CN105801765A - Preparation method of anti-segregation type polycarboxylic acid water reducer of concrete - Google Patents

Preparation method of anti-segregation type polycarboxylic acid water reducer of concrete Download PDF

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CN105801765A
CN105801765A CN201610115439.8A CN201610115439A CN105801765A CN 105801765 A CN105801765 A CN 105801765A CN 201610115439 A CN201610115439 A CN 201610115439A CN 105801765 A CN105801765 A CN 105801765A
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solution
concrete
reducer
preparation
agent
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吴峰
何年
梁青松
马春城
李浪
杨志飞
舒豆豆
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Sichuan Tong Zhou Chemical Industry Science Co Ltd
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Sichuan Tong Zhou Chemical Industry Science Co Ltd
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    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08FMACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • 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
    • 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
    • C04B24/00Use of organic materials as active ingredients for mortars, concrete or artificial stone, e.g. plasticisers
    • C04B24/24Macromolecular compounds
    • C04B24/26Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
    • C04B24/2688Copolymers containing at least three different monomers
    • C04B24/2694Copolymers containing at least three different monomers containing polyether side chains
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08FMACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F2/00Processes of polymerisation
    • C08F2/04Polymerisation in solution
    • C08F2/10Aqueous solvent
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08FMACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F2/00Processes of polymerisation
    • C08F2/38Polymerisation using regulators, e.g. chain terminating agents, e.g. telomerisation
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08FMACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F4/00Polymerisation catalysts
    • C08F4/40Redox systems
    • 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
    • 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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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Organic Chemistry (AREA)
  • Health & Medical Sciences (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Engineering & Computer Science (AREA)
  • Ceramic Engineering (AREA)
  • Materials Engineering (AREA)
  • Structural Engineering (AREA)
  • Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)

Abstract

The invention discloses a preparation method of an anti-segregation type polycarboxylic acid water reducer of concrete. The preparation method comprises: preparing a solution A, preparing a solution B and generating a product. An aqueous solution free radical polymerization method is adopted in the synthetic process of the polycarboxylic acid water reducer, the method is simple and is low in cost and strong in operability, the synthesized polycarboxylic acid water reducer is colorless viscous liquid, and is large in molecular weight and stable in storage time, and the original characteristics of the polycarboxylic acid water reducer cannot be changed easily. The polycarboxylic acid water reducer synthesized by the method disclosed by the invention has a high water reducing rate, the use method is the same as that of a conventional water reducer, and the polycarboxylic acid water reducer can significantly improve the workability of concrete, and cannot change the gradual loss of the concrete within 60-90 minutes to enable the concrete to have a pumpable property; and more importantly, the polycarboxylic acid water reducer can effectively hold back concrete segregation caused by adding an admixture for the second time or the third time because of floor material changes, careless increase of the content of the admixture in operation, and long-time transportation.

Description

A kind of preparation method of agent on crack resistance of concrete isolation type polycarboxylate water-reducer
Technical field
The present invention relates to cement water reducing agent, be specifically related to the preparation method of a kind of agent on crack resistance of concrete isolation type polycarboxylate water-reducer.
Background technology
Building fast development with China, concrete also occurs that the speed of more than 10 increases, and concrete is as main building Material, serves the most important effect for nation-building and development.Poly carboxylic acid series water reducer is as the efficient diminishing of the third generation A kind of concrete that agent is current forefront the most in the world, scientific and technological content is the highest, application prospect is best, combination property is optimum is super plasticized Agent.Poly carboxylic acid series water reducer, as the important component of concrete admixture, is possible not only to reduce concrete Water Usage Per Unit Volume, The service behaviour of ready-mixed concrete can also be promoted and improve the intensity of maturing, increasing the service life.Polycarboxylate water-reducer has Have that volume is low, water-reducing rate is high, good with the cement-based gelling material compatibility, the concrete strength advantage such as good high, slump-retaining, The most obtain and developed rapidly, become the critical material manufacturing high performance concrete, also promote concrete technology progress One of important additives.The first in the world is occupied at China's cement output and concrete square amount, along with the fast development of China's economy, National basis Facilities Construction and the increasing of housing construction dynamics, demand and performance requirement to amount of concrete rise year by year, and naphthalene system subtracts Water preparation is to the pollution of environment and usage amount rapid drawdown, and therefore, the market demand of polycarboxylate water-reducer the most constantly increases.
During concrete uses, the water-reducing rate of water reducer and workability and function of slump protection are its of paramount importance two reference indexs, Especially under the conditions of summer high temperature, the difference of material, transportation range and construction technology in addition, collapsing, to mix degree of falling loss be that solidifying soil makes A most commonly seen problem in.The problem too fast in order to solve fresh concrete slump-loss, can take polycarboxylic acids to subtract The methods such as water preparation and retarder are mixed again, latter admixing method and the method for mixing to improve the service behaviour of concrete more.But, on the one hand, mixed Add water after after mixing additive or long-time transport arrival building site after solidifying soil, operate careless slightly and concrete easily occurs Isolation, the accident such as stifled pump, or during concrete departures, concrete slump is put big especially, thus cause concrete from Analysis.The operating process of latter admixing method and the method for mixing complicated more, and higher to equipment requirements, Financial cost is higher, and practical value is little.Separately On the one hand, the answering of retarder mixes the problems such as the compatibility that may cause the excessive slow setting of cement, cement with retarder, thus affects The construction speed of concrete and the quality of concrete, not only increase cost and also can arrive delayed impact.Finally, for solving to add Concrete water bleeding yellowing after additive, isolates and wraps up sex chromosome mosaicism, can compound with water-keeping thickening component, the most virtually increase Also bringing along the increase of later stage integrated cost while the volume of poly carboxylic acid series water reducer, therefore, traditional method is the most inadvisable But also the appearance of compounding additive and the incompatibility problem of water-keeping thickening component can be brought.
Summary of the invention
It is an object of the invention to overcome the shortcoming of prior art, it is provided that the preparation of a kind of agent on crack resistance of concrete isolation type polycarboxylate water-reducer Method.
The purpose of the present invention is achieved through the following technical solutions: the preparation method of a kind of agent on crack resistance of concrete isolation type polycarboxylate water-reducer, It comprises the following steps:
S1. solution A is prepared: by acrylic compounds that molal weight is 0.23~0.84mol, reducing agent, prenol Polyoxyethylene ether and molecular weight regulator are configured to the solution that mass percent concentration is 50~80%, are solution A;Wherein, Described reducing agent is one or both the combination in vitamin C or Brueggemann;Described molecular weight regulator be mercaptoethanol, The combination of one or more in TGA or mercaptopropionic acid;
S2. B solution is prepared: the acrylamides that molal weight is 0.33~0.76mol is configured to mass percent Concentration is the solution of 5~25%, is B solution;
S3. generating product: isopentenol polyoxyethylene ether adds in deionized water, the stirring that heats up is to isopentenol polyoxyethylene ether Add initiator after being completely dissolved, then drip solution A and B solution;Wherein, described initiator is Ammonium persulfate., potassium peroxydisulfate Or the combination of one or more in hydrogen peroxide.
Further, described acrylic compounds is acrylic acid, methacrylic acid, methyl methacrylate, methacrylic acid The combination of one or more in ethyl ester.
Further, described isopentenol polyoxyethylene ether be molecular weight be 1200,2000,2400,2600 or 3000 different The mixing of one or more in pentenol polyoxyethylene ether.
Further, described reducing agent is 1:1000~2500 with the mass ratio of isopentenol polyoxyethylene ether.
Further, described molecular weight regulator is 1:120~200 with the mass ratio of isopentenol polyoxyethylene ether.
Further, described acrylamides is acrylamide, n-methylolacrylamide, hydroxyethyl acrylamide or third The combination of one or more in acrylamide base dimethyl ethyl sulfonic acid.
Further, the temperature stirred that heats up described in step S3 is 10~35 DEG C.
Further, it is further continued for after step S3 first drips solution A 10~30min dripping solution A and B solution, described dropping Time for adding≤the 3.5h of solution A, the time for adding≤3h of described dropping B solution.
Further, initiator described in step S3 is 1:150~220 with the mass ratio of isopentenol polyoxyethylene ether.
In the present invention, acrylic compounds and acrylamide compounds can not be prepared in a vessel, to prevent phase simultaneously Implode and autohemagglutination with this understanding occurring between Hu, therefore uses and prepare A, B solution respectively, the mode of dropping joins substrate In.
The present invention is using first dropping solution A 10~30min, is being further continued for dripping solution A and B solution, first drips solution A Purpose be in order to make B solution add after can be abundant, lasting reaction, owing to B solution is easily absorbed heat, be initially charged B solution meeting Reaction temperature is caused to reduce so that reaction is stagnated.
The invention have the advantages that
(1) present invention is by aqueous free radical polymerization in polycarboxylate water-reducer building-up process, and method is simple, low cost, Workable, synthesized polycarboxylate water-reducer is colorless viscous liquid, and molecular weight is big, and standing time is stable, not malleable Its original characteristic;
(2) polycarboxylate water-reducer synthesized by the present invention possesses high water-reducing rate (>=25%), using method and conventional water reducer one Sample and can significantly improve the workability energy of concrete, does not change the gradual loss of concrete, makes concrete have in 60min-90min Have pumpable performance, this type of polycarboxylate water-reducer prior can effectively check because of ground material change (sandstone water content increases suddenly), In operating process admixture dosage accidentally strengthen, for a long time transport after second time or third time add the caused coagulation of additive The isolation of soil.
Accompanying drawing explanation
Fig. 1 is the infrared spectrogram of agent on crack resistance of concrete isolation type polycarboxylate water-reducer of the present invention.
Detailed description of the invention
Below in conjunction with embodiment, the present invention will be further described, and protection scope of the present invention is not limited to the following stated:
Embodiment 1:
A kind of preparation method of agent on crack resistance of concrete isolation type polycarboxylate water-reducer, it comprises the following steps:
S1. prepare solution A: by molal weight be the acrylic acid of 0.35mol, reducing agent, isopentenol polyoxyethylene ether and point Son amount regulator is configured to the solution that mass percent concentration is 60%, is solution A;Wherein, described reducing agent is vitamin C; Reducing agent is 1:1250 with the mass ratio of isopentenol polyoxyethylene ether;Molecular weight regulator is mercaptoethanol;Molecular weight regulator It is 1:140 with the mass ratio of isopentenol polyoxyethylene ether;
S2. prepare B solution: the acrylamide that molal weight is 0.48mol is configured to mass percent concentration be 10% molten Liquid, is B solution;
S3. generate product: isopentenol polyoxyethylene ether adds in deionized water, be warmed up to 15 DEG C of stirrings to prenol polyoxy Vinyl Ether adds initiator after being completely dissolved, then drips solution A and B solution;First it is further continued for dropping after dropping solution A 16min Solution A and B solution, the time for adding≤3.5h of described dropping solution A, the time for adding≤3h of described dropping B solution;Its In, described initiator is Ammonium persulfate., and initiator is 1:160 with the mass ratio of isopentenol polyoxyethylene ether;
Described isopentenol polyoxyethylene ether be molecular weight be the isopentenol polyoxyethylene ether of 1200.
Embodiment 2:
A kind of preparation method of agent on crack resistance of concrete isolation type polycarboxylate water-reducer, it comprises the following steps:
S1. solution A is prepared: be the acrylic compounds of 0.23mol, reducing agent, prenol polyoxy second by molal weight Alkene ether and molecular weight regulator are configured to the solution that mass percent concentration is 50%, are solution A;Wherein, acrylic compounds Compound is the mixed solution of methacrylic acid and methyl methacrylate, and weight ratio is 1:1, and described reducing agent is Brueggemann; Reducing agent is 1:1000 with the mass ratio of isopentenol polyoxyethylene ether;Described molecular weight regulator is TGA and mercaptopropionic acid Mixture, and weight ratio is 1:1;Molecular weight regulator is 1:120 with the mass ratio of isopentenol polyoxyethylene ether;
S2. B solution is prepared: the acrylamides that molal weight is 0.33mol is configured to mass percent concentration is The solution of 5%, is B solution;Described acrylamides be n-methylolacrylamide and hydroxyethyl acrylamide mixing molten Liquid, and weight ratio is 2:1;
S3. generate product: isopentenol polyoxyethylene ether adds in deionized water, be warmed up to 10 DEG C of stirrings to prenol polyoxy Vinyl Ether adds initiator, then dropping solution A and B solution respectively after being completely dissolved;First it is further continued for after dropping solution A 10min Dropping solution A and B solution, the time for adding≤3.5h of described dropping solution A, the time for adding≤3h of described dropping B solution; Wherein, described initiator was the mixed solution of potassium peroxydisulfate and hydrogen peroxide, and weight ratio is 1:1;Initiator and prenol The mass ratio of polyoxyethylene ether is 1:150;
Described isopentenol polyoxyethylene ether be molecular weight be the mixed solution of the isopentenol polyoxyethylene ether of 2000 and 2400.
Embodiment 3:
A kind of preparation method of agent on crack resistance of concrete isolation type polycarboxylate water-reducer, it comprises the following steps:
S1. solution A is prepared: be the acrylic compounds of 0.84mol, reducing agent, prenol polyoxy second by molal weight Alkene ether and molecular weight regulator are configured to the solution that mass percent concentration is 80%, are solution A;Wherein, acrylic compounds Compound is the mixed solution of methacrylic acid, methyl methacrylate and ethyl methacrylate, and weight ratio is 3:2:1;Institute Stating reducing agent is one or both the combination in Brueggemann;Reducing agent with the mass ratio of isopentenol polyoxyethylene ether is 1:2500;Described molecular weight regulator is the combination of one or more in mercaptoethanol, TGA or mercaptopropionic acid;Molecule Amount regulator is 1:200 with the mass ratio of isopentenol polyoxyethylene ether;
S2. B solution is prepared: the acrylamides that molal weight is 0.76mol is configured to mass percent concentration is The solution of 25%, is B solution;Wherein, described acrylamides is n-methylolacrylamide, hydroxyethyl acrylamide With the mixed solution of acrylamido dimethyl ethyl sulfonic acid, and weight ratio is 2:3:1;
S3. generate product: isopentenol polyoxyethylene ether adds in deionized water, be warmed up to 35 DEG C of stirrings to prenol polyoxy Vinyl Ether adds initiator, then dropping solution A and B solution respectively after being completely dissolved;First it is further continued for after dropping solution A 30min Dropping solution A and B solution, the time for adding≤3.5h of described dropping solution A, the time for adding≤3h of described dropping B solution; Wherein, described initiator is the mixed solution of Ammonium persulfate., potassium peroxydisulfate and hydrogen peroxide, and weight ratio is 1:1:4;Initiator It is 1:220 with the mass ratio of isopentenol polyoxyethylene ether;
Described isopentenol polyoxyethylene ether be molecular weight be the mixing of the isopentenol polyoxyethylene ether of 2400,2600 and 3000 Solution, mixes with arbitrary proportion.
Embodiment 4:
A kind of preparation method of agent on crack resistance of concrete isolation type polycarboxylate water-reducer, it comprises the following steps:
S1. solution A is prepared: be the acrylic compounds of 0.58mol, reducing agent, prenol polyoxy second by molal weight Alkene ether and molecular weight regulator are configured to the solution that mass percent concentration is 62%, are solution A;Wherein, acrylic compounds Compound is the mixed solution of acrylic acid, methacrylic acid, methyl methacrylate and ethyl methacrylate, mixes with arbitrary proportion Closing, described reducing agent is the mixing of vitamin C and Brueggemann, and weight ratio is 3:1;Reducing agent and prenol polyoxy second The mass ratio of alkene ether is 1:1840;Described molecular weight regulator is TGA, molecular weight regulator and prenol polyoxyethylene The mass ratio of ether is 1:165;
S2. B solution is prepared: the acrylamides that molal weight is 0.60mol is configured to mass percent concentration is The solution of 15%, is B solution;Acrylamides is hydroxyethyl acrylamide;
S3. generate product: isopentenol polyoxyethylene ether adds in deionized water, be warmed up to 23 DEG C of stirrings to prenol polyoxy Vinyl Ether adds initiator, then dropping solution A and B solution respectively after being completely dissolved;First it is further continued for after dropping solution A 20min Dropping solution A and B solution, the time for adding≤3.5h of described dropping solution A, the time for adding≤3h of described dropping B solution; Wherein, described initiator is hydrogen peroxide, and initiator is 1:180 with the mass ratio of isopentenol polyoxyethylene ether;
Described isopentenol polyoxyethylene ether be molecular weight be the isopentenol polyoxyethylene ether of 2000,2400,2600 and 3000 Mixed solution, with arbitrary proportion mix.
Embodiment 5:
A kind of preparation method of agent on crack resistance of concrete isolation type polycarboxylate water-reducer, it comprises the following steps:
S1. solution A is prepared: be the acrylic compounds of 0.72mol, reducing agent, prenol polyoxy second by molal weight Alkene ether and molecular weight regulator are configured to the solution that mass percent concentration is 72%, are solution A;Wherein, acrylic compounds Compound is the mixed solution of acrylic acid, methacrylic acid and methyl methacrylate, and weight ratio is 5:3:2;Described reducing agent For vitamin C, reducing agent is 1:2300 with the mass ratio of isopentenol polyoxyethylene ether;Described molecular weight regulator is sulfydryl second Alcohol and the mixed solution of TGA, and weight ratio is 3:2;Molecular weight regulator and the mass ratio of isopentenol polyoxyethylene ether For 1:185;
S2. B solution is prepared: the acrylamides that molal weight is 0.72mol is configured to mass percent concentration is The solution of 22%, is B solution;Acrylamides is n-methylolacrylamide, hydroxyethyl acrylamide, acrylamide The mixing of base dimethyl ethyl sulfonic acid, mixes with arbitrary proportion;
S3. product is generated: isopentenol polyoxyethylene ether adds in deionized water, be warmed up to/32 DEG C of stirrings are to prenol polyoxy Vinyl Ether adds initiator, then dropping solution A and B solution respectively after being completely dissolved;First it is further continued for after dropping solution A 28min Dropping solution A and B solution, the time for adding≤3.5h of described dropping solution A, the time for adding≤3h of described dropping B solution; Wherein, described initiator is the mixing of Ammonium persulfate. and potassium peroxydisulfate, and weight ratio is 5:1;Initiator and prenol polyoxy The mass ratio of vinyl Ether is 1:210;
Described isopentenol polyoxyethylene ether be molecular weight be the prenol polyoxy of 1200,2000,2400,2600 and 3000 The mixed solution of vinyl Ether, mixes with arbitrary proportion.
Below by way of description of test beneficial effects of the present invention:
1. cement paste experiment: the anti-isolation type polycarboxylate water-reducer of the embodiment of the present invention 1 synthesis is carried out cement paste experiment, The performance indications of polycarboxylate water-reducer are according to industry standard JG/T223-2007 " polycarboxylate high performance water-reducing agent ";Cement paste Fluidity experiment is tested according to GB GB/T8077-2000 " concrete admixture homogeneity test method ", and water reducer is rolled over Gu volume is 0.1%, the anti-isolation type polycarboxylate water-reducer (abbreviation experimental group) of synthesis and commercially sample 1 (ordinary water-reducing agent type Water reducer), 2 (high diminishing dosage form water reducers), 3 (collapse protection type water reducer) contrast test the results are shown in Table shown in 1 above-mentioned commercially 1, Commercially 2, commercially 3 all have Sichuan Tong Zhou Chemical Industry Science Co., Ltd to produce;
Table 1: only starch result of the test
Illustrating: the solid volume of polycarboxylate water-reducer folding is 0.1%, cement is middle P.O 42.5R cement (China's associating Cement Group Beichuan Zhong Lian Cement Co., Ltd produces).
1. concrete experiments: concrete test is according to GB GB/T50080-2002 " normal concrete mix performance test mark Accurate ", the solid volume of water reducer folding is 0.2%;GB-T50081-2002 " standard for test methods of mechanical properties of ordinary concrete " is carried out Test, the solid volume of the folding of water reducer is 0.16%, compared for commercially 3 polycarboxylate water-reducers and synthesis with different volumes respectively Anti-isolation type polycarboxylate water-reducer contrast test, test result is shown in Table 2.
Table 2: concrete test result
Illustrate: commercially the 3 solid volumes of water reducer folding are 0.18%, and C30 concrete folk prescription water consumption is 170kg/L;Anti-isolation type gathers The solid volume of carboxylic acid water reducer experimental group 1 folding is 0.18%, the solid volume of experimental group 2 folding is 0.19%, the solid volume of experimental group 3 folding is 0.2%, and C30 concrete folk prescription water consumption is 170kg/L;The solid volume of experimental group 4, experimental group 5, experimental group 6 folding is 0.18%, C30 concrete folk prescription water consumption is respectively 180kg/L, 190kg/L, 200kg/L.Employing joins P.O 42.5R water Mud, medium sand (Machine-made Sand, containing mud 5%, sand aqueous 0%), 5~25 continuous size fraction rubbles, cement often side's consumption 260, river Oil coal ash often side consumption 80kg, sand coarse aggregate ratio is 44.5%.
3. infrared spectrum experiment, carries out infrared spectrum experiment to the anti-isolation type polycarboxylate water-reducer of present invention synthesis, result such as figure Shown in 1, its abscissa is wave number (cm-1), vertical coordinate be transmitance (%);In infrared spectrum, 1728.59cm-1For carboxylic acid Carbonyl C=O shrinks vibration peak;1113.42cm-1、952.74cm-1And 843.03cm-1The absworption peak at place is the polymeric monomer of long-chain branch Characteristic absorption peak, wherein 1113.42cm-1It is the stretching vibration peak of C-O, 952.74cm in C-O-C structure-1And 843.03cm-1 It is C-C and the C-O stretching vibration in polyoxyethylene groups respectively;1644.48cm-1、1467.59cm-1、1344.41cm-1、 1243.11cm-1、531.12cm-1Characteristic absorption peak for amides compound;Features above peak can show that minor comonomer and polyethers are big Monomer creates copolymerization in aqueous, generates polycarboxylate water-reducer.

Claims (9)

1. the preparation method of an agent on crack resistance of concrete isolation type polycarboxylate water-reducer, it is characterised in that it comprises the following steps:
S1. solution A is prepared: acrylic compounds, reducing agent, isopentenol polyoxyethylene ether and molecular weight regulator that molal weight is 0.23~0.84mol are configured to the solution that mass percent concentration is 50~80%, are solution A;Wherein, one or both the combination during described reducing agent is vitamin C or Brueggemann;Described molecular weight regulator is the combination of one or more in mercaptoethanol, TGA or mercaptopropionic acid;
S2. B solution is prepared: the acrylamides that molal weight is 0.33~0.76mol is configured to the solution that mass percent concentration is 5~25%, is B solution;
S3. generating product: isopentenol polyoxyethylene ether adds in deionized water, the stirring that heats up adds initiator after being completely dissolved to isopentenol polyoxyethylene ether, then drips solution A and B solution;Wherein, the combination of one or more during described initiator is Ammonium persulfate., potassium peroxydisulfate or hydrogen peroxide.
The preparation method of a kind of agent on crack resistance of concrete isolation type polycarboxylate water-reducer the most as claimed in claim 1, it is characterized in that, described acrylic compounds is the combination of one or more in acrylic acid, methacrylic acid, methyl methacrylate, ethyl methacrylate.
The preparation method of a kind of agent on crack resistance of concrete isolation type polycarboxylate water-reducer the most as claimed in claim 1, it is characterized in that, described isopentenol polyoxyethylene ether be molecular weight be the mixing of one or more in the isopentenol polyoxyethylene ether of 1200,2000,2400,2600 or 3000.
4. the preparation method of a kind of agent on crack resistance of concrete isolation type polycarboxylate water-reducer as described in claim 1 or 3, it is characterised in that described reducing agent is 1:1000~2500 with the mass ratio of isopentenol polyoxyethylene ether.
5. the preparation method of a kind of agent on crack resistance of concrete isolation type polycarboxylate water-reducer as described in claim 1 or 3, it is characterised in that described molecular weight regulator is 1:120~200 with the mass ratio of isopentenol polyoxyethylene ether.
The preparation method of a kind of agent on crack resistance of concrete isolation type polycarboxylate water-reducer the most as claimed in claim 1, it is characterized in that, described acrylamides is the combination of one or more in acrylamide, n-methylolacrylamide, hydroxyethyl acrylamide or acrylamido dimethyl ethyl sulfonic acid.
The preparation method of a kind of agent on crack resistance of concrete isolation type polycarboxylate water-reducer the most as claimed in claim 1, it is characterised in that the temperature of the stirring that heats up described in step S3 is 10~35 DEG C.
The preparation method of a kind of agent on crack resistance of concrete isolation type polycarboxylate water-reducer the most as claimed in claim 1, it is characterized in that, it is further continued for after step S3 first drips solution A 10~30min dripping solution A and B solution, time for adding≤the 3.5h of described dropping solution A, the time for adding≤3h of described dropping B solution.
9. the preparation method of a kind of agent on crack resistance of concrete isolation type polycarboxylate water-reducer as described in claim 1 or 3, it is characterised in that initiator described in step S3 is 1:150~220 with the mass ratio of isopentenol polyoxyethylene ether.
CN201610115439.8A 2016-03-01 2016-03-01 Preparation method of anti-segregation type polycarboxylic acid water reducer of concrete Pending CN105801765A (en)

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Cited By (5)

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CN106699986A (en) * 2016-12-06 2017-05-24 长江大学 Acrylic acid-acrylamide-allyl polyether copolymer and preparation method thereof
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CN113929835A (en) * 2021-11-01 2022-01-14 江苏兆佳建材科技有限公司 Polycarboxylate superplasticizer for machine-made sand and preparation method thereof

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CN106517859A (en) * 2016-10-18 2017-03-22 贵州建工混凝土有限责任公司 Concrete anti-segregation method
CN106632884A (en) * 2016-10-24 2017-05-10 湖北江城子建材科技股份有限公司 Method for preparing polycarboxylate superplasticizer
CN106699986A (en) * 2016-12-06 2017-05-24 长江大学 Acrylic acid-acrylamide-allyl polyether copolymer and preparation method thereof
CN106699986B (en) * 2016-12-06 2019-06-25 长江大学 A kind of acrylic acid-acrylamide-allyl polyether copolymer and preparation method thereof
CN113121736A (en) * 2021-04-22 2021-07-16 河北三楷深发科技股份有限公司 Preparation method of hydrophilic solvent type polycarboxylate superplasticizer
CN113929835A (en) * 2021-11-01 2022-01-14 江苏兆佳建材科技有限公司 Polycarboxylate superplasticizer for machine-made sand and preparation method thereof

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Application publication date: 20160727