CN108516724A - A kind of double preparation methods for causing high stability polycarboxylate water-reducer - Google Patents
A kind of double preparation methods for causing high stability polycarboxylate water-reducer Download PDFInfo
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- CN108516724A CN108516724A CN201810295002.6A CN201810295002A CN108516724A CN 108516724 A CN108516724 A CN 108516724A CN 201810295002 A CN201810295002 A CN 201810295002A CN 108516724 A CN108516724 A CN 108516724A
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B40/00—Processes, in general, for influencing or modifying the properties of mortars, concrete or artificial stone compositions, e.g. their setting or hardening ability
- C04B40/0028—Aspects relating to the mixing step of the mortar preparation
- C04B40/0039—Premixtures of ingredients
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F2/00—Processes of polymerisation
- C08F2/38—Polymerisation using regulators, e.g. chain terminating agents, e.g. telomerisation
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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
- 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
- C08F4/00—Polymerisation catalysts
- C08F4/04—Azo-compounds
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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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Abstract
The present invention provides a kind of double preparation methods for causing high stability polycarboxylate water-reducer, includes the following steps：1) a certain proportion of polyether macromonomer and water are added in reaction kettle, agitating and heating waits for its dissolving；2) control temperature is initially added into a certain amount of hydrogen peroxide, bleeding agent, chain-transferring agent at 50 58 DEG C；3) after 5min, start that solution B is added dropwise, 10min starts that solution A is added dropwise, and solution A time for adding is a hours, and solution B time for adding is a+0.5 hours；Solution A is made of a certain proportion of acrylic acid and water, and solution B is made of medium temperature initiator, alcohol organic solvent and water；4) after completion of dropwise addition, keep temperature constant, curing causes high stability polycarboxylate water-reducer in b hours to get described one kind is double.The present invention is selected by rational technological design and raw material, and the polycarboxylate water-reducer water-reducing rate of preparation is high, adaptability is good, stability is high, the anti-adsorption capacity of anti-mud is strong, has excellent concrete workability.
Description
Technical field
The invention belongs to building material technical fields, are related to concrete admixture field, and specifically a kind of double initiations are high
The preparation method of stability polycarboxylate water-reducer.
Background technology
With the rapid development of technology of high performance concrete, requirement of the engineer application for water-reducing agent performance also constantly carries
It is high.With the continuous propulsion of engineering construction, various trans-regional, cross-region engineering projects continue to bring out, and polycarboxylate water-reducer exists
The case where often will appear " not acclimatized " during use；It is excellent along with sandstone material is limited by regions and multifarious
The influence for the problems such as matter sand and stone resources are again increasingly in short supply, the polycarboxylic acids that market is stable to performance, adaptability is good, water-reducing rate is high
Water-reducing agent is in great demand.
It takes suitable technique and raw material to select, prepares molecular weight stabilizers distribution, the good polycarboxylic acids diminishing of adaptability
Agent, one of key are the selections of initiator, must allow the steady controllable of initiation system；Moreover, double initiation systems are conducive to selectivity
Prepare specific molecular configuration.
Patent CN106046269A discloses a kind of preparation side of cross-linking type muting sensitive sense ester ether copoly type polycarboxylate water-reducer
Method, the invention is by hydroxyl butyl vinyl polyoxyethylene ether, unsaturated acids, unsaturated phosphate monoester and unsaturated di-phosphate ester
Polycarboxylate water-reducer made of copolymerization has higher water-reducing rate under the synergistic effect of various groups, has certain guarantor
Collapsing property, workability, anti-mud and low-dosage sensibility.
Patent CN106008854A discloses a kind of preparation method of polycarboxylate water-reducer, which is specifically：Water,
In the presence of water-soluble chain transfer agent and radical initiator, at a temperature of between 5 DEG C with 45 DEG C so that following substance occurs
Reaction：At least one unsaturated carboxylic acid；And at least one polyethers, there is the polymer that can be formed with unsaturated carboxylic acid
The free hydroxyl that reacts of carboxyl functional group.The preparation method of the polycarboxylate water-reducer of the invention reacts mild, operation side
Just, raw material selection is free.
Patent CN106008853A discloses a kind of preparation method of anti-mud collapse protection type phosphate ester-containing based polycarboxylic acid water-reducing agent,
Specific step is first prepares the polycarboxylate water-reducer performed polymer containing halogen, then by the polycarboxylate water-reducer performed polymer containing halogen
Polymerisation is carried out with alkyl phosphate and obtains the copolymerization product of phosphoric acid ester group, adjusts pH value after the completion of reaction, water is added to obtain
Poly carboxylic acid series water reducer.The polycarboxylate water-reducer has the advantages that volume is low, water-reducing rate is high, it is strong to protect time of collapsing long and anti-mud.
It is different from the above patent, the method that the present invention goes residual initiator using curing is heated after double initiations-uses initiation
The stable medium temperature initiator of effect, and selected by the technological design of optimization and raw material, it is ripe for a long time that curing method is heated after
Change, removes extra initiator, obtain the diminishing agent molecule of more reasonable structure.Final to prepare water-reducing rate height, adaptability is good, resists
The anti-adsorption capacity of mud is strong, the high polycarboxylate water-reducer of stability.
Invention content
Technical problem to be solved by the present invention lies in provide a kind of double preparations for causing high stability polycarboxylate water-reducer
Method.
Polycarboxylate water-reducer is in use, however it remains some problems, it is more perfect that performance is developed in an urgent demand
High-performance water reducing agent, meet the needs of different engineerings, varying environment are to concrete performance Multifunctional multilayer time.
The present invention first uses hydrogen peroxide work is initial to cause using double methods caused, drives reaction progress, reuses initiation
The stable medium temperature initiator of effect carries out continuing to be added dropwise causing, and obtains the initiation system that transition is steady, process is controllable.
The invention selects the medium temperature initiator of suitable half-life period for the technological temperature of reaction, it is not easy to induction point occur
Solution, is easy to form the polymer of high molecule mass；Novel carboxylic function monomer is introduced, using its special structure with linked rings, is generated
Good anti-mud effect；The bleeding agent of introducing has hydrophilic radical, is aligned in the surface energy of solution, and can make surface
Power is remarkably decreased, and obtains excellent emulsification, dispersibility, and each component raw material is enable to be sufficiently mixed reaction, greatly improves reaction effect
Rate and monomer conversion.It is cured for a long time using the rear way of distillation, extra initiator is removed, after eliminating residual initiator water-reducing agent
The unstability of phase performance influences, and promotes the reaction was complete to carry out, and obtains the diminishing agent molecule of more reasonable structure.Final system
High for water-reducing rate is gone out, adaptability is good, and the anti-anti- adsorption capacity of mud is strong, the good polycarboxylate water-reducer of workability.
Technical scheme is as follows：
A kind of double preparation methods for causing high stability polycarboxylate water-reducer, double initiation high stability polycarboxylic acids diminishings
Agent is mainly prepared from the following components：Polyether macromonomer, medium temperature releaser, alcohol organic solvent, hydrogen peroxide, acrylic acid, chain
Transfer agent, bleeding agent, neutralizer, water；1000 parts of gross mass, preparation method includes the following steps：
1) 390-420 parts of polyether macromonomers and 200-240 parts of water are added in reaction kettle, agitating and heating waits for its dissolving；
2) temperature in the kettle is measured, control temperature after temperature is stablized, is added at one time 0.1-0.3 parts of infiltrations at 50-58 DEG C
Agent, 3-7 parts of chain-transferring agents, 0.2-0.5 parts of hydrogen peroxide；
3) after 5min, start that solution B, solution A is added dropwise successively, start to be added dropwise after solution B is added dropwise, in 10min molten
Liquid A, solution A time for adding are a hours, and solution B time for adding is a+0.5 hours；Solution B is caused by 2.5-4.5 parts of medium temperatures
Agent, 10-15 parts of alcohol organic solvents and 50-60 parts of water compositions, solution A are made of 55-75 parts of acrylic acid and 60-70 parts of water；
4) after completion of dropwise addition, 65-70 DEG C is heated, keeps temperature constant, cures b hours, waits for that reaction solution temperature is less than
At 30 DEG C, be slowly added to 6-11 parts of neutralizers, moisturizing to 1000 parts be 50% to get mass fraction double initiation high stabilities
Polycarboxylate water-reducer finished product.
The polyether macromonomer is by allyl polyethenoxy ether, methyl allyl polyoxyethylene ether, prenol polyoxy second
One or more of alkene ether, vinyl butyl ether polyoxyethylene ether form；It is preferred that isoamyl alcohol polyoxyethylene ether.
The medium temperature initiator is initiator of the 1h half life temperatures at 50-75 DEG C, specifically by azobisisoheptonitrile, azo
One or more of dicyano valeric acid, di-isopropyl peroxydicarbonate, di-cyclohexylperoxy di-carbonate form；It is preferred that
Mass ratio is 1:1 is the composition of azobisisoheptonitrile and azo dicyano valeric acid.
The alcohol organic solvent is by one or more of methanol, ethyl alcohol, benzyl alcohol, ethylene glycol, propylene glycol, glycerine
Composition；It is preferred that the alcohol with certain chain transfer ability；Preferred mass ratio is 1:1 ethyl alcohol and the composition of propylene glycol.
The bleeding agent is by sulfated castor oil, sodium alkyl sulfonate, sodium alkyl benzene sulfonate, alkyl sulfate sodium, secondary alkyl
Sodium sulfonate, secondary alkyl sulphate sodium, Negel, succinic acid alkyl ester sulfonate sodium, one kind in sulfamic acid sodium or several
Kind composition；Preferred anionic type bleeding agent；Preferred mass ratio is 1:1 sodium alkyl sulfonate and the composition of sodium alkyl benzene sulfonate.
The chain-transferring agent is by thioacetic acid, mercaptopropionic acid, mercaptoethanol, sodium vinyl sulfonate, acrylic sodium sulfonate, first
One or more of base sodium allylsulfonate, sodium styrene sulfonate, 2- acrylamide-2-methyl propane sulfonics, sodium hypophosphite group
At；It is preferred that weak chain-transferring agent；Preferred mass ratio is 1:1 sodium vinyl sulfonate and the composition of sodium hypophosphite.
The neutralizer is sodium hydroxide, potassium hydroxide, sodium carbonate, sodium bicarbonate, potassium carbonate, sodium methoxide, sodium ethoxide, second
One or more of hydramine, diethanol amine, triethanolamine, triisopropanolamine form；Preferred mass ratio is 1:1 three ethyl alcohol
The composition of amine and triisopropanolamine.
The hydrogen peroxide is that mass percent is 27.5% industrial grade hydrogen peroxide.
The solution A time for adding a is 2-4h；Preferably 2.5h.
The curing time b is 1-3h；Preferably 1.5h.
The beneficial effects of the invention are as follows：
1, it using the method for double initiations, first uses hydrogen peroxide to make initial initiation, drives reaction to carry out, reuse initiation effect
Stable medium temperature initiator carries out continuing to be added dropwise causing, and obtains the initiation system that transition is steady, process is controllable；Medium temperature initiator
Induction is less likely to occur to decompose, is easy to form the polymer of high molecule mass；In conjunction with entire reaction process temperature, selection partly declines
The slightly lower medium temperature initiator of phase temperature coordinates the alcohol organic solvent with certain chain tra nsfer function, and azo-initiator is molten
It is re-dissolved in water after alcohols, using the method being at the uniform velocity added dropwise, rationally controls reaction rate, is conducive to industrial production.
2, the bleeding agent introduced has hydrophilic radical, is aligned in the surface energy of solution, and surface tension can be made notable
Decline, obtains excellent emulsification, dispersibility, each component raw material is enable to be sufficiently mixed reaction, greatly improve reaction efficiency and list
Transformation rate；And the bleeding agent introduced belongs to anion surfactant, even if final residue also contributes to pair in the product
The peptizaiton of cement slurry.
3, residual method is heated after, two-part temperature, the later stage carries out long-time heat preservation curing, by composite initiation system
In remaining initiator eliminated in heating maturing process, prevent residual initiator to the unstable of water-reducing agent later stage performance
Property influence, moreover it is possible to promote the reaction was complete carry out, water-reducing agent molecular weight can be allowed more optimized, obtain ideal molecular weight and molecule structure
Type.
4, it is selected by rational technological design and raw material, the polycarboxylate water-reducer water-reducing rate height of preparation, adaptability are good, steady
Qualitative height, the anti-anti- adsorption capacity of mud are strong, have excellent concrete workability.
Specific implementation mode
For the ease of those of ordinary skill in the art understand and implement the present invention, with reference to embodiment to the present invention make into
The detailed description of one step, it should be appreciated that embodiment described herein is merely to illustrate and explain the present invention, and is not had to
It is of the invention in limiting.
Embodiment 1
A kind of double preparation methods for causing high stability polycarboxylate water-reducer, double initiation high stability polycarboxylic acids diminishings
Agent is prepared from the following components：Polyether macromonomer, medium temperature releaser, alcohol organic solvent, hydrogen peroxide, acrylic acid, chain tra nsfer
Agent, bleeding agent, neutralizer, water；1000 parts of gross mass, preparation method includes the following steps：
1) 410 parts of isoamyl alcohol polyoxyethylene ethers and 200 parts of water are added in reaction kettle, agitating and heating waits for its dissolving；
2) temperature in the kettle is measured, control temperature is at 50 DEG C, and after temperature is stablized, it is 1 to be added at one time 0.3 part of mass ratio:1
The composition of sodium alkyl sulfonate and sodium alkyl benzene sulfonate, 7 parts of mass ratioes are 1:1 sodium vinyl sulfonate and sodium hypophosphite
Composition, 0.2 part of hydrogen peroxide；
3) after 5min, start that solution B, solution A is added dropwise successively, start to be added dropwise after solution B is added dropwise, in 10min molten
Liquid A, solution A time for adding are 2 hours, and solution B time for adding is 2.5 hours；Solution B is 1 by 3.5 parts of mass ratioes:1 is
The composition of azobisisoheptonitrile and azo dicyano valeric acid, 15 parts of mass ratioes are 1:1 ethyl alcohol and the composition of propylene glycol and
60 parts of water compositions, solution A are made of 60 parts of acrylic acid and 60 parts of water；
4) it after completion of dropwise addition, heats to 70 DEG C, keeps temperature constant, cure 1 hour, wait for that reaction solution temperature is less than 30 DEG C
When, it is 1 to be slowly added to 10 parts of mass ratioes:1 triethanolamine and the composition of triisopropanolamine, moisturizing is to 1000 parts to get matter
Measure double initiation high stability polycarboxylate water-reducers that score is 50%.
Embodiment 2
A kind of double preparation methods for causing high stability polycarboxylate water-reducer, it is characterised in that：Double initiation high stables
Property polycarboxylate water-reducer is prepared from the following components：Polyether macromonomer, medium temperature releaser, alcohol organic solvent, hydrogen peroxide,
Acrylic acid, chain-transferring agent, bleeding agent, neutralizer；1000 parts of gross mass, preparation method includes the following steps：
1) 390 parts of vinyl butyl ether polyoxyethylene ether and 240 parts of water are added in reaction kettle, agitating and heating waits for that its is molten
Solution；
2) temperature in the kettle is measured, control temperature after temperature is stablized, is added at one time 0.1 part of sodium alkyl sulfonate, 6 at 52 DEG C
Part mass ratio is 1:The composition of 2 2- acrylamide-2-methyl propane sulfonics and the composition of sodium hypophosphite, 0.3 part of dioxygen
Water；
3) after 5min, start that solution B, solution A is added dropwise successively, start to be added dropwise after solution B is added dropwise, in 10min molten
Liquid A, solution A time for adding are 2.5 hours, and solution B time for adding is 3 hours；Solution B by 4.5 parts of azo dicyano valeric acids,
14 parts of mass ratioes 1:2 ethyl alcohol and the composition of ethylene glycol and 50 parts of water compositions, solution A is by 75 parts of acrylic acid and 60 parts of water groups
At；
4) it after completion of dropwise addition, heats to 69 DEG C, keeps temperature constant, cure 1.5 hours, wait for that reaction solution temperature is less than 30
DEG C when, be slowly added to 11 parts of triethanolamines, moisturizing gathers to double initiation high stabilities that 1000 parts are 50% to get mass fraction
Carboxylic acid water reducer.
Embodiment 3
A kind of double preparation methods for causing high stability polycarboxylate water-reducer, it is characterised in that：Double initiation high stables
Property polycarboxylate water-reducer is prepared from the following components：Polyether macromonomer, medium temperature releaser, alcohol organic solvent, hydrogen peroxide,
Acrylic acid, chain-transferring agent, bleeding agent, neutralizer；1000 parts of gross mass, final product quality score is 50% after preparation, preparation method
Include the following steps：
1) 420 parts of methyl allyl polyoxyethylene ethers and 200 parts of water are added in reaction kettle, agitating and heating waits for that its is molten
Solution；
2) measure temperature in the kettle, control temperature is at 54 DEG C, after temperature is stablized, be added at one time 0.3 part of sodium alkyl benzene sulfonate,
5 parts of sodium hypophosphites, 0.5 part of hydrogen peroxide；
3) after 5min, start that solution B, solution A is added dropwise successively, start to be added dropwise after solution B is added dropwise, in 10min molten
Liquid A, solution A time for adding are 3 hours, and solution B time for adding is 3.5 hours；Solution B is by 2.5 parts of azobisisoheptonitrile, 11
Part ethylene glycol and 55 parts of water compositions, solution A are made of 55 parts of acrylic acid and 70 parts of water；
4) it after completion of dropwise addition, heats to 68 DEG C, keeps temperature constant, cure 2.5 hours, wait for that reaction solution temperature is less than 30
DEG C when, be slowly added to 7 parts of triisopropanolamines, moisturizing gathers to double initiation high stabilities that 1000 parts are 50% to get mass fraction
Carboxylic acid water reducer.
Embodiment 4
A kind of double preparation methods for causing high stability polycarboxylate water-reducer, it is characterised in that：Double initiation high stables
Property polycarboxylate water-reducer is prepared from the following components：Polyether macromonomer, medium temperature releaser, alcohol organic solvent, hydrogen peroxide,
Acrylic acid, chain-transferring agent, bleeding agent, neutralizer；1000 parts of gross mass, final product quality score is 50% after preparation, preparation method
Include the following steps：
1) it is that allyl polyethenoxy ether and 210 parts of water are added in reaction kettle by 400 parts of polyether macromonomers, agitating and heating
Wait for its dissolving；
2) temperature in the kettle is measured, control temperature after temperature is stablized, is added at one time 0.25 part of alkyl naphthalene sulfonic acid at 56 DEG C
Sodium, 4 parts of 2- acrylamide-2-methyl propane sulfonics, 0.3 part of hydrogen peroxide；
3) after 5min, start that solution B, solution A is added dropwise successively, start to be added dropwise after solution B is added dropwise, in 10min molten
Liquid A, solution A time for adding are 3.5 hours, and solution B time for adding is 4 hours；Solution B is 1 by 3.5 parts of mass ratioes:1 peroxide
Change the composition, 13 parts of glycerine and 58 parts of water compositions of two diisopropyl carbonates and di-cyclohexylperoxy di-carbonate, solution A
It is made of 71 parts of acrylic acid and 65 parts of water；
4) it after completion of dropwise addition, heats to 66 DEG C, keeps temperature constant, cure 2 hours, wait for that reaction solution temperature is less than 30 DEG C
When, 8 parts of sodium methoxides are slowly added to, moisturizing subtracts to double initiation high stability polycarboxylic acids that 1000 parts are 50% to get mass fraction
Aqua.
Embodiment 5
A kind of double preparation methods for causing high stability polycarboxylate water-reducer, it is characterised in that：Double initiation high stables
Property polycarboxylate water-reducer is prepared from the following components：Polyether macromonomer, medium temperature releaser, alcohol organic solvent, hydrogen peroxide,
Acrylic acid, chain-transferring agent, bleeding agent, neutralizer；1000 parts of gross mass, final product quality score is 50% after preparation, preparation method
Include the following steps：
1) 405 parts of isoamyl alcohol polyoxyethylene ethers and 215 parts of water are added in reaction kettle, agitating and heating waits for its dissolving；
2) temperature in the kettle is measured, control temperature after temperature is stablized, is added at one time 0.15 part of secondary alkyl sulphate at 58 DEG C
Sodium, 4.5 parts of sodium styrene sulfonate, 0.25 part of hydrogen peroxide；
3) after 5min, start that solution B, solution A is added dropwise successively, start to be added dropwise after solution B is added dropwise, in 10min molten
Liquid A, solution A time for adding are 4 hours, and solution B time for adding is 4.5 hours；Solution B is different by 3.2 parts of dicetyl peroxydicarbonates two
Propyl ester, 12 parts of benzyl alcohols and 56 parts of water compositions, solution A are made of 65 parts of acrylic acid and 70 parts of water；
4) it after completion of dropwise addition, heats to 67 DEG C, keeps temperature constant, cure 2.5 hours, wait for that reaction solution temperature is less than 30
DEG C when, be slowly added to 8.5 parts of ethanol amines, moisturizing to 1000 parts be 50% to get mass fraction double poly- carboxylics of initiation high stability
Sour water-reducing agent.
Embodiment 6
A kind of double preparation methods for causing high stability polycarboxylate water-reducer, it is characterised in that：Double initiation high stables
Property polycarboxylate water-reducer is prepared from the following components：Polyether macromonomer, medium temperature releaser, alcohol organic solvent, hydrogen peroxide,
Acrylic acid, chain-transferring agent, bleeding agent, neutralizer；1000 parts of gross mass, final product quality score is 50% after preparation, preparation method
Include the following steps：
1) it is 1 by 412 parts of mass ratioes:The group of 1 isoamyl alcohol polyoxyethylene ether and vinyl butyl ether polyoxyethylene ether
Conjunction object, 220 parts of water are added in reaction kettle, and agitating and heating waits for its dissolving；
2) measure temperature in the kettle, control temperature is at 55 DEG C, after temperature is stablized, be added at one time 0.32 part of sulfamic acid sodium,
6.5 parts of acrylic sodium sulfonates, 0.38 part of hydrogen peroxide；
3) after 5min, start that solution B, solution A is added dropwise successively, start to be added dropwise after solution B is added dropwise, in 10min molten
Liquid A, solution A time for adding are 2.7 hours, and solution B time for adding is 3.2 hours；Solution B is by 2.8 parts of dicetyl peroxydicarbonates two
Cyclohexyl, 11 parts of mass ratioes 1:1 ethyl alcohol and the composition of benzyl alcohol and 58 parts of water compositions, solution A is by 60 parts of acrylic acid and 65
Part water composition；
4) it after completion of dropwise addition, heats to 65 DEG C, keeps temperature constant, cure 2 hours, wait for that reaction solution temperature is less than 30 DEG C
When, be slowly added to 7.5 parts of diethanol amine, moisturizing to 1000 parts be 50% to get mass fraction double poly- carboxylics of initiation high stability
Sour water-reducing agent.
Double initiation high stability polycarboxylate water-reducers of test above-described embodiment 1,2,3,4,5,6 and common polycarboxylic acids respectively
The net slurry initial fluidity in different cement, 1h mobility and concrete under water-reducing agent mother liquor comparable sodium initially collapse
Degree of falling/divergence and through when the slump/divergence.Experiment cement used is new 42.5 ordinary portland cement of China, 42.5 Pu Guishui of conch
Mud, 42.5 ordinary portland cement of Yadong, with reference to GB/8076-2008《Concrete admixture》Testing standard.
The different Water-reducing Admixtures To Cements net slurry flow effects of table 1 (new 42.5 ordinary portland cement of China)
| Water-reducing agent type | Initial fluidity mm | 1h mobility mm |
| Ordinary water-reducing agent | 255 | 235 |
| Embodiment 1 | 245 | 235 |
| Embodiment 2 | 235 | 220 |
| Embodiment 3 | 235 | 225 |
| Embodiment 4 | 250 | 230 |
| Embodiment 5 | 240 | 220 |
| Embodiment 6 | 240 | 230 |
The different Water-reducing Admixtures To Cements net slurry flow effects (42.5 ordinary portland cement of conch) of table 2
The different water-reducing agents of table 3 influence (new 42.5 ordinary portland cement of China) concrete flowability
The different water-reducing agents of table 4 influence (42.5 ordinary portland cement of conch) to concrete flowability
According to above-mentioned initial fluidity, 1h mobility and concrete it is initial and through when mobility compare, double initiation high stables
Property polycarboxylate water-reducer embodiment 1,2,3,4,5,6 from ordinary water-reducing agent when using different cement experiments, initial fluidity,
1h mobility is showed compared with ordinary water-reducing agent mother liquor relatively to be stablized, and adaptability is preferable, concrete flowability data comparison, embodiment 1,
2,3,4,5,6 concrete flowability performance tends towards stability in different brands cement, and it is high steady that overall data illustrates that this pair causes
Qualitative polycarboxylate water-reducer formula and mature preparation process are reliable, compared with 40% water-reducing agent mother liquor of common liq, water-reducing rate
It is not much different, it is adaptable, face stable work in work when different brands cement.
Claims (10)
1. a kind of double preparation methods for causing high stability polycarboxylate water-reducer, it is characterised in that：Double initiation high stabilities
Polycarboxylate water-reducer is mainly prepared from the following components：Polyether macromonomer, medium temperature releaser, alcohol organic solvent, hydrogen peroxide,
Acrylic acid, chain-transferring agent, bleeding agent, neutralizer, water；1000 parts of gross mass, preparation method includes the following steps：
1) 390-420 parts of polyether macromonomers and 200-240 parts of water are added in reaction kettle, agitating and heating waits for its dissolving；
2) temperature in the kettle is measured, control temperature after temperature is stablized, is added at one time 0.1-0.3 parts of bleeding agents, 3-7 at 50-58 DEG C
Part chain-transferring agent, 0.2-0.5 parts of hydrogen peroxide；
3) after 5min, start that solution B, solution A is added dropwise successively, start that solution A is added dropwise after solution B is added dropwise, in 10min,
Solution A time for adding is a hours, and solution B time for adding is a+0.5 hours；Solution B is by 2.5-4.5 parts of medium temperature initiators, 10-
15 parts of alcohol organic solvents and 50-60 parts of water compositions, solution A are made of 55-75 parts of acrylic acid and 60-70 parts of water；
4) after completion of dropwise addition, 65-70 DEG C is heated, keeps temperature constant, is cured b hours, waits for that reaction solution temperature is less than 30 DEG C
When, be slowly added to 6-11 parts of neutralizers, moisturizing to 1000 parts be 50% to get mass fraction double initiation high stability polycarboxylic acids
Water-reducing agent finished product.
2. a kind of double initiation high stability polycarboxylate water-reducers according to claim 1, it is characterised in that：The big list of polyethers
Body is by allyl polyethenoxy ether, methyl allyl polyoxyethylene ether, isoamyl alcohol polyoxyethylene ether, vinyl butyl ether polyoxy
One or more of vinethene forms.
3. a kind of double initiation high stability polycarboxylate water-reducers according to claim 1, it is characterised in that：The medium temperature causes
Agent is initiator of the 1h half life temperatures at 50-75 DEG C, specifically by azobisisoheptonitrile, azo dicyano valeric acid, peroxidating two
One or more of diisopropyl carbonate, di-cyclohexylperoxy di-carbonate form.
4. a kind of double initiation high stability polycarboxylate water-reducers according to claim 1, it is characterised in that：The alcohols is organic
Solvent is made of one or more of methanol, ethyl alcohol, benzyl alcohol, ethylene glycol, propylene glycol, glycerine.
5. a kind of double initiation high stability polycarboxylate water-reducers according to claim 1, it is characterised in that：The bleeding agent by
Sulfated castor oil, sodium alkyl sulfonate, sodium alkyl benzene sulfonate, alkyl sulfate sodium, sodium secondary alkyl sulfonate, secondary alkyl sulphate
One or more of sodium, Negel, succinic acid alkyl ester sulfonate sodium, sulfamic acid sodium form.
6. a kind of double initiation high stability polycarboxylate water-reducers according to claim 1, it is characterised in that：The chain-transferring agent
By thioacetic acid, mercaptopropionic acid, mercaptoethanol, sodium vinyl sulfonate, acrylic sodium sulfonate, methylpropene sodium sulfonate, styrene
One or more of sodium sulfonate, 2- acrylamide-2-methyl propane sulfonics, sodium hypophosphite form.
7. a kind of double initiation high stability polycarboxylate water-reducers according to claim 1, it is characterised in that：The neutralizer by
Sodium hydroxide, potassium hydroxide, sodium carbonate, sodium bicarbonate, potassium carbonate, sodium methoxide, sodium ethoxide, ethanol amine, diethanol amine, three ethyl alcohol
One or more of amine, triisopropanolamine form.
8. a kind of double initiation high stability polycarboxylate water-reducers according to claim 1, it is characterised in that：The hydrogen peroxide is
Mass percent is 27.5% industrial grade hydrogen peroxide.
9. a kind of double initiation high stability polycarboxylate water-reducers according to claim 1, it is characterised in that：The solution A drop
A is 2-4h between added-time.
10. a kind of double initiation high stability polycarboxylate water-reducers according to claim 1, it is characterised in that：When the curing
Between b be 1-3h.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109503773A (en) * | 2018-10-15 | 2019-03-22 | 湖州绿色新材股份有限公司 | High-slump-retentionpolycarboxylate polycarboxylate water reducer and its synthetic method |
| CN109776739A (en) * | 2018-12-29 | 2019-05-21 | 广州星业科技股份有限公司 | A kind of anti-colour contamination builder of novel high polymer |
| CN110240676A (en) * | 2019-04-10 | 2019-09-17 | 武汉理工大学 | A kind of preparation method of solid polycarboxylic acid water reducing agent |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0960021A4 (en) * | 1997-01-31 | 2001-05-02 | Seydel Res Inc | Water dispersible/redispersible hydrophobic polyester resins and their application in coatings |
| CN105254822A (en) * | 2015-11-20 | 2016-01-20 | 科之杰新材料集团有限公司 | Preparation method of polycarboxylate superplasticizer |
-
2018
- 2018-03-30 CN CN201810295002.6A patent/CN108516724A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0960021A4 (en) * | 1997-01-31 | 2001-05-02 | Seydel Res Inc | Water dispersible/redispersible hydrophobic polyester resins and their application in coatings |
| CN105254822A (en) * | 2015-11-20 | 2016-01-20 | 科之杰新材料集团有限公司 | Preparation method of polycarboxylate superplasticizer |
Non-Patent Citations (2)
| Title |
|---|
| 姚志光等: "《高分子化学》", 31 January 2013, 北京理工大学出版社 * |
| 韦军等: "《高分子合成工艺学》", 28 February 2011, 华东理工大学出版社 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109503773A (en) * | 2018-10-15 | 2019-03-22 | 湖州绿色新材股份有限公司 | High-slump-retentionpolycarboxylate polycarboxylate water reducer and its synthetic method |
| CN109776739A (en) * | 2018-12-29 | 2019-05-21 | 广州星业科技股份有限公司 | A kind of anti-colour contamination builder of novel high polymer |
| CN109776739B (en) * | 2018-12-29 | 2021-09-14 | 广州星业科技股份有限公司 | Macromolecular anti-cross-color builder |
| CN110240676A (en) * | 2019-04-10 | 2019-09-17 | 武汉理工大学 | A kind of preparation method of solid polycarboxylic acid water reducing agent |
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