CN112028533A - Early-strength viscosity-reduction type polycarboxylate superplasticizer and preparation method thereof - Google Patents

Early-strength viscosity-reduction type polycarboxylate superplasticizer and preparation method thereof Download PDF

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CN112028533A
CN112028533A CN202010977563.1A CN202010977563A CN112028533A CN 112028533 A CN112028533 A CN 112028533A CN 202010977563 A CN202010977563 A CN 202010977563A CN 112028533 A CN112028533 A CN 112028533A
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dropping liquid
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宋欣
倪涛
汪咏梅
刘昭洋
王进春
刘翠芬
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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
    • C04B40/00—Processes, in general, for influencing or modifying the properties of mortars, concrete or artificial stone compositions, e.g. their setting or hardening ability
    • C04B40/0028—Aspects relating to the mixing step of the mortar preparation
    • C04B40/0039—Premixtures of ingredients
    • C04B40/0046—Premixtures of ingredients characterised by their processing, e.g. sequence of mixing the ingredients when preparing the premixtures
    • C—CHEMISTRY; METALLURGY
    • 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
    • C04B24/2641—Polyacrylates; Polymethacrylates
    • C04B24/2647—Polyacrylates; Polymethacrylates containing polyether side chains
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F283/00—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G
    • C08F283/06—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G on to polyethers, polyoxymethylenes or polyacetals
    • C08F283/065—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G on to polyethers, polyoxymethylenes or polyacetals on to unsaturated polyethers, polyoxymethylenes or polyacetals
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2103/00—Function or property of ingredients for mortars, concrete or artificial stone
    • C04B2103/30—Water reducers, plasticisers, air-entrainers, flow improvers
    • C04B2103/302—Water reducers

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  • Structural Engineering (AREA)
  • Health & Medical Sciences (AREA)
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  • Polymers & Plastics (AREA)
  • Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)

Abstract

An early-strength viscosity-reduction type polycarboxylate superplasticizer and a preparation method thereof are disclosed, wherein the early-strength viscosity-reduction type polycarboxylate superplasticizer is prepared from the following raw materials: 90-100 parts of polyether monomer, 1-10 parts of inorganic early strength component A, 1-5 parts of dispersing agent, 100 parts of water, 1-10 parts of inorganic early strength component B, and dropping liquid X1Dropping liquid X20.5-4.0 parts of initiator, namely hydrogen peroxide. The inorganic early strength component A is one or more of calcium nitrate, calcium formate, calcium bicarbonate, calcium chloride and calcium acetate, the inorganic early strength component B is one or more of sodium silicate, potassium silicate, lithium silicate and magnesium fluosilicate, and the liquid X is dripped1The preparation method comprises dissolving thioglycollic acid and sodium formaldehyde sulfoxylate in deionized water to obtain dropping solution X1Dropping liquid X2The preparation method is that acrylic acid is dissolved in deionized water to obtain dropping liquid X2. The invention also provides a preparation method of the early-strength viscosity-reduction type polycarboxylate superplasticizer. By introducing the inorganic early-strength component and the polyether monomer, the water reducer has the effects of early strength and viscosity reduction.

Description

Early-strength viscosity-reduction type polycarboxylate superplasticizer and preparation method thereof
Technical Field
The invention relates to a polycarboxylate superplasticizer, in particular to an early-strength viscosity-reduction polycarboxylate superplasticizer. The invention also relates to a preparation method of the early-strength viscosity-reduction type polycarboxylate superplasticizer.
Background
In recent years, large-scale construction projects in China are continuously eager for using precast concrete. Precast concrete is also required to have a certain early strength development rate to improve the turnover rate of the formwork or to be suitable for use in a low temperature environment, extending its production cycle to a cold season. The high-strength concrete pipe pile is a product which is developed rapidly in a short period of time and has a wide application range, has the advantages of high strength, strong bearing capacity, convenience in application and the like, and is applied to many fields. For the production, it is desirable to reduce some steam-curing steps to achieve zero energy consumption. At present, the early strength type polycarboxylate superplasticizer generally adopts a superplasticizer with longer side chain and shorter main chain, so that the shape of molecules is changed from comb type to inverted T type, and the length of the side chain exceeds the length of the main chain. However, since the water-gel ratio of high-strength concrete is low, the viscosity of concrete is high, and the viscosity of concrete is high due to the long side chain of the common early-strength water reducing agent. However, the side chain of the general viscosity reduction type water reducing agent is short, so that the effect of early strength cannot be achieved, and even concrete retardation may be caused.
The inventors searched the following related patent documents: CN109749020A discloses an alkyl-containing early-strength viscosity-reduction type polycarboxylate superplasticizer and a preparation method thereof, wherein the components and functional groups of the early-strength viscosity-reduction type polycarboxylate superplasticizer are synergistic, compared with the early-strength polycarboxylate superplasticizer synthesized by the prior art, the early-strength viscosity-reduction type polycarboxylate superplasticizer has superior early-strength and viscosity-reduction effects, and the water reduction rate is not influenced, and meanwhile, a large amount of hydrophobic alkyl is introduced into a PEG side chain, so that the HLB value is reduced, the surface activity effect is enhanced, and the polycarboxylate superplasticizer has good shrinkage reduction performance.
The technology can achieve good early strength and viscosity reduction effects on how to make the early strength viscosity reduction type polycarboxylate superplasticizer, and a specific guidance scheme is not given.
Disclosure of Invention
The invention aims to solve the technical problem of providing an early-strength viscosity-reduction type polycarboxylate superplasticizer which has good early-strength and viscosity-reduction effects.
Therefore, the invention also aims to solve another technical problem of providing a preparation method of the early-strength viscosity-reduction type polycarboxylate superplasticizer.
In order to solve the technical problems, the technical scheme adopted by the invention is as follows:
the technical scheme of the early-strength viscosity-reduction type polycarboxylate superplasticizer is that the early-strength viscosity-reduction type polycarboxylate superplasticizer is prepared from the following raw materials in parts by weight: 90-100 parts of polyether monomer (polyether macromonomer), 1-10 parts of inorganic early strength component A, 1-5 parts of dispersing agent and 100 parts of water (not including dropping liquid X)1Dropping liquid X2Water), 1-10 parts of inorganic early strength component B, and dropping liquid X1Dropping liquid X20.5-4.0 parts of initiator, namely hydrogen peroxide.
The polyether monomer is methyl allyl alcohol polyoxyethylene ether, and the molecular formula is as follows:
CH2＝C(CH3)CH2O(CH2CH2O)nH
the early strength inorganic component A is one or a mixture of more of calcium nitrate, calcium formate, calcium bicarbonate, calcium chloride and calcium acetate, the early strength inorganic component B is one or a mixture of more of sodium silicate, potassium silicate, lithium silicate and magnesium fluosilicate, and the dispersing agent is one or a mixture of more of fatty alcohol-polyoxyethylene ether sodium sulfate, fatty alcohol-polyoxyethylene ether ammonium sulfate, sodium dodecyl sulfate and sodium dodecyl benzene sulfonate; the dropping liquid X1The preparation method comprises the steps of dissolving 0.1-1.0 part of thioglycolic acid and 0.1-1.0 part of sodium formaldehyde sulfoxylate in 30 parts of deionized water to obtain a dropping liquid X1Dropping liquid X2The preparation method comprises the step of dissolving 5-20 parts of acrylic acid in 30 parts of deionized water to obtain dropping liquid X2。
Preparation of early-strength viscosity-reduction type polycarboxylate superplasticizerThe preparation method comprises the following process steps: firstly, according to the weight parts, adding 90-100 parts of polyether monomer, 1-10 parts of inorganic early strength component A, 1-5 parts of dispersing agent and 50 parts of water into a reaction kettle, dissolving 1-10 parts of inorganic early strength component B in (another) 50 parts of water, adding into the reaction kettle, stirring for reaction for 0.5-1 h, and performing ultrasonic dispersion; ② then preparing dropping liquid X1Dropping liquid X2(ii) a Thirdly, raising the temperature of the reaction kettle to 35-60 ℃, adding 0.5-4.0 parts of initiator into the reaction kettle, stirring for 1-2 min, and then beginning to simultaneously dropwise add dropping liquid X1Dropping liquid X2And the dripping time is 1-2 h, and after the dripping is finished, the heat preservation and stirring are carried out for 0.5-1 h, so that the finally obtained product is the early-strength viscosity reduction type polycarboxylate superplasticizer.
In the above technical solution, a preferable technical solution may be: the weight average molecular weight of the polyether monomer is 800-1500. The rotating speed of stirring in the step (i) is 300-500 rpm, and the rotating speed of stirring in the step (iii) is 100-200 rpm. The time of ultrasonic dispersion in the step I is 0.5-1.5 h.
Among the above-described technical solutions, the following embodiments 1 to 5 are also preferable.
Referring to the comparative test later in the specification, compared with the commercial early-strength water reducing agent, the early-strength viscosity-reducing polycarboxylate water reducing agent provided by the invention has the advantages that the T500 flow rate is obviously higher, the viscosity reducing effect is achieved, and the strength is not reduced in 12h, 7d and 28 d. Compared with the commercially available viscosity reduction type water reducer, the early-strength viscosity reduction type polycarboxylate water reducer disclosed by the invention has the advantages that the strength is obviously improved in 12h, 7d and 28d, and the T500 flow rate is not reduced. According to the invention, by introducing the inorganic early-strength component and the polyether monomer, the water reducer has the effects of early strength and viscosity reduction. The early-strength viscosity-reduction type polycarboxylate superplasticizer prepared by the invention has good early-strength and viscosity-reduction effects and also has a good water-reduction effect. The method is applied to the precast concrete, promotes the early strength development of the concrete, shortens the turnover period of the mould, realizes the steam curing-free and pressure steam-free single-double-free process, and reduces the construction by more than 12 percent.
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 clearly and completely described below with reference to the embodiments. Embodiments 1 to 5 are the early-strength viscosity-reduction type polycarboxylate superplasticizer and the preparation method thereof. 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 embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1: the early-strength viscosity-reduction type polycarboxylate superplasticizer is prepared from the following raw materials in parts by weight: 90 parts of polyether monomer namely methyl allyl alcohol polyoxyethylene ether (molecular weight is 800), 1 part of inorganic early strength component A namely calcium nitrate, 2 parts of dispersing agent namely sodium dodecyl sulfate, 100 parts of water, 1.6 parts of inorganic early strength component B namely a combination of 1.2 parts of magnesium fluosilicate and 0.4 part of sodium silicate, and dripping liquid X1Dropping liquid X22 parts of initiator namely hydrogen peroxide; the preparation method of the early-strength viscosity-reduction type polycarboxylate superplasticizer comprises the following process steps: firstly, adding 90 parts of polyether monomer, 1 part of inorganic early strength component A, 2 parts of dispersing agent and 50 parts of water into a reaction kettle, dissolving 1.2 parts of magnesium fluosilicate and 0.4 part of sodium silicate in 50 parts of water, dropwise adding into the reaction kettle, stirring and reacting for 0.5h at the stirring speed of 300rpm, and ultrasonically dispersing for 0.5 h; ② then preparing dropping liquid X1Dropping liquid X2Dropping liquid X1The preparation method is that 0.7 part of thioglycollic acid and 0.1 part of sodium formaldehyde sulfoxylate are dissolved in 30 parts of deionized water to obtain dropping liquid X1Dropping liquid X2The preparation method is that 6 parts of acrylic acid is dissolved in 30 parts of deionized water to obtain dropping liquid X2(ii) a Thirdly, raising the temperature of the reaction kettle to 35 ℃, adding 2 parts of initiator into the reaction kettle, stirring for 1min, and then beginning to simultaneously dropwise add dropping liquid X1Dropping liquid X2The dripping time is 1.5h, the heat preservation and the stirring are carried out for 0.5h after the dripping is finished, the stirring rotating speed is 100rpm, and the finally obtained product is the early-strength viscosity-reduction type polycarboxylate superplasticizer.
Example 2: the early-strength viscosity-reduction type polycarboxylate superplasticizer is prepared from the following raw materials in parts by weight: 90 parts of polyether monomer, i.e.methylenePropanol polyoxyethylene ether (molecular weight is 1000), 2 parts of inorganic early strength component A, namely calcium bicarbonate, 5 parts of dispersing agent, namely sodium dodecyl sulfate, 100 parts of water, 1 part of inorganic early strength component B, namely a combination of 0.6 part of magnesium fluosilicate and 0.4 part of lithium silicate, and dripping liquid X1Dropping liquid X21.5 parts of initiator namely hydrogen peroxide; the preparation method of the early-strength viscosity-reduction type polycarboxylate superplasticizer comprises the following process steps: firstly, adding 90 parts of polyether monomer, 2 parts of inorganic early strength component A, 5 parts of dispersing agent and 50 parts of water into a reaction kettle, dissolving 0.6 part of magnesium fluosilicate and 0.4 part of lithium silicate in 50 parts of water, dropwise adding into the reaction kettle, stirring and reacting for 1 hour, wherein the stirring speed is 400rpm, and ultrasonically dispersing for 1 hour; ② then preparing dropping liquid X1Dropping liquid X2Dropping liquid X1The preparation method is that 0.9 part of thioglycollic acid and 0.2 part of sodium formaldehyde sulfoxylate are dissolved in 30 parts of deionized water to obtain dropping liquid X1Dropping liquid X2The preparation method is that 10 parts of acrylic acid is dissolved in 30 parts of deionized water to obtain dropping liquid X2(ii) a Thirdly, raising the temperature of the reaction kettle to 45 ℃, adding 1.5 parts of initiator into the reaction kettle, stirring for 1min, and then simultaneously dropwise adding the dropping liquid X1Dropping liquid X2The dripping time is 2h, the mixture is stirred for 1h under the condition of heat preservation after the dripping is finished, the stirring speed is 120rpm, and the finally obtained product is the early-strength viscosity-reduction type polycarboxylate superplasticizer.
Example 3: the early-strength viscosity-reduction type polycarboxylate superplasticizer is prepared from the following raw materials in parts by weight: 90 parts of polyether monomer namely methyl allyl alcohol polyoxyethylene ether (molecular weight is 1200), 5 parts of inorganic early strength component A namely calcium acetate, 5 parts of dispersing agent namely fatty alcohol polyoxyethylene ether sodium sulfate, 100 parts of water, 5 parts of inorganic early strength component B namely potassium silicate, and dropping liquid X1Dropping liquid X23 parts of initiator namely hydrogen peroxide; the preparation method of the early-strength viscosity-reduction type polycarboxylate superplasticizer comprises the following process steps: firstly, according to the weight parts, adding 90 parts of polyether monomer, 5 parts of inorganic early strength component A, 5 parts of dispersing agent and 50 parts of water into a reaction kettle, dissolving 5 parts of inorganic early strength component B in 50 parts of water, adding the solution into the reaction kettle, stirring and reacting for 1 hour, wherein the stirring speed is 500rpm, and ultrasonically dispersing for 1 hour; ② then preparing dropping liquid X1Dropping liquid X2Dropping liquid X1The preparation method is that 0.9 part of thioglycollic acid and 0.3 part of sodium formaldehyde sulfoxylate are dissolved in 30 parts of deionized water to obtain dropping liquid X1Dropping liquid X2The preparation method is that 15 parts of acrylic acid is dissolved in 30 parts of deionized water to obtain dropping liquid X2(ii) a Thirdly, raising the temperature of the reaction kettle to 45 ℃, adding 3 parts of initiator into the reaction kettle, stirring for 1min, and then simultaneously dropwise adding dropping liquid X1Dropping liquid X2The dripping time is 1.5h, the heat preservation and the stirring are carried out for 0.8h after the dripping is finished, the stirring rotating speed is 150rpm, and the finally obtained product is the early-strength viscosity-reduction type polycarboxylate superplasticizer.
Example 4: the early-strength viscosity-reduction type polycarboxylate superplasticizer is prepared from the following raw materials in parts by weight: 90 parts of polyether monomer namely methyl allyl alcohol polyoxyethylene ether (molecular weight is 1500), 10 parts of inorganic early strength component A namely the combination of 4 parts of calcium chloride and 6 parts of calcium acetate, 5 parts of dispersing agent namely the combination of 3 parts of sodium dodecyl benzene sulfonate and 2 parts of fatty alcohol polyoxyethylene ether ammonium sulfate, 100 parts of water, 5.2 parts of inorganic early strength component B namely the combination of 3.2 parts of potassium silicate, 1.5 parts of magnesium fluosilicate and 0.5 part of lithium silicate, and dripping liquid X1Dropping liquid X24 parts of initiator namely hydrogen peroxide; the preparation method of the early-strength viscosity-reduction type polycarboxylate superplasticizer comprises the following process steps: firstly, according to the weight parts, adding 90 parts of polyether monomer, 4 parts of calcium chloride, 6 parts of calcium acetate, 3 parts of sodium dodecyl benzene sulfonate, 2 parts of fatty alcohol-polyoxyethylene ether ammonium sulfate and 50 parts of water into a reaction kettle, dissolving 3.2 parts of potassium silicate, 1.5 parts of magnesium fluosilicate and 0.5 part of lithium silicate in 50 parts of water, adding the mixture into the reaction kettle, stirring and reacting for 0.8h at the stirring speed of 390rpm, and ultrasonically dispersing for 1 h; ② then preparing dropping liquid X1Dropping liquid X2Dropping liquid X1The preparation method is that 0.7 part of thioglycollic acid and 0.5 part of sodium formaldehyde sulfoxylate are dissolved in 30 parts of deionized water to obtain dropping liquid X1Dropping liquid X2The preparation method is that 10 parts of acrylic acid is dissolved in 30 parts of deionized water to obtain dropping liquid X2(ii) a Thirdly, the temperature of the reaction kettle is raised to 50 ℃, 4.0 parts of initiator is added into the reaction kettle, and after stirring for 1min, dropwise adding liquid X simultaneously1Dropping liquid X2Dropwise addition ofThe time is 2h, the mixture is stirred for 1h under the condition of heat preservation after the dripping is finished, the stirring speed is 100rpm, and the finally obtained product is the early-strength viscosity-reduction type polycarboxylate superplasticizer.
Example 5: the early-strength viscosity-reduction type polycarboxylate superplasticizer is prepared from the following raw materials in parts by weight: 90 parts of polyether monomer namely methyl allyl alcohol polyoxyethylene ether (molecular weight is 1000), 4 parts of inorganic early strength component A namely calcium formate, 2 parts of dispersing agent namely fatty alcohol polyoxyethylene ether ammonium sulfate, 100 parts of water, 1.5 parts of inorganic early strength component B namely a combination of 0.8 part of potassium silicate and 0.7 part of sodium silicate, and dropping liquid X1Dropping liquid X23.5 parts of an initiator, namely hydrogen peroxide; the preparation method of the early-strength viscosity-reduction type polycarboxylate superplasticizer comprises the following process steps: firstly, adding 90 parts of polyether monomer, 4 parts of inorganic early strength component A, 2 parts of dispersing agent and 50 parts of water into a reaction kettle, dissolving 0.8 part of potassium silicate and 0.7 part of sodium silicate in 50 parts of water, dropwise adding into the reaction kettle, stirring and reacting for 1 hour, wherein the stirring speed is 450rpm, and ultrasonically dispersing for 0.5 hour; ② then preparing dropping liquid X1Dropping liquid X2Dropping liquid X1The preparation method is that 0.8 part of thioglycollic acid and 0.4 part of sodium formaldehyde sulfoxylate are dissolved in 30 parts of deionized water to obtain dropping liquid X1Dropping liquid X2The preparation method is that 13 parts of acrylic acid is dissolved in 30 parts of deionized water to obtain dropping liquid X2(ii) a Thirdly, the temperature of the reaction kettle is raised to 50 ℃, 3.5 parts of initiator is added into the reaction kettle, and after stirring for 1min, dropwise adding liquid X simultaneously1Dropping liquid X2The dripping time is 1.5h, the heat preservation and the stirring are carried out for 0.5h after the dripping is finished, the stirring rotating speed is 120rpm, and the finally obtained product is the early-strength viscosity reduction type polycarboxylate superplasticizer.
The early-strength viscosity-reduction type polycarboxylate water reducer synthesized in the embodiments 1 to 5 of the invention is compared with commercially available early-strength type water reducers and viscosity-reduction type water reducers. Concrete was prepared according to the formulation shown in Table 1 below, and the slump, the spreading, the t500 and the 12h, and the 7d and 28d strengths of the concrete were measured.
TABLE 1 concrete mix proportion (kg/m)3)
Cement Fly ash Coarse sand Fine sand Stone (stone) Water (W)
432 108 450 198 1034 165
TABLE 2 evaluation results of concrete
Figure BDA0002686316900000061
In Table 2, the commercial early strength water reducer is the mother liquor ESP3511 of the Honghang early strength type polycarboxylate superplasticizer. In table 2, the commercial viscosity-reducing water reducer is the header body viscosity-reducing polycarboxylate superplasticizer mother liquor LVP 4511.
As can be seen from the concrete evaluation data in Table 2, compared with the commercially available early strength type water reducing agent, the early strength viscosity reduction type polycarboxylate superplasticizer has a significantly higher T500 flow rate, and has a viscosity reduction effect, and the strength of the polycarboxylate superplasticizer is not reduced for 12h, 7d and 28 d. Compared with the commercially available viscosity reduction type water reducer, the early-strength viscosity reduction type polycarboxylate superplasticizer has the advantages that the strength of 12h, 7d and 28d is obviously improved, and the T500 flow rate is not reduced. In conclusion, the early-strength viscosity-reducing polycarboxylate superplasticizer has good early-strength and viscosity-reducing effects.
In conclusion, the early-strength viscosity-reducing polycarboxylate superplasticizer prepared by the embodiments of the invention has good early-strength and viscosity-reducing effects, and also has good water-reducing effect. The method is applied to the precast concrete, promotes the early strength development of the concrete, shortens the turnover period of the mould, realizes the steam curing-free and pressure steam-free single-double-free process, and reduces the construction by more than 12 percent.

Claims (10)

1. The early-strength viscosity-reduction type polycarboxylate superplasticizer is characterized by being prepared from the following raw materials in parts by weight: 90-100 parts of polyether monomer, 1-10 parts of inorganic early strength component A, 1-5 parts of dispersing agent, 100 parts of water, 1-10 parts of inorganic early strength component B, and dropping liquid X1Dropping liquid X20.5-4.0 parts of initiator, namely hydrogen peroxide;
the polyether monomer is methyl allyl alcohol polyoxyethylene ether; the early strength inorganic component A is one or a mixture of more of calcium nitrate, calcium formate, calcium bicarbonate, calcium chloride and calcium acetate, the early strength inorganic component B is one or a mixture of more of sodium silicate, potassium silicate, lithium silicate and magnesium fluosilicate, and the dispersing agent is one or a mixture of more of fatty alcohol-polyoxyethylene ether sodium sulfate, fatty alcohol-polyoxyethylene ether ammonium sulfate, sodium dodecyl sulfate and sodium dodecyl benzene sulfonate; the dropping liquid X1The preparation method comprises the steps of dissolving 0.1-1.0 part of thioglycolic acid and 0.1-1.0 part of sodium formaldehyde sulfoxylate in 30 parts of deionized water to obtain a dropping liquid X1Dropping liquid X2The preparation method comprises the step of dissolving 5-20 parts of acrylic acid in 30 parts of deionized water to obtain dropping liquid X2；
The preparation method of the early-strength viscosity-reduction type polycarboxylate superplasticizer comprises the following process steps: firstly, according to the weight parts, adding 90-100 parts of polyether monomer, 1-10 parts of inorganic early strength component A, 1-5 parts of dispersing agent and 50 parts of water into a reaction kettle, dissolving 1-10 parts of inorganic early strength component B into 50 parts of water, dropwise adding into the reaction kettle, stirring for reaction for 0.5-1 h, and performing ultrasonic dispersion; ② then preparing dropping liquid X1Dropping liquidX2(ii) a Thirdly, raising the temperature of the reaction kettle to 35-60 ℃, adding 0.5-4.0 parts of initiator into the reaction kettle, stirring for 1-2 min, and then beginning to simultaneously dropwise add dropping liquid X1Dropping liquid X2And the dripping time is 1-2 h, and after the dripping is finished, the heat preservation and stirring are carried out for 0.5-1 h, so that the finally obtained product is the early-strength viscosity reduction type polycarboxylate superplasticizer.
2. The early strength viscosity reduction type polycarboxylate superplasticizer according to claim 1, wherein the molecular weight of the polyether monomer is 800-1500.
3. The early strength viscosity reduction type polycarboxylate superplasticizer according to claim 1, wherein the stirring speed in the step (i) is 300-500 rpm, and the stirring speed in the step (iii) is 100-200 rpm.
4. The early strength viscosity reduction type polycarboxylate superplasticizer according to claim 1, wherein the time of ultrasonic dispersion in the step (i) is 0.5-1.5 hours.
5. The early strength viscosity reduction type polycarboxylate superplasticizer according to claim 1, characterized by being prepared from the following raw materials in parts by weight: 90 parts of polyether monomer, 1 part of inorganic early strength component A, namely calcium nitrate, 2 parts of dispersing agent, namely sodium dodecyl sulfate, 100 parts of water, 1.6 parts of inorganic early strength component B, namely the combination of 1.2 parts of magnesium fluosilicate and 0.4 part of sodium silicate, and dripping liquid X1Dropping liquid X22 parts of initiator namely hydrogen peroxide; the preparation method of the early-strength viscosity-reduction type polycarboxylate superplasticizer comprises the following process steps: firstly, adding 90 parts of polyether monomer, 1 part of inorganic early strength component A, 2 parts of dispersing agent and 50 parts of water into a reaction kettle, dissolving 1.2 parts of magnesium fluosilicate and 0.4 part of sodium silicate in 50 parts of water, dropwise adding into the reaction kettle, stirring and reacting for 0.5h at the stirring speed of 300rpm, and ultrasonically dispersing for 0.5 h; ② then preparing dropping liquid X1Dropping liquid X2Dropping liquid X1The preparation method is that 0.7 part of thioglycollic acid and 0.1 part of sodium formaldehyde sulfoxylate are dissolved in 30 parts of deionized water to obtain dropping liquid X1Is droppedLiquid feeding X2The preparation method is that 6 parts of acrylic acid is dissolved in 30 parts of deionized water to obtain dropping liquid X2(ii) a Thirdly, raising the temperature of the reaction kettle to 35 ℃, adding 2 parts of initiator into the reaction kettle, stirring for 1min, and then beginning to simultaneously dropwise add dropping liquid X1Dropping liquid X2The dripping time is 1.5h, the heat preservation and the stirring are carried out for 0.5h after the dripping is finished, the stirring rotating speed is 100rpm, and the finally obtained product is the early-strength viscosity-reduction type polycarboxylate superplasticizer.
6. The early strength viscosity reduction type polycarboxylate superplasticizer according to claim 1, characterized by being prepared from the following raw materials in parts by weight: 90 parts of polyether monomer, 2 parts of inorganic early strength component A, namely calcium bicarbonate, 5 parts of dispersant, namely sodium dodecyl sulfate, 100 parts of water, 1 part of inorganic early strength component B, namely the combination of 0.6 part of magnesium fluosilicate and 0.4 part of lithium silicate, and dripping liquid X1Dropping liquid X21.5 parts of initiator namely hydrogen peroxide; the preparation method of the early-strength viscosity-reduction type polycarboxylate superplasticizer comprises the following process steps: firstly, adding 90 parts of polyether monomer, 2 parts of inorganic early strength component A, 5 parts of dispersing agent and 50 parts of water into a reaction kettle, dissolving 0.6 part of magnesium fluosilicate and 0.4 part of lithium silicate in 50 parts of water, dropwise adding into the reaction kettle, stirring and reacting for 1 hour, wherein the stirring speed is 400rpm, and ultrasonically dispersing for 1 hour; ② then preparing dropping liquid X1Dropping liquid X2Dropping liquid X1The preparation method is that 0.9 part of thioglycollic acid and 0.2 part of sodium formaldehyde sulfoxylate are dissolved in 30 parts of deionized water to obtain dropping liquid X1Dropping liquid X2The preparation method is that 10 parts of acrylic acid is dissolved in 30 parts of deionized water to obtain dropping liquid X2(ii) a Thirdly, raising the temperature of the reaction kettle to 45 ℃, adding 1.5 parts of initiator into the reaction kettle, stirring for 1min, and then simultaneously dropwise adding the dropping liquid X1Dropping liquid X2The dripping time is 2h, the mixture is stirred for 1h under the condition of heat preservation after the dripping is finished, the stirring speed is 120rpm, and the finally obtained product is the early-strength viscosity-reduction type polycarboxylate superplasticizer.
7. The early-strength viscosity-reduction type polycarboxylate superplasticizer according to claim 1, characterized by comprising the following components in parts by weightThe raw materials are as follows: 90 parts of polyether monomer, 10 parts of inorganic early strength component A, namely the combination of 4 parts of calcium chloride and 6 parts of calcium acetate, 5 parts of dispersing agent, namely the combination of 3 parts of sodium dodecyl benzene sulfonate and 2 parts of fatty alcohol-polyoxyethylene ether ammonium sulfate, 100 parts of water, 5.2 parts of inorganic early strength component B, namely the combination of 3.2 parts of potassium silicate, 1.5 parts of magnesium fluosilicate and 0.5 part of lithium silicate, and dripping liquid X1Dropping liquid X24 parts of initiator namely hydrogen peroxide; the preparation method of the early-strength viscosity-reduction type polycarboxylate superplasticizer comprises the following process steps: firstly, according to the weight parts, adding 90 parts of polyether monomer, 4 parts of calcium chloride, 6 parts of calcium acetate, 3 parts of sodium dodecyl benzene sulfonate, 2 parts of fatty alcohol-polyoxyethylene ether ammonium sulfate and 50 parts of water into a reaction kettle, dissolving 3.2 parts of potassium silicate, 1.5 parts of magnesium fluosilicate and 0.5 part of lithium silicate in 50 parts of water, adding the mixture into the reaction kettle, stirring and reacting for 0.8h at the stirring speed of 390rpm, and ultrasonically dispersing for 1 h; ② then preparing dropping liquid X1Dropping liquid X2Dropping liquid X1The preparation method is that 0.7 part of thioglycollic acid and 0.5 part of sodium formaldehyde sulfoxylate are dissolved in 30 parts of deionized water to obtain dropping liquid X1Dropping liquid X2The preparation method is that 10 parts of acrylic acid is dissolved in 30 parts of deionized water to obtain dropping liquid X2(ii) a Thirdly, the temperature of the reaction kettle is raised to 50 ℃, 4.0 parts of initiator is added into the reaction kettle, and after stirring for 1min, dropwise adding liquid X simultaneously1Dropping liquid X2The dripping time is 2h, the mixture is stirred for 1h under the condition of heat preservation after the dripping is finished, the stirring speed is 100rpm, and the finally obtained product is the early-strength viscosity-reduction type polycarboxylate superplasticizer.
8. The early strength viscosity reduction type polycarboxylate superplasticizer according to claim 1, characterized by being prepared from the following raw materials in parts by weight: 90 parts of polyether monomer, 4 parts of inorganic early strength component A, namely calcium formate, 2 parts of dispersing agent, namely fatty alcohol-polyoxyethylene ether ammonium sulfate, 100 parts of water, 1.5 parts of inorganic early strength component B, namely the combination of 0.8 part of potassium silicate and 0.7 part of sodium silicate, and dripping liquid X1Dropping liquid X23.5 parts of an initiator, namely hydrogen peroxide; the preparation method of the early-strength viscosity-reduction type polycarboxylate superplasticizer comprises the following process steps: firstly, according to the weight portion, 90 portions of polyether monomer are firstly addedAdding 4 parts of inorganic early strength component A, 2 parts of dispersing agent and 50 parts of water into a reaction kettle, dissolving 0.8 part of potassium silicate and 0.7 part of sodium silicate in 50 parts of water, adding into the reaction kettle, stirring and reacting for 1h, wherein the stirring speed is 450rpm, and performing ultrasonic dispersion for 0.5 h; ② then preparing dropping liquid X1Dropping liquid X2Dropping liquid X1The preparation method is that 0.8 part of thioglycollic acid and 0.4 part of sodium formaldehyde sulfoxylate are dissolved in 30 parts of deionized water to obtain dropping liquid X1Dropping liquid X2The preparation method is that 13 parts of acrylic acid is dissolved in 30 parts of deionized water to obtain dropping liquid X2(ii) a Thirdly, the temperature of the reaction kettle is raised to 50 ℃, 3.5 parts of initiator is added into the reaction kettle, and after stirring for 1min, dropwise adding liquid X simultaneously1Dropping liquid X2The dripping time is 1.5h, the heat preservation and the stirring are carried out for 0.5h after the dripping is finished, the stirring rotating speed is 120rpm, and the finally obtained product is the early-strength viscosity reduction type polycarboxylate superplasticizer.
9. The preparation method of the early-strength viscosity-reduction type polycarboxylate superplasticizer according to claim 1, which is characterized in that the early-strength viscosity-reduction type polycarboxylate superplasticizer is prepared from the following raw materials in parts by weight: 90-100 parts of polyether monomer, 1-10 parts of inorganic early strength component A, 1-5 parts of dispersing agent, 100 parts of water, 1-10 parts of inorganic early strength component B, and dropping liquid X1Dropping liquid X20.5-4.0 parts of initiator, namely hydrogen peroxide;
the polyether monomer is methallyl alcohol polyoxyethylene ether, the inorganic early strength component A is one or a mixture of more of calcium nitrate, calcium formate, calcium bicarbonate, calcium chloride and calcium acetate, the inorganic early strength component B is one or a mixture of more of sodium silicate, potassium silicate, lithium silicate and magnesium fluosilicate, and the dispersing agent is one or a mixture of more of fatty alcohol-polyoxyethylene ether sodium sulfate, fatty alcohol-polyoxyethylene ether ammonium sulfate, sodium dodecyl sulfonate and sodium dodecyl benzene sulfonate; the dropping liquid X1The preparation method comprises the steps of dissolving 0.1-1.0 part of thioglycolic acid and 0.1-1.0 part of sodium formaldehyde sulfoxylate in 30 parts of deionized water to obtain a dropping liquid X1Dropping liquid X2The preparation method comprises the step of dissolving 5-20 parts of acrylic acid in 30 parts of deionized water to obtain dropping liquid X2；
The preparation method of the early-strength viscosity-reduction type polycarboxylate superplasticizer comprises the following process steps: firstly, according to the weight parts, adding 90-100 parts of polyether monomer, 1-10 parts of inorganic early strength component A, 1-5 parts of dispersing agent and 50 parts of water into a reaction kettle, dissolving 1-10 parts of inorganic early strength component B into 50 parts of water, dropwise adding into the reaction kettle, stirring for reaction for 0.5-1 h, and performing ultrasonic dispersion; ② then preparing dropping liquid X1Dropping liquid X2(ii) a Thirdly, raising the temperature of the reaction kettle to 35-60 ℃, adding 0.5-4.0 parts of initiator into the reaction kettle, stirring for 1-2 min, and then beginning to simultaneously dropwise add dropping liquid X1Dropping liquid X2And the dripping time is 1-2 h, and after the dripping is finished, the heat preservation and stirring are carried out for 0.5-1 h, so that the finally obtained product is the early-strength viscosity reduction type polycarboxylate superplasticizer.
10. The preparation method of the early-strength viscosity-reducing polycarboxylate superplasticizer according to claim 9, wherein the molecular weight of the polyether monomer is 500-1500; the stirring speed in the first step is 300-500 rpm, and the stirring speed in the third step is 100-200 rpm; the time of ultrasonic dispersion in the step I is 0.5-1.5 h.
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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113201101A (en) * 2021-05-26 2021-08-03 山西佳维新材料股份有限公司 Viscosity-reducing water reducer and preparation method and application thereof
CN114133164A (en) * 2022-01-29 2022-03-04 唐山市筑业新材料有限公司 Alkali-free chlorine-free non-autoclaved concrete additive for prefabricated part and rapid preparation method thereof

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113201101A (en) * 2021-05-26 2021-08-03 山西佳维新材料股份有限公司 Viscosity-reducing water reducer and preparation method and application thereof
CN114133164A (en) * 2022-01-29 2022-03-04 唐山市筑业新材料有限公司 Alkali-free chlorine-free non-autoclaved concrete additive for prefabricated part and rapid preparation method thereof
CN114133164B (en) * 2022-01-29 2022-05-13 唐山市筑业新材料有限公司 Alkali-free chlorine-free non-autoclaved concrete additive for prefabricated part and rapid preparation method thereof

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