CN108484840A - A kind of anti-chamotte mould polycarboxylate water-reducer of ester ether mixed structure and preparation method thereof - Google Patents
A kind of anti-chamotte mould polycarboxylate water-reducer of ester ether mixed structure and preparation method thereof Download PDFInfo
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- CN108484840A CN108484840A CN201810249461.0A CN201810249461A CN108484840A CN 108484840 A CN108484840 A CN 108484840A CN 201810249461 A CN201810249461 A CN 201810249461A CN 108484840 A CN108484840 A CN 108484840A
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- reducer
- weight
- solution
- mixed structure
- polycarboxylate water
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Classifications
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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
- C04B24/24—Macromolecular compounds
- C04B24/26—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
- C04B24/2605—Macromolecular compounds 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
- 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
The invention discloses anti-chamotte mould polycarboxylate water-reducers of a kind of ester ether mixed structure and preparation method thereof.It is prepared by the component containing following parts by weight, 180~220 parts by weight polyether macromonomers；140~180 parts by weight are esterified polymeric monomer；30~40 parts by weight unsaturated acids；1~5 parts by weight cationic monomer；2~4 parts by weight oxidants；0.5~2.5 parts by weight tartaric acid；0.5~1.5 parts by weight chain-transferring agent；400~500 parts by weight of deionized water；140~160 parts by weight, 32 mass volume % liquid caustic soda.The anti-chamotte mould polycarboxylate water-reducer of ester ether mixed structure has the advantages that volume is low, water-reducing rate is high, anti-mud is good, even if the clay content of aggregate is higher, which can still keep higher water-reducing rate.It is simple for process simultaneously, it is prepared under normal temperature condition, easy control of reaction conditions, low energy consumption, pollution-free.
Description
Technical field
The present invention relates to technical field of concrete additives more particularly to a kind of anti-chamotte mould polycarboxylic acids of ester ether mixed structure to subtract
Aqua and preparation method thereof.
Background technology
Polycarboxylate water-reducer has many advantages, such as that volume is low, water-reducing rate is high, slump retaining is good, environmentally protective, railway, highway,
It is used widely in the engineerings such as bridge, tunnel, skyscraper.With the rapid growth of concrete usage amount in recent years, meet
The quality sand and stone aggregate resources that clay content requires have been unable to meet present needs, therefore the sandstone bone of high clay content on the market
The usage amount of material is continuously improved.Traditional polycarboxylate water-reducer is very sensitive to the clay content in aggregate, because as aggregate contains
The raising of mud amount, a part of polycarboxylate water-reducer is by adsorption by clay so that its dispersion performance and function of slump protection are substantially reduced.Cause
This, it not is necessary by the polycarboxylate water-reducer that clay content is influenced to prepare a kind of dispersion performance and function of slump protection.
The adverse effect brought for solving aggregate clay content, it is mainly special by changing the structure of polycarboxylate water-reducer
Sign synthesizes a kind of anti-chamotte mould polycarboxylate water-reducer.But there is synthesis in the existing technology for preparing anti-chamotte mould polycarboxylate water-reducer
The shortcomings of time is long, energy consumption is high, side-chain structure is single, anti-mud is poor.
Invention content
In order to overcome, generated time present in existing anti-chamotte mould polycarboxylate water-reducer technology of preparing is long, energy consumption is high, divides
The defects of minor structure is single, anti-mud is poor, the present invention provide the ester ether mixing knot that a kind of volume is low, water-reducing rate is high, anti-mud is good
The anti-chamotte mould polycarboxylate water-reducer of structure, even if the clay content of aggregate is higher, which can still keep higher water-reducing rate.
To achieve the above object, the present invention provides a kind of anti-chamotte mould polycarboxylate water-reducer of ester ether mixed structure, and feature exists
In, it is prepared by the component containing following parts by weight,
Further, the polyether macromonomer be molecular weight be 2200~3000 isobutene alcohol polyoxyethylene ether, iso-amylene
One kind in alcohol polyoxyethylene ether, 4- hydroxy butyl vinyl ethers.
Further, the esterification polymeric monomer is the methoxy polyethylene glycol methacrylate-styrene polymer that molecular weight is 1000~1200
Or methoxy polyethylene glycol acrylate.
Further, the unsaturated acids is acrylic or methacrylic acid.
Further, the cationic monomer is MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride or acrylyl oxy-ethyl front three
Ammonium chloride.
Further, the oxidant is one kind in hydrogen peroxide, ammonium persulfate, sodium peroxydisulfate.
Further, the chain-transferring agent is one kind in mercaptoethanol, 3- mercaptopropionic acids, thioacetic acid.
The present invention also provides a kind of preparation method of the anti-chamotte mould polycarboxylate water-reducer of ester ether mixed structure, feature exists
In steps are as follows：
Under normal temperature condition, polyether monomer and deionized water are put into reaction kettle；Oxidant is put into reaction kettle again
In, after stirring and dissolving, while solution A, solution B and solution C is added dropwise, time for adding is 2~3 hours (in the synthesis of water-reducing agent
The time for adding of Cheng Zhong, solution have a significant impact to the conversion ratio and performance of product, and time for adding is too fast, and chemical reaction is violent,
Molecular weight is excessive, and performance declines；Time for adding is excessively slow, and the production cycle is long, uneconomical, it is found by the applicant that when titration in 2-3 hours
Between it is most suitable), constant temperature 0.5~1 hour after completion of dropwise addition, carry out free radicals copolymerization reaction；After reaction, it is adjusted with liquid caustic soda molten
The pH value of liquid is 6.0~7.0 (pH value within this range stable storing, be unlikely to deteriorate), and obtained clear solution is that ester ether is mixed
Close the anti-chamotte mould polycarboxylate water-reducer of structure；
Wherein, the deionized water for being prepared as unsaturated acids and cationic monomer being dissolved in 1/16-7/100 weight of solution A
In, it is configured to the solution A that mass fraction is 40-60%；Preferably, the solution A that mass fraction is 50%；
The preparation of solution B：Tartaric acid and chain-transferring agent are dissolved in the deionized water of 1/16-7/100 weight, are configured to matter
Measure the solution B that score is 0.5-2%；Preferably, the solution B that mass fraction is 1%；
The preparation of solution C：Esterification polymeric monomer is dissolved in remaining deionized water, it is 70-90% to be configured to mass fraction
Solution C；Preferably, the solution C that mass fraction is 80%.
For polyether monomer in entire reaction system, reactivity is low, so first putting into reaction as reaction bottom material with water, carries
Its high conversion ratio；The reactivity for being esterified polymeric monomer is high, need use and be added dropwise, reduce its concentration in system, prevent implode；It is whole
A reaction system uses redox initiation system, the content of oxidant to be in water greater than the amount of reducing agent, therefore oxidant
It is added at one time, reducing agent is added dropwise with solution B；Oxidant one be added, to proceed by chemical reaction, must be added dropwise simultaneously solution A,
B, C makes synthetic reaction be normally carried out.
Room temperature of the present invention refers to 5-40 DEG C, no matter winter or summer, can be carried out.
The beneficial effects of the invention are as follows：
1,140-180 parts by weight are introduced in the anti-chamotte mould polycarboxylate water-reducer molecule structure of ester ether mixed structure of the invention
Ester-containing based structures side chain esterification polymeric monomer, this esters side-chain structure can significantly reduce sensitivity of the water-reducing agent to soil
Property.The anti-chamotte mould polycarboxylate water-reducer of ester ether mixed structure realize ethers polycarboxylic acid water reducing agent high water reducing rate and high fluidity and
The adaptability and slump retaining of esters polycarboxylate water-reducer, can be complementary in performance and promote, even if containing mud in aggregate
Measure it is higher in the case of use, can also keep its good dispersion performance and function of slump protection.
The cation of 1-5 parts by weight is introduced in the anti-chamotte mould polycarboxylate water-reducer molecule structure of ester ether mixed structure of the present invention
Monomer, after introducing cationic monomer in molecular structure, polycarboxylate water-reducer molecule shows ambisexuality, can be adsorbed onto band just
It on electrical mineral, and can be adsorbed onto on electronegative mineral, adsorption capacity and adsorbance are improved, polycarboxylate water-reducer
Steric hindrance effect and electrostatic repulsion effect all increase, thus dispersibility improve.But when cationic monomer introduces
After amount is more than 5 parts by weight, the dispersibility of polycarboxylate water-reducer can weaken.This is because the introduction volume of cationic monomer reaches one
After definite value, positive elecrtonegativity " neutralization " can occur for cation group and anionic group in molecular structure, influence polycarboxylic acids diminishing
Agent molecule adsorbs on cement granules, its dispersibility is made to weaken.
2, the present invention introduces in the raw material of the anti-chamotte mould polycarboxylate water-reducer of synthetic ester ether mixed structure while having also
The tartaric acid of originality and chain transfer is aided with chain-transferring agent and is controlled so that the anti-chamotte mould polycarboxylic acids of ester ether mixed structure subtracts
The molecular weight of aqua is effectively controlled.
3, present invention process is simple, is prepared under normal temperature condition, and easy control of reaction conditions, low energy consumption, pollution-free.
Specific implementation mode
The embodiment of the present invention is described below in detail, the examples of the embodiments are being intended to be used to explain the present invention, without
It can be interpreted as limitation of the present invention.In the examples where no specific technique or condition is specified, it is retouched according to document in the art
The technology or condition stated are carried out according to product description.Reagents or instruments used without specified manufacturer, being can be with
Conventional products that are commercially available.
Embodiment 1：The preparation of the anti-chamotte mould polycarboxylate water-reducer of ester ether mixed structure
Raw material：It is shown in Table 1.Wherein polyether macromonomer is isobutene alcohol polyoxyethylene ether (molecular weight 2400)；It is esterified polymeric monomer
For methoxy poly (ethylene glycol) methyl methacrylate (molecular weight 1200)；Unsaturated acids is acrylic acid；Cationic monomer is methyl
Acrylyl oxy-ethyl-trimethyl salmiac；Oxidant is hydrogen peroxide；Chain-transferring agent is mercaptoethanol.
1 each ingredients of embodiment 1-5 of table use scale (parts by weight)
| Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 | |
| Polyether macromonomer | 210 | 200 | 180 | 220 |
| It is esterified polymeric monomer | 150 | 160 | 180 | 140 |
| Unsaturated acids | 33 | 35 | 30 | 40 |
| Cationic monomer | 2 | 1 | 5 | 1 |
| Oxidant | 3 | 4 | 2 | 2 |
| Tartaric acid | 1 | 0.5 | 0.5 | 2.5 |
| Chain-transferring agent | 0.5 | 1 | 1 | 1.5 |
| Deionized water | 450 | 445 | 400 | 440 |
| Liquid caustic soda | Surplus | Surplus | Surplus | Surplus |
Note:Liquid caustic soda concentration can be different, for example can be 32 mass fraction %.
Preparation method：Each starting components are weighed by the dosage of table 1；
The preparation of solution A：Acrylic acid and MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride are dissolved in deionized water, configured
The solution A for being 50% at mass fraction；
The preparation of solution B：Tartaric acid and mercaptoethanol are dissolved in deionized water, be configured to mass fraction be 1% it is molten
Liquid B；
The preparation of solution C：Methoxy poly (ethylene glycol) methyl methacrylate is dissolved in deionized water, quality point is configured to
The solution C that number is 80%.
Under the conditions of room temperature (5~40 DEG C), isobutene alcohol polyoxyethylene ether and remaining parts by weight are put into reaction kettle
Deionized water；Hydrogen peroxide input is added in reaction kettle again, after stirring and dissolving, while solution A, solution B, solution C is added dropwise,
Time for adding is 2 hours, and constant temperature 0.5 hour after completion of dropwise addition carries out free radicals copolymerization reaction；Free radicals copolymerization reaction terminates
Afterwards, the pH value for solution being adjusted with 32% liquid caustic soda is 7.0, the as described anti-chamotte mould polycarboxylic acids diminishing of obtained clear solution
Agent.
Embodiment 2：The preparation of the anti-chamotte mould polycarboxylate water-reducer of ester ether mixed structure
Raw material：It is shown in Table 1.Wherein polyether macromonomer is isoamyl alcohol polyoxyethylene ether (molecular weight 2400)；It is esterified polymeric monomer
For methoxypolyethylene glycol methacrylate (molecular weight 1200)；Unsaturated acids is methacrylic acid；Cationic monomer is propylene
Acyloxyethyl trimethyl ammonium chloride；Oxidant is ammonium persulfate；Chain-transferring agent is thioacetic acid.
Preparation method：Time for adding therein is 3 hours, constant temperature 1 hour after completion of dropwise addition.The same embodiment of other steps
1。
Embodiment 3：The preparation of the anti-chamotte mould polycarboxylate water-reducer of ester ether mixed structure
Raw material：It is shown in Table 1.Wherein polyether macromonomer is 4- hydroxy butyl vinyl ethers (molecular weight 2400)；Being esterified polymeric monomer is
Methoxy poly (ethylene glycol) methyl methacrylate (molecular weight 1200)；Unsaturated acids is methacrylic acid；Cationic monomer is third
Alkene acyloxyethyl trimethyl ammonium chloride；Oxidant is sodium peroxydisulfate；Chain-transferring agent is 3- mercaptopropionic acids.
Preparation method：Time for adding therein is 2.5 hours, constant temperature 1 hour after completion of dropwise addition.Other steps are the same as implementation
Example 1.
Embodiment 4：Compliance test result is tested
The anti-chamotte mould polycarboxylate water-reducer of ester ether mixed structure that embodiment 1-3 is synthesized, according to GB 8076-2008
《Concrete admixture》, survey its concrete water-reducing ratio, the slump and through when slump-loss.It the results are shown in Table 2.Comparison used is
Plain edition water-reducing agent, specially platform circle chemical industry TJ-288 conventional types water-reducing agent mother liquor.
2 embodiment performance comparison table of table
From the results shown in Table 2, in aggregate in the case of containing mud, the poly- carboxylic of the anti-chamotte mould of ester ether mixed structure of the invention
Its dispersion effect of sour water-reducing agent is substantially better than conventional water reducing agents, and retention property is more preferable.That is ester ether of the invention is mixed
Closing the anti-chamotte mould polycarboxylate water-reducer of structure has many advantages, such as that volume is low, water-reducing rate is high, anti-mud is good, even if the clay content of aggregate reaches
To 4%, which can still keep higher water-reducing rate.
Although the embodiments of the present invention has been shown and described above, it is to be understood that above-described embodiment is example
Property, it is not considered as limiting the invention, those skilled in the art are not departing from the principle of the present invention and objective
In the case of can make changes, modifications, alterations, and variations to the above described embodiments within the scope of the invention.
Claims (8)
1. a kind of anti-chamotte mould polycarboxylate water-reducer of ester ether mixed structure, which is characterized in that by the component system containing following parts by weight
It is standby to obtain,
2. the anti-chamotte mould polycarboxylate water-reducer of ester ether mixed structure as described in claim 1, which is characterized in that the polyether macromonomer
For molecular weight be 2200~3000 isobutene alcohol polyoxyethylene ether, isoamyl alcohol polyoxyethylene ether, 4- hydroxy butyl vinyl ethers
In one kind.
3. the anti-chamotte mould polycarboxylate water-reducer of ester ether mixed structure as described in claim 1, which is characterized in that the esterification polymeric monomer
The methoxy polyethylene glycol methacrylate-styrene polymer or methoxy polyethylene glycol acrylate for being 1000~1200 for molecular weight.
4. the anti-chamotte mould polycarboxylate water-reducer of ester ether mixed structure as described in claim 1, which is characterized in that the unsaturated acids is
Acrylic or methacrylic acid.
5. the anti-chamotte mould polycarboxylate water-reducer of ester ether mixed structure as described in claim 1, which is characterized in that the cationic monomer
For MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride or acrylyl oxy-ethyl-trimethyl salmiac.
6. the anti-chamotte mould polycarboxylate water-reducer of ester ether mixed structure as described in claim 1, which is characterized in that the oxidant was
One kind in hydrogen oxide, ammonium persulfate, sodium peroxydisulfate.
7. the anti-chamotte mould polycarboxylate water-reducer of ester ether mixed structure as described in claim 1, which is characterized in that the chain-transferring agent is
One kind in mercaptoethanol, 3- mercaptopropionic acids, thioacetic acid.
8. a kind of preparation method of the anti-chamotte mould polycarboxylate water-reducer of any one of claim 1 to 7 ester ether mixed structure,
It is characterized in that, steps are as follows：
Under normal temperature condition, polyether monomer and deionized water are put into reaction kettle；Oxidant is put into reaction kettle again, is stirred
After mixing dissolving, while solution A, solution B and solution C is added dropwise, time for adding is 2~3 hours, and constant temperature 0.5~1 is small after completion of dropwise addition
When, carry out free radicals copolymerization reaction；After reaction, it is 6.0~7.0 to adjust the pH value of solution with liquid caustic soda, and obtained clarification is molten
Liquid is the anti-chamotte mould polycarboxylate water-reducer of ester ether mixed structure；
Wherein, solution A is prepared as unsaturated acids and cationic monomer being dissolved in the deionized water of 1/16-7/100 weight, matches
It is set to the solution A that mass fraction is 40-60%；The solution A that preferred mass score is 50%；
The preparation of solution B：Tartaric acid and chain-transferring agent are dissolved in the deionized water of 1/16-7/100 weight, are configured to quality point
Number is the solution B of 0.5-2%；The solution A that preferred mass score is 1%；
The preparation of solution C：Esterification polymeric monomer is dissolved in remaining deionized water, it is the molten of 70-90% to be configured to mass fraction
Liquid C；The solution A that preferred mass score is 80%.
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Cited By (5)
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| CN109881288A (en) * | 2019-02-27 | 2019-06-14 | 圣华盾防护科技股份有限公司 | Alkali-resistant glass fiber, protective garment and protective garment fabric |
| CN112645630A (en) * | 2020-12-19 | 2021-04-13 | 厦门宏发先科新型建材有限公司 | Fluorine-containing early-strength polycarboxylate superplasticizer, preparation method thereof and early-strength concrete |
| CN113980202A (en) * | 2021-11-17 | 2022-01-28 | 科之杰新材料集团有限公司 | Polycarboxylate superplasticizer and preparation method thereof |
| CN114085335A (en) * | 2021-11-17 | 2022-02-25 | 重庆建研科之杰新材料有限公司 | Water-reducing polycarboxylate superplasticizer with vinyl ether ester mixed structure and preparation method thereof |
| CN114369208A (en) * | 2021-12-29 | 2022-04-19 | 科之杰新材料集团有限公司 | Preparation method and application of anti-mud high-adsorption water-reducing polycarboxylate superplasticizer |
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| CN114369208A (en) * | 2021-12-29 | 2022-04-19 | 科之杰新材料集团有限公司 | Preparation method and application of anti-mud high-adsorption water-reducing polycarboxylate superplasticizer |
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Application publication date: 20180904 |