CN108164173A - A kind of concrete slump retaining agent and preparation method thereof - Google Patents
A kind of concrete slump retaining agent and preparation method thereof Download PDFInfo
- Publication number
- CN108164173A CN108164173A CN201711310750.9A CN201711310750A CN108164173A CN 108164173 A CN108164173 A CN 108164173A CN 201711310750 A CN201711310750 A CN 201711310750A CN 108164173 A CN108164173 A CN 108164173A
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- Prior art keywords
- unsaturated
- polymeric monomer
- beta
- agent
- slump retaining
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Classifications
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B24/00—Use of organic materials as active ingredients for mortars, concrete or artificial stone, e.g. plasticisers
- C04B24/16—Sulfur-containing compounds
- C04B24/161—Macromolecular compounds comprising sulfonate or sulfate groups
- C04B24/163—Macromolecular compounds comprising sulfonate or sulfate groups obtained by reactions only involving carbon-to-carbon unsaturated bonds
- C04B24/165—Macromolecular compounds comprising sulfonate or sulfate groups obtained by reactions only involving carbon-to-carbon unsaturated bonds containing polyether side chains
-
- 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
-
- 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
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/10—Esters
- C08F220/38—Esters containing sulfur
-
- 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
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/10—Esters
- C08F220/38—Esters containing sulfur
- C08F220/387—Esters containing sulfur and containing nitrogen and oxygen
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Curing Cements, Concrete, And Artificial Stone (AREA)
Abstract
The invention discloses a kind of concrete slump retaining agents and preparation method thereof, belong to concrete admixture field.Its primary raw material includes polymeric monomer, unsaturated acids, beta-unsaturated esters, unsaturated amides, initiator and chain conversion agent, polymeric monomer, unsaturated acids, beta-unsaturated esters and unsaturated amides molar ratio be 1：1~3.5：1~3：1~3, initiator accounts for the 0.5~1.8% of polymeric monomer, unsaturated acids, beta-unsaturated esters and unsaturated amides gross mass, chain conversion agent accounts for the 0.1~0.5% of polymeric monomer, unsaturated acids, beta-unsaturated esters and unsaturated amides gross mass, wherein, polymeric monomer is allyl polyethenoxy ether ichthyodin.The slump retaining agent function of slump protection that the present invention synthesizes is good, convenient for production.
Description
Technical field
The invention belongs to concrete admixture fields, and in particular to a kind of concrete slump retaining agent.
Background technology
Concrete is that purposes is most wide in modern civil engineering, a kind of construction material of dosage maximum.As present commodity mix
The widespread adoption of soil is coagulated, centralized mixing and commercialized supply become its main feature, and this requires concrete have passed through
The transport of long period and remain able to maintain the bigger slump after parking.
At present, the method for the damage that solves to collapse mainly has：（1）Latter admixing method,（2）Mixing applied force method,（3）Comminution granulation.Wherein,
Latter admixing method is easy to operate, and damage of collapsing to inhibition has positive effect, but this method is not easy to quality control, and have regular hour limitation,
Problem can not be fully solved.Comminution granulation is the granular substance that water-reducing agent is made to different-grain diameter, different rate of dissolutions, is formed not
Same dissolving gradient, makes the water-reducing agent in system maintain critical micell state always, the slump is finally made not lose or lose
Very little, but the control wherein to grain size and rate of dissolution, need very accurate equipment, and input cost is higher.Mixing applied force method
As slump retaining agent due to it is at low cost, effect is good, so as to be widely applied.
Invention content
In view of the deficiencies of the prior art, the present invention provides a kind of good, convenient for production, the lower-cost coagulations of function of slump protection
Native slump retaining agent.
To solve the above-mentioned problems, the technical solution adopted by the present invention is that：
A kind of concrete slump retaining agent, the structural formula of active ingredient is as follows, and molecular weight is 15000~100000：
Its primary raw material includes polymeric monomer, unsaturated acids, beta-unsaturated esters, unsaturated amides, initiator and chain conversion agent, big single
Body, unsaturated acids, beta-unsaturated esters and unsaturated amides molar ratio be 1：1~3.5：1~3：1~3, initiator account for polymeric monomer,
The 0.5~1.8% of unsaturated acids, beta-unsaturated esters and unsaturated amides gross mass, chain conversion agent accounts for polymeric monomer, unsaturated acids, insatiable hunger
With the 0.1~0.5% of ester and unsaturated amides gross mass,
Wherein, polymeric monomer is allyl polyethenoxy ether ichthyodin, and structural formula is：R1HC=CHCH2O(CH2CH2O)nSO3NH4,
The structural formula of unsaturated acids is R2CH=CHCOOH, the structural formula of beta-unsaturated esters are：R2CH=CR1COOR3, the knot of unsaturated amides
Structure formula is：CH2=CHCONR4R5, R1For H or CH3, R2For H, CH3At least one of with COONa, R3For H, CH3And CH2CH2OH
At least one of, R4、R5Mutually independent is hydrogen atom, CH3And CH2CH3At least one of.
Further, the molecular weight of the polymeric monomer is 400 ~ 2000.
Further, the initiator is redox initiator, and wherein oxidant is hydrogen peroxide, ammonium persulfate, mistake
At least one of sodium sulphate and tert-butyl hydroperoxide, reducing agent is hangs informal voucher, ascorbic acid, sodium sulfite and hypophosphites
At least one of.
Further, the chain conversion agent is thioacetic acid or mercaptopropionic acid.
A kind of preparation method of above-mentioned concrete slump retaining agent, includes the following steps：
（1）Deionized water is warming up to 58 DEG C, adds in the polymeric monomer, stirring is to being completely dissolved；
（2）Oxidizing agent solution is added dropwise in above-mentioned solution, and is warming up to 60 DEG C；
（3）By the mixed solution of the unsaturated acids, beta-unsaturated esters and unsaturated amides and the chain conversion agent and reducing agent
Mixed solution is added drop-wise to respectively while at the uniform velocity in above-mentioned solution, and total duration was added dropwise at 1.5~2 hours in control, during dropwise addition
60 DEG C of constant temperature, after being added dropwise to complete, constant temperature stirs 1 hour；
（4）Slowly reduce temperature to 50~55 DEG C, while stirring be added dropwise sodium hydroxide solution adjust pH to 6.8 to get.
The beneficial effects of the invention are as follows：
1. polymeric monomer uses allyl polyethenoxy ether ichthyodin, the allyl polyethenoxy ether of long side chain is compared, is copolymerized effect
More preferably.
2. the sulfonic acid group introduced in molecular structure, the preferential disperse cement particles of energy, delay hydrated cementitious.
3. introducing ester group in molecular structure, hydrolyzed in the alkaline environment of cement slurry, release carboxyl adsorption group compared with
Soon, early stage guarantor can be played the role of to collapse.
4. introducing amide group in molecular structure, hydrolyzed in the alkaline environment of cement slurry and release adsorption group,
But its rate of release is slower than ester-type hydrolysis speed, collapses so as to play the role of later stage guarantor.
The raw material sources that the present invention uses are extensive, of low cost, and preparation process is simple, and the reaction time is short and reaction temperature
It is low, while protect and collapse that effect is good, and the duration is long, application easy to spread.
Specific embodiment
The embodiment of the present invention is described below in detail, the example of the embodiment is intended to be used to explain the present invention, and cannot
It is interpreted as limitation of the present invention.
Embodiment 1：The preparation of concrete slump retaining agent
115g deionized waters is taken to put into reaction vessel, are warming up to 58 DEG C.Put into 240.0g allyl polyethenoxy ether sulfonic acid
Ammonium ASPEG-1200（Molecular weight 1200）Stirring to monomer is completely dissolved.It keeps temperature-resistant, it is molten that first is at the uniform velocity added dropwise into container
Liquid continues stirring 2~3 minutes after completion of dropwise addition, while is warming up to 60 DEG C.Start at the uniform velocity to be added dropwise second solution and third molten into container
Liquid, time for adding are 2 hours, and reaction temperature is controlled at 60 DEG C, and 1 hour is kept the temperature after being added dropwise.Temperature is reduced to 54 DEG C, is added in
30% sodium hydroxide solution adjusts pH to 6.8 to get finished product.
Wherein, first solution is made of 1.8g sodium peroxydisulfates and 8.2g deionized waters；Second solution by 26.0g methacrylic acids,
46.0g hydroxy-ethyl acrylates, 39.6gN, N- dimethacrylamide and 40.0g deionized waters composition；Third solution is anti-bad by 1.0g
Hematic acid, 1.0g thioacetic acid and 18.0g deionized waters composition.
Embodiment 2：The preparation of concrete slump retaining agent
86g deionized waters is taken to put into reaction vessel, are warming up to 58 DEG C.Put into 180.0g allyl polyethenoxy ether ichthyodins
ASPEG-1200（Molecular weight 1200）Stirring to monomer is completely dissolved.It keeps temperature-resistant, first solution is at the uniform velocity added dropwise into container,
Continue stirring after completion of dropwise addition 2~3 minutes, while be warming up to 60 DEG C.Start that second solution and the third solution are at the uniform velocity added dropwise into container,
Time for adding is 2 hours, and reaction temperature is controlled at 60 DEG C, and 1 hour is kept the temperature after being added dropwise.Temperature is reduced to 54 DEG C, adds in 30%
Sodium hydroxide solution adjusts pH to 6.8 to get finished product.
Wherein, first solution is made of 1.5g sodium peroxydisulfates and 6g deionized waters；Second solution by 25.5g methacrylic acids,
52.2g hydroxy-ethyl acrylates, 29.7gN, N- dimethacrylamide and 30.0g deionized waters composition；Third solution is anti-bad by 0.9g
Hematic acid, 0.8g thioacetic acid and 10.0g deionized waters composition.
Embodiment 3：The preparation of concrete slump retaining agent
110.0g deionized waters is taken to put into reaction vessel, are warming up to 58 DEG C.Put into 228.0g allyl polyethenoxy ether sulphurs
Sour ammonium ASPEG-1200（Molecular weight 1200）Stirring to monomer is completely dissolved.It keeps temperature-resistant, first is at the uniform velocity added dropwise into container
Solution continues stirring 2~3 minutes after completion of dropwise addition, while is warming up to 60 DEG C.Start that second solution and third are at the uniform velocity added dropwise into container
Solution, time for adding are 2 hours, and reaction temperature is controlled at 60 DEG C, and 1 hour is kept the temperature after being added dropwise.Temperature is reduced to 54 DEG C, is added
Enter 30% sodium hydroxide solution, adjust pH to 6.8 to get finished product.
Wherein, first solution is made of 2.0g sodium peroxydisulfates and 8.0g deionized waters；Second solution by 32.3g methacrylic acids,
66.1g hydroxy-ethyl acrylates, 56.4gN, N- dimethacrylamide and 38.0g deionized waters composition；Third solution is anti-bad by 1.1g
Hematic acid, 1.0g thioacetic acid and 17.0g deionized waters composition.
The product of above example is evaluated：
More than 3 embodiment products, carry out flowing degree of net paste of cement and the slump test.
Cement paste experiment according to《Methods for testing uniformity of concrete admixture》（GB/T 8076-2008）It carries out, collapses
Degree test reference《Normal concrete mix method for testing performance standard》（GB/T 50080-2016）It carries out, experimental result is such as
Following table.
By above-mentioned data it is found that the slump retaining agent that the present invention synthesizes can make fresh concrete initial slump in 2 hours
Substantially it does not lose, and fluidity is kept not lost in 2 hours.
Certainly, described above is only presently preferred embodiments of the present invention, not limitation of the present invention, and the present invention is not yet
Be only limitted to the example above, variation that those skilled in the art are made in the essential scope of the present invention, remodeling,
Addition is replaced, and also belongs to protection scope of the present invention.
Claims (5)
1. a kind of concrete slump retaining agent, which is characterized in that the structural formula of its active ingredient is as follows, molecular weight for 15000~
100000：
Its primary raw material includes polymeric monomer, unsaturated acids, beta-unsaturated esters, unsaturated amides, initiator and chain conversion agent, big single
Body, unsaturated acids, beta-unsaturated esters and unsaturated amides molar ratio be 1：1~3.5：1~3：1~3, initiator account for polymeric monomer,
The 0.5~1.8% of unsaturated acids, beta-unsaturated esters and unsaturated amides gross mass, chain conversion agent accounts for polymeric monomer, unsaturated acids, insatiable hunger
With the 0.1~0.5% of ester and unsaturated amides gross mass,
Wherein, polymeric monomer is allyl polyethenoxy ether ichthyodin, and structural formula is：R1HC=CHCH2O(CH2CH2O)nSO3NH4,
The structural formula of unsaturated acids is R2CH=CHCOOH, the structural formula of beta-unsaturated esters are：R2CH=CR1COOR3, the knot of unsaturated amides
Structure formula is：CH2=CHCONR4R5, R1For H or CH3, R2For H, CH3At least one of with COONa, R3For H, CH3And CH2CH2OH
At least one of, R4、R5Mutually independent is hydrogen atom, CH3And CH2CH3At least one of.
2. a kind of concrete slump retaining agent according to claim 1, which is characterized in that the molecular weight of the polymeric monomer is 400
~2000.
3. a kind of concrete slump retaining agent according to claim 1, which is characterized in that the initiator is Redox Initiator
Agent, wherein oxidant are at least one of for hydrogen peroxide, ammonium persulfate, sodium peroxydisulfate and tert-butyl hydroperoxide, reducing agent
To hang at least one of informal voucher, ascorbic acid, sodium sulfite and hypophosphites.
4. a kind of concrete slump retaining agent according to claim 1, which is characterized in that the chain conversion agent for thioacetic acid or
Mercaptopropionic acid.
5. according to a kind of preparation method of concrete slump retaining agent of Claims 1 to 4 any one of them, which is characterized in that including
Following steps：
（1）Deionized water is warming up to 58 DEG C, adds in the polymeric monomer, stirring is to being completely dissolved；
（2）Oxidizing agent solution is added dropwise in above-mentioned solution, and is warming up to 60 DEG C；
（3）By the mixed solution of the unsaturated acids, beta-unsaturated esters and unsaturated amides and the chain conversion agent and reducing agent
Mixed solution is added drop-wise to respectively while at the uniform velocity in above-mentioned solution, and total duration was added dropwise at 1.5~2 hours in control, during dropwise addition
60 DEG C of constant temperature, after being added dropwise to complete, constant temperature stirs 1 hour；
（4）Slowly reduce temperature to 50~55 DEG C, while stirring be added dropwise sodium hydroxide solution adjust pH to 6.8 to get.
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| CN201711310750.9A CN108164173A (en) | 2017-12-11 | 2017-12-11 | A kind of concrete slump retaining agent and preparation method thereof |
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| CN201711310750.9A CN108164173A (en) | 2017-12-11 | 2017-12-11 | A kind of concrete slump retaining agent and preparation method thereof |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102924669A (en) * | 2011-08-10 | 2013-02-13 | 广州泰祥混凝土外加剂有限公司 | Preparation method of polycarboxylate superplasticizer |
| US20130172505A1 (en) * | 2010-07-27 | 2013-07-04 | Jian Fang | Synthesis method of polycarboxylic acid water-reducing agent |
| CN103788307A (en) * | 2012-10-27 | 2014-05-14 | 北京市建筑工程研究院有限责任公司 | Preparation method of novel concrete slump retaining agent based on allyl polyoxyethylene ether |
| CN105294953A (en) * | 2015-11-26 | 2016-02-03 | 科之杰新材料集团有限公司 | Preparation method of polycarboxylic acid super slump retaining agent |
| CN105712651A (en) * | 2015-12-15 | 2016-06-29 | 江苏苏博特新材料股份有限公司 | Concrete slump retaining agent for very-long-time slump retaining and preparation method thereof |
-
2017
- 2017-12-11 CN CN201711310750.9A patent/CN108164173A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20130172505A1 (en) * | 2010-07-27 | 2013-07-04 | Jian Fang | Synthesis method of polycarboxylic acid water-reducing agent |
| CN102924669A (en) * | 2011-08-10 | 2013-02-13 | 广州泰祥混凝土外加剂有限公司 | Preparation method of polycarboxylate superplasticizer |
| CN103788307A (en) * | 2012-10-27 | 2014-05-14 | 北京市建筑工程研究院有限责任公司 | Preparation method of novel concrete slump retaining agent based on allyl polyoxyethylene ether |
| CN105294953A (en) * | 2015-11-26 | 2016-02-03 | 科之杰新材料集团有限公司 | Preparation method of polycarboxylic acid super slump retaining agent |
| CN105712651A (en) * | 2015-12-15 | 2016-06-29 | 江苏苏博特新材料股份有限公司 | Concrete slump retaining agent for very-long-time slump retaining and preparation method thereof |
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