CN108484839A - A kind of amphipathic carboxylic dispersants and preparation method thereof - Google Patents
A kind of amphipathic carboxylic dispersants and preparation method thereof Download PDFInfo
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- CN108484839A CN108484839A CN201810247647.2A CN201810247647A CN108484839A CN 108484839 A CN108484839 A CN 108484839A CN 201810247647 A CN201810247647 A CN 201810247647A CN 108484839 A CN108484839 A CN 108484839A
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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
- C04B24/24—Macromolecular compounds
- C04B24/26—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
- C04B24/2664—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds of ethylenically unsaturated dicarboxylic acid polymers, e.g. maleic anhydride copolymers
- C04B24/267—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds of ethylenically unsaturated dicarboxylic acid polymers, e.g. maleic anhydride copolymers 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
- C04B24/00—Use of organic materials as active ingredients for mortars, concrete or artificial stone, e.g. plasticisers
- C04B24/24—Macromolecular compounds
- C04B24/26—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
- C04B24/2688—Copolymers containing at least three different monomers
- C04B24/2694—Copolymers containing at least three different monomers containing polyether side chains
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F2/00—Processes of polymerisation
- C08F2/04—Polymerisation in solution
- C08F2/10—Aqueous solvent
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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
- C04B2103/40—Surface-active agents, dispersants
- C04B2103/408—Dispersants
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Abstract
A kind of amphipathic carboxylic dispersants and preparation method thereof, dispersant is made of the raw material of following portions by weight：72~76 parts of unsaturated polyoxyethylene ether polymeric monomer, 0~2 part of oiliness monomer, 3~4 parts of maleic anhydride, 1~1.5 part of aqueous initiator, 0.001~0.01 part of oiliness initiator, 30 parts of deionized water, A feed liquids, B feed liquids.The polymeric monomer is methyl allyl polyoxyethylene ether, allyl polyethenoxy ether, isoamyl alcohol polyoxyethylene ether, isobutene alcohol polyoxyethylene ether；Oiliness monomer is styrene or styrene derivative；Aqueous initiator is hydrogen peroxide, persulfate, azo-bis-isobutyrate hydrochloride；Oiliness initiator is azo-bis-isobutyl cyanide, benzoyl peroxide.The present invention also provides preparation methods.The present invention prepares amphipathic carboxylic dispersants by environmentally protective no soap technique at low cost, effectively increases self-compacting concrete flow velocity, improves concrete workability, preparation process is simple, environmentally protective.
Description
Technical field
It is specifically a kind of amphipathic the present invention relates to a kind of concrete admixture more particularly to a kind of polycarboxylate dispersant
Polycarboxylate dispersant belongs to building material technical field.The invention further relates to a kind of preparation methods of polycarboxylate dispersant, specifically
It is a kind of preparation method of amphipathic carboxylic dispersants.
Background technology
With the popularization of green building, third generation polycarboxylate water-reducer is widely used by people, is applied to various work China Democratic National Construction Associations
In.Polycarboxylate water-reducer can promote the various performances of concrete, such as compression strength, workability, pumpability.Due to polycarboxylic acids skill
The raising of art also allows and prepares super high strength concrete, flowing concrete, self-compacting concrete, and underwater concrete and injection are mixed
Solidifying soil technology has obtained large increase.In practical applications, people have also discovered one existing for traditional polycarboxylate water-reducer simultaneously
A little problems, for example in self-compacting concrete application, concrete flow velocity prepared by traditional polycarboxylic acids is not high enough, penetrates steel bar piece
Ability is limited, influences construction speed and its construction quality.In the undesirable concrete of low-grade concrete or sand grading, usually
It is not rich enough to will appear slurry, package is not good enough, and dew stone is serious, affects workability, has seriously affected concrete durability.
Inventor retrieves following Patents documents：CN107602773A discloses a kind of poly- carboxylic for oil-well cement
Acid dispersant and preparation method thereof, the polycarboxylate dispersant are with acrylic acid, n-vinyl pyrrolidone, itaconic acid, 2- propylene
Amide groups -2- methyl propane sulfonic acids, sodium vinyl sulfonate, vinylbenzenesulfonic acid sodium and allyl polyglycol are the copolymerization of monomer
Object；The weight average molecular weight of allyl polyglycol is 300~2400；It is the quality of acrylic acid in terms of 100% by the gross mass of monomer
Percentage is 0.5%~20%, and the mass percent of n-vinyl pyrrolidone is 0.5%~15%, the quality hundred of itaconic acid
The mass percent than being 0.5%~10%, 2- acrylamide-2-methylpro panesulfonic acids is divided to be 5%~60%, vinyl sulfonic acid
The mass percent of sodium is 0.5%~30%, and the mass percent of vinylbenzenesulfonic acid sodium is 0.5%~30%, and allyl is poly-
The mass percent of ethylene glycol is 20%~70%；The weight average molecular weight of polycarboxylate dispersant is 5000~250000.
CN103406067A discloses a kind of polycarboxylate dispersant and the preparation method and application thereof.The polycarboxylate dispersant by 1.0~
3.0 parts by weight contain the unsaturated monomer of carboxyl, the sulfonic unsaturated monomer of 1.1~2.2 parts by weight and 0.6~1.2 weight
Part other free-radical polymerised unsaturated base monomers, 25~35 parts by weight water, 0.11~0.22 parts by weight initiator,
Free radical polymerization occurs under the conditions of 0.03~0.06 parts by weight chain-transferring agent and 1.5~4.0 parts by weight alkali compounds are existing
It is obtained by the reaction.CN106519151A discloses amphipathic poly-carboxylic-acid cement dispersant and preparation method thereof.The amphipathic carboxylic
Sour water cement dispersant is a kind of dispersion liquid of the polycarboxylic acids particle with vermiform microscopic pattern；Its composition includes amphipathic carboxylic
Sour nano-particle and water；The weight average molecular weight of the amphipathic carboxylic acid particle is 15000~40000, and it is poly- which employs RAFT
Conjunction method, but RAFT polymerizations are with high costs, chain-transferring agent is more difficult to buy.It has difficulties in industrial practical application.
United States Patent 4792360 are disclosed makes amphipathic carboxylic acid by introducing the method for styrene sulfonic acid
Dispersant.But the price of styrene sulfonic acid is very high, has equally existed the problem of being difficult to promote.US Patent
5158996 disclose the method for synthesizing amphoteric dispersant as solvent by using acetone, but can be made to environment using solvent
It at pollution, and must also be removed by distillation in follow-up use, cost increases.
The above technology improves coagulation for how to enable polycarboxylate dispersant effectively improve self-compacting concrete flow velocity
Native workability does not provide specific guidance program.
Invention content
The technical problem to be solved by the invention is to provide a kind of amphipathic carboxylic dispersants, the polycarboxylate dispersants
Self-compacting concrete flow velocity can be effectively improved, improves concrete workability, while the preparation process of the polycarboxylate dispersant is simple,
It is environmentally protective.
For this purpose, another technical problem to be solved by this invention is to provide a kind of system of amphipathic carboxylic dispersants
Preparation Method.
In order to solve the above technical problems, the technical solution adopted by the present invention is as follows：
A kind of amphipathic carboxylic dispersants, its technical solution is that it is made of the raw material of following portions by weight：
72~76 parts of unsaturated polyoxyethylene ether polymeric monomer, 0~2 part of oiliness monomer, 3~4 parts of maleic anhydride, aqueous initiator 1~1.5
Part, 0.001~0.01 part of oiliness initiator, 30 parts of deionized water, A feed liquids, B feed liquids.Wherein, above-mentioned unsaturated polyoxyethylene
Ether polymeric monomer is methyl allyl polyoxyethylene ether, allyl polyethenoxy ether, isoamyl alcohol polyoxyethylene ether, isobutene alcohol are poly-
One kind in ethylene oxide ether；Unsaturated polyoxyethylene ether is selected, steric hindrance is improved.Above-mentioned oiliness monomer be styrene or
Styrene derivative；Above-mentioned aqueous initiator is hydrogen peroxide, persulfate (in potassium peroxydisulfate, ammonium persulfate, sodium peroxydisulfate
It is a kind of), the one or any two kinds compositions (mixture) for pressing arbitrary quality proportioning in azo-bis-isobutyrate hydrochloride；On
The oiliness initiator stated is one or two kinds of combination by arbitrary quality proportioning in azo-bis-isobutyl cyanide, benzoyl peroxide
Object (mixture).Above-mentioned A feed liquids are mixed by 5~11 parts of acrylic acid, 0~4 part of oiliness monomer and 10 parts of deionized waters
(be mixed in beaker and be formulated), B feed liquids are by 0.08~0.12 part of reducing agent, 0.3-~0.5 part chain-transferring agent and 10 parts
Deionized water mixes and (is mixed in beaker and is formulated), and reducing agent is mixed by L-AA and phosphorous acid,
Chain-transferring agent is mercaptopropionic acid (β-mercaptopropionic acid).
The preparation method of the amphipathic carboxylic dispersants comprises the technical steps that：1. (fritting) is unsaturated poly-
3~4 parts and 10 parts 72~76 parts of ethylene oxide ether polymeric monomer, 0~2 part of oiliness monomer, maleic anhydride deionized water input reactions
In kettle (reaction kettle is the three-necked flask with magnetic agitation of 500ml), 45~50 DEG C are warming up to, stirring to unsaturated polyoxy second
Alkene ether polymeric monomer is completely dissolved；2. aqueous initiator, oiliness initiator are added in reaction kettle, reaction 15~after twenty minutes, it adopts
Started that A feed liquids and B feed liquids are added dropwise simultaneously with constant flow pump, A feed liquids were added dropwise to complete at 2.5~3 hours, and B feed liquids were at 3~3.5 hours
It is added dropwise to complete, after all feed liquids are added dropwise to complete, the product of gained is finally down to room temperature, added by insulation reaction 1.5~2 hours
Enter liquid caustic soda (30wt% sodium hydroxide solutions) and adjusts pH value to 7 to get amphipathic carboxylic dispersants (high-molecular copolymer).
In above-mentioned technical proposal, currently preferred technical solution can be, in the reducing agent, L-AA and
The weight ratio of phosphorous acid is preferably 5:1.
Currently preferred technical solution is referring also to the following examples 1~5.
The present invention passes through acrylic acid, maleic anhydride, oiliness monomer (Styrene and its derivatives), unsaturated polyoxyethylene ether
Polymeric monomer carries out soap-free polymerization, prepares amphiphilic dispersant (water-reducing agent).The present invention be directed to that traditional polycarboxylic acids encounters it is above-mentioned these
Problem cuts means by molecule and is addressed, introduces hydrophobic rigid radical and change molecule hydrophilic and oleophilic value, utilize lipophilic group
Part heat resistance and salt tolerance, increase slurry flowing, slurry allowed more preferably to wrap up coarse aggregate, reduce weak transition zone.Increase main chain
Rigidity, allows molecule more to unfold in slurry, improves Molecular Adsorption rate so that slurry flow velocity can further increase.The present invention
Change the hydrophilic and oleophilic value of polycarboxylic acids molecule by introducing hydrophobic functional groups, introduces rigid functional group and change the rigid of strand
Property so that polycarboxylic acids Molecular Adsorption kenel is changed, and can effectively improve self-compacting concrete flow velocity, is improved concrete and is passed through steel
The ability of rib.Low glue material concrete wrapping property and workability can be obviously improved simultaneously.Present invention use is without soap aqueous solution polymerization.
Not applicable organic solvent, will not make troubles to environment and subsequent processing.Without using expensive chain-transferring agent, without using costliness
Hydrophily phenyl ring monomer has commercial introduction value.It prepares amphipathic carboxylic by environmentally protective no soap technique at low cost
Acid dispersant effectively increases self-compacting concrete flow velocity, improves concrete workability.
The dispersant of the present invention has high diminishing, high holding capacity, and can effectively improve concrete by reinforcing bar ability,
Improve concrete package and workability.The present invention uses soap-free polymerization, environmentally protective, avoids conventional emulsion polymerizations and solvent
Polymerization uses the pollution of emulsifier and organic solvent for environment.
Description of the drawings
Fig. 1 is that different sample concrete go out machine package status figure.
Fig. 2 is self-compacting concrete T500 and V slot test chart.
Specific implementation mode
Embodiment 1：Amphipathic carboxylic dispersants of the present invention are made of the raw material of following portions by weight：No
It (can be 72g, 0.03mol to be saturated polyoxyethylene ether polymeric monomer, that is, 72 parts of methyl allyl polyoxyethylene ether (TPEG2400)
TPEG 2400), 3 parts of maleic anhydride, 1.2 parts of aqueous initiator, that is, hydrogen peroxide (30% concentration, mass fraction), oiliness initiator
That is 0.001 part of azo-bis-isobutyl cyanide, 30 parts of deionized water, A feed liquids, B feed liquids；Above-mentioned A feed liquids by 8.6 parts of acrylic acid, 10 parts
Deionized water mixes and (is mixed in beaker and is formulated).B feed liquids are by 0.12 part of reducing agent, 0.3 part of chain-transferring agent, that is, mercapto
Base propionic acid and 10 parts of deionized waters mix and (are mixed in beaker and are formulated), and reducing agent is by 0.05 part of L- Vitamin C
Acid and 0.07 part of phosphorous acid mix.
The preparation method of the amphipathic carboxylic dispersants comprises the technical steps that：1. by unsaturated polyoxyethylene
(reaction kettle is 500ml with magnetic force in 3 parts and 10 parts 72 parts of ether polymeric monomer, maleic anhydride deionized water input reaction kettles
The three-necked flask of stirring), 50 DEG C are warming up to, stirring to unsaturated polyoxyethylene ether polymeric monomer is completely dissolved；2. in reaction kettle
1.2 parts of aqueous initiator, that is, hydrogen peroxide, oiliness initiator, that is, 0.001 part of azo-bis-isobutyl cyanide is added, after reacting 15 minutes, uses
Constant flow pump starts that A feed liquids and B feed liquids are added dropwise simultaneously, and A feed liquids were added dropwise to complete at 3 hours, and B feed liquids were added dropwise to complete at 3.5 hours, when
After all feed liquids are added dropwise to complete, the product of gained is finally down to room temperature by insulation reaction 1.5 hours, and liquid caustic soda (30wt% hydrogen is added
Sodium hydroxide solution) pH value is adjusted to 7 to get amphipathic carboxylic dispersants (high-molecular copolymer).Here it will use and be added without
Hydrophobic monomer carries out polycarboxylic acids synthesis, while product will be used as basic pattern and carry out amphipathic carboxylic dispersants and carry out pair
Than.
Embodiment 2：Amphipathic carboxylic dispersants of the present invention are made of the raw material of following portions by weight：No
It is saturated polyoxyethylene ether polymeric monomer, that is, 72 parts of methyl allyl polyoxyethylene ether (TPEG2400), oiliness monomer, that is, styrene 0.1
Part, 3 parts of maleic anhydride, 1.2 parts of aqueous initiator, that is, hydrogen peroxide (30% concentration, mass fraction), oiliness initiator, that is, azo two
0.001 part of isobutyl cyanogen, 30 parts of deionized water, A feed liquids, B feed liquids；Above-mentioned A feed liquids are by 8.6 parts of acrylic acid, 0.3 part of oiliness monomer
That is styrene and 10 parts of deionized waters mixes, B feed liquids by 0.1 part of reducing agent, 0.3 part of chain-transferring agent, that is, mercaptopropionic acid with
And 10 parts of deionized waters mix, reducing agent is mixed by 0.03 part of L-AA and 0.07 part of phosphorous acid.
The preparation method of the amphipathic carboxylic dispersants comprises the technical steps that：1. by unsaturated polyoxyethylene
It is (anti-in 3 parts and 10 parts 72 parts of ether polymeric monomer, oiliness monomer, that is, 0.1 part of styrene, maleic anhydride deionized water input reaction kettles
It is the three-necked flask with magnetic agitation of 500ml to answer kettle), 50 DEG C are warming up to, stirring to unsaturated polyoxyethylene ether polymeric monomer
It is completely dissolved；2. 1.2 parts of aqueous initiator, that is, hydrogen peroxide, oiliness initiator, that is, azo-bis-isobutyl cyanide are added in reaction kettle
0.001 part, after reacting 15 minutes, starting that A feed liquids and B feed liquids are added dropwise simultaneously using constant flow pump, A feed liquids were added dropwise to complete at 3 hours,
B feed liquids were added dropwise to complete at 3.5 hours, after all feed liquids are added dropwise to complete, insulation reaction 1.5 hours, finally by the product of gained
It is down to room temperature, liquid caustic soda (30wt% sodium hydroxide solutions) is added and adjusts pH value to 7 to get amphipathic carboxylic dispersants (high score
Sub- copolymer).The present embodiment reaction condition is same as Example 1, except that hydrophobic monomer styrene is added in the present embodiment
Carry out soap-free polymerization.
Embodiment 3：Amphipathic carboxylic dispersants of the present invention are made of the raw material of following portions by weight：No
Be saturated polyoxyethylene ether polymeric monomer, that is, 76 parts of methyl allyl polyoxyethylene ether (TPEG2400), oiliness monomer, that is, 1 part of styrene,
4 parts of maleic anhydride, 1.5 parts of aqueous initiator, that is, hydrogen peroxide (30% concentration, mass fraction), oiliness initiator, that is, two isobutyl of azo
0.01 part of cyanogen, 30 parts of deionized water, A feed liquids, B feed liquids；Above-mentioned A feed liquids are by 8.6 parts of acrylic acid, 3 parts of oiliness monomer, that is, benzene second
Alkene and 10 parts of deionized waters mix, and B feed liquids are by 0.12 part of reducing agent, 0.5 part of chain-transferring agent, that is, mercaptopropionic acid and 10
Part deionized water mixes and (is mixed in beaker and is formulated), and reducing agent is by 0.05 part of L-AA and 0.07 part of phosphorous
Acid mixes.
The preparation method of the amphipathic carboxylic dispersants comprises the technical steps that：1. by unsaturated polyoxyethylene
(reaction in 4 parts and 10 parts 76 parts of ether polymeric monomer, oiliness monomer, that is, 1 part of styrene, maleic anhydride deionized water input reaction kettles
Kettle is the three-necked flask with magnetic agitation of 500ml), 50 DEG C are warming up to, stirring is complete to unsaturated polyoxyethylene ether polymeric monomer
Fully dissolved；2. 1.5 parts of aqueous initiator, that is, hydrogen peroxide, oiliness initiator, that is, azo-bis-isobutyl cyanide 0.01 are added in reaction kettle
Part, after reacting 15 minutes, start that A feed liquids and B feed liquids are added dropwise simultaneously using constant flow pump, A feed liquids were added dropwise to complete at 3 hours, B feed liquids
It was added dropwise to complete at 3.5 hours, after all feed liquids are added dropwise to complete, the product of gained is finally down to room by insulation reaction 1.5 hours
Temperature is added liquid caustic soda (30wt% sodium hydroxide solutions) and adjusts pH value to 7 to get amphipathic carboxylic dispersants (polymer copolymerization
Object).
Embodiment 4：Amphipathic carboxylic dispersants of the present invention are made of the raw material of following portions by weight：No
Saturation polyoxyethylene ether polymeric monomer 72 parts of (TPEG 2400), 3 parts of maleic anhydride, aqueous draws oiliness monomer, that is, 0.5 part of styrene
Send out 1.5 parts of agent, that is, hydrogen peroxide (30% concentration, mass fraction), oiliness initiator, that is, 0.005 part of azo-bis-isobutyl cyanide, deionized water
30 parts, A feed liquids, B feed liquids；Above-mentioned A feed liquids are mixed by 8.6 parts of acrylic acid, 1 part of oiliness monomer, that is, styrene and 10 parts of deionizations
It closes, B feed liquids are mixed by 0.12 part of reducing agent, 0.4 part of chain-transferring agent, that is, mercaptopropionic acid and 10 parts of deionized waters, also
Former agent is mixed by 0.05 part of L-AA and 0.07 part of phosphorous acid.
The preparation method of the amphipathic carboxylic dispersants comprises the technical steps that：1. by unsaturated polyoxyethylene
It is (anti-in 3 parts and 10 parts 72 parts of ether polymeric monomer, oiliness monomer, that is, 0.5 part of styrene, maleic anhydride deionized water input reaction kettles
It is the three-necked flask with magnetic agitation of 500ml to answer kettle), 50 DEG C are warming up to, stirring to unsaturated polyoxyethylene ether polymeric monomer
It is completely dissolved；2. 1.5 parts of aqueous initiator, that is, hydrogen peroxide, oiliness initiator, that is, azo-bis-isobutyl cyanide are added in reaction kettle
0.005 part, after reacting 15 minutes, starting that A feed liquids and B feed liquids are added dropwise simultaneously using constant flow pump, A feed liquids were added dropwise to complete at 3 hours,
B feed liquids were added dropwise to complete at 3.5 hours, after all feed liquids are added dropwise to complete, insulation reaction 1.5 hours, finally by the product of gained
It is down to room temperature, liquid caustic soda (30wt% sodium hydroxide solutions) is added and adjusts pH value to 7 to get amphipathic carboxylic dispersants (high score
Sub- copolymer).
Embodiment 5：Amphipathic carboxylic dispersants of the present invention are made of the raw material of following portions by weight：No
It is saturated 74 parts of polyoxyethylene ether polymeric monomer, 1.8 parts of oiliness monomer, 3.5 parts of maleic anhydride, 1 part of aqueous initiator, oiliness initiator
0.01 part, 30 parts of deionized water, A feed liquids, B feed liquids.Wherein, above-mentioned unsaturated polyoxyethylene ether polymeric monomer is poly- for isobutene alcohol
Ethylene oxide ether.Above-mentioned oiliness monomer is styrene；Above-mentioned aqueous initiator is potassium peroxydisulfate (or ammonium persulfate), azo
The weight ratio of the composition (mixture) of two two kinds of NSC 18620 hydrochlorides, potassium peroxydisulfate and azo-bis-isobutyrate hydrochloride is 1：
0.5.Above-mentioned oiliness initiator is benzoyl peroxide.Above-mentioned A feed liquids are by 10 parts of acrylic acid, 2 parts of oiliness monomer, that is, benzene second
Alkene and 10 parts of deionized waters mix and (are mixed in beaker and are formulated), and B feed liquids are by 0.10 part of reducing agent, 0.4 part of chain
Transfer agent and 10 parts of deionized waters mix and (are mixed in beaker and are formulated), and reducing agent is by L-AA and Asia
Phosphoric acid mixes, and the weight ratio of L-AA and phosphorous acid is 5:1.Chain-transferring agent is mercaptopropionic acid.
The preparation method of the amphipathic carboxylic dispersants comprises the technical steps that：1. by unsaturated polyoxyethylene
74 parts of ether polymeric monomer, 1.8 parts of oiliness monomer, (reaction kettle is in maleic anhydride 3.5 parts and 10 parts deionized waters input reaction kettles
The three-necked flask with magnetic agitation of 500ml), 45 DEG C are warming up to, stirring is completely molten to unsaturated polyoxyethylene ether polymeric monomer
Solution；2. aqueous initiator, oiliness initiator are added in reaction kettle, reaction after twenty minutes, starts that A is added dropwise simultaneously using constant flow pump
Feed liquid and B feed liquids, A feed liquids were added dropwise to complete at 3 hours, and B feed liquids were added dropwise to complete at 3.5 hours, after all feed liquids are added dropwise to complete,
The product of gained is finally down to room temperature by insulation reaction 2 hours, be added liquid caustic soda (30wt% sodium hydroxide solutions) adjust pH value to
7 to get amphipathic carboxylic dispersants (high-molecular copolymer).
It is the performance evaluation that the amphipathic carboxylic dispersants (product) of 1~4 gained of above example are carried out below.
Flowing degree of net paste of cement is tested according to GB8077-2012《Methods for testing uniformity of concrete admixture》Provide into
Row weighs cement 300g, and 87g water is added, and net slurry test is carried out according to the ratio of mud 0,29.The high victory cement P.O42.5 of cement selection.
1 quiet slurry test data of table
It can be seen from Table 1 that polycarboxylate dispersant after introducing portion hydrophobic grouping in the early stage can be on dispersion effect
It the increase of hydrophobic group content and reduces, but increasing with hydrophobic grouping, holding capacity can gradually increase.
Concrete test below, concrete mix is as shown in table 2, concrete slump and divergence experiment according to
GB/T50080-2002《Standard for test methods of properties of ordinary concrete mixture standard (attached provision explanation)》Regulation carries out, and result is such as
Shown in table 3.
2 concrete mix of table, cement selection high victory P.O.42,5
3 concrete experiments result of table
From table 3 it can be seen that concrete test result is identical as quiet slurry result.Polycarboxylic acids after introducing portion hydrophobic grouping
Dispersant can reduce on dispersion effect in the early stage with the increase of hydrophobic group content, because reaching the same slump, need
The dispersion dosage wanted is more.But increasing with hydrophobic grouping, holding capacity can gradually increase.
As shown in Figure 1, label 1, label 2, label 4, label 3 are respectively embodiment 1, embodiment 2, embodiment 4, embodiment
3 package status figure.When as seen from Figure 1, using traditional polycarboxylate dispersant, goes out machine concrete and there is leakage stone, slurry packet
Insufficient disadvantage is wrapped up in, the workability of concrete is affected, to affect concrete construction and beauty after molding.But
The dispersant that amphiphilic is modified is used, concrete leakage stone phenomenon has obtained apparent solution, and slurry obviously enriches, whole to wrap
The property wrapped up in is improved.Floating operation is carried out to levelling concrete surface after initially going out machine using spatula simultaneously, until surface occurs
Until slurry.It tests different example sample concrete and reaches the surface pulp required floating time.Also may be used by floating number
It finds to be easier to smooth out (being shown in Table 4) by modified amphiphilic polycarboxylate dispersant with apparent, its slurry of surface is more rich, workability
More preferably, it is easier to construct.
Table 4, which reaches, smoothes out number needed for pulp
| Sample | Smooth out number |
| Embodiment 1 | 7 |
| Embodiment 2 | 5 |
| Embodiment 3 | 2 |
| Embodiment 4 | 3 |
The interaction of sample and self-compacting concrete is evaluated, T500 and V-shaped groove flow time conduct are used
Evaluation index judges its flow velocity.C60 mix parameters of high-strength self-compacting concrete is as shown in table 5.The self-compacting concrete slump is shown in Table 6.
5 mix parameters of high-strength self-compacting concrete of table
| Cement | Flyash | Miberal powder | Sand | Stone |
| 292 | 158 | 100 | 782 | 954 |
The 6 self-compacting concrete slump of table
Reach identical initial slump by changing the volume of additive in experiment, is then surveyed respectively in 5 minutes again
T500 times and V-shaped groove flow time are tried, test results are shown in figure 2.
As seen in Figure 2, amphipathic carboxylic dispersants compared with traditional polycarboxylate dispersant for, can obviously reduce
Concrete T 500 and V slot flow times can accelerate construction progress to improve self-compacting concrete flow velocity, promote coagulation
Soil improves construction quality by reinforcing bar ability.Simultaneously it has also been found that passing through the ratio for improving hydrophobic grouping, concrete flow velocity also can phase
It should improve, but it can promote the required volume of dispersant.
5 obtained data of embodiment are close with embodiment 2.
The dispersant of the present invention has high diminishing, high holding capacity, and can effectively improve concrete by reinforcing bar ability,
Improve concrete package and workability.The present invention uses soap-free polymerization, environmentally protective, avoids conventional emulsion polymerizations and solvent
Polymerization uses the pollution of emulsifier and organic solvent for environment.
In conclusion the present invention effectively increases self-compacting concrete flow velocity, concrete workability is improved, while this is poly-
The preparation process of carboxylic dispersants is simple, environmentally protective.
Claims (9)
1. a kind of amphipathic carboxylic dispersants, it is characterised in that it is made of the raw material of following portions by weight：It is unsaturated
72~76 parts of polyoxyethylene ether polymeric monomer, 0~2 part of oiliness monomer, 3~4 parts of maleic anhydride, 1~1.5 part of aqueous initiator, oil
0.001~0.01 part of initiator of property, 30 parts of deionized water, A feed liquids, B feed liquids；
Wherein, above-mentioned unsaturated polyoxyethylene ether polymeric monomer be methyl allyl polyoxyethylene ether, allyl polyethenoxy ether,
One kind in isoamyl alcohol polyoxyethylene ether, isobutene alcohol polyoxyethylene ether；Above-mentioned oiliness monomer is styrene or benzene second
Ene derivative；Above-mentioned aqueous initiator is one or any in hydrogen peroxide, persulfate, azo-bis-isobutyrate hydrochloride
Two kinds of compositions for pressing arbitrary quality proportioning；Above-mentioned oiliness initiator is one in azo-bis-isobutyl cyanide, benzoyl peroxide
Kind or two kinds of compositions for pressing arbitrary quality proportioning；
Above-mentioned A feed liquids are mixed by 5~11 parts of acrylic acid, 0~4 part of oiliness monomer and 10 parts of deionized waters, B feed liquids by
0.08~0.12 part of reducing agent, 0.3-~0.5 part chain-transferring agent and 10 parts of deionized waters mix, and reducing agent is resisted by L-
Bad hematic acid and phosphorous acid mix, and chain-transferring agent is mercaptopropionic acid；
The preparation method of the amphipathic carboxylic dispersants comprises the technical steps that：1. unsaturated polyoxyethylene ether is big
3~4 parts and 10 parts 72~76 parts of monomer, 0~2 part of oiliness monomer, maleic anhydride deionized waters are put into reaction kettles, are warming up to
45~50 DEG C, stirring to unsaturated polyoxyethylene ether polymeric monomer is completely dissolved；2. aqueous initiator, oiliness are added in reaction kettle
Initiator, reaction 15~after twenty minutes, start that A feed liquids and B feed liquids are added dropwise simultaneously using constant flow pump, A feed liquids were at 2.5~3 hours
It being added dropwise to complete, B feed liquids were added dropwise to complete at 3~3.5 hours, after all feed liquids are added dropwise to complete, insulation reaction 1.5~2 hours, most
The product of gained is down to room temperature afterwards, liquid caustic soda is added and adjusts pH value to 7 to get amphipathic carboxylic dispersants.
2. amphipathic carboxylic dispersants according to claim 1, it is characterised in that in above-mentioned reducing agent, L-AA
Weight ratio with phosphorous acid is 5:1.
3. amphipathic carboxylic dispersants according to claim 1, it is characterised in that it is the original by following portions by weight
Made of material：Unsaturated polyoxyethylene ether polymeric monomer, that is, 2,400 72 parts of methyl allyl polyoxyethylene ether TPEG, maleic anhydride 3
Part, 1.2 parts of aqueous initiator, that is, hydrogen peroxide, oiliness initiator, that is, 0.001 part of azo-bis-isobutyl cyanide, 30 parts of deionized water, A material
Liquid, B feed liquids；Above-mentioned A feed liquids are mixed by 8.6 parts of acrylic acid, 10 parts of deionized waters, B feed liquids by 0.12 part of reducing agent,
0.3 part of chain-transferring agent, that is, mercaptopropionic acid and 10 parts of deionized waters mix, reducing agent be by 0.05 part of L-AA and
0.07 part of phosphorous acid mixes；
The preparation method of the amphipathic carboxylic dispersants comprises the technical steps that：1. unsaturated polyoxyethylene ether is big
In 3 parts and 10 parts 72 parts of monomer, maleic anhydride deionized water input reaction kettles, 50 DEG C are warming up to, stirring to unsaturated polyoxy
Vinethene polymeric monomer is completely dissolved；2. 1.2 parts of aqueous initiator, that is, hydrogen peroxide, oiliness initiator, that is, azo are added in reaction kettle
Two 0.001 part of isobutyl cyanogen start that A feed liquids and B feed liquids are added dropwise simultaneously using constant flow pump, A feed liquids were at 3 hours after reacting 15 minutes
It being added dropwise to complete, B feed liquids were added dropwise to complete at 3.5 hours, after all feed liquids are added dropwise to complete, insulation reaction 1.5 hours, finally by institute
The product obtained is down to room temperature, and liquid caustic soda is added and adjusts pH value to 7 to get amphipathic carboxylic dispersants.
4. amphipathic carboxylic dispersants according to claim 1, it is characterised in that it is the original by following portions by weight
Made of material：Unsaturated polyoxyethylene ether polymeric monomer, that is, 2,400 72 parts of methyl allyl polyoxyethylene ether TPEG, oiliness monomer
That is 0.1 part of styrene, 3 parts of maleic anhydride, 1.2 parts of aqueous initiator, that is, hydrogen peroxide, oiliness initiator, that is, azo-bis-isobutyl cyanide
0.001 part, 30 parts of deionized water, A feed liquids, B feed liquids；Above-mentioned A feed liquids are by 8.6 parts of acrylic acid, 0.3 part of oiliness monomer, that is, benzene second
Alkene and 10 parts of deionized waters mix, and B feed liquids are by 0.1 part of reducing agent, 0.3 part of chain-transferring agent, that is, mercaptopropionic acid and 10 parts
Deionized water mixes, and reducing agent is mixed by 0.03 part of L-AA and 0.07 part of phosphorous acid；
The preparation method of the amphipathic carboxylic dispersants comprises the technical steps that：1. unsaturated polyoxyethylene ether is big
In 3 parts and 10 parts 72 parts of monomer, oiliness monomer, that is, 0.1 part of styrene, maleic anhydride deionized water input reaction kettles, it is warming up to
50 DEG C, stirring to unsaturated polyoxyethylene ether polymeric monomer is completely dissolved；2. aqueous initiator, that is, hydrogen peroxide is added in reaction kettle
1.2 parts, oiliness initiator, that is, 0.001 part of azo-bis-isobutyl cyanide after reacting 15 minutes, start that A material are added dropwise simultaneously using constant flow pump
Liquid and B feed liquids, A feed liquids were added dropwise to complete at 3 hours, and B feed liquids were added dropwise to complete at 3.5 hours, after all feed liquids are added dropwise to complete, were protected
Temperature reaction 1.5 hours, is finally down to room temperature by the product of gained, and liquid caustic soda is added and adjusts pH value to 7 to get amphipathic carboxylic acid point
Powder.
5. amphipathic carboxylic dispersants according to claim 1, it is characterised in that it is the original by following portions by weight
Made of material：Unsaturated polyoxyethylene ether polymeric monomer, that is, 2,400 76 parts of methyl allyl polyoxyethylene ether TPEG, oiliness monomer
That is 1 part of styrene, 4 parts of maleic anhydride, 1.5 parts of aqueous initiator, that is, hydrogen peroxide, oiliness initiator, that is, azo-bis-isobutyl cyanide 0.01
Part, 30 parts of deionized water, A feed liquids, B feed liquids；Above-mentioned A feed liquids by 8.6 parts of acrylic acid, 3 parts of oiliness monomer, that is, styrene and
10 parts of deionized waters mix, B feed liquids by 0.12 part of reducing agent, 0.5 part of chain-transferring agent, that is, mercaptopropionic acid and 10 parts go from
Sub- water mixes, and reducing agent is mixed by 0.05 part of L-AA and 0.07 part of phosphorous acid；
The preparation method of the amphipathic carboxylic dispersants comprises the technical steps that：1. unsaturated polyoxyethylene ether is big
In 4 parts and 10 parts 76 parts of monomer, oiliness monomer, that is, 1 part of styrene, maleic anhydride deionized water input reaction kettles, it is warming up to 50
DEG C, stirring to unsaturated polyoxyethylene ether polymeric monomer is completely dissolved；2. aqueous initiator, that is, hydrogen peroxide 1.5 is added in reaction kettle
Part, oiliness initiator, that is, 0.01 part of azo-bis-isobutyl cyanide after reacting 15 minutes start that A feed liquids and B are added dropwise simultaneously using constant flow pump
Feed liquid, A feed liquids were added dropwise to complete at 3 hours, and B feed liquids were added dropwise to complete at 3.5 hours, and after all feed liquids are added dropwise to complete, heat preservation is anti-
It answers 1.5 hours, the product of gained is finally down to room temperature, liquid caustic soda is added and adjusts pH value to 7 to get the dispersion of amphipathic carboxylic acid
Agent.
6. amphipathic carboxylic dispersants according to claim 1, it is characterised in that it is the original by following portions by weight
Made of material：Unsaturated 2,400 72 parts of polyoxyethylene ether polymeric monomer TPEG, oiliness monomer, that is, 0.5 part of styrene, maleic anhydride 3
Part, 1.5 parts of aqueous initiator, that is, hydrogen peroxide, oiliness initiator, that is, 0.005 part of azo-bis-isobutyl cyanide, 30 parts of deionized water, A material
Liquid, B feed liquids；Above-mentioned A feed liquids are mixed by 8.6 parts of acrylic acid, 1 part of oiliness monomer, that is, styrene and 10 parts of deionizations, B
Feed liquid is mixed by 0.12 part of reducing agent, 0.4 part of chain-transferring agent, that is, mercaptopropionic acid and 10 parts of deionized waters, reducing agent by
0.05 part of L-AA and 0.07 part of phosphorous acid mix；
The preparation method of the amphipathic carboxylic dispersants comprises the technical steps that：1. unsaturated polyoxyethylene ether is big
In 3 parts and 10 parts 72 parts of monomer, oiliness monomer, that is, 0.5 part of styrene, maleic anhydride deionized water input reaction kettles, it is warming up to
50 DEG C, stirring to unsaturated polyoxyethylene ether polymeric monomer is completely dissolved；2. aqueous initiator, that is, hydrogen peroxide is added in reaction kettle
1.5 parts, oiliness initiator, that is, 0.005 part of azo-bis-isobutyl cyanide after reacting 15 minutes, start that A material are added dropwise simultaneously using constant flow pump
Liquid and B feed liquids, A feed liquids were added dropwise to complete at 3 hours, and B feed liquids were added dropwise to complete at 3.5 hours, after all feed liquids are added dropwise to complete, were protected
Temperature reaction 1.5 hours, is finally down to room temperature by the product of gained, and liquid caustic soda is added and adjusts pH value to 7 to get amphipathic carboxylic acid point
Powder.
7. amphipathic carboxylic dispersants according to claim 1, it is characterised in that it is the original by following portions by weight
Made of material：74 parts of unsaturated polyoxyethylene ether polymeric monomer, 1.8 parts of oiliness monomer, 3.5 parts of maleic anhydride, aqueous initiator 1
Part, 0.01 part of oiliness initiator, 30 parts of deionized water, A feed liquids, B feed liquids；Wherein, the above-mentioned big list of unsaturated polyoxyethylene ether
Body is isobutene alcohol polyoxyethylene ether, and above-mentioned oiliness monomer is styrene, and above-mentioned aqueous initiator is potassium peroxydisulfate, azo
The weight ratio of the composition of two two kinds of NSC 18620 hydrochlorides, potassium peroxydisulfate and azo-bis-isobutyrate hydrochloride is 1：0.5, it is above-mentioned
Oiliness initiator be benzoyl peroxide, above-mentioned A feed liquids are by 10 parts of acrylic acid, 2 parts of oiliness monomer, that is, styrene and 10
Part deionized water mixes, and B feed liquids are mixed by 0.10 part of reducing agent, 0.4 part of chain-transferring agent and 10 parts of deionized waters,
Reducing agent is mixed by L-AA and phosphorous acid, and the weight ratio of L-AA and phosphorous acid is 5:1, chain tra nsfer
Agent is mercaptopropionic acid；
The preparation method of the amphipathic carboxylic dispersants comprises the technical steps that：1. unsaturated polyoxyethylene ether is big
3.5 parts and 10 parts 74 parts of monomer, 1.8 parts of oiliness monomer, maleic anhydride deionized waters are put into reaction kettles, are warming up to 45 DEG C,
Stirring to unsaturated polyoxyethylene ether polymeric monomer is completely dissolved；2. aqueous initiator, oiliness initiator are added in reaction kettle, instead
It should start that A feed liquids and B feed liquids are added dropwise simultaneously using constant flow pump, A feed liquids were added dropwise to complete at 3 hours, and B feed liquids are 3.5 after twenty minutes
Hour is added dropwise to complete, and after all feed liquids are added dropwise to complete, the product of gained is finally down to room temperature by insulation reaction 2 hours, is added
Liquid caustic soda adjusts pH value to 7 to get amphipathic carboxylic dispersants.
8. a kind of preparation method of amphipathic carboxylic dispersants described in claim 1, it is characterised in that it includes following work
Skill step：1. by 72~76 parts of unsaturated polyoxyethylene ether polymeric monomer, 0~2 part of oiliness monomer, 3~4 parts of maleic anhydride and 10
In part deionized water input reaction kettle, 45~50 DEG C are warming up to, stirring to unsaturated polyoxyethylene ether polymeric monomer is completely dissolved；②
Addition aqueous initiator, oiliness initiator in reaction kettle, reaction 15~after twenty minutes, start that A is added dropwise simultaneously using constant flow pump
Feed liquid and B feed liquids, A feed liquids were added dropwise to complete at 2.5~3 hours, and B feed liquids were added dropwise to complete at 3~3.5 hours, when all feed liquids are dripped
After the completion of adding, the product of gained is finally down to room temperature by insulation reaction 1.5~2 hours, be added liquid caustic soda adjust pH value to 7 to get
Amphipathic carboxylic dispersants.
9. the preparation method of amphipathic carboxylic dispersants according to claim 8, it is characterised in that in above-mentioned reducing agent,
The weight ratio of L-AA and phosphorous acid is 5:1.
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