CN107902939A - A kind of anti-freezing type polycarboxylate water-reducer and its synthesis technique - Google Patents
A kind of anti-freezing type polycarboxylate water-reducer and its synthesis technique Download PDFInfo
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- CN107902939A CN107902939A CN201711198447.4A CN201711198447A CN107902939A CN 107902939 A CN107902939 A CN 107902939A CN 201711198447 A CN201711198447 A CN 201711198447A CN 107902939 A CN107902939 A CN 107902939A
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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
- C04B24/16—Sulfur-containing compounds
- C04B24/161—Macromolecular compounds comprising sulfonate or sulfate groups
- C04B24/163—Macromolecular compounds comprising sulfonate or sulfate groups obtained by reactions only involving carbon-to-carbon unsaturated bonds
- C04B24/165—Macromolecular compounds comprising sulfonate or sulfate groups obtained by reactions only involving carbon-to-carbon unsaturated bonds containing polyether side chains
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- 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
- C08F2/38—Polymerisation using regulators, e.g. chain terminating agents, e.g. telomerisation
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- 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
- C08F2/44—Polymerisation in the presence of compounding ingredients, e.g. plasticisers, dyestuffs, fillers
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- 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
- C08F251/00—Macromolecular compounds obtained by polymerising monomers on to polysaccharides or derivatives thereof
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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
- C08F251/00—Macromolecular compounds obtained by polymerising monomers on to polysaccharides or derivatives thereof
- C08F251/02—Macromolecular compounds obtained by polymerising monomers on to polysaccharides or derivatives thereof on to cellulose or derivatives thereof
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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
- C08F283/04—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G on to polycarbonamides, polyesteramides or polyimides
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- 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
- 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
- C08F289/00—Macromolecular compounds obtained by polymerising monomers on to macromolecular compounds not provided for in groups C08F251/00 - C08F287/00
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/12—Powdering or granulating
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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
- 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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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2351/00—Characterised by the use of graft polymers in which the grafted component is obtained by reactions only involving carbon-to-carbon unsaturated bonds; Derivatives of such polymers
- C08J2351/08—Characterised by the use of graft polymers in which the grafted component is obtained by reactions only involving carbon-to-carbon unsaturated bonds; Derivatives of such polymers grafted on to macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2451/00—Characterised by the use of graft polymers in which the grafted component is obtained by reactions only involving carbon-to-carbon unsaturated bonds; Derivatives of such polymers
- C08J2451/02—Characterised by the use of graft polymers in which the grafted component is obtained by reactions only involving carbon-to-carbon unsaturated bonds; Derivatives of such polymers grafted on to polysaccharides
Abstract
The invention discloses a kind of anti-freezing type polycarboxylate water-reducer and its synthesis technique, raw material to include：Antifreeze, acrylic acid, hydrogen peroxide, β propyloic acrylic esters, maleic anhydride monomer, initiator, molecular weight regulator, fatty alcohol polyoxyethylene ether, unitary unsaturated carboxylic acid and its derivative, alkene ether polyoxyethylene, catalyst, γ polyglutamic acids, Artemisia Glue, microcrystalline cellulose, feather protein；The raw material of antifreeze includes：3 allyloxy, 2 hydroxypropionate sodium, allyl polyglycol, calcium chloride, ammonium sulfate, silicon ash, microdenier staple.The present invention not only has water reducing ability, slump retaining, and the workability of concrete is set to significantly improve, greatly reduce sensitiveness of the water-reducing agent to water consumption, obtained Water-reducing Admixtures To Cements have good compatibility, and volume is small, and water-reducing rate is high, cryoprotective effects are good, the frost-proof test of concrete is remarkably improved, is used suitable for cold district engineering, there is higher practical value.
Description
Technical field
The present invention relates to chemical assistant technical field, is specifically a kind of anti-freezing type polycarboxylate water-reducer and its synthesis technique.
Background technology
High-efficiency water-reducing agent of poly-carboxylic acid is third generation water-reducing agent, and well-known with its environmental protection and high water reducing rate, current application is more next
It is more extensive, C40-C100 high-strength concretes are applied not only to, C10-C30 low-grade concretes can be additionally used in by compounding, it is economical
Superior performance is in naphthalene water reducer, and the concrete properties for mixing high-efficiency water-reducing agent of poly-carboxylic acid are better than mixing naphthalene water reducer
(fresh concrete workability, the performance ratio such as intensity and durability mixes the coagulation of naphthalene water reducer to concrete on the coagulation after hardening
Soil has qualitative leap).At present research poly carboxylic acid series water reducer by more from the intensity of concrete, application property, durability and
The various aspects such as price consider.As synthesis is with characterizing the research of polyalcohol water reducing agent and its chemical constitution and property relationship not
Disconnected to go deep into, poly carboxylic acid series water reducer will develop further towards high-performance multifunction, ecology, International standardization direction.
Water-reducing agent is a kind of important concrete admixture, is one of staple product of building material pillar industry.Efficiently
Water-reducing agent not only substantially increases the mechanical property of high-strength concrete, and provides easy-to-use construction technology.At present I
The widely used high efficiency water reducing agent of state is mainly naphthalene system product.
The ratio of mud can be greatly lowered in polycarboxylate water-reducer, improve early stage and the later strength of concrete, have concrete
There are high compact and volume stability, greatly improve concrete performance and cost can be reduced, easy to construct.But poly- shuttle acid at present
Technique is complex in high efficiency water reducing agent building-up process, the more difficult grasp of technical process control, and current water-reducing agent is liquid,
It is high there are freight, the shortcomings of storage period is short；In addition, in high latitude and plateau and cold climate area a reinforced, the resistance to frost of concrete
It is important inspection target.When temperature is low, the growth of concrete strength can be seriously affected, the moisture in concrete also can be in the external world
Temperature causes frost heave when raising, and causes the rupture of concrete, influences the structure of concrete, further reduces the intensity of concrete；
The water-reducing agent used in cold district engineering needs have good anti-freezing property, so as to improve the frost resistance of concrete.
The content of the invention
It is an object of the invention to provide the anti-freezing type polycarboxylate water-reducer and its conjunction that a kind of cryoprotective effects are good, water-reducing rate is high
Into technique, to solve the problems mentioned in the above background technology.
To achieve the above object, the present invention provides following technical solution：
A kind of anti-freezing type polycarboxylate water-reducer, includes according to the raw material of parts by weight：46-76 parts of antifreeze, acrylic acid 30-50
Part, 80-100 parts of hydrogen peroxide, β -10-15 parts of propyloic acrylic ester, 1-3 parts of maleic anhydride monomer, 3-5 parts of initiator, molecule
1-2 parts of conditioning agent of amount, 3-5 parts of fatty alcohol polyoxyethylene ether, unitary unsaturated carboxylic acid and its 10-20 parts of derivative, alkene ether gather
5-7 parts of ethylene oxide, 2-4 parts of catalyst, 0.1-0.3 parts of gamma-polyglutamic acid, 2-4 parts of Artemisia Glue, 4-6 parts of microcrystalline cellulose, feather
1-3 parts of albumen；The antifreeze includes according to the raw material of parts by weight：3-5 parts of 3- allyloxys -2- hydroxypropionate sodiums, allyl
4-6 parts of base polyethylene glycol, 15-25 parts of calcium chloride, 6-8 parts of ammonium sulfate, 10-20 parts of silicon ash, 8-12 parts of microdenier staple.
The anti-freezing type polycarboxylate water-reducer, includes according to the raw material of parts by weight：It is 61 parts of antifreeze, 40 parts of acrylic acid, double
90 parts of oxygen water, 12 parts of β-propyloic acrylic ester, 2 parts of maleic anhydride monomer, 4 parts of initiator, 1.5 parts of molecular weight regulator, fat
15 parts of 4 parts of fat alcohol polyoxyethylene ether, unitary unsaturated carboxylic acid and its derivative, 6 parts of alkene ether polyoxyethylene, 3 parts of catalyst,
0.2 part of gamma-polyglutamic acid, 3 parts of Artemisia Glue, 5 parts of microcrystalline cellulose, 2 parts of feather protein；The antifreeze according to parts by weight original
Material includes：4 parts of 3- allyloxy -2- hydroxypropionate sodiums, 5 parts of allyl polyglycol, 20 parts of calcium chloride, 7 parts of ammonium sulfate, silicon
Grey 15 parts, 10 parts of microdenier staple.
As the further scheme of the present invention：The molecular weight regulator presses 1 for methylpropene sodium sulfonate and mercaptopropionic acid：
The mixture that 4 ratio is mixed to get.
As the further scheme of the present invention：The initiator is dibenzoyl peroxide, dicetyl peroxydicarbonate 26
Ester and dicetyl peroxydicarbonate dihexyl.
As further scheme of the invention：The catalyst presses 1 for vitamin C, Ge(SO) and amion acetic acid propyl ester：
1.5：2 obtained mixtures.
The synthesis technique of the anti-freezing type polycarboxylate water-reducer, comprises the following steps that：
(1) by β-propyloic acrylic ester, fatty alcohol polyoxyethylene ether, unitary unsaturated carboxylic acid and its derivative, alkene ether
70-90 DEG C of stirring 0.5-1h obtains A liquid in the water of base polyoxyethylene addition 1/2-2/3 amounts；By hydrogen peroxide, maleic anhydride monomer, draw
Hair agent, molecular weight regulator, catalyst, gamma-polyglutamic acid, Artemisia Glue, microcrystalline cellulose, feather protein are uniformly mixed to obtain B liquid；
(2) in a kettle, 100-140 parts of water and acrylic acid are added, sequentially adds the 3- allyloxys -2- in antifreeze
Hydroxypropionate sodium, allyl polyglycol, calcium chloride, ammonium sulfate, silicon ash, microdenier staple, after stirring evenly, by A liquid and B
The speed that liquid is dripped off by 3-5h is added dropwise into reaction kettle, after B liquid 5min is added dropwise first is started that A liquid is added dropwise again, is added in A drops
After continue stir 0.5-1h；
(3) product that step (2) obtains is added on liquid distribution trough by feeding valve, then is cast by liquid distribution trough
To conveyer belt, conveyer belt at the uniform velocity advances in vacuum temp control case, controls the heating system of vacuum temp control case, makes vacuum temp control case
Interior temperature is kept for 40-60 DEG C；The pace of conveyer belt is controlled, moisture is constantly evaporated, is exported from vacuum temp control case defeated
Send material solid content >=95% that band is taken out of；
(4) peel off：After material is taken out of by conveyer belt from the outlet of vacuum temp control case, continue as conveyer belt is advanced forward,
In traveling process, natural cooling；After material is with conveyor belt turn-over, shelled by being arranged on the hoe scaler below conveyer belt
From；
(5) crush：After material is stripped knife stripping conveyer belt, under the action of self gravitation, fall into pulverizer, by powder
Broken machine is crushed, that is, anti-freezing type polycarboxylate water-reducer finished product is made.
Compared with prior art, the beneficial effects of the invention are as follows：
The present invention is pulvis, is easy to store, transports, can more reduce packaging and freight, it may have storage period
The features such as long, easy to use, in use, being dissolved in water, not only with water reducing ability, slump retaining, but also make the sum of concrete
Easy property significantly improves, and greatly reduces sensitiveness of the water-reducing agent to water consumption, by the compounding of various raw materials, makes obtained
Water-reducing Admixtures To Cements have good compatibility, and volume is small, and water-reducing rate is high, and cryoprotective effects are good, are remarkably improved concrete
Frost-proof test, uses suitable for cold district engineering, has higher practical value.
Embodiment
The technical solution of this patent is described in more detail with reference to embodiment.
Embodiment 1
A kind of anti-freezing type polycarboxylate water-reducer, includes according to the raw material of parts by weight：It is 46 parts of antifreeze, 30 parts of acrylic acid, double
80 parts of oxygen water, 10 parts of β-propyloic acrylic ester, 1 part of maleic anhydride monomer, 3 parts of initiator, 1 part of molecular weight regulator, fat
10 parts of 3 parts of alcohol polyoxyethylene ether, unitary unsaturated carboxylic acid and its derivative, 5 parts of alkene ether polyoxyethylene, 2 parts of catalyst, γ-
0.1 part of polyglutamic acid, 2 parts of Artemisia Glue, 4 parts of microcrystalline cellulose, 1 part of feather protein；The antifreeze according to parts by weight raw material
Including：3 parts of 3- allyloxy -2- hydroxypropionate sodiums, 4 parts of allyl polyglycol, 15 parts of calcium chloride, 6 parts of ammonium sulfate, silicon ash
10 parts, 8 parts of microdenier staple.
The synthesis technique of the anti-freezing type polycarboxylate water-reducer, comprises the following steps that：
(1) by β-propyloic acrylic ester, fatty alcohol polyoxyethylene ether, unitary unsaturated carboxylic acid and its derivative, alkene ether
70 DEG C of stirring 0.5h obtain A liquid in the water of base polyoxyethylene 1/2 amount of addition；By hydrogen peroxide, maleic anhydride monomer, initiator, molecule
Amount conditioning agent, catalyst, gamma-polyglutamic acid, Artemisia Glue, microcrystalline cellulose, feather protein are uniformly mixed to obtain B liquid；
(2) in a kettle, 100 parts of water and acrylic acid are added, sequentially adds the 3- allyloxy -2- hydroxyls in antifreeze
Propanesulfonate, allyl polyglycol, calcium chloride, ammonium sulfate, silicon ash, microdenier staple, after stirring evenly, A liquid and B liquid are pressed
The speed that 3h is dripped off is added dropwise into reaction kettle, after B liquid 5min is added dropwise first starts that A liquid is added dropwise again, after A drops add
Continue to stir 0.5h；
(3) product that step (2) obtains is added on liquid distribution trough by feeding valve, then is cast by liquid distribution trough
To conveyer belt, conveyer belt at the uniform velocity advances in vacuum temp control case, controls the heating system of vacuum temp control case, makes vacuum temp control case
Interior temperature is kept for 40 DEG C；The pace of conveyer belt is controlled, moisture is constantly evaporated, is exported from vacuum temp control case by conveyer belt
Material solid content >=95% taken out of；
(4) peel off：After material is taken out of by conveyer belt from the outlet of vacuum temp control case, continue as conveyer belt is advanced forward,
In traveling process, natural cooling；After material is with conveyor belt turn-over, shelled by being arranged on the hoe scaler below conveyer belt
From；
(5) crush：After material is stripped knife stripping conveyer belt, under the action of self gravitation, fall into pulverizer, by powder
Broken machine is crushed, that is, anti-freezing type polycarboxylate water-reducer finished product is made.
Embodiment 2
A kind of anti-freezing type polycarboxylate water-reducer, includes according to the raw material of parts by weight：It is 61 parts of antifreeze, 40 parts of acrylic acid, double
90 parts of oxygen water, 12 parts of β-propyloic acrylic ester, 2 parts of maleic anhydride monomer, 4 parts of initiator, 1.5 parts of molecular weight regulator, fat
15 parts of 4 parts of fat alcohol polyoxyethylene ether, unitary unsaturated carboxylic acid and its derivative, 6 parts of alkene ether polyoxyethylene, 3 parts of catalyst,
0.2 part of gamma-polyglutamic acid, 3 parts of Artemisia Glue, 5 parts of microcrystalline cellulose, 2 parts of feather protein；The antifreeze according to parts by weight original
Material includes：4 parts of 3- allyloxy -2- hydroxypropionate sodiums, 5 parts of allyl polyglycol, 20 parts of calcium chloride, 7 parts of ammonium sulfate, silicon
Grey 15 parts, 10 parts of microdenier staple.
The synthesis technique of the anti-freezing type polycarboxylate water-reducer, comprises the following steps that：
(1) by β-propyloic acrylic ester, fatty alcohol polyoxyethylene ether, unitary unsaturated carboxylic acid and its derivative, alkene ether
80 DEG C of stirring 0.8h obtain A liquid in the water of base polyoxyethylene 7/12 amount of addition；By hydrogen peroxide, maleic anhydride monomer, initiator, molecule
Amount conditioning agent, catalyst, gamma-polyglutamic acid, Artemisia Glue, microcrystalline cellulose, feather protein are uniformly mixed to obtain B liquid；
(2) in a kettle, 120 parts of water and acrylic acid are added, sequentially adds the 3- allyloxy -2- hydroxyls in antifreeze
Propanesulfonate, allyl polyglycol, calcium chloride, ammonium sulfate, silicon ash, microdenier staple, after stirring evenly, A liquid and B liquid are pressed
The speed that 4h is dripped off is added dropwise into reaction kettle, after B liquid 5min is added dropwise first starts that A liquid is added dropwise again, after A drops add
Continue to stir 0.8h；
(3) product that step (2) obtains is added on liquid distribution trough by feeding valve, then is cast by liquid distribution trough
To conveyer belt, conveyer belt at the uniform velocity advances in vacuum temp control case, controls the heating system of vacuum temp control case, makes vacuum temp control case
Interior temperature is kept for 50 DEG C；The pace of conveyer belt is controlled, moisture is constantly evaporated, is exported from vacuum temp control case by conveyer belt
Material solid content >=95% taken out of；
(4) peel off：After material is taken out of by conveyer belt from the outlet of vacuum temp control case, continue as conveyer belt is advanced forward,
In traveling process, natural cooling；After material is with conveyor belt turn-over, shelled by being arranged on the hoe scaler below conveyer belt
From；
(5) crush：After material is stripped knife stripping conveyer belt, under the action of self gravitation, fall into pulverizer, by powder
Broken machine is crushed, that is, anti-freezing type polycarboxylate water-reducer finished product is made.
Embodiment 3
A kind of anti-freezing type polycarboxylate water-reducer, includes according to the raw material of parts by weight：It is 76 parts of antifreeze, 50 parts of acrylic acid, double
100 parts of oxygen water, 15 parts of β-propyloic acrylic ester, 3 parts of maleic anhydride monomer, 5 parts of initiator, 2 parts of molecular weight regulator, fat
20 parts of 5 parts of alcohol polyoxyethylene ether, unitary unsaturated carboxylic acid and its derivative, 7 parts of alkene ether polyoxyethylene, 4 parts of catalyst, γ-
0.3 part of polyglutamic acid, 4 parts of Artemisia Glue, 6 parts of microcrystalline cellulose, 3 parts of feather protein；The antifreeze according to parts by weight raw material
Including：5 parts of 3- allyloxy -2- hydroxypropionate sodiums, 6 parts of allyl polyglycol, 25 parts of calcium chloride, 8 parts of ammonium sulfate, silicon ash
20 parts, 12 parts of microdenier staple.
The synthesis technique of the anti-freezing type polycarboxylate water-reducer, comprises the following steps that：
(1) by β-propyloic acrylic ester, fatty alcohol polyoxyethylene ether, unitary unsaturated carboxylic acid and its derivative, alkene ether
90 DEG C of stirring 1h obtain A liquid in the water of base polyoxyethylene addition 1/2-2/3 amounts；By hydrogen peroxide, maleic anhydride monomer, initiator, point
Son amount conditioning agent, catalyst, gamma-polyglutamic acid, Artemisia Glue, microcrystalline cellulose, feather protein are uniformly mixed to obtain B liquid；
(2) in a kettle, 140 parts of water and acrylic acid are added, sequentially adds the third sulphur of allyloxy-hydroxyl in antifreeze
Sour sodium, allyl polyglycol, calcium chloride, ammonium sulfate, silicon ash, microdenier staple, after stirring evenly, 5h drops are pressed by A liquid and B liquid
Complete speed is added dropwise into reaction kettle, after B liquid 5min is added dropwise first is started that A liquid is added dropwise again, is continued after A drops add
Stir 1h；
(3) product that step (2) obtains is added on liquid distribution trough by feeding valve, then is cast by liquid distribution trough
To conveyer belt, conveyer belt at the uniform velocity advances in vacuum temp control case, controls the heating system of vacuum temp control case, makes vacuum temp control case
Interior temperature is kept for 60 DEG C；The pace of conveyer belt is controlled, moisture is constantly evaporated, is exported from vacuum temp control case by conveyer belt
Material solid content >=95% taken out of；
(4) peel off：After material is taken out of by conveyer belt from the outlet of vacuum temp control case, continue as conveyer belt is advanced forward,
In traveling process, natural cooling；After material is with conveyor belt turn-over, shelled by being arranged on the hoe scaler below conveyer belt
From；
(5) crush：After material is stripped knife stripping conveyer belt, under the action of self gravitation, fall into pulverizer, by powder
Broken machine is crushed, that is, anti-freezing type polycarboxylate water-reducer finished product is made.
Using reference cement, above-mentioned obtained water-reducing agent is tested, it is as a result as shown in the table：
Table one：Concrete mixture characteristic (water-reducing agent consolidates volume 0.5%)
Paste flowing degree test is carried out to the cement of different compositions with water-reducing agent obtained above, it is as a result as follows：
Table two：Dispersiveness of the water-reducing agent in different composition cement
The molecular weight regulator presses 1 for methylpropene sodium sulfonate and mercaptopropionic acid：The mixing that 4 ratio is mixed to get
Thing；The initiator is dibenzoyl peroxide, two hexadecyl ester of dicetyl peroxydicarbonate and dicetyl peroxydicarbonate dihexyl；It is described to urge
Agent presses 1 for vitamin C, Ge(SO) and amion acetic acid propyl ester：1.5：2 obtained mixtures.
The present invention is pulvis, is easy to store, transports, can more reduce packaging and freight, it may have storage period
The features such as long, easy to use, in use, being dissolved in water, not only with water reducing ability, slump retaining, but also make the sum of concrete
Easy property significantly improves, and greatly reduces sensitiveness of the water-reducing agent to water consumption, by the compounding of various raw materials, makes obtained
Water-reducing Admixtures To Cements have good compatibility, and volume is small, and water-reducing rate is high, and cryoprotective effects are good, are remarkably improved concrete
Frost-proof test, uses suitable for cold district engineering, has higher practical value.
The better embodiment of this patent is explained in detail above, but this patent is not limited to above-mentioned embodiment party
Formula, can also be on the premise of this patent objective not be departed from the knowledge that one skilled in the relevant art possesses
Various changes can be made.
Claims (6)
1. a kind of anti-freezing type polycarboxylate water-reducer, it is characterised in that include according to the raw material of parts by weight：46-76 parts of antifreeze, third
30-50 parts of olefin(e) acid, 80-100 parts of hydrogen peroxide, β -10-15 parts of propyloic acrylic ester, 1-3 parts of maleic anhydride monomer, initiator 3-
10-20 parts of 5 parts, 1-2 parts of molecular weight regulator, 3-5 parts of fatty alcohol polyoxyethylene ether, unitary unsaturated carboxylic acid and its derivative,
5-7 parts of alkene ether polyoxyethylene, 2-4 parts of catalyst, 0.1-0.3 parts of gamma-polyglutamic acid, 2-4 parts of Artemisia Glue, microcrystalline cellulose 4-
6 parts, 1-3 parts of feather protein；The antifreeze includes according to the raw material of parts by weight：3- allyloxy -2- hydroxypropionate sodiums 3-5
Part, 4-6 parts of allyl polyglycol, 15-25 parts of calcium chloride, 6-8 parts of ammonium sulfate, 10-20 parts of silicon ash, microdenier staple 8-12
Part.
2. anti-freezing type polycarboxylate water-reducer according to claim 1, it is characterised in that include according to the raw material of parts by weight：
61 parts of antifreeze, 40 parts of acrylic acid, 90 parts of hydrogen peroxide, 12 parts of β-propyloic acrylic ester, 2 parts of maleic anhydride monomer, initiator 4
Part, 1.5 parts of molecular weight regulator, 4 parts of fatty alcohol polyoxyethylene ether, unitary unsaturated carboxylic acid and its 15 parts of derivative, alkene ether
6 parts of polyoxyethylene, 3 parts of catalyst, 0.2 part of gamma-polyglutamic acid, 3 parts of Artemisia Glue, 5 parts of microcrystalline cellulose, 2 parts of feather protein；Institute
State antifreeze includes according to the raw material of parts by weight：4 parts of 3- allyloxy -2- hydroxypropionate sodiums, 5 parts of allyl polyglycol,
20 parts of calcium chloride, 7 parts of ammonium sulfate, 15 parts of silicon ash, 10 parts of microdenier staple.
3. according to any anti-freezing type polycarboxylate water-reducers of claim 1-2, it is characterised in that the molecular weight regulator
1 is pressed for methylpropene sodium sulfonate and mercaptopropionic acid：The mixture that 4 ratio is mixed to get.
4. according to any anti-freezing type polycarboxylate water-reducers of claim 1-2, it is characterised in that the initiator is peroxide
Change dibenzoyl, two hexadecyl ester of dicetyl peroxydicarbonate and dicetyl peroxydicarbonate dihexyl.
5. according to any anti-freezing type polycarboxylate water-reducers of claim 1-2, it is characterised in that the catalyst is given birth to for dimension
Plain C, Ge(SO) and amion acetic acid propyl ester press 1：1.5：2 obtained mixtures.
6. the synthesis technique of a kind of anti-freezing type polycarboxylate water-reducer as described in claim 1-2 is any, it is characterised in that specific
Step is as follows：
(1) β-propyloic acrylic ester, fatty alcohol polyoxyethylene ether, unitary unsaturated carboxylic acid and its derivative, alkene ether are gathered
70-90 DEG C of stirring 0.5-1h obtains A liquid in the water of ethylene oxide addition 1/2-2/3 amounts；By hydrogen peroxide, maleic anhydride monomer, initiator,
Molecular weight regulator, catalyst, gamma-polyglutamic acid, Artemisia Glue, microcrystalline cellulose, feather protein are uniformly mixed to obtain B liquid；
(2) in a kettle, 100-140 parts of water and acrylic acid are added, sequentially adds the 3- allyloxy -2- hydroxyls in antifreeze
Propanesulfonate, allyl polyglycol, calcium chloride, ammonium sulfate, silicon ash, microdenier staple, after stirring evenly, A liquid and B liquid are pressed
The speed that 3-5h is dripped off is added dropwise into reaction kettle, after B liquid 5min is added dropwise first starts that A liquid is added dropwise again, in A liquid completion of dropwise addition
After continue stir 0.5-1h；
(3) product that step (2) obtains is added on liquid distribution trough by feeding valve, then is cast to by liquid distribution trough defeated
Send and take, conveyer belt at the uniform velocity advances in vacuum temp control case, controls the heating system of vacuum temp control case, makes in vacuum temp control case
Temperature is kept for 40-60 DEG C；The pace of conveyer belt is controlled, moisture is constantly evaporated, is exported from vacuum temp control case by conveyer belt
Material solid content >=95% taken out of；
(4) peel off：After material is taken out of by conveyer belt from the outlet of vacuum temp control case, continue, as conveyer belt is advanced forward, advancing
During, natural cooling；After material is with conveyor belt turn-over, peeled off by being arranged on the hoe scaler below conveyer belt；
(5) crush：After material is stripped knife stripping conveyer belt, under the action of self gravitation, fall into pulverizer, by pulverizer
Crushed, that is, anti-freezing type polycarboxylate water-reducer finished product is made.
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