals
- C08F283/065—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G on to polyethers, polyoxymethylenes or polyacetals on to unsaturated polyethers, polyoxymethylenes or polyacetals
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B24/00—Use of organic materials as active ingredients for mortars, concrete or artificial stone, e.g. plasticisers
- C04B24/24—Macromolecular compounds
- C04B24/26—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
- C04B24/2688—Copolymers containing at least three different monomers
- C04B24/2694—Copolymers containing at least three different monomers containing polyether side chains
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- C04B40/00—Processes, in general, for influencing or modifying the properties of mortars, concrete or artificial stone compositions, e.g. their setting or hardening ability
- C04B40/0028—Aspects relating to the mixing step of the mortar preparation
- C04B40/0039—Premixtures of ingredients
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F2/00—Processes of polymerisation
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- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F2/00—Processes of polymerisation
- C08F2/38—Polymerisation using regulators, e.g. chain terminating agents, e.g. telomerisation
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- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F4/00—Polymerisation catalysts
- C08F4/40—Redox systems
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- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2103/00—Function or property of ingredients for mortars, concrete or artificial stone
- C04B2103/30—Water reducers, plasticisers, air-entrainers, flow improvers
- C04B2103/302—Water reducers
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Abstract
The invention provides a polycarboxylate superplasticizer mother liquor and a preparation method thereof, and a polycarboxylate superplasticizer and a preparation method thereof, and solves the technical problems that the production time is too long in the existing concrete production technology, so that the production construction and production efficiency of a construction site are influenced, and the workload of operators is increased. The mother solution comprises the following raw materials: ether macromonomer, unsaturated acid, oxidant reducing agent, catalyst, chain transfer agent, liquid alkali and water; the water reducing agent comprises the following raw materials: water, a retarding component, a water retention component and an air entraining and defoaming component. According to the mother liquor and the preparation method thereof, and the water reducing agent and the preparation method thereof, provided by the invention, when the temperature is low in winter, the reaction speed of concrete can be increased, the production efficiency can be improved, and the problems of post-bleeding segregation, poor workability and the like of concrete can be effectively prevented; the production process is optimized, the synthesis process time is shortened, the labor cost is saved, and the synthesis time is increased.
Description
Technical Field
The invention relates to a polycarboxylate superplasticizer mother solution for accelerating the initial reaction speed of concrete and a preparation method thereof, and a polycarboxylate superplasticizer for accelerating the initial reaction speed of concrete and a preparation method thereof.
Background
The rapid development of social economy creates wide market space for the building industry, and in addition, the competition of the concrete industry is fierce, the demand of concrete on the market is large, each concrete merchant concrete station occupies the market in order to improve the market competitiveness, and the market is mainly devised in the aspects of reducing materials and cost and improving efficiency, and the concrete merchant concrete station is mainly embodied in that the water consumption is low, the water-cement ratio is reduced by high doping of a water reducing agent, the using amount of a cementing material is saved, and the purpose of reducing cost is achieved.
In the prior art, the problems of poor concrete workability, increased mixing difficulty, slow reaction speed and the like caused by high admixture doping and water consumption reduction are solved; and when the concrete is stirred in large production in winter due to various reasons such as poor quality of the existing ground materials, the condition that the stirring time reaches 120-150 s and the concrete can not be discharged frequently occurs, so that the production time of the concrete is greatly prolonged, the production construction and production efficiency of a construction site are influenced, and the workload of workers in an operation building is increased.
Disclosure of Invention
The invention aims to provide a polycarboxylate superplasticizer mother solution for accelerating the initial reaction speed of concrete, a preparation method thereof, a polycarboxylate superplasticizer for accelerating the initial reaction speed of concrete and a preparation method thereof, and aims to solve the technical problems that the production time is too long in the existing concrete production technology, so that the production construction and production efficiency of construction sites are influenced, and the workload of operators is increased. The technical effects that can be produced by the preferred technical scheme in the technical schemes provided by the invention are described in detail in the following.
In order to achieve the purpose, the invention provides the following technical scheme:
the invention provides a polycarboxylate superplasticizer mother liquor for accelerating the initial reaction speed of concrete, which is prepared from the following raw materials in parts by weight: 20-40 parts of ether macromonomer; 4-10 parts of unsaturated acid; 0.5-1.0 part of oxidant; 0.15-0.25 part of reducing agent; 0.05-0.1 part of catalyst; 0.1-0.3 part of chain transfer agent; 5-10 parts of liquid caustic soda; 40-50 parts of deionized water.
Further, the mother liquor is prepared from the following raw materials in parts by weight: 25-35 parts of ether macromonomer; 6-8 parts of unsaturated acid; 0.6-0.8 part of oxidant; 0.18-0.22 part of reducing agent; 0.06-0.08 part of catalyst; 0.15-0.25 part of chain transfer agent; 6-8 parts of liquid caustic soda; 42-48 parts of deionized water.
Further, the mother liquor is prepared from the following raw materials in parts by weight: 30 parts of ether macromonomer; 7 parts of unsaturated acid; 0.7 part of an oxidizing agent; 0.2 part of a reducing agent; 0.07 part of a catalyst; 0.2 part of chain transfer agent; 7 parts of liquid caustic soda; 45 parts of deionized water.
Further, the ether macromonomer is allyl polyoxyethylene ether;
the unsaturated acid is acrylic acid and maleic anhydride;
the main component of the reducing agent is sodium formaldehyde sulfoxylate sodium formaldehyde sulfate;
the oxidant is hydrogen peroxide;
the chain transfer agent is mercaptopropionic acid or mercaptoacetic acid;
the catalyst is ferrous sulfate heptahydrate;
the liquid alkali is sodium hydroxide solution.
The preparation method of the polycarboxylate superplasticizer mother liquor for accelerating the initial reaction speed of concrete provided by the invention comprises the following steps:
a1, preparing a polycarboxylic acid water reducer mother liquor raw material for accelerating the initial reaction speed of concrete according to a ratio;
a2, preparation of solution A: preparing prepared acrylic acid and mercaptopropionic acid into solution A by using deionized water;
a3, preparation of solution B: dissolving the prepared reducing agent in deionized water, and stirring and dissolving to prepare a solution B;
a4, adding the rest deionized water into a reaction kettle, adding the prepared allyl polyoxyethylene ether and maleic anhydride under the stirring state, heating to 25-30 ℃, controlling the constant temperature to be 25-30 ℃, adding the prepared hydrogen peroxide and ferrous sulfate heptahydrate after the hydrogen peroxide and the ferrous sulfate heptahydrate are completely dissolved, and uniformly stirring;
a5, stabilizing the temperature of the reaction kettle to 25-30 ℃, simultaneously dripping the solution A and the solution B in a stirring state, and controlling the temperature of the reaction kettle to be below 40 ℃ in the dripping process after finishing dripping within 85-95 minutes; after the dropwise addition is finished, continuously preserving the heat in the reaction kettle for 25-35 minutes to obtain a mixed material;
and A6, after the mixed material obtained in the step A5 is cooled to room temperature, adjusting the pH value to 6.0-7.0 by using liquid alkali to obtain the polycarboxylate superplasticizer mother liquor for accelerating the initial reaction speed of the concrete.
The invention provides a polycarboxylic acid water reducing agent for accelerating the initial reaction speed of concrete, which is prepared from the following raw materials in parts by weight: 4-6 parts of the prepared water reducer mother liquor; 4-6 parts of water-reducing or slump-retaining polycarboxylic mother liquor; 70-80 parts of water; 2-3 parts of a retarding component; 3-5 parts of a water retention component; 0.05-0.1 part of air-entraining defoaming component.
Further, the preparation of the water reducing agent comprises the following raw materials in parts by weight: 5 parts of the prepared water reducing agent mother liquor; 5 parts of water-reducing or slump-retaining polycarboxylic mother liquor; 75 parts of water; 2.5 parts of a retarding component; 4 parts of a water retention component; 0.07 part of air entraining defoaming component.
Further, the retarding component is sodium gluconate and white sugar.
Further, the water-retaining component was a 0.4% cellulose dilution.
Further, the air-entraining defoaming component comprises ZY-99 air-entraining agent and DF-210 defoaming agent.
The preparation method of the polycarboxylic acid water reducer for accelerating the initial reaction speed of the concrete, provided by the invention, comprises the following steps:
b1, preparing raw materials for preparing the polycarboxylate superplasticizer for accelerating the initial reaction speed of the concrete according to the mixture ratio;
b2, putting the prepared water, retarding components, water retention components and air entraining and defoaming components into a stirring tank and uniformly stirring;
b3, injecting the prepared water-reducing or slump-retaining type polycarboxylic mother liquor and the prepared polycarboxylic mother liquor for accelerating the initial reaction speed of the concrete into a stirring tank, and uniformly stirring to obtain a mixed material;
and B4, filtering the mixed material obtained in the step B3 by using a filter screen to obtain the polycarboxylic acid water reducing agent for accelerating the initial reaction speed of the concrete.
Furthermore, the mixing amount of the water reducing agent is 1.0-2.0% of the weight of cementing materials such as cement when in use.
The reaction mechanism and the action mechanism of the invention are as follows:
free radicals are generated through a redox initiation system, the polymerization reaction is initiated under the synergistic action of a catalyst, a chain transfer agent and the like, and functional groups on the main chain and the long side chain provide water reduction and slump retention and accelerate the cement hydration rate through the rapid adsorption dispersion and steric hindrance effects, so that the concrete reaction rate is improved; the equation for the reaction is shown below:
based on the technical scheme, the embodiment of the invention can at least produce the following technical effects:
(1) according to the mother liquor of the polycarboxylate superplasticizer and the preparation method thereof, as well as the polycarboxylate superplasticizer and the preparation method thereof, the optimized stirring, dripping and curing time is mainly adopted, so that the production process is optimized, the synthesis process time is shortened, the production can be completed from the original 7-8 hours to the current 3-4 hours, the labor cost is greatly saved, and the synthesis time is increased;
(2) the invention provides a polycarboxylate water reducer mother liquor and a preparation method thereof, and a polycarboxylate water reducer and a preparation method thereof, wherein new unsaturated acid and catalyst are introduced into the polycarboxylate water reducer,
free radicals generated by a redox initiation system initiate the polymerization reaction under the synergistic action of a catalyst, a chain transfer agent and the like, and functional groups of a main chain and a long side chain provide water reduction and slump retention and accelerate the hydration rate of cement through the rapid adsorption dispersion and steric hindrance effects so as to improve the reaction rate of concrete, thereby shortening the machine-out time of the concrete by 40-75s and greatly improving the production efficiency;
(3) according to the polycarboxylate superplasticizer mother liquor and the preparation method thereof, and the polycarboxylate superplasticizer and the preparation method thereof, the newly synthesized polycarboxylate superplasticizer is endowed with high dispersibility and retentivity in concrete by introducing the allyl micromolecule polyether monomer and a new synthesis process; thereby effectively preventing the problems of the post-arranged bleeding and segregation, poor workability and the like of the concrete.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the technical solutions of the present invention will be described in detail below. It is to be understood that the described embodiments are merely exemplary of the invention, and not restrictive of the full scope of the invention. All other embodiments, which can be derived by a person skilled in the art from the examples given herein without any inventive step, are within the scope of the present invention.
Description of raw materials:
allyl polyoxyethylene ether: molecular weight is 1000-;
hydrogen peroxide: the purity is analytical grade, and the concentration is 28-32%;
maleic anhydride: is industrial grade maleic anhydride, and the purity is more than 98 percent;
mercaptopropionic acid: the purity is more than 99 percent;
ferrous sulfate heptahydrate: the purity is analytical grade;
sodium formaldehyde sulfoxylate: the purity is more than 99 percent and is of industrial grade;
acrylic acid: the purity is more than 99 percent in industrial grade;
liquid caustic soda: sodium hydroxide solution with concentration of 30%;
reducing agent: the adopted reducing agent is produced by German Bruggeman company, and the model is E51;
water-reducing polycarboxylic acid mother liquor: the model of the water-reducing polycarboxylic mother liquor produced by Sichuan Xin New Material Co., Ltd is PC 250;
slump-retaining polycarboxylic mother liquor: the model of the slump-retaining polycarboxylic mother liquor of Sichuan Xin New Material Co., Ltd is PC 340.
First, preparation example
Example 1:
preparing a polycarboxylic acid water reducing agent:
(1) preparation of mother liquor
1.1.1 raw materials:
the preparation method of the polycarboxylate superplasticizer mother liquor for accelerating the initial reaction speed of concrete comprises the following raw materials in parts by weight:
20 parts of allyl polyoxyethylene ether; 2 parts of acrylic acid; 3 parts of maleic anhydride; 0.5 part of hydrogen peroxide; 0.15 part of a reducing agent; 0.05 part of ferrous sulfate heptahydrate; 5 parts of 30% sodium hydroxide solution; 0.1 part of mercaptopropionic acid; and 40 parts of water.
1.1.2 preparation method:
the method comprises the following steps:
a1, preparing a polycarboxylic acid water reducer mother liquor raw material for accelerating the initial reaction speed of concrete according to a ratio;
a2, preparation of solution A: preparing prepared acrylic acid and mercaptopropionic acid into solution A by using deionized water;
a3, preparation of solution B: dissolving the prepared reducing agent in deionized water, and stirring and dissolving to prepare a solution B;
a4, adding the rest deionized water into a reaction kettle, adding the prepared allyl polyoxyethylene ether and maleic anhydride under the stirring state, heating to 25 ℃, controlling the constant temperature to be 25 ℃, adding the prepared hydrogen peroxide and ferrous sulfate heptahydrate after the hydrogen peroxide and the ferrous sulfate heptahydrate are completely dissolved, and stirring for 8 minutes at the speed of 60 revolutions per minute;
a5, stabilizing the temperature of the reaction kettle to 25 ℃, simultaneously dripping the solution A and the solution B in a stirring state, and controlling the temperature of the reaction kettle to be 35 ℃ in the dripping process after the dripping is finished within 85 minutes; after the dropwise addition is finished, continuously keeping the temperature in the reaction kettle for 25 minutes to obtain a mixed material;
and A6, after the mixed material obtained in the step A5 is cooled to room temperature, adjusting the pH value to 6.0 by using liquid alkali to obtain the polycarboxylic acid water reducer mother liquor for accelerating the initial reaction speed of the concrete.
(2) Preparation of finished product of polycarboxylic acid water reducing agent
1.2.1 raw materials:
the preparation of the polycarboxylate superplasticizer for accelerating the initial reaction speed of concrete comprises the following raw materials in parts by weight:
70 parts of water, 1.5 parts of sodium gluconate serving as a slow-setting component and 0.5 part of white sugar, 3 parts of 0.4% cellulose diluent serving as a water retention component, 0.04 part of ZY-99 air entraining agent and 0.01 part of DF-210 defoaming agent, 3 parts of polycarboxylic acid mother liquor which is prepared in the step (1) and is used for accelerating the initial reaction speed of the concrete, and 3 parts of slump-retaining polycarboxylic acid mother liquor.
1.2.2 preparation method:
the method comprises the following steps:
b1, preparing raw materials for preparing the polycarboxylate superplasticizer for accelerating the initial reaction speed of the concrete according to the mixture ratio;
b2, putting water, sodium gluconate and white sugar serving as retarding components, 0.4% cellulose diluent serving as a water retention component, ZY-99 air entraining agent and DF-210 defoaming agent into a stirring tank, stirring and dissolving for 15 minutes;
b3, injecting the slump-retaining polycarboxylic acid mother liquor and the polycarboxylic acid mother liquor which is prepared in the step (1) and accelerates the initial reaction speed of the concrete into a stirring tank, and continuously stirring for 15min to obtain a mixed material;
and B4, filtering the mixed material obtained in the step B3 by using a filter screen to obtain the polycarboxylic acid water reducer for accelerating the initial reaction speed of the concrete.
Example 2:
preparing a polycarboxylic acid water reducing agent:
(1) preparation of mother liquor
2.1.1 raw materials:
the preparation method of the polycarboxylate superplasticizer mother liquor for accelerating the initial reaction speed of concrete comprises the following raw materials in parts by weight:
40 parts of allyl polyoxyethylene ether; 5 parts of acrylic acid; 5 parts of maleic anhydride; 1.0 part of hydrogen peroxide; 0.25 part of a reducing agent; 0.1 part of ferrous sulfate heptahydrate; 10 parts of 30% sodium hydroxide solution; 0.3 part of mercaptopropionic acid; 50 parts of water.
2.1.2 preparation method:
the method comprises the following steps:
a1, preparing a polycarboxylic acid water reducer mother liquor raw material for accelerating the initial reaction speed of concrete according to a ratio;
a2, preparation of solution A: preparing prepared acrylic acid and mercaptopropionic acid into solution A by using deionized water;
a3, preparation of solution B: dissolving the prepared reducing agent in deionized water, and stirring and dissolving to prepare a solution B;
a4, adding the rest deionized water into a reaction kettle, adding the prepared allyl polyoxyethylene ether and maleic anhydride under the stirring state, heating to 30 ℃, controlling the constant temperature to be 30 ℃, adding the prepared hydrogen peroxide and ferrous sulfate heptahydrate after the hydrogen peroxide and the ferrous sulfate heptahydrate are completely dissolved, and stirring for 14 minutes at the speed of 65 revolutions per minute;
a5, stabilizing the temperature of the reaction kettle to 30 ℃, simultaneously dripping the solution A and the solution B in a stirring state, finishing dripping within 95 minutes, and controlling the temperature of the reaction kettle to be 40 ℃ in the dripping process; after the dropwise addition is finished, continuously keeping the temperature in the reaction kettle for 28 minutes to obtain a mixed material;
and A6, after the mixed material obtained in the step A5 is cooled to room temperature, adjusting the pH value to 7.0 by using liquid alkali to obtain the polycarboxylic acid water reducer mother liquor for accelerating the initial reaction speed of the concrete.
(2) Preparation of finished product of polycarboxylic acid water reducing agent
2.2.1 raw materials:
the preparation of the polycarboxylate superplasticizer for accelerating the initial reaction speed of concrete comprises the following raw materials in parts by weight:
80 parts of water, 2.25 parts of sodium gluconate serving as a slow-setting component and 0.75 part of white sugar, 5 parts of 0.4% cellulose diluent serving as a water retention component, 0.08 part of ZY-99 air entraining agent and 0.02 part of DF-210 defoaming agent, 7 parts of polycarboxylic acid mother liquor which is prepared in the step (1) and is used for accelerating the initial reaction speed of the concrete, and 7 parts of water-reducing polycarboxylic acid mother liquor.
2.2.2 preparation method:
b1, preparing raw materials for preparing the polycarboxylate superplasticizer for accelerating the initial reaction speed of the concrete according to the mixture ratio;
b2, putting water, sodium gluconate and white sugar serving as retarding components, 0.4% cellulose diluent serving as a water retention component, ZY-99 air entraining agent and DF-210 defoaming agent into a stirring tank, stirring and dissolving for 20 minutes;
b3, injecting the water-reducing polycarboxylic mother liquor and the polycarboxylic mother liquor which is prepared in the step (1) and accelerates the initial reaction speed of the concrete into a stirring tank, and continuously stirring for 20min to obtain a mixed material;
and B4, filtering the mixed material obtained in the step B3 by using a filter screen to obtain the polycarboxylic acid water reducer for accelerating the initial reaction speed of the concrete.
Example 3:
preparing a polycarboxylic acid water reducing agent:
(1) preparation of mother liquor
3.1.1 raw materials:
the preparation method of the polycarboxylate superplasticizer mother liquor for accelerating the initial reaction speed of concrete comprises the following raw materials in parts by weight:
25 parts of allyl polyoxyethylene ether; 3 parts of acrylic acid; 3 parts of maleic anhydride; 0.6 part of hydrogen peroxide; 0.18 part of reducing agent; 0.06 part of ferrous sulfate heptahydrate; 6 parts of 30% sodium hydroxide solution; 0.15 part of mercaptopropionic acid; 42 parts of water.
3.1.2 preparation method:
a1, preparing a polycarboxylic acid water reducer mother liquor raw material for accelerating the initial reaction speed of concrete according to a ratio;
a2, preparation of solution A: preparing prepared acrylic acid and mercaptopropionic acid into solution A by using deionized water;
a3, preparation of solution B: dissolving the prepared reducing agent in deionized water, and stirring and dissolving to prepare a solution B;
a4, adding the rest deionized water into a reaction kettle, adding the prepared allyl polyoxyethylene ether and maleic anhydride under the stirring state, heating to 26 ℃, controlling the constant temperature to be 26 ℃, adding the prepared hydrogen peroxide and ferrous sulfate heptahydrate after the hydrogen peroxide and the ferrous sulfate heptahydrate are completely dissolved, and stirring for 12 minutes at the speed of 62 revolutions per minute;
a5, stabilizing the temperature of the reaction kettle to 30 ℃, simultaneously dripping the solution A and the solution B in a stirring state, finishing dripping within 95 minutes, and controlling the temperature of the reaction kettle to be 36 ℃ in the dripping process; after the dropwise addition is finished, continuously keeping the temperature in the reaction kettle for 35 minutes to obtain a mixed material;
and A6, after the mixed material obtained in the step A5 is cooled to room temperature, adjusting the pH value to 6.2 by using liquid alkali to obtain the polycarboxylic acid water reducer mother liquor capable of accelerating the initial reaction speed of concrete.
(2) Preparation of finished product of polycarboxylic acid water reducing agent
3.2.1 raw materials:
the preparation of the polycarboxylate superplasticizer for accelerating the initial reaction speed of concrete comprises the following raw materials in parts by weight:
72 parts of water, 1.65 parts of sodium gluconate serving as a slow-setting component and 0.55 part of white sugar, 3.5 parts of 0.4% cellulose diluent serving as a water retention component, 0.05 part of ZY-99 air entraining agent and 0.01 part of DF-210 defoaming agent, 4 parts of polycarboxylic acid mother liquor which is prepared in the step (1) and is used for accelerating the initial reaction speed of the concrete, and 4 parts of slump-retaining polycarboxylic acid mother liquor.
3.2.2 preparation method:
b1, preparing raw materials for preparing the polycarboxylate superplasticizer for accelerating the initial reaction speed of the concrete according to the mixture ratio;
b2, putting water, sodium gluconate and white sugar serving as retarding components, 0.4% cellulose diluent serving as a water retention component, ZY-99 air entraining agent and DF-210 defoaming agent into a stirring tank, stirring and dissolving for 16 minutes;
b3, injecting the water-reducing polycarboxylic mother liquor and the polycarboxylic mother liquor which is prepared in the step (1) and accelerates the initial reaction speed of the concrete into a stirring tank, and continuously stirring for 16min to obtain a mixed material;
and B4, filtering the mixed material obtained in the step B3 by using a filter screen to obtain the polycarboxylic acid water reducer for accelerating the initial reaction speed of the concrete.
Example 4:
preparing a polycarboxylic acid water reducing agent:
(1) preparation of mother liquor
4.1.1 raw materials:
the preparation method of the polycarboxylate superplasticizer mother liquor for accelerating the initial reaction speed of concrete comprises the following raw materials in parts by weight:
35 parts of allyl polyoxyethylene ether; 4 parts of acrylic acid; 4 parts of maleic anhydride; 0.8 part of hydrogen peroxide; 0.22 part of reducing agent; 0.08 part of ferrous sulfate heptahydrate; 8 parts of 30% sodium hydroxide solution; 0.25 part of mercaptopropionic acid; 48 parts of water.
4.1.2 preparation method:
the method comprises the following steps:
a1, preparing a polycarboxylic acid water reducer mother liquor raw material for accelerating the initial reaction speed of concrete according to a ratio;
a2, preparation of solution A: preparing prepared acrylic acid and mercaptopropionic acid into solution A by using deionized water;
a3, preparation of solution B: dissolving the prepared reducing agent in deionized water, and stirring and dissolving to prepare a solution B;
a4, adding the rest deionized water into a reaction kettle, adding the prepared allyl polyoxyethylene ether and maleic anhydride under the stirring state, heating to 28 ℃, controlling the constant temperature to be 28 ℃, adding the prepared hydrogen peroxide and ferrous sulfate heptahydrate after the hydrogen peroxide and the ferrous sulfate heptahydrate are completely dissolved, and stirring for 13 minutes at the speed of 64 revolutions per minute;
a5, stabilizing the temperature of the reaction kettle to 30 ℃, simultaneously dripping the solution A and the solution B in a stirring state, finishing dripping within 95 minutes, and controlling the temperature of the reaction kettle to be 38 ℃ in the dripping process; after the dropwise addition is finished, continuously keeping the temperature in the reaction kettle for 35 minutes to obtain a mixed material;
and A6, after the mixed material obtained in the step A5 is cooled to room temperature, adjusting the pH value to 6.8 by using liquid alkali to obtain the polycarboxylic acid water reducer mother liquor capable of accelerating the initial reaction speed of concrete.
(2) Preparation of finished product of polycarboxylic acid water reducing agent
4.2.1 raw materials:
the preparation of the polycarboxylate superplasticizer for accelerating the initial reaction speed of concrete comprises the following raw materials in parts by weight:
78 parts of water, 2.1 parts of sodium gluconate serving as a slow-setting component and 0.7 part of white sugar, 4.5 parts of 0.4% cellulose diluent serving as a water retention component, 0.06 part of ZY-99 air entraining agent and 0.02 part of DF-210 defoaming agent, 6 parts of polycarboxylic acid mother liquor which is prepared in the step (1) and is used for accelerating the initial reaction speed of the concrete, and 6 parts of water-reducing polycarboxylic acid mother liquor.
4.2.2 preparation method:
the method comprises the following steps:
b1, preparing raw materials for preparing the polycarboxylate superplasticizer for accelerating the initial reaction speed of the concrete according to the mixture ratio;
b2, putting water, sodium gluconate and white sugar serving as retarding components, 0.4% cellulose diluent serving as a water retention component, ZY-99 air entraining agent and DF-210 defoaming agent into a stirring tank, stirring and dissolving for 18 minutes;
b3, injecting the water-reducing polycarboxylic mother liquor and the polycarboxylic mother liquor which is prepared in the step (1) and accelerates the initial reaction speed of the concrete into a stirring tank, and continuously stirring for 18min to obtain a mixed material;
and B4, filtering the mixed material obtained in the step B3 by using a filter screen to obtain the polycarboxylic acid water reducer for accelerating the initial reaction speed of the concrete.
Example 5:
preparing a polycarboxylic acid water reducing agent:
(1) preparation of mother liquor
5.1.1 raw materials:
the preparation of the polycarboxylate superplasticizer mother liquor for accelerating the initial reaction speed of concrete requires the following raw materials:
30 parts of allyl polyoxyethylene ether; 3 parts of acrylic acid; 4 parts of maleic anhydride; 0.7 part of hydrogen peroxide; 0.2 part of a reducing agent; 0.07 part of ferrous sulfate heptahydrate; 7 parts of 30% sodium hydroxide solution; 0.2 part of mercaptopropionic acid; and 45 parts of water.
5.1.2 preparation method:
the method comprises the following steps:
a1, preparing a polycarboxylic acid water reducer mother liquor raw material for accelerating the initial reaction speed of concrete according to a ratio;
a2, preparation of solution A: preparing prepared acrylic acid and mercaptopropionic acid into solution A by using deionized water;
a3, preparation of solution B: dissolving the prepared reducing agent in deionized water, and stirring and dissolving to prepare a solution B;
a4, adding the rest deionized water into a reaction kettle, adding the prepared allyl polyoxyethylene ether and maleic anhydride under the stirring state, heating to 25 ℃, controlling the constant temperature to be 25 ℃, adding the prepared hydrogen peroxide and ferrous sulfate heptahydrate after the hydrogen peroxide and the ferrous sulfate heptahydrate are completely dissolved, and stirring for 10 minutes at the speed of 63 revolutions per minute;
a5, stabilizing the temperature of the reaction kettle to 25 ℃, simultaneously dripping the solution A and the solution B in a stirring state, and controlling the temperature of the reaction kettle to be 38 ℃ in the dripping process after finishing dripping for 90 minutes; after the dropwise addition is finished, continuously keeping the temperature in the reaction kettle for 25 minutes to obtain a mixed material;
and A6, after the mixed material obtained in the step A5 is cooled to room temperature, adjusting the pH value to 6.5 by using liquid alkali to obtain the polycarboxylic acid water reducer mother liquor for accelerating the initial reaction speed of the concrete.
(2) Preparation of finished product of polycarboxylic acid water reducing agent
5.2.1 raw materials:
the preparation of the polycarboxylate superplasticizer for accelerating the initial reaction speed of concrete comprises the following raw materials in parts by weight:
75 parts of water, 1.87 parts of sodium gluconate and 0.63 part of white sugar which are used as retarding components, 4 parts of 0.4 percent cellulose diluent which is used as a water retention component, 0.06 part of ZY-99 air entraining agent and 0.01 part of DF-210 defoaming agent, 5 parts of polycarboxylic acid mother liquor which is prepared in the step (1) and is used for accelerating the initial reaction speed of the concrete, and 5 parts of slump-retaining polycarboxylic acid mother liquor.
5.2.2 preparation method:
the method comprises the following steps:
b1, preparing raw materials for preparing the polycarboxylate superplasticizer for accelerating the initial reaction speed of the concrete according to the mixture ratio;
b2, putting water, sodium gluconate and white sugar serving as retarding components, 0.4% cellulose diluent serving as a water retention component, ZY-99 air entraining agent and DF-210 defoaming agent into a stirring tank, stirring and dissolving for 15 minutes;
b3, injecting the water-reducing polycarboxylic mother liquor and the polycarboxylic mother liquor which is prepared in the step (1) and accelerates the initial reaction speed of the concrete into a stirring tank, and continuously stirring for 15min to obtain a mixed material;
and B4, filtering the mixed material obtained in the step B3 by using a filter screen to obtain the polycarboxylic acid water reducer for accelerating the initial reaction speed of the concrete.
Second, Experimental example
(1) The concrete is prepared according to the proportioning mode of c30
According to the weight portion, 955 parts of macadam, 955 parts of sand, 250 parts of cement and 60 parts of fly ash; the cement is 42.5R common silicate cement in a Desheng cement plant to obtain a concrete primary product, and then the obtained concrete primary product is divided into six parts according to weight average;
(2) taking five parts of the concrete primary product obtained in the step (1), adding the polycarboxylic acid water reducing agent which is prepared in the embodiment 1-5 and is used for accelerating the initial reaction speed of the concrete, and adding the rest part of the concrete primary product into a normal product (Xin leading building materials, Limited liability company, PC150H) on the market, wherein the amount of the added water reducing agent in each part is 1.5 percent of the weight of the concrete primary product in each part; obtaining a concrete experimental product;
(3) and (3) comparing the machine-out time, the concrete slump/fluidity, the concrete workability and the concrete strength of the concrete experiment product obtained in the step (2).
Compared with the application test of the normal product concrete through five groups of embodiments, the product of the invention is obviously improved by 40-75s when being taken out of the machine, the concrete strength is slightly improved, the water reducing rate and the slump retaining property are basically equivalent, the normal product basically shows the phenomenon of backward expansion in the later period, the concrete retentivity of the product of the invention is good, and the five groups of test conclusions are basically consistent; after the product is added in a concrete workability contrast test, the concrete state is obviously improved, the segregation and bleeding phenomena are avoided, the concrete is mixed to be soft, the wrapping performance is good, and the slurry is rich; the comparison results (standard of slump/fluidity is GB8076-2008 concrete admixture, standard of strength is GB/T50081-2002 common concrete mechanical property test method, and workability is mainly judged by empirical observation) are shown in the following table 1:
TABLE 1 comparison of concrete Performance Using the product of the invention with the product of the invention without it
The above description is only for the specific embodiment of the present invention, but the scope of the present invention is not limited thereto, and any changes or substitutions that can be easily conceived by those skilled in the art within the technical scope of the present invention are included in the scope of the present invention.
Claims (10)
1. A polycarboxylate water reducing agent mother liquor for accelerating the initial reaction speed of concrete is characterized in that: the preparation of the mother solution comprises the following raw materials in parts by weight: 20-40 parts of ether macromonomer; 5-10 parts of unsaturated acid; 0.5-1.0 part of oxidant; 0.15-0.25 part of reducing agent; 0.05-0.1 part of catalyst; 0.1-0.3 part of chain transfer agent; 5-10 parts of liquid caustic soda; 40-50 parts of deionized water.
2. The polycarboxylate superplasticizer mother liquor capable of accelerating the initial reaction speed of concrete as claimed in claim 1, wherein: the weight parts of the raw materials are respectively as follows: 25-35 parts of ether macromonomer; 6-8 parts of unsaturated acid; 0.6-0.8 part of oxidant; 0.18-0.22 part of reducing agent; 0.06-0.08 part of catalyst; 0.15-0.25 part of chain transfer agent; 6-8 parts of liquid caustic soda; 42-48 parts of deionized water.
3. The polycarboxylate superplasticizer mother liquor capable of accelerating the initial reaction speed of concrete as claimed in claim 2, wherein: the weight parts of the raw materials are respectively as follows: 30 parts of ether macromonomer; 7 parts of unsaturated acid; 0.7 part of an oxidizing agent; 0.2 part of a reducing agent; 0.07 part of a catalyst; 0.2 part of chain transfer agent; 7 parts of liquid caustic soda; 45 parts of deionized water.
4. The polycarboxylate superplasticizer mother liquor capable of accelerating the initial reaction speed of concrete as claimed in any one of claims 1 to 3, wherein:
the ether macromonomer is allyl polyoxyethylene ether;
the unsaturated acid is acrylic acid and maleic anhydride;
the oxidant is hydrogen peroxide;
the chain transfer agent is mercaptopropionic acid or mercaptoacetic acid;
the catalyst is ferrous sulfate heptahydrate;
the liquid alkali is sodium hydroxide solution.
5. The method for preparing the polycarboxylate superplasticizer mother liquor capable of accelerating the initial reaction speed of concrete according to any one of claims 1 to 4, which is characterized by comprising the following steps: the method comprises the following steps:
a1, preparing a polycarboxylic acid water reducer mother liquor raw material for accelerating the initial reaction speed of concrete according to a ratio;
a2, preparation of solution A: preparing prepared acrylic acid and mercaptopropionic acid into solution A by using deionized water;
a3, preparation of solution B: dissolving the prepared reducing agent in deionized water, and stirring and dissolving to prepare a solution B;
a4, adding the rest deionized water into a reaction kettle, adding the prepared allyl polyoxyethylene ether and maleic anhydride under the stirring state, heating to 25-30 ℃, controlling the constant temperature to be 25-30 ℃, adding the prepared hydrogen peroxide and ferrous sulfate heptahydrate after the hydrogen peroxide and the ferrous sulfate heptahydrate are completely dissolved, and uniformly stirring;
a5, stabilizing the temperature of the reaction kettle to 25-30 ℃, simultaneously dripping the solution A and the solution B in a stirring state, and controlling the temperature of the reaction kettle to be below 40 ℃ in the dripping process after finishing dripping within 85-95 minutes; after the dropwise addition is finished, continuously preserving the heat in the reaction kettle for 25-35 minutes to obtain a mixed material;
and A6, after the mixed material obtained in the step A5 is cooled to room temperature, adjusting the pH value to 6.0-7.0 by using liquid alkali to obtain the polycarboxylate superplasticizer mother liquor for accelerating the initial reaction speed of the concrete.
6. A polycarboxylate water reducing agent for accelerating the initial reaction speed of concrete is characterized in that: the water reducing agent is prepared from the following components in parts by weight: 3-7 parts of a water reducer mother liquor prepared in claim 5; 3-7 parts of water-reducing or slump-retaining polycarboxylic mother liquor; 70-80 parts of water; 2-3 parts of a retarding component; 3-5 parts of a water retention component; 0.05-0.1 part of air-entraining defoaming component.
7. The polycarboxylate superplasticizer mother liquor capable of accelerating the initial reaction speed of concrete as claimed in claim 6, wherein: the weight parts of each component are respectively as follows: 4-6 parts of a water reducer mother liquor prepared in the method of claim 5; 4-6 parts of water-reducing or slump-retaining polycarboxylic mother liquor; 72-78 parts of water; 2.2-2.8 parts of a retarding component; 3.5-4.5 parts of a water retention component; 0.06-0.08 part of air-entraining defoaming component.
8. The polycarboxylic acid water reducer for accelerating the initial reaction speed of concrete according to claim 7, which is characterized in that: the weight parts of each component are respectively as follows: 5 parts of a water reducer mother liquor prepared in the method of claim 5; 5 parts of water-reducing or slump-retaining polycarboxylic mother liquor; 75 parts of water; 2.5 parts of a retarding component; 4 parts of a water retention component; 0.07 part of air entraining defoaming component.
9. The polycarboxylic acid water reducer for accelerating the initial reaction speed of concrete according to any one of claims 6 to 8, which is characterized in that: the retarding component is sodium gluconate and white sugar; the water-retaining component is 0.4% of cellulose diluent; the air-entraining and defoaming components comprise ZY-99 air-entraining agent and DF-210 defoaming agent.
10. The method for preparing the polycarboxylic acid water reducer for accelerating the initial reaction speed of concrete according to any one of claims 6 to 9, which is characterized in that: the method comprises the following steps:
b1, preparing raw materials for preparing the polycarboxylate superplasticizer for accelerating the initial reaction speed of the concrete according to the mixture ratio;
b2, putting the prepared water, retarding components, water retention components and air entraining and defoaming components into a stirring tank and uniformly stirring;
b3, injecting the prepared water-reducing or slump-retaining polycarboxylic acid mother liquor and the water reducer mother liquor prepared in the claim 5 into a stirring tank, and uniformly stirring to obtain a mixed material;
and B4, filtering the mixed material obtained in the step B3 by using a filter screen to obtain the polycarboxylic acid water reducer for accelerating the initial reaction speed of the concrete.
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