CN106749970B - A kind of sheet polycarboxylic acid slump retaining agent and preparation method thereof admittedly - Google Patents
A kind of sheet polycarboxylic acid slump retaining agent and preparation method thereof admittedly Download PDFInfo
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- CN106749970B CN106749970B CN201611116665.4A CN201611116665A CN106749970B CN 106749970 B CN106749970 B CN 106749970B CN 201611116665 A CN201611116665 A CN 201611116665A CN 106749970 B CN106749970 B CN 106749970B
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F283/00—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G
- C08F283/06—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G on to polyethers, polyoxymethylenes or polyacetals
- C08F283/065—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G on to polyethers, polyoxymethylenes or polyacetals on to unsaturated polyethers, polyoxymethylenes or polyacetals
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B24/00—Use of organic materials as active ingredients for mortars, concrete or artificial stone, e.g. plasticisers
- C04B24/16—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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- 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
- C04B2103/308—Slump-loss preventing agents
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- Engineering & Computer Science (AREA)
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Abstract
The invention discloses a kind of solid sheet polycarboxylic acid slump retaining agents and preparation method thereof.Specific step is as follows: 805-845 parts of polyether macromonomers being placed in reaction kettle, heating stirring, until dissolution is complete；Equilibrium temperature is 65-75 DEG C, disposably puts into 5-10 parts of weak chain-transferring agents, 2.0-4.5 parts of organic peroxy class initiators, 5.5-10.5 parts of unsaturated dicarboxylic acids and 5.0-11.5 parts of unsaturated sulfonic acid class minor comonomers；Then, the 5-10 parts of concentrated sulfuric acids, adjustment bottom liquid pH value to 5.0 is added；Start the mixed solution that 35-65 parts of acrylic acid, 70-115 parts of acrylic acid hydroxy alkyl esters and 2.8-4.6 parts strong chain-transferring agent are added dropwise, during dropwise addition, puts into azo-initiator in two times；After being added dropwise, 1-2h is cured, 5.5-12.0 parts of neutralizers are added, are sliced after cooling to get finished product.The solid sheet polycarboxylate water-reducer, convenient for storage, long-distance transportation logistics cost is low, completely water-soluble, is suitable for cement-based gelling material civil engineering.
Description
Technical field
The present invention relates to a kind of cement-based gelling material polycarboxylate water-reducers, are adapted to the storage of additive mother liquor and pin
Sell-production area haul distance too far the case where, and in particular to a kind of solid sheet polycarboxylate water-reducer and preparation method thereof.
Background technique
Poly carboxylic acid series water reducer preparation at present is based on liquid, and mother liquor solid content is within the scope of 35-60%, long-distance transportation
Cost limitation manufacturing enterprise operation region.Polycarboxylate water-reducer mainly passes through also with the presence of a small amount of powder in the market
Spray drying gained is heated to liquid polycarboxylate water-reducer, since its application field is mostly dry method mortar, grouting agent, Self-leveling sand
Slurry etc. is special engineered.It is usually outer to mix auxiliary agent to adjust mortar workability and pulvis cost, diminishing for the workability for guaranteeing mortar
Rate and price have not been suitable for general quotient's concrete concrete works needs.Exploitation is not necessarily to heat spraying solid polycarboxylic acids product, is
It reduces transportation cost and promotes polycarboxylate water-reducer in the widely used essential condition in various regions, solid state is also not limited to powder
Shape has good water solubility.
102993387 A of CN discloses the method that a step directly synthesizes pure solid high-performance polycarboxylate water-reducer, with propylene
Acid compounds and unsaturated polyoxyethylene ether are polymerization reaction monomer, molecular weight regulator are added, under the action of initiator
It is made in the environment of without any solvent by free radical bulk polymerization.Process of the present invention controllability is strong, the degree of polymerization is high, at
This is cheap, environment friendly and pollution-free, and the preparation of complete anhydrous pure solid high-performance polycarboxylate water-reducer is realized by bulk polymerization,
Not only have flowing degree of net paste of cement similar in the polycarboxylate water-reducer for polymerizeing preparation with regular solution and holding capacity, cement suitable
Ying Xing, concrete application performance can be prepared any according to actual needs simultaneously because the product of direct polymerization is anhydrous pure solid
Strength solution.
105061690 A of CN discloses a kind of preparation method of high water reduction type solid high-performance polycarboxylate water-reducer, specifically
Steps are as follows: after the unsaturated polyoxyethylene ether combination polymeric monomer heating melting of two kinds of different molecular weights, acting in initiator
The lower mixed liquor that unsaturated carboxylic acid class minor comonomer, unsaturated acyl amine minor comonomer and chain-transferring agent is added dropwise, by poly- from basic body
Close reaction be made, use after the reaction was completed neutralizer adjustment pH for 5-6, cooling after by grinding be solid granular.
104628969 A of CN discloses a kind of preparation method of slow-release solid polycarboxylate water-reducer, has first with amine
Machine small molecule pre-processes the carboxylic acids minor comonomer containing unsaturated double-bond；Then by above-mentioned pretreated unsaturation third
After olefin(e) acid class minor comonomer and unsaturated polyoxyethylene ether polymeric monomer heating melting, it is added dropwise not under initiator and chain-transferring agent effect
It is saturated esters minor comonomer, reaction process is placed in the environment of anhydrous organic solvent-free to be made by bulk polymerization.
Summary of the invention
Technical problem to be solved by the invention is to provide a kind of solid sheet polycarboxylic acid slump retaining agents, are polymerize by following each components
It forms, total mass of raw material is 1000 parts, and each component includes:
Polyether macromonomer: 800-830；
Unsaturated dicarboxylic acid: 5.5-10.5；
Unsaturated sulfonic acid class minor comonomer: 5.0-11.5；
Weak chain-transferring agent: 5-10；
Peroxide type initiators: 2.0 ~ 4.5；
The concentrated sulfuric acid: 5-10；
Acrylic acid: 35-65；
Acrylic acid hydroxy alkyl ester: 70-115；
Azo-initiator: 2.0-6.0；
Strong chain-transferring agent: 2.8 ~ 4.6；
Neutralizer: 5.5-12.0.
The polyether macromonomer is allyl polyethenoxy ether, methyl allyl polyoxyethylene ether, prenol polyoxy second
One or more of compositions of alkene ether, vinyl butyl ether polyoxyethylene ether；Anhydrous solvent-free in view of synthetic system, viscosity is larger,
It is necessary to select the polyether macromonomer of high reaction activity, preferably isoamyl alcohol polyoxyethylene ether, vinyl butyl ether polyoxy second
One or two kinds of compositions of alkene ether；
The polyether macromonomer judges from the angle of slump retaining, preferably isoamyl alcohol polyoxyethylene ether；
The unsaturated dicarboxylic acid is one or two kinds of compositions of itaconic acid, fumaric acid；
The weak chain-transferring agent is one or more of compositions of sodium hypophosphite, sodium formate, polyphosphate sodium；
The unsaturated sulfonic acid class minor comonomer is sodium vinyl sulfonate, acrylic sodium sulfonate, methylpropene sodium sulfonate, benzene second
One or more of compositions of alkene sodium sulfonate, 2- acrylamide-2-methyl propane sulfonic；The sulphonic acids chain-transferring agent preferably reacts
The biggish sulphonic acids chain-transferring agent of activity, i.e. one kind or several of sodium vinyl sulfonate, acrylic sodium sulfonate, methylpropene sodium sulfonate
Kind composition；
The concentrated sulfuric acid is the H that mass fraction is 98.3%2SO4Solution.
The peroxide type initiators be isopropyl benzene hydroperoxide, tert-butyl hydroperoxide, cumyl peroxide,
Di-t-butyl peroxide, dibenzoyl peroxide, dilauroyl peroxide, peroxidized t-butyl perbenzoate, peroxidating trimethylacetic acid uncle
Butyl ester, di-isopropyl peroxydicarbonate, the one or more of of di-cyclohexylperoxy di-carbonate form；The organic peroxy
Half-life period is dilauroyl peroxide, the peroxidating trimethylacetic acid tert-butyl ester, mistake of 1h at 65-75 DEG C of class initiator preferably synthetic temperature
Aoxidize one or more of compositions of two dicyclohexyl carbonates；
The azo-initiator is azodiisobutyronitrile, azobisisoheptonitrile, azo-bis-iso-dimethyl, azo
Isobutyl cyano formamide, two isobutyl imidazoline hydrochloride of azo, the one or more of of azo-bis-isobutyrate hydrochloride form；It is described
Azo-initiator be preferably oiliness azo-initiator, i.e. azodiisobutyronitrile, azobisisoheptonitrile, two isobutyric acid of azo
One or more of compositions of dimethyl ester, azo isobutyl cyano formamide；
The strong chain-transferring agent is aliphatic mercaptan, lauryl mercaptan, dithioesters, mercaptopropionic acid, thioacetic acid, mercapto
One or more of compositions of base ethyl alcohol, mercaprol；The strong chain-transferring agent is preferably oiliness or alcohols chain-transferring agent, i.e. rouge
Fat race mercaptan, lauryl mercaptan, dithioesters, mercaptoethanol, the one or more of of mercaprol form；
The acrylic acid hydroxy alkyl ester is one or two kinds of compositions of hydroxy-ethyl acrylate and hydroxypropyl acrylate；It is described
Acrylic acid hydroxy alkyl ester be preferably hydroxy-ethyl acrylate and hydroxypropyl acrylate composition；The acrylic acid hydroxy alkyl ester
Preferably mass ratio is the hydroxy-ethyl acrylate of 1:1 and the composition of hydroxypropyl acrylate.
The neutralizer is sodium hydroxide, potassium hydroxide, triethanolamine, diethanol amine, triisopropanolamine, diisopropanol
One or more of compositions of amine, monoisopropanolamine；It is not easy in view of sodium hydroxide, potassium hydroxide dissolution, triethanolamine, diethanol amine
Excite C3A mineral aquation causes to adsorb water-reducing agent, and the neutralizer is preferably triisopropanolamine, diisopropanolamine (DIPA), an isopropyl
One or more of compositions of hydramine.
A kind of preparation method of solid sheet polycarboxylic acid slump retaining agent of the invention, successively includes following operating procedure:
(1) polyether macromonomer is placed in reaction vessel, does not add water and any organic solvent, is heated to 65-75 DEG C；
Stirring is up to no obvious bulk or sheet material；
(2) by weak chain-transferring agent, peroxide type initiators, unsaturated dicarboxylic acid and unsaturated sulfonic acid class minor comonomer
It is added in the polyether macromonomer melted；Add the 5-20 parts of concentrated sulfuric acids, adjustment pH value to 5.0；
(3) start the mixed solution that acrylic acid, acrylic acid hydroxy alkyl ester and strong chain-transferring agent is added dropwise, time for adding is that a is small
When；After when dropwise addition a/3 is small, the disposable azo-initiator for putting into half amount；After when dropwise addition 2a/3 is small, disposably
Put into the azo-initiator of remaining half amount；
(4) after being added dropwise, 1-2h is cured, is cooled to 30 DEG C, neutralizer is added, stirs evenly, is sliced after cooling, i.e.,
Obtain finished product.
Time for adding a described in step (4) is 2-4h.
The beneficial effects of the present invention are:
1. acrylic acid dosage is relatively fewer in slump retaining agent, be not suitable for first throwing, but to ensure that the pH value of bottom material is in faintly acid
Range adds sulfuric acid to adjust, and the conversion ratio of initiator can be improved in weak acid environment.By 65 ~ 75 degree of half-life period 1h strong initiation
Agent-initiation of the organic peroxy class initiator as the initial stage of acrylic acid in bottom material and unsaturated dicarboxylic acid, in synthesis
In the stage afterwards, supplement, which is stablized, in two times decomposes azo-initiator without induction, makes up under high viscosity environment polymer as far as possible to drawing
The cage effect of agent is sent out with side reaction；The multiple elements design of initiator causes and alternately supplement initiation is to ensure that the anhydrous nothing of the high viscosity
The high conversion of polymerization reaction under solvent.
2. unsaturated dicarboxylic acid minor comonomer mass ratio is unsaturated in synthetic ratio design on an equal basis under anchoring adsorption capacity
The quality of monocarboxylic acid minor comonomer is small, synthesizes the anchoring contact point three dimensional stress of short-chain branch, and the design of polyether macromonomer dosage can be inclined
Greatly, branch chain density is relatively higher, and slump retaining is more preferably；In high-temperature high viscosity polymerization reaction, acrylic acid is easy autohemagglutination, the bottom of at
It is added weak chain-transferring agent in material, and the strong chain-transferring agent of simultaneously match in conjunction with the polynary design of initiator prevents third during being added dropwise
A possibility that olefin(e) acid autohemagglutination or too long polycarboxylic acids molecular backbone.
Specific embodiment
Below by example, the present invention will be further elaborated, and following the description is not right only for explaining the present invention
Content is defined.
Embodiment 1
A kind of solid sheet polycarboxylic acid slump retaining agent ontology, the water-reducing agent are polymerized by following each components, and total mass of raw material is
1000 parts, each component and technological parameter are as follows:
810 parts of allyl polyethenoxy ethers are placed in reaction vessel, water and any organic solvent is not added, is heated to 65
℃；It is slowly stirred, control revolving speed is 15 rpm/min, until solution is without obvious bulk or sheet material；
Until allyl polyethenoxy ether dissolution is completely, quickening speed of agitator to 85 rpm/min, and continue to stir；
5.5 parts of sodium hypophosphites, 2.2 parts of dilauroyl peroxides, 5.8 parts of itaconic acids and 6.5 parts of sodium vinyl sulfonates are placed in
In the polyether macromonomer melted；Add 7.5 parts of concentrated sulfuric acids, adjustment bottom liquid pH value to 5.0；
After being added at one time above-mentioned material, start that 48.5 parts of acrylic acid, 100 parts of hydroxy-ethyl acrylates and 3.5 part ten are added dropwise
The mixed solution of dialkyl group mercaptan, time for adding are 3 hours；After when dropwise addition 1 is small, 2 parts of azo isobutyl cyano are disposably put into
Formamide；After when dropwise addition 2 is small, property puts into 2 parts of azo isobutyl cyano formamides again；
After being added dropwise, 1h is cured, 30 DEG C is cooled to, is slowly added to 6.5 parts of triisopropanolamines, stirs evenly, it is then, cold
But it is sliced afterwards to get finished product.
Embodiment 2
A kind of solid sheet polycarboxylic acid slump retaining agent ontology, the water-reducing agent are polymerized by following each components, and total mass of raw material is
1000 parts, each component and technological parameter are as follows:
822 parts of isoamyl alcohol polyoxyethylene ethers are placed in reaction vessel, water and any organic solvent is not added, is heated to
70℃；It is slowly stirred, control revolving speed is 20 rpm/min, until solution is without obvious bulk or sheet material；
Until isoamyl alcohol polyoxyethylene ether dissolution is completely, quickening speed of agitator to 90 rpm/min, and continue to stir；
By 5 parts of sodium hypophosphites, 1.5 parts of sodium tripolyphosphates, 3.5 parts of peroxidating trimethylacetic acid tert-butyl esters, 7.5 parts of fumaric acid and
7.6 parts of acrylic sodium sulfonates are placed in the polyether macromonomer melted；9.5 parts of concentrated sulfuric acids are added, adjustment bottom liquid pH value is extremely
5.0；
After being added at one time above-mentioned material, start that 56.5 parts of acrylic acid, 71.4 parts of hydroxypropyl acrylates and 4.5 parts of mercaptos are added dropwise
The mixed solution of base ethyl alcohol, time for adding are 2.5 hours；After when dropwise addition 2.5/3 is small, it is different disposably to put into 1.5 parts of azos two
Butyronitrile；After when dropwise addition 5/3 is small, property puts into 1.5 parts of azodiisobutyronitriles again；
After being added dropwise, 2h is cured, 30 DEG C is cooled to, is slowly added to 8 parts of diisopropanolamine (DIPA)s, stirs evenly, it is then, cooling
After be sliced to get finished product.
Embodiment 3
A kind of solid sheet polycarboxylic acid slump retaining agent ontology, the water-reducing agent are polymerized by following each components, and total mass of raw material is
1000 parts, each component and technological parameter are as follows:
805 parts of vinyl butyl ether polyoxyethylene ether are placed in reaction vessel, water and any organic solvent is not added, adds
Heat is to 75 DEG C；It is slowly stirred, control revolving speed is 30rpm/min, until solution is without obvious bulk or sheet material；
Until the dissolution of vinyl butyl ether polyoxyethylene is completely, quickening speed of agitator to 100rpm/min, and continue to stir；
By 8.5 parts of sodium tripolyphosphates, 4.2 parts of di-cyclohexylperoxy di-carbonates, 9.1 parts of fumaric acid and 10.7 parts of methyl-props
Alkene sodium sulfonate is placed in the polyether macromonomer melted；Add 5.5 parts of concentrated sulfuric acids, adjustment bottom liquid pH value to 5.0；
After being added at one time above-mentioned material, start that 36.5 parts of acrylic acid, 50 parts of hydroxy-ethyl acrylates, 50 parts of acrylic acid are added dropwise
The mixed solution of hydroxypropyl acrylate and 4.5 parts of mercaprols, time for adding are 4 hours；After when dropwise addition 4/3 is small, 2.5 are disposably put into
Part azo-bis-iso-dimethyl；After when dropwise addition 8/3 is small, property puts into 2.5 parts of azo-bis-iso-dimethyls again；
After being added dropwise, 1.5h is cured, 30 DEG C is cooled to, is slowly added to 10 parts of monoisopropanolamines, stirs evenly, then,
Slice is after cooling to get finished product.
Solid sheet polycarboxylic acid slump retaining agent and water prepared by embodiment 1,2,3 are dissolved in water in the ratio of 4:6, determine that its is water-soluble
Property is preferable.
Solid sheet polycarboxylic acid slump retaining agent and the common polycarboxylic acid slump retaining agent mother liquor for testing above-described embodiment 1,2,3 respectively are same
Cement paste initial fluidity, 1,2h mobility and concrete initial slump/divergence under concentration and through when the slump/expansion
The latitude of emulsion.Testing cement used is new 42.5 ordinary portland cement of China, with reference to GB/8076-2008 " concrete admixture " testing standard.
Different slump retaining agents influence pulp flowage
| Water-reducing agent type | Initial fluidity mm | 1h mobility mm | 2h mobility mm |
| Common slump retaining agent | - | 240 | 210 |
| Embodiment 1 | - | 235 | 230 |
| Embodiment 2 | - | 225 | 230 |
| Embodiment 3 | - | 230 | 245 |
Different slump retaining agents influence concrete flowability
| Water-reducing agent type | Initial slump/divergence mm | Through when the slump/divergence mm |
| Ordinary water-reducing agent | 160/420 | 190/520 |
| Embodiment 1 | 150/400 | 185/510 |
| Embodiment 2 | 165/435 | 195/525 |
| Embodiment 3 | 160/410 | 190/530 |
According to above-mentioned initial fluidity, 1,2h mobility and concrete it is initial and through when mobility compare, Gu the poly- carboxylic of sheet
The more common slump retaining agent mother liquor of the net slurry initial fluidity of sour slump retaining agent embodiment 1,2,3 is slightly not good enough, but slump retaining is preferable；Coagulation
Native mobility data comparison, the function of slump protection of embodiment 1,2,3 reach unanimity or slightly better with common, and overall data explanation should
Gu sheet polycarboxylic acid slump retaining agent formula and mature preparation process are reliable, in high viscosity reaction environment, high conversion rate, with liquid at this stage
40% slump retaining agent mother liquor performance of body reaches unanimity, and slump retaining is slightly good.
Claims (6)
1. a kind of preparation method of solid sheet polycarboxylic acid slump retaining agent, the solid sheet polycarboxylic acid slump retaining agent are polymerize by following each components
It forms, total mass of raw material is 1000 parts, and each component includes:
Polyether macromonomer: 800-830 parts；
Unsaturated dicarboxylic acid: 5.5-10.5 parts；
Unsaturated sulfonic acid class minor comonomer: 5.0-11.5 parts；
Weak chain-transferring agent: 5-10 parts；
Peroxide type initiators: 2.0-4.5 parts；
The concentrated sulfuric acid: 5-10 parts；
Acrylic acid: 35-65 parts；
Acrylic acid hydroxy alkyl ester: 70-115 parts；
Azo-initiator: 2.0-6.0 parts；
Strong chain-transferring agent: 2.8-4.6 parts；
Neutralizer: 5.5-12.0 parts；
It is characterized in that, preparation method successively includes following operating procedure:
(1) polyether macromonomer is placed in reaction vessel, does not add water and any organic solvent, is heated to 65-75 DEG C；Stirring is straight
To no obvious bulk or sheet material；
(2) weak chain-transferring agent, peroxide type initiators, unsaturated dicarboxylic acid and unsaturated sulfonic acid class minor comonomer are added
In the polyether macromonomer of thawing；Add the 5-10 parts of concentrated sulfuric acids, adjustment pH value to 5.0；
(3) start the mixed solution that acrylic acid, acrylic acid hydroxy alkyl ester and strong chain-transferring agent is added dropwise, time for adding is a hours, drop
A is 2-4h between added-time；After when dropwise addition a/3 is small, the disposable azo-initiator for putting into half amount；When being added dropwise, 2a/3 is small
Shi Hou, the disposable azo-initiator for putting into remaining half amount；
(4) after being added dropwise, cure 1-2h, be cooled to 30 DEG C, neutralizer is added, stirs evenly, it is cooling after slice to get at
Product；
The polyether macromonomer be allyl polyethenoxy ether, methyl allyl polyoxyethylene ether, isoamyl alcohol polyoxyethylene ether,
One or more of compositions of vinyl butyl ether polyoxyethylene ether；
The unsaturated dicarboxylic acid is one or two kinds of compositions of itaconic acid, fumaric acid；
The weak chain-transferring agent is one or more of compositions of sodium hypophosphite, sodium formate, polyphosphate sodium；
The unsaturated sulfonic acid class minor comonomer is sodium vinyl sulfonate, acrylic sodium sulfonate, methylpropene sodium sulfonate, styrene sulphur
One or more of compositions of sour sodium, 2- acrylamide-2-methyl propane sulfonic；
The peroxide type initiators are dilauroyl peroxide, the peroxidating trimethylacetic acid tert-butyl ester, two ring of dicetyl peroxydicarbonate
One or more of compositions of own ester.
2. preparation method according to claim 1, which is characterized in that the azo-initiator is two isobutyl of azo
Nitrile, azobisisoheptonitrile, azo-bis-iso-dimethyl, azo isobutyl cyano formamide, two isobutyl imidazoline hydrochloride of azo,
One or more of compositions of azo-bis-isobutyrate hydrochloride.
3. preparation method according to claim 1, which is characterized in that the strong chain-transferring agent be lauryl mercaptan,
Dithioesters, mercaptopropionic acid, thioacetic acid, mercaptoethanol, the one or more of of mercaprol form.
4. preparation method according to claim 1, which is characterized in that the acrylic acid hydroxy alkyl ester is acrylic acid hydroxyl second
One or two kinds of compositions of ester and hydroxypropyl acrylate.
5. preparation method according to claim 1, which is characterized in that the neutralizer be sodium hydroxide, potassium hydroxide,
Triethanolamine, diethanol amine, triisopropanolamine, diisopropanolamine (DIPA), the one or more of of monoisopropanolamine form.
6. preparation method according to claim 1, which is characterized in that the concentrated sulfuric acid is that mass fraction is 98.3%
H2SO4Solution.
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| CN107325236A (en) * | 2017-07-15 | 2017-11-07 | 刘翠芬 | A kind of non-soil responsive type polycarboxylate water-reducer and preparation method thereof |
| CN108503255A (en) * | 2018-03-30 | 2018-09-07 | 湖北工业大学 | A kind of preparation method of the solid sheet polycarboxylic acid slump retaining agent of bulk polymerization |
| CN110845172A (en) * | 2018-08-20 | 2020-02-28 | 辽宁奥克化学股份有限公司 | Preparation method of solid polycarboxylic acid slump retaining agent |
| CN111170671A (en) * | 2018-11-13 | 2020-05-19 | 北京市建筑工程研究院有限责任公司 | Preparation method of slump-retaining solid polycarboxylate superplasticizer |
| CN109880020B (en) * | 2019-01-28 | 2021-05-25 | 中铁四局集团有限公司 | Concrete workability regulator and preparation method thereof |
| CN110951008A (en) * | 2019-11-19 | 2020-04-03 | 湖北工业大学 | Solid sheet-shaped polycarboxylic slump retaining agent prepared by soap-free emulsion polymerization method and method |
| CN110951010A (en) * | 2019-11-19 | 2020-04-03 | 湖北工业大学 | Solid sheet-shaped polycarboxylic slump retaining agent and method for preparing same by using ultra-concentrated emulsion method |
| CN112851877A (en) * | 2020-12-31 | 2021-05-28 | 陕西友邦新材料科技有限公司 | Solid polycarboxylic acid water reducing agent and preparation method thereof |
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| CN105061690A (en) * | 2015-07-22 | 2015-11-18 | 江苏奥莱特新材料有限公司 | Preparation method for high performance water reducer made from high water reducing solid polycarboxylic acid |
| CN105801764A (en) * | 2016-02-25 | 2016-07-27 | 南京师范大学 | Preparation method of all-solid high-performance polycarboxylate superplasticizer |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102993387A (en) * | 2012-09-13 | 2013-03-27 | 北京工业大学 | Method for directly synthesizing pure solid high-performance polycarboxylate water-reducer in one step |
| CN105017490A (en) * | 2015-07-14 | 2015-11-04 | 唐山市龙亿科技开发有限公司 | Method for preparing polycarboxylate superplasticizer by nonaqueous technique |
| CN105061689A (en) * | 2015-07-17 | 2015-11-18 | 北京市建筑工程研究院有限责任公司 | Preparation method of powdery polycarboxylic acid high-performance water reducing agent |
| CN105061690A (en) * | 2015-07-22 | 2015-11-18 | 江苏奥莱特新材料有限公司 | Preparation method for high performance water reducer made from high water reducing solid polycarboxylic acid |
| CN105801764A (en) * | 2016-02-25 | 2016-07-27 | 南京师范大学 | Preparation method of all-solid high-performance polycarboxylate superplasticizer |
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