CN106589253A - Preparation method of mud-resistant polycarboxylic acid water-reducing agent - Google Patents
Preparation method of mud-resistant polycarboxylic acid water-reducing agent Download PDFInfo
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- CN106589253A CN106589253A CN201611095721.0A CN201611095721A CN106589253A CN 106589253 A CN106589253 A CN 106589253A CN 201611095721 A CN201611095721 A CN 201611095721A CN 106589253 A CN106589253 A CN 106589253A
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- mixed liquor
- polyethenoxy ether
- allyl polyethenoxy
- ether mixed
- reducing agent
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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
-
- 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
-
- 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
Abstract
A preparation method of a mud-resistant polycarboxylic acid water-reducing agent comprises three steps: equally diving allyl polyethenoxy ether mixed liquid into three parts; adding methacrylamide and an initiator into the first part of allyl polyethenoxy ether mixed liquid and dropwise adding end-sealing amide phosphate, a reducing agent and a chain transfer agent simultaneously to obtain mixed liquid I; adding an initiator into the second part of allyl polyethenoxy ether mixed liquid and dropwise adding sodium methallyl sulfonate to obtain mixed liquid II; adding an initiator into the third part of allyl polyethenoxy ether mixed liquid and dropwise adding acrylic acid, a reducing agent and a chain transfer agent simultaneously, adding the mixed liquid I and the mixed liquid II, and then continuously adding the acrylic acid, the reducing agent and the chain transfer agent dropwise. The acrylic acid, a reducing agent and a chain transfer agent adopts normal-pressure production, and is low in equipment requirement, convenient to operate and favorable for industrialized production; the water-reducing agent synthesized by the method is adopted when the mud content of aggregate is high, so that the sensitiveness of the water-reducing agent on the mud content of the aggregate can be reduced and the flowability of concrete is improved on the premise of not increasing the doping amounting of the water-reducing agent.
Description
Technical field
The invention belongs to concrete additives in building materials technical field, and in particular to a kind of anti-chamotte mould polycarboxylic acids diminishing
The preparation method of agent.
Background technology
Polycarboxylate water-reducer is by the polyether monomer with double bond and other unsaturated small molecules with double bond or effective base
The high molecular polymer of group's copolymerization, because which has, volume is low, water-reducing rate is high, slump retaining is high, environmental protection and height are durable
The advantages of and be widely used in Concrete Industry.However, substantial amounts of case history and research show, with naphthalene system, trimerization
The water reducer such as cyanamide system and amido sulfoacid series is compared, and polycarboxylate water-reducer is particularly sensitive to the clay content of aggregate.With in recent years
The explosive growth of concrete construction amount, quality sand and stone aggregate resources fall sharply, and aggregate clay content is improved constantly, with clay content
Increase, mix the initial fluidity of plain edition polycarboxylate water-reducer concrete and it is slump-retaining constantly can reduce, it is particularly bright
Aobvious is that mobility is substantially reduced, sandstone of the general plain edition polycarboxylate water-reducer to clay content more than 3%, the flowing of concrete
Property disappears very fast, far can not meet construction party to concrete transportation construction requirement.Although can be with by improving water reducer volume
It is eased, but the problems such as being easily caused concrete coagulating time overlength and compressive strength rate and reduce, and greatly increase into
This, this is also the major reason for affecting poly carboxylic acid series water reducer in ready-mixed concrete industry large-scale promotion.
One kind is disclosed in patent CN 101798197A and suppresses the clay content slow release polycarboxylate water reducing agent that gathers materials, it leads
To be formed by anti-chamotte mould polycarboxylate water-reducer, retarder and natural zeolite powder compounding.Because clay mineral can be preferentially adsorbed on
Natural zeolite powder particle surface, so anti-chamotte mould polycarboxylate water-reducer molecule is liberated, it is easier to be adsorbed in cement granules table
Face, the problem excessive to polycarboxylic acids Molecular Adsorption so as to alleviate clay.But as zeolite loose structure can also adsorb excessive gathering
Carboxylic acid molecules, therefore ready-mixed concrete will reach identical fluidity, can still increase the volume of water reducer, increase cost.
A kind of preparation method of the anti-mud agent of amphoteric ethylene polymer concrete is disclosed in patent CN102617811A,
Method using post polymerization is first esterified, introduces cation group in the molecular structure, obtains a kind of anti-mud agent, but the method ester
Change and polymerization temperature is higher, be unfavorable for industrial applications, more due to introducing the vinyl monomer containing chloride ion, may cause
Steel bar corrosion.
The content of the invention
It is an object of the invention to provide a kind of preparation method of anti-chamotte mould polycarboxylate water-reducer, the preparation method is using normal
Pressure production, equipment requirements are low, easy to operate, beneficial to industrialized production；When aggregate clay content is higher using present invention synthesis
Water reducer, can reduce sensitivity of the polycarboxylate water-reducer to aggregate clay content on the premise of water reducer volume is not improved, carry
The mobility of high concrete；Not chloride ion-containing in product, will not produce corrosion harm to the reinforcing bar in concrete.
For achieving the above object, the present invention provides a kind of preparation method of anti-chamotte mould polycarboxylate water-reducer, including following step
Suddenly：
(1) a certain amount of allyl polyethenoxy ether is added in the container equipped with deionized water and is diluted, and stir intensification
To 45 DEG C -65 DEG C, allyl polyethenoxy ether mixed liquor is uniformly divided into into three parts after stirring, respectively pi-allyl polyoxy second
Alkene ether mixed liquor I, allyl polyethenoxy ether mixed liquor II and allyl polyethenoxy ether mixed liquor III；
(2-1) equipped with thermometer, agitator, disposably add pi-allyl polyoxy in five mouthfuls of flasks of constant pressure funnel successively
Vinyl Ether mixed liquor I, a certain amount of Methacrylamide and a certain amount of initiator, keeping temperature is 45- under agitation
65 DEG C, then at the uniform velocity a certain amount of end-blocking amidophosphoric acid ester of Deca, reducing agent and chain-transferring agent simultaneously in 1～2h, drip
The state of being kept stirring for obtains mixed liquor I；
(2-2) it is disposable in equipped with thermometer, agitator, the there-necked flask of constant pressure funnel to add allyl polyethenoxy
Ether mixed liquor II and a certain amount of initiator, keeping temperature is 45-65 DEG C under agitation, is then at the uniform velocity dripped in 1～2h
Plus a certain amount of methylpropene sodium sulfonate, drip the state of being kept stirring for and obtain mixed liquor II；
(2-3) equipped with thermometer, agitator, disposably add pi-allyl polyoxy in five mouthfuls of flasks of constant pressure funnel successively
Vinyl Ether mixed liquor III and a certain amount of initiator, keeping temperature is 45-65 DEG C under agitation, then same in 1～3h
When at the uniform velocity a certain amount of acrylic acid of Deca, reducing agent and chain-transferring agent, the state of being kept stirring for obtains mixed liquor III；
The step (2-1), step (2-2) and step (2-3) are while carry out；
(3), after disposably adding mixed liquor I and mixed liquor II in mixed liquor III, continue simultaneously at the uniform velocity to drip in 1h
Acrylic acid, reducing agent and chain-transferring agent, are down to room temperature after continuing stirring 1h, that is, obtain a kind of anti-chamotte mould polycarboxylic acids and subtract after dripping
Water preparation.
Preferably, allyl polyethenoxy ether mixed liquor is warming up to into 55 DEG C in the step (1), the step (2-1)
Into step (2-3), keeping temperature is 55 DEG C under agitation；In the step (2-1) in the 2h at the uniform velocity Deca end-blocking amide
Phosphate ester, reducing agent and chain-transferring agent, in the step (2-2) in the 2h at the uniform velocity Deca methylpropene sodium sulfonate, the step
(2-3) in the 2h at the uniform velocity Deca acrylic acid, reducing agent and chain-transferring agent.
Preferably, in the step (1), allyl polyethenoxy ether and the mass ratio of deionized water are 1:0.5～1:1.2.
Preferably, in the step (2-1), allyl polyethenoxy ether mixed liquor I with the mol ratio of Methacrylamide is
1:0.5～1:1, in the step (2-1), allyl polyethenoxy ether mixed liquor I and the mol ratio of end-blocking amidophosphoric acid ester are 1:
0.6～1:0.9.
Preferably, in the step (2-2) allyl polyethenoxy ether mixed liquor II and methylpropene sodium sulfonate mole
Than for 1:0.06～1:0.08.
Preferably, the mole of allyl polyethenoxy ether mixed liquor III and step (2-3) and step in the step (2-3)
Suddenly the ratio between acrylic acid integral molar quantity needed for (3) is 1:2.5～1:2.7.
Preferably, the initiator is hydrogen peroxide or sodium peroxydisulfate, the initiator respectively with allyl polyethenoxy ether
Mol ratio between mixed liquor I, allyl polyethenoxy ether mixed liquor II and allyl polyethenoxy ether mixed liquor III is 1:
0.35～1:0.55.
Preferably, the reducing agent be ascorbic acid, sodium ascorbate, the one kind in 2,2'-Azobis(2,4-dimethylvaleronitrile)；The reduction
Agent is 1 with the mol ratio between allyl polyethenoxy ether mixed liquor I and allyl polyethenoxy ether mixed liquor III respectively:
0.009～1:0.015.
Preferably, the chain-transferring agent is TGA or mercaptopropionic acid；The chain-transferring agent respectively with pi-allyl polyoxy
Mol ratio between vinyl Ether mixed liquor I and allyl polyethenoxy ether mixed liquor III is 1:0.05～1:0.09.
Preferably, the molecular weight of the allyl polyethenoxy ether is 2000～2400.
Compared with prior art, effective radical polymerisation is become effective small molecule by the present invention first, then by effective small molecule
It is copolymerized into high molecular polymer so that effectively group can preferably copolymerization be together；The preparation method is produced using normal pressure, equipment
Low, low production cost is required, it is easy to operate, beneficial to industrialized production；When aggregate clay content is higher using present invention synthesis
Anti- chamotte mould polycarboxylate water-reducer, realizes the resistant function to clay on the premise of polycarboxylate water-reducer volume is not improved, drop
Low sensitivity of the polycarboxylate water-reducer to aggregate clay content, improves the water-reducing effect of polycarboxylate water-reducer, so as to improve
The mobility of concrete, and not chloride ion-containing in product, endanger to the reinforcing bar non-corroding in concrete.
Specific embodiment
With reference to embodiments the present invention is described in further detail.
Embodiment 1
A kind of preparation method of anti-chamotte mould polycarboxylate water-reducer, comprises the following steps：
(1) a certain amount of allyl polyethenoxy ether is added in the container equipped with deionized water and is diluted, pi-allyl polyoxy
The molecular weight of vinyl Ether is 2000, and allyl polyethenoxy ether is 1 with the mass ratio of deionized water:1.2, and stirring is warming up to 45
DEG C, allyl polyethenoxy ether mixed liquor is uniformly divided into into three parts after stirring, respectively allyl polyethenoxy ether mixing
Liquid I, allyl polyethenoxy ether mixed liquor II and allyl polyethenoxy ether mixed liquor III；
(2-1) equipped with thermometer, agitator, disposably add pi-allyl polyoxy in five mouthfuls of flasks of constant pressure funnel successively
Vinyl Ether mixed liquor I, a certain amount of Methacrylamide and a certain amount of hydrogen peroxide；Keeping temperature is 45 under agitation
DEG C, then at the uniform velocity a certain amount of end-blocking amidophosphoric acid ester of Deca, ascorbic acid and TGA simultaneously in the 1h, drip holding
Stirring obtains mixed liquor I；The allyl polyethenoxy ether mixed liquor I and Methacrylamide and end-blocking amidophosphoric acid ester
Mol ratio be 1:0.5:0.6, the hydrogen peroxide is 1 with the mol ratio of allyl polyethenoxy ether mixed liquor I:0.35, it is described
Mol ratio between ascorbic acid and allyl polyethenoxy ether mixed liquor I is 1:0.009, the TGA is gathered with pi-allyl
Mol ratio between oxygen vinyl Ether mixed liquor I is 1:0.05；
(2-2) it is disposable in equipped with thermometer, agitator, the there-necked flask of constant pressure funnel to add allyl polyethenoxy
Ether mixed liquor II and a certain amount of hydrogen peroxide, keeping temperature is 45 DEG C under agitation, and then at the uniform velocity Deca is certain in the 1h
The methylpropene sodium sulfonate of amount, drips the state of being kept stirring for and obtains mixed liquor II；The allyl polyethenoxy ether mixed liquor
II is 1 with the mol ratio of methylpropene sodium sulfonate:0.06, the hydrogen peroxide and allyl polyethenoxy ether mixed liquor II mole
Than for 1:0.35；
(2-3) equipped with thermometer, agitator, disposably add pi-allyl polyoxy in five mouthfuls of flasks of constant pressure funnel successively
Vinyl Ether mixed liquor III and a certain amount of hydrogen peroxide, the hydrogen peroxide with the mol ratio of allyl polyethenoxy ether mixed liquor III is
1:0.35, keeping temperature is 45 DEG C under agitation, then at the uniform velocity a certain amount of acrylic acid of Deca, Vitamin C simultaneously in the 1h
Acid and TGA, the state of being kept stirring for obtain mixed liquor III；The ascorbic acid and allyl polyethenoxy ether mixed liquor III
Between mol ratio be 1:0.009, the mol ratio between the TGA and allyl polyethenoxy ether mixed liquor III is
1:0.05；
The step (2-1), step (2-2) and step (2-3) are while carry out；
(3), after disposably adding mixed liquor I and mixed liquor II in mixed liquor III, continue simultaneously at the uniform velocity to drip in 1h
Acrylic acid, ascorbic acid and TGA, the mole of allyl polyethenoxy ether mixed liquor III and step in the step (2-3)
Suddenly (2-3) and the ratio needed for step (3) between acrylic acid integral molar quantity are 1:2.5, drop after continuing stirring 1h after dripping
To room temperature, that is, obtain a kind of anti-chamotte mould polycarboxylate water-reducer.
Embodiment 2
A kind of preparation method of anti-chamotte mould polycarboxylate water-reducer, comprises the following steps：
(1) a certain amount of allyl polyethenoxy ether is added in the container equipped with deionized water and is diluted, pi-allyl polyoxy
The molecular weight of vinyl Ether is 2200, and allyl polyethenoxy ether is 1 with the mass ratio of deionized water:0.85, and stirring be warming up to
55 DEG C, allyl polyethenoxy ether mixed liquor is uniformly divided into into three parts after stirring, respectively allyl polyethenoxy ether is mixed
Close liquid I, allyl polyethenoxy ether mixed liquor II and allyl polyethenoxy ether mixed liquor III；
(2-1) equipped with thermometer, agitator, disposably add pi-allyl polyoxy in five mouthfuls of flasks of constant pressure funnel successively
Vinyl Ether mixed liquor I, a certain amount of Methacrylamide and a certain amount of sodium peroxydisulfate；Keeping temperature is 55 under agitation
DEG C, then at the uniform velocity a certain amount of end-blocking amidophosphoric acid ester of Deca, sodium ascorbate and mercaptopropionic acid simultaneously in the 2h, drip guarantor
Hold stirring and obtain mixed liquor I；The allyl polyethenoxy ether mixed liquor I and Methacrylamide and end-blocking amidophosphoric acid
The mol ratio of ester is 1:0.75:0.75, the sodium peroxydisulfate is 1 with the mol ratio of allyl polyethenoxy ether mixed liquor III:
0.45, the mol ratio between the sodium ascorbate and allyl polyethenoxy ether mixed liquor I is 1:0.012, the sulfydryl third
Mol ratio between acid and allyl polyethenoxy ether mixed liquor I is 1:0.07；
(2-2) it is disposable in equipped with thermometer, agitator, the there-necked flask of constant pressure funnel to add allyl polyethenoxy
Ether mixed liquor II and a certain amount of sodium peroxydisulfate, keeping temperature is 55 DEG C under agitation, then the at the uniform velocity Deca one in the 2h
Quantitative methylpropene sodium sulfonate, drips the state of being kept stirring for and obtains mixed liquor II；The allyl polyethenoxy ether mixing
Liquid II is 1 with the mol ratio of methylpropene sodium sulfonate:0.07, the sodium peroxydisulfate and allyl polyethenoxy ether mixed liquor III
Mol ratio is 1:0.45；
(2-3) equipped with thermometer, agitator, disposably add pi-allyl polyoxy in five mouthfuls of flasks of constant pressure funnel successively
Vinyl Ether mixed liquor III and a certain amount of sodium peroxydisulfate, the sodium peroxydisulfate and allyl polyethenoxy ether mixed liquor III mole
Than for 1:0.45, keeping temperature is 55 DEG C under agitation, then at the uniform velocity a certain amount of acrylic acid of Deca, anti-simultaneously in the 2h
Bad hematic acid sodium and mercaptopropionic acid, the state of being kept stirring for obtain mixed liquor III；The sodium ascorbate and allyl polyethenoxy ether
Mol ratio between mixed liquor III is 1:0.012, between the mercaptopropionic acid and allyl polyethenoxy ether mixed liquor III
Mol ratio is 1:0.07；
The step (2-1), step (2-2) and step (2-3) are while carry out；
(3), after disposably adding mixed liquor I and mixed liquor II in mixed liquor III, continue simultaneously at the uniform velocity to drip in 1h
Acrylic acid, sodium ascorbate and mercaptopropionic acid, in the step (2-3) mole of allyl polyethenoxy ether mixed liquor III with
Step (2-3) and the ratio needed for step (3) between acrylic acid integral molar quantity are 1:2.6, after continuing stirring 1h after dripping
Room temperature is down to, that is, obtains a kind of anti-chamotte mould polycarboxylate water-reducer.
Embodiment 3
A kind of preparation method of anti-chamotte mould polycarboxylate water-reducer, comprises the following steps：
(1) a certain amount of allyl polyethenoxy ether is added in the container equipped with deionized water and is diluted, pi-allyl polyoxy
The molecular weight of vinyl Ether is 2400, and allyl polyethenoxy ether is 1 with the mass ratio of deionized water:0.5, and stirring is warming up to 65
DEG C, allyl polyethenoxy ether mixed liquor is uniformly divided into into three parts after stirring, respectively allyl polyethenoxy ether mixing
Liquid I, allyl polyethenoxy ether mixed liquor I I and allyl polyethenoxy ether mixed liquor III；
(2-1) equipped with thermometer, agitator, disposably add pi-allyl polyoxy in five mouthfuls of flasks of constant pressure funnel successively
Vinyl Ether mixed liquor I, a certain amount of Methacrylamide and a certain amount of hydrogen peroxide；Keeping temperature is 65 under agitation
DEG C, then at the uniform velocity a certain amount of end-blocking amidophosphoric acid ester of Deca, 2,2'-Azobis(2,4-dimethylvaleronitrile) and TGA simultaneously in the 2h, drip
The state of being kept stirring for obtains mixed liquor I；The allyl polyethenoxy ether mixed liquor I and Methacrylamide and end-blocking amide phosphorus
The mol ratio of acid esters is 1:1:0.9, the hydrogen peroxide is 1 with the mol ratio of allyl polyethenoxy ether mixed liquor III:0.55, institute
It is 1 to state the mol ratio between 2,2'-Azobis(2,4-dimethylvaleronitrile) and allyl polyethenoxy ether mixed liquor I:0.015, the TGA and alkene
Mol ratio between propyl group polyoxyethylene ether mixed liquor I is 1:0.09；
(2-2) it is disposable in equipped with thermometer, agitator, the there-necked flask of constant pressure funnel to add allyl polyethenoxy
Ether mixed liquor I I and a certain amount of hydrogen peroxide, keeping temperature is 65 DEG C under agitation, and then at the uniform velocity Deca is certain in the 2h
The methylpropene sodium sulfonate of amount, drips the state of being kept stirring for and obtains mixed liquor I I；The allyl polyethenoxy ether mixed liquor
II is 1 with the mol ratio of methylpropene sodium sulfonate:0.08, the hydrogen peroxide and allyl polyethenoxy ether mixed liquor III mole
Than for 1:0.55；
(2-3) equipped with thermometer, agitator, disposably add pi-allyl polyoxy in five mouthfuls of flasks of constant pressure funnel successively
Vinyl Ether mixed liquor III and a certain amount of hydrogen peroxide, the hydrogen peroxide with the mol ratio of allyl polyethenoxy ether mixed liquor III is
1:0.55, keeping temperature is 65 DEG C under agitation, then at the uniform velocity a certain amount of acrylic acid of Deca, azo two simultaneously in the 3h
Different heptonitrile and TGA, the state of being kept stirring for obtain mixed liquor III；The 2,2'-Azobis(2,4-dimethylvaleronitrile) and allyl polyethenoxy ether
Mol ratio between mixed liquor III is 1:0.015, between the TGA and allyl polyethenoxy ether mixed liquor III
Mol ratio is 1:0.09；
The step (2-1), step (2-2) and step (2-3) are while carry out；
(3), after disposably adding mixed liquor I and mixed liquor I I in mixed liquor III, continue simultaneously at the uniform velocity to drip in 1h
Acrylic acid, 2,2'-Azobis(2,4-dimethylvaleronitrile) and TGA, the mole of allyl polyethenoxy ether mixed liquor III in the step (2-3)
It is 1 with step (2-3) and the ratio needed for step (3) between acrylic acid integral molar quantity:2.7, continue stirring 1h after dripping
After be down to room temperature, that is, obtain a kind of anti-chamotte mould polycarboxylate water-reducer.
Implementation result
1st, Mortar'S Flowability experiment
Experiment cement adopts Carnis Rapanae thomasianae P.O42.5 cement, and experiment sand is normal sand, and soil replaces the normal sand of respective amount
(mud takes the mud in common yellow ground using 75 μm of sieve sieve, mixes in normal sand by different proportion), mortar mix ratio is shown in Table 1：
1 mortar of table tests match ratio
| Sand | Cement | Water | Water reducer |
| 1424 | 824 | 292 | 4.532 |
(selected with polycarboxylate water-reducer sample of the anti-chamotte mould polycarboxylate water-reducer obtained in the embodiment of the present invention 1～3 with contrast
With commercial general polycarboxylate water-reducer) contrasted, mortar mobility contrast experiment, sand are carried out with the sand of different clay contents
Slurry fluidity is with reference to GB GB/T 2419-2005《Test method for fluidity of cement mortar》Step is carried out, and mortar test result is shown in
Table 2：
The mobility contrast of 2 mortar of table
2nd, concrete performance experiment
Experiment cement adopts Carnis Rapanae thomasianae P.O42.5 cement, and experiment sand is the clean sand (clay content is 0%) of washing, and soil takes
Clean sand (mud takes the mud in common yellow ground using 75 μm of sieve sieve, mixes in clean sand by different proportion) for respective amount,
Concrete mix is shown in Table 3：
3 concrete experiments match ratio of table
| Sand | Cement | Rubble | Water | Water reducer |
| 795 | 375 | 1048 | 164 | 5.428 |
(selected with polycarboxylate water-reducer sample of the anti-chamotte mould polycarboxylate water-reducer obtained in the embodiment of the present invention 1～3 with contrast
With commercial general polycarboxylate water-reducer) contrasted, concrete performance contrast experiment is carried out with the sand of different clay contents, join
According to GB GB/T 50080-2011《Standard for test methods of properties of ordinary concrete mixture standard》Step is carried out, concrete test knot
Fruit is shown in Table 4：
The performance test contrast of 4 concrete of table
As the divergence of concrete is relevant with its mobility, mobility is bigger, and divergence is bigger.When the slump is more than
During 220mm, the slump can not accurately reflect the mobility of concrete, be slump flow test with the average diameter after concrete extension
It is used as the liquidity scale, so as to more accurately reflect the mobility of concrete.
By in table 2 and table 4 as can be seen that the anti-chamotte mould polycarboxylate water-reducer that will be synthesized using this method mixes mortar and mixed
In solidifying soil, as the initial fluidity of the increase of clay content in sand, mortar and concrete is not interfered substantially, Er Qiezhong
Later stage mortar and concrete flowability also have excellent retentivity, the anti-chamotte mould polycarboxylate water-reducer of this explanation present invention synthesis
The resistant function to clay can be realized on the premise of polycarboxylate water-reducer volume is not improved, and polycarboxylate water-reducer is reduced to bone
The sensitivity of material clay content, so as to improve the water-reducing effect and mortar and the mobility of concrete of polycarboxylate water-reducer, and
Containing mud or without in the case of mud, water-reducing property is above commercial general polycarboxylate water-reducer sample.
Claims (10)
1. a kind of preparation method of anti-chamotte mould polycarboxylate water-reducer, it is characterised in that comprise the following steps：
(1) a certain amount of allyl polyethenoxy ether is added in the container equipped with deionized water and is diluted, and stirring is warming up to 45-
65 DEG C, allyl polyethenoxy ether mixed liquor is uniformly divided into into three parts after stirring, respectively allyl polyethenoxy ether is mixed
Close liquid I, allyl polyethenoxy ether mixed liquor II and allyl polyethenoxy ether mixed liquor III；
(2-1) allyl polyethenoxy is disposably added successively in equipped with thermometer, agitator, five mouthfuls of flasks of constant pressure funnel
Ether mixed liquor I, a certain amount of Methacrylamide and a certain amount of initiator, keeping temperature is 45-65 DEG C under agitation,
Then at the uniform velocity a certain amount of end-blocking amidophosphoric acid ester of Deca, reducing agent and chain-transferring agent simultaneously in 1～2h, drip holding and stir
The state of mixing obtains mixed liquor I；
(2-2) it is disposable in equipped with thermometer, agitator, the there-necked flask of constant pressure funnel to add allyl polyethenoxy ether to mix
Liquid II and a certain amount of initiator are closed, keeping temperature is 45-65 DEG C under agitation, then the at the uniform velocity Deca one in 1～2h
Quantitative methylpropene sodium sulfonate, drips the state of being kept stirring for and obtains mixed liquor II；
(2-3) allyl polyethenoxy is disposably added successively in equipped with thermometer, agitator, five mouthfuls of flasks of constant pressure funnel
Ether mixed liquor III and a certain amount of initiator, keeping temperature is 45-65 DEG C under agitation, then simultaneously even in 1～3h
A certain amount of acrylic acid of fast Deca, reducing agent and chain-transferring agent, the state of being kept stirring for obtain mixed liquor III；
The step (2-1), step (2-2) and step (2-3) are while carry out；
(3), after disposably adding mixed liquor I and mixed liquor II in mixed liquor III, continue simultaneously at the uniform velocity to drip propylene in 1h
Acid, reducing agent and chain-transferring agent, are down to room temperature after continuing stirring 1h, that is, obtain a kind of anti-chamotte mould polycarboxylic acids diminishing after dripping
Agent.
2. a kind of preparation method of anti-chamotte mould polycarboxylate water-reducer according to claim 1, it is characterised in that the step
(1) allyl polyethenoxy ether mixed liquor is warming up to into 55 DEG C in, in stirring condition in the step (2-1) to step (2-3)
Lower keeping temperature is 55 DEG C；In the step (2-1) in the 2h at the uniform velocity Deca end-blocking amidophosphoric acid ester, reducing agent and chain tra nsfer
Agent, in the step (2-2) in the 2h at the uniform velocity Deca methylpropene sodium sulfonate, in the step (2-3) in the 2h at the uniform velocity Deca
Acrylic acid, reducing agent and chain-transferring agent.
3. the preparation method of a kind of anti-chamotte mould polycarboxylate water-reducer according to claim 1 and 2, it is characterised in that described
In step (1), allyl polyethenoxy ether and the mass ratio of deionized water are 1:0.5～1:1.2.
4. the preparation method of a kind of anti-chamotte mould polycarboxylate water-reducer according to claim 1 and 2, it is characterised in that described
In step (2-1), allyl polyethenoxy ether mixed liquor I and the mol ratio of Methacrylamide are 1:0.5～1:1, the step
(2-1) in, allyl polyethenoxy ether mixed liquor I and the mol ratio of end-blocking amidophosphoric acid ester are 1:0.6～1:0.9.
5. the preparation method of a kind of anti-chamotte mould polycarboxylate water-reducer according to claim 1 and 2, it is characterised in that described
In step (2-2), allyl polyethenoxy ether mixed liquor II and the mol ratio of methylpropene sodium sulfonate are 1:0.06～1:0.08.
6. the preparation method of a kind of anti-chamotte mould polycarboxylate water-reducer according to claim 1 and 2, it is characterised in that described
In step (2-3), the mole of allyl polyethenoxy ether mixed liquor III is acrylic acid with needed for step (2-3) and step (3)
Ratio between integral molar quantity is 1:2.5～1:2.7.
7. the preparation method of a kind of anti-chamotte mould polycarboxylate water-reducer according to claim 1 and 2, it is characterised in that described
Initiator is hydrogen peroxide or sodium peroxydisulfate, the initiator respectively with allyl polyethenoxy ether mixed liquor I, pi-allyl polyoxy second
Mol ratio between alkene ether mixed liquor II and allyl polyethenoxy ether mixed liquor III is 1:0.35～1:0.55.
8. the preparation method of a kind of anti-chamotte mould polycarboxylate water-reducer according to claim 1 and 2, it is characterised in that described
Reducing agent is ascorbic acid, sodium ascorbate, the one kind in 2,2'-Azobis(2,4-dimethylvaleronitrile)；The reducing agent respectively with pi-allyl polyoxy second
Mol ratio between alkene ether mixed liquor I and allyl polyethenoxy ether mixed liquor III is 1:0.009～1:0.015.
9. the preparation method of a kind of anti-chamotte mould polycarboxylate water-reducer according to claim 1 and 2, it is characterised in that described
Chain-transferring agent is TGA or mercaptopropionic acid；The chain-transferring agent respectively with allyl polyethenoxy ether mixed liquor I and allyl
Mol ratio between base polyoxyethylene ether mixed liquor III is 1:0.05～1:0.09.
10. the preparation method of a kind of anti-chamotte mould polycarboxylate water-reducer according to claim 1 and 2, it is characterised in that described
The molecular weight of allyl polyethenoxy ether is 2000～2400.
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| CN107129180A (en) * | 2017-05-11 | 2017-09-05 | 长沙加美乐素化工有限公司 | A kind of synthesis of clay inhibitor and preparation method |
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| CN109553729A (en) * | 2018-11-28 | 2019-04-02 | 中国建材检验认证集团厦门宏业有限公司 | A kind of anti-chamotte mould water-reducing agent of both sexes and preparation method thereof |
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| CN109650762B (en) * | 2018-12-24 | 2020-08-11 | 科之杰新材料集团有限公司 | Phosphate type polycarboxylate superplasticizer and preparation method thereof |
| CN111087516A (en) * | 2019-12-18 | 2020-05-01 | 深圳大学 | Mud-resistant polycarboxylic water reducer and preparation method and application thereof |
| CN111087552A (en) * | 2019-12-22 | 2020-05-01 | 同济大学 | Synthetic method of polycarboxylic acid water reducer with high water reducing rate and mud resistance |
| CN111019064A (en) * | 2019-12-26 | 2020-04-17 | 河北铁园科技发展有限公司 | Polycarboxylate superplasticizer and preparation method thereof |
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