CN109400825A - A kind of low responsive type polycarboxylate water-reducer and preparation method thereof with anti-mud effect - Google Patents
A kind of low responsive type polycarboxylate water-reducer and preparation method thereof with anti-mud effect Download PDFInfo
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- CN109400825A CN109400825A CN201811469078.2A CN201811469078A CN109400825A CN 109400825 A CN109400825 A CN 109400825A CN 201811469078 A CN201811469078 A CN 201811469078A CN 109400825 A CN109400825 A CN 109400825A
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- acid
- reducer
- polycarboxylate water
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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
- C08F289/00—Macromolecular compounds obtained by polymerising monomers on to macromolecular compounds not provided for in groups C08F251/00 - C08F287/00
-
- 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
- C04B24/243—Phosphorus-containing polymers
- C04B24/246—Phosphorus-containing polymers containing polyether side chains
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F2/00—Processes of polymerisation
- C08F2/38—Polymerisation using regulators, e.g. chain terminating agents, e.g. telomerisation
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2103/00—Function or property of ingredients for mortars, concrete or artificial stone
- C04B2103/30—Water reducers, plasticisers, air-entrainers, flow improvers
- C04B2103/302—Water reducers
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- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Macromonomer-Based Addition Polymer (AREA)
Abstract
A kind of low responsive type polycarboxylate water-reducer and preparation method thereof with anti-mud effect, be prepared by methyl allyl polyoxyethylene ether, acrylic acid, sodium hypophosphite, ammonium persulfate, hydrogen peroxide, L-AA, thioacetic acid, humic acid by redox Raolical polymerizable, it is characterised in that: methyl allyl polyoxyethylene ether, acrylic acid, sodium hypophosphite, ammonium persulfate, hydrogen peroxide, L-AA, thioacetic acid, humic acid mass ratio be 1:0.11:0.014:0.008:0.005:0.002:0.005:0.06；Beneficial effect is: largely avoiding Preferential adsorption of the polycarboxylic acids molecule on soil, improves the retention property of water-reducing agent；With significant anti-mud effect, preparation process is simple, at low cost.
Description
Technical field
The present invention relates to a kind of low responsive type polycarboxylate water-reducer and preparation method thereof with anti-mud effect, belongs to coagulation
Native additive technical field.
Background technique
Polycarboxylate high performance water-reducing agent by feat of its volume low, high water reduction, high-collapse-retentivity, concrete high-durability and
Environmentally protective equal excellent characteristics have been widely used in concrete works.But a large amount of Practical case and correlation
Application study shows poly carboxylic acid series water reducer to the clay content of aggregate compared to traditional naphthalene system, melamine series, sulfamate
The high efficiency water reducing agents such as system are more sensitive.Especially along with the rapid degradation of various regions sand and stone resources, contain silt particle and tailing using height
The case where sand, grows in intensity, and leads to the dispersion performance degradation of polycarboxylate water-reducer, protects effect of collapsing and have a greatly reduced quality, harden coagulation
The phenomenons such as native intensity is low emerge one after another, seriously affected poly carboxylic acid series water reducer in the large-scale promotion of ready-mixed concrete industry and
It uses.
In order to solve this problem, the method for improving water-reducing agent volume, compounding extraneous component is generallyd use in construction at present
To alleviate.But these methods inevitably bring the increase of concrete construction cost and complexity of constructing, and it is initial also to will cause concrete
Serious isolation, the problems such as air content is excessively high, setting time is too long, intensity is insufficient.Therefore, there is an urgent need to develop a kind of pair of cement contents
Change the polycarboxylate water-reducer with hyposensitivity, clay can effectively be inhibited to adsorb the intercalation of polycarboxylate water-reducer, improves poly-
The dispersion efficiency of carboxylic acid water reducer, to solve this big common problem of sandstone aggregate clay content in engineer application conscientiously.
Therefore, there is an urgent need to develop a kind of novel concrete early strength agent, early strength of concrete, right can be effectively improved
Later strength can effectively avoid the corrosiveness to reinforcing bar, concrete without negative interaction, while scum, alkali-aggregate will not occur
Reaction, has many advantages, such as that cement adaptability is good, volume susceptibility is small.
Summary of the invention
Purpose of the present invention overcome the deficiencies in the prior art is started with from water-reducing agent MOLECULE DESIGN, is provided a kind of with anti-mud
The low responsive type polycarboxylate water-reducer and preparation method thereof of effect improves polycarboxylate water-reducer point by the introducing of specific functional groups
Son is introduced by the method for graft copolymerization to the affinity and the rate of adsorption of cement and has inhibition and peptizaiton to soil
Molecular structure, reduction soil realize the work of anti-mud to reduce the sensibility of polycarboxylate water-reducer to the competitive Adsorption of polycarboxylic acids
With.
In order to reach the goals above, technical scheme is as follows:
A kind of low responsive type polycarboxylate water-reducer with anti-mud effect, by methyl allyl polyoxyethylene ether, acrylic acid, secondary phosphorus
Sour sodium, ammonium persulfate, hydrogen peroxide, L-AA, thioacetic acid, humic acid are prepared by redox Raolical polymerizable
It forms, it is characterised in that: methyl allyl polyoxyethylene ether, acrylic acid, sodium hypophosphite, ammonium persulfate, hydrogen peroxide, L- Vitamin C
Acid, thioacetic acid, humic acid mass ratio be 1:0.11:0.014:0.008:0.005:0.002:0.005:0.06；
Structural formula is as follows:
Phosphoryl functional group-H in structural formula2PO3It is introduced into main chain-C-C- by telomerization effect, X indicates humic acid structure,
Humic acid structure is introduced into main chain by the method for graft copolymerization.
A kind of preparation method of the low responsive type polycarboxylate water-reducer with anti-mud effect, it is characterised in that: methallyl
Base polyoxyethylene ether, acrylic acid, sodium hypophosphite, ammonium persulfate, hydrogen peroxide, L-AA, thioacetic acid, the quality of humic acid
Than for 1:0.11:0.014:0.008:0.005:0.002:0.005:0.06, preparation step is as follows:
(1) methyl allyl polyoxyethylene ether of 1 part of quality is added in four-hole boiling flask and flask is placed in 40 DEG C of water-baths, adds
Enter the deionized water of 1 part of quality, stirring to solid is completely dissolved；
(2) sodium hypophosphite of 0.014 part of quality is added in flask, stirring to dissolution；
(3) thioacetic acid of the acrylic acid of 0.11 part of quality, the L-AA of 0.002 part of quality, 0.005 part of quality is prepared
At the aqueous solution a of 50% concentration, the ammonium persulfate of 0.008 part of quality is made into certain density aqueous solution b, is controlled with peristaltic pump
A, b solution is added dropwise in 2h and 2.5h respectively, then insulation reaction 0.5h；
(4) humic acid of 0.06 part of quality is added in flask, the hydrogen peroxide of 0.005 part of quality is added after its dissolution, sufficiently
2.5h is reacted, is after reaction the low responsive type polycarboxylate water-reducer with anti-mud effect.
As optimization: according to the above-described low responsive type polycarboxylate water-reducer with anti-mud effect and its preparation side
Method, it is characterised in that: the substitute of thioacetic acid is mercaptopropionic acid or mercaptoethanol.
As optimization: according to the above-described low responsive type polycarboxylate water-reducer with anti-mud effect and its preparation side
Method, it is characterised in that: methyl allyl polyoxyethylene ether, acrylic acid, humic acid mass ratio adjusted in the range of ± 15%.
Compared with the prior art, the invention has the advantages that:
1. the Molecular Design thinking of low responsive type polycarboxylate water-reducer is in Raolical polymerizable in reaction system
Middle addition sodium phosphite forms the polymers of carboxylic acid of phosphorous acyl function by telomerization effect in the molecular structure.Phosphoryl
To cement molecule have more strong affinity and anchorage effect, the rate of adsorption faster, to reduce polycarboxylic acids molecule to soil
Preferential adsorption degree.On the other hand, using the method for graft copolymerization, humic acid molecule is introduced in polycarboxylic acid structure.Humic acid
The functional groups such as carboxyl rich in, phenolic hydroxyl group in molecule, have the space structure unfolded, polycarboxylic acids molecule can be helped to mud
Soil plays the role of inhibition and dispersion, largely avoids Preferential adsorption of the polycarboxylic acids molecule on soil, it is same these
Structure, which can also cooperate with, improves polycarboxylic acids to the dispersibility and retentivity of cement；
2. the method for using the secondary initiation of segmented in low responsive type polycarboxylate water-reducer synthesis process, mentions to a certain extent
High monomer conversion, to improve the retention property of water-reducing agent；
3. the sensitivity to aggregate containing mud can be effectively reduced in a low responsive type polycarboxylate water-reducer, there is significant anti-mud effect, energy
Effectively inhibit soil to adsorb the intercalation of polycarboxylate water-reducer, improves the dispersion effect and retentivity of water-reducing agent；
4. low responsive type polycarboxylate water-reducer preparation process is simple, at low cost.
Specific embodiment
In order to absolutely prove characteristic of the invention and implement mode of the invention, embodiment is given below.
Embodiment 1
A kind of low responsive type polycarboxylate water-reducer with anti-mud effect, by methyl allyl polyoxyethylene ether (M=2400), third
Olefin(e) acid, sodium hypophosphite, ammonium persulfate, hydrogen peroxide, L-AA, thioacetic acid, humic acid pass through redox radical polymerization
It closes reaction to be prepared, the mass ratio of each component is 1 part of methyl allyl polyoxyethylene ether, 0.11 part of acrylic acid, sodium hypophosphite
0.014, ammonium persulfate 0.008, hydrogen peroxide 0.005, L-AA 0.002, thioacetic acid 0.005, humic acid 0.06；
A kind of structural formula of the low responsive type polycarboxylate water-reducer with anti-mud effect is as follows:
Phosphoryl functional group-H in structural formula2PO3It is introduced into main chain-C-C- by telomerization effect, X indicates humic acid structure,
Humic acid structure is introduced into main chain by the method for graft copolymerization.
A kind of preparation method of the low responsive type polycarboxylate water-reducer with anti-mud effect, according to methacrylic polyoxy second
Alkene ether, acrylic acid, sodium hypophosphite, ammonium persulfate, hydrogen peroxide, L-AA, thioacetic acid, humic acid mass ratio 1:
0.11:0.014:0.008:0.005:0.002:0.005:0.06 prepares sample, and preparation step is as follows:
(1) methyl allyl polyoxyethylene ether of 180g is added in four-hole boiling flask and flask is placed in 40 DEG C of water-baths, is added
The deionized water of 180g, stirring to solid are completely dissolved；
(2) 2.524g sodium hypophosphite is added in flask, stirring to dissolution；
(3) thioacetic acid of 19.8g acrylic acid, the L-AA of 0.36g, 0.9g are configured to the aqueous solution a of 50% concentration,
1.44g ammonium persulfate is made into certain density aqueous solution b, is dripped respectively in 2h and 2.5h with peristaltic pump control a, b solution
Finish, then insulation reaction 0.5h；
(4) humic acid of 10.8g is added in flask, the hydrogen peroxide of 0.9g, sufficiently reaction 2.5h, reaction is added after its dissolution
After be with anti-mud effect low responsive type polycarboxylate water-reducer.
Embodiment 2
According to the low responsive type polycarboxylate water-reducer and preparation method thereof described in embodiment 1 with anti-mud effect, feature exists
In: thioacetic acid has mercaptopropionic acid, mercaptoethanol etc. as chain-transferring agent, alternative substitute.
Embodiment 3
According to the low responsive type polycarboxylate water-reducer and preparation method thereof described in embodiment 1 with anti-mud effect, feature exists
It can be adjusted in the range of ± 15% in the mass ratio of: methyl allyl polyoxyethylene ether, acrylic acid, humic acid, to obtain not
With the low responsive type polycarboxylate water-reducer of water-reducing rate and retentivity.
Claims (6)
1. a kind of low responsive type polycarboxylate water-reducer with anti-mud effect, by methyl allyl polyoxyethylene ether, acrylic acid, secondary
Sodium phosphate, ammonium persulfate, hydrogen peroxide, L-AA, thioacetic acid, humic acid pass through redox Raolical polymerizable system
It is standby to form, it is characterised in that: methyl allyl polyoxyethylene ether, acrylic acid, sodium hypophosphite, ammonium persulfate, hydrogen peroxide, L- are anti-bad
Hematic acid, thioacetic acid, humic acid mass ratio be 1:0.11:0.014:0.008:0.005:0.002:0.005:0.06；
Structure is as follows:
Phosphoryl functional group-H in structural formula2PO3It is introduced into main chain-C-C- by telomerization effect, X indicates humic acid structure, rotten
It grows sour structure and main chain is introduced by the method for graft copolymerization.
2. a kind of preparation method of the low responsive type polycarboxylate water-reducer with anti-mud effect, it is characterised in that: methacrylic
Polyoxyethylene ether, acrylic acid, sodium hypophosphite, ammonium persulfate, hydrogen peroxide, L-AA, thioacetic acid, humic acid mass ratio
For 1:0.11:0.014:0.008:0.005:0.002:0.005:0.06, preparation step is as follows:
(1) methyl allyl polyoxyethylene ether of 1 part of quality is added in four-hole boiling flask and flask is placed in 40 DEG C of water-baths, adds
Enter the deionized water of 1 part of quality, stirring to solid is completely dissolved；
(2) sodium hypophosphite of 0.014 part of quality is added in flask, stirring to dissolution；
(3) thioacetic acid of the acrylic acid of 0.11 part of quality, the L-AA of 0.002 part of quality, 0.005 part of quality is prepared
At the aqueous solution a of 50% concentration, the ammonium persulfate of 0.008 part of quality is made into certain density aqueous solution b, is controlled with peristaltic pump
A, b solution is added dropwise in 2h and 2.5h respectively, then insulation reaction 0.5h；
(4) humic acid of 0.06 part of quality is added in flask, the hydrogen peroxide of 0.005 part of quality is added after its dissolution, sufficiently
2.5h is reacted, is after reaction the low responsive type polycarboxylate water-reducer with anti-mud effect.
3. the low responsive type polycarboxylate water-reducer according to claim 1 with anti-mud effect, it is characterised in that: sulfydryl second
The substitute of acid is mercaptopropionic acid or mercaptoethanol.
4. the preparation method of the low responsive type polycarboxylate water-reducer according to claim 2 with anti-mud effect, feature
Be: the substitute of thioacetic acid is mercaptopropionic acid or mercaptoethanol.
5. the low responsive type polycarboxylate water-reducer according to claim 1 with anti-mud effect, it is characterised in that: methyl alkene
Propyl polyoxyethylene ether, acrylic acid, humic acid mass ratio adjusted in the range of ± 15%.
6. the preparation method of the low responsive type polycarboxylate water-reducer according to claim 2 with anti-mud effect, feature
Be: methyl allyl polyoxyethylene ether, acrylic acid, humic acid mass ratio adjusted in the range of ± 15%.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110054429A (en) * | 2019-04-24 | 2019-07-26 | 海南太和科技有限公司 | A kind of polycarboxylate water-reducer and preparation method thereof based on humic acid base polyether monomer |
| CN111560121A (en) * | 2020-04-03 | 2020-08-21 | 安徽工业大学 | Preparation method of modified lignite humic acid water reducer |
| CN115093514A (en) * | 2022-07-22 | 2022-09-23 | 小飞鱼高新科技发展有限公司 | High-efficiency environment-friendly water reducing agent suitable for mortar and premixed concrete and preparation method thereof |
| CN115432953A (en) * | 2022-08-08 | 2022-12-06 | 中交二航武汉港湾新材料有限公司 | Polycarboxylate superplasticizer for micro-expansive type ultrahigh-performance concrete and preparation method and application thereof |
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| JPS5997563A (en) * | 1982-11-26 | 1984-06-05 | 日本重化学工業株式会社 | Chemical admixing agent for concrete and manufacture |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110054429A (en) * | 2019-04-24 | 2019-07-26 | 海南太和科技有限公司 | A kind of polycarboxylate water-reducer and preparation method thereof based on humic acid base polyether monomer |
| CN110054429B (en) * | 2019-04-24 | 2021-09-10 | 海南太和科技有限公司 | Polycarboxylic acid water reducing agent based on humic acid-based polyether monomer and preparation method thereof |
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| CN111560121B (en) * | 2020-04-03 | 2022-03-04 | 安徽工业大学 | Preparation method of modified lignite humic acid water reducer |
| CN115093514A (en) * | 2022-07-22 | 2022-09-23 | 小飞鱼高新科技发展有限公司 | High-efficiency environment-friendly water reducing agent suitable for mortar and premixed concrete and preparation method thereof |
| CN115432953A (en) * | 2022-08-08 | 2022-12-06 | 中交二航武汉港湾新材料有限公司 | Polycarboxylate superplasticizer for micro-expansive type ultrahigh-performance concrete and preparation method and application thereof |
| CN115432953B (en) * | 2022-08-08 | 2023-09-22 | 中交二航武汉港湾新材料有限公司 | Polycarboxylate superplasticizer for micro-expansion type ultra-high performance concrete, and preparation method and application thereof |
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