CN109485801A - A kind of manufacturing method of high performance water reducing agent of polyocarboxy acid - Google Patents
A kind of manufacturing method of high performance water reducing agent of polyocarboxy acid Download PDFInfo
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- CN109485801A CN109485801A CN201811257835.XA CN201811257835A CN109485801A CN 109485801 A CN109485801 A CN 109485801A CN 201811257835 A CN201811257835 A CN 201811257835A CN 109485801 A CN109485801 A CN 109485801A
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- Prior art keywords
- reducing agent
- high performance
- added
- water reducing
- performance 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
- 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
- C04B24/2688—Copolymers containing at least three different monomers
- C04B24/2694—Copolymers containing at least three different monomers containing polyether side chains
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- 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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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)
- Graft Or Block Polymers (AREA)
Abstract
The invention discloses a kind of manufacturing method of high performance water reducing agent of polyocarboxy acid, include the following steps: that raw material prepare；Mixing heating；Hydrogen peroxide addition；Polymerization；It neutralizes；The beneficial effects of the present invention are: the high performance water reducing agent of polyocarboxy acid of preparation, has good adaptability, excellent function of slump protection.
Description
Technical field
The invention belongs to high performance water reducing agent of polyocarboxy acid preparation technical fields, and in particular to a kind of poly-carboxylic high-performance diminishing
The manufacturing method of agent.
Background technique
High performance water reducing agent of polyocarboxy acid is a variety of macromolecular organic compounds based on polycarboxylate, through graft copolymerization
It generates, there is extremely strong water-reducing property, belong to the environment-friendly type concrete additive of technological precedence in the world today.It has been widely used
It is applied in the concrete that water conservancy, electric power, harbour, railway, bridge, highway, airport, military engineering and various citizens build main structure
Work.
The development of water-reducing agent is divided into three phases: using calcium lignosulfonate as the first generation ordinary water-reducing agent stage of representative；
Using naphthalene system as the second generation high efficiency water reducing agent stage of representative, using polycarboxylic-acid as the third generation high-performance water reducing agent stage of representative；
Polycarboxylate high performance water-reducing agent has many features: on synthesis technology, polycarboxylate high performance water-reducing agent is using unsaturated single
The polycondensation synthesis that body copolymerization rather than conventional water reducing agents use, the synthesis material of such water-reducing agent is many, usually has
Polyethylene glycol, (methyl) acrylic acid, allyl alcohol polyethenoxy ether etc.；On molecular structure, polycarboxylate high performance water-reducing agent
Molecular structure is Linear comb structure, rather than the linear structure that conventional water reducing agents are single；Polymerizeing on such water-reducing agent main chain has
A variety of different active groups, such as carboxylic acid group (- COOH), hydroxyl group (- OH), sulfonic group (- SO3Na), can produce
Raw electrostatic repulsive force；Its side chain is with hydrophilic nonpolar active group, space steric effect with higher.
However some unreasonable factors are remained during existing high performance water reducing agent of polyocarboxy acid preparation, it is existing
There is the deficiencies of following aspect in the preparation for some high performance water reducing agent of polyocarboxy acid:
1. in terms of adaptability, there is deficiencies；
2. there is deficiencies for function of slump protection.
Summary of the invention
The purpose of the present invention is to provide a kind of manufacturing methods of high performance water reducing agent of polyocarboxy acid, to solve above-mentioned background skill
Some unreasonable factors are remained during the existing high performance water reducing agent of polyocarboxy acid preparation proposed in art, it is existing
High performance water reducing agent of polyocarboxy acid there is there is deficiencies in terms of adaptability in the preparation；Function of slump protection is asked there is insufficient
Topic.
To achieve the above object, the invention provides the following technical scheme: a kind of manufacturer of high performance water reducing agent of polyocarboxy acid
Method includes the following steps:
Step 1: raw material prepare: isopentene group polyoxyethylene ether, hydrogen peroxide, initiator, acrylic acid, acrylic acid hydroxyl second
Ester, hydroxy methyl methacrylate, 2- acrylamide-2-methylpro panesulfonic acid AMPS, chain-transferring agent, piece alkali, deionized water；
Step 2: mixing heating: deionized water and isopentene group polyoxyethylene ether are added in reaction kettle, and it is risen
Temperature:
Step 3: hydrogen peroxide addition: hydrogen peroxide is added in the mixed liquor of step 2；
Step 4: acrylic acid, hydroxy-ethyl acrylate, methyl uniformly polymerization reaction: are added dropwise into the mixed liquor of step 3
Acrylate, 2- acrylamide-2-methylpro panesulfonic acid AMPS, chain-transferring agent and water mixed liquor, after completion of dropwise addition plus
Enter initiator, and stir, keeps the temperature；
Step 5: neutralization reaction: the polymer of step 4 is cooled down, and piece alkali is added while stirring, is adjusted pH value, can be obtained
To high performance water reducing agent of polyocarboxy acid.
As a preferred technical solution of the invention, the initiator is benzoyl peroxide, persulfate, over cure
One of sour potassium, reducing agent sodium hydrogensulfite, azodiisobutyronitrile or at least two.
As a preferred technical solution of the invention, deionized water and different is added in the step 2, in reaction kettle
Pentenyl polyoxyethylene ether, and 55 DEG C are warming up to it.
As a preferred technical solution of the invention, dropwise addition time-consuming≤3.5h in the step 4, the temperature of heat preservation
Degree is 58-62 DEG C.
As a preferred technical solution of the invention, in the step 5, polymer is cooled to 50 DEG C hereinafter, side is stirred
It mixes side and piece alkali is added, adjust pH value 6-7.
Compared with prior art, the beneficial effects of the present invention are: the high performance water reducing agent of polyocarboxy acid of preparation, has good
Adaptability, excellent function of slump protection.
Detailed description of the invention
Fig. 1 is flow chart of the invention；
Specific embodiment
Embodiment 1
A kind of manufacturing method of high performance water reducing agent of polyocarboxy acid, includes the following steps:
Step 1: raw material prepare: isopentene group polyoxyethylene ether, hydrogen peroxide, initiator, acrylic acid, acrylic acid hydroxyl second
Ester, hydroxy methyl methacrylate, 2- acrylamide-2-methylpro panesulfonic acid AMPS, chain-transferring agent, piece alkali, deionized water；Cause
Agent is for one of benzoyl peroxide, persulfate, potassium peroxydisulfate, reducing agent sodium hydrogensulfite, azodiisobutyronitrile or extremely
It is two kinds few；
Step 2: mixing heating: deionized water and isopentene group polyoxyethylene ether are added in reaction kettle, and heats up to it
To 55 DEG C:
Step 3: hydrogen peroxide addition: hydrogen peroxide is added in the mixed liquor of step 2；
Step 4: acrylic acid, hydroxy-ethyl acrylate, methyl uniformly polymerization reaction: are added dropwise into the mixed liquor of step 3
Acrylate, 2- acrylamide-2-methylpro panesulfonic acid AMPS, chain-transferring agent and water mixed liquor, be added dropwise it is time-consuming≤
3.5h is added initiator, and stirs after completion of dropwise addition, keep the temperature at 58 DEG C；
Step 5: neutralization reaction: by the polymer of step 4 be cooled to 50 DEG C hereinafter, while stirring be added piece alkali, adjust
PH value 6, can be obtained high performance water reducing agent of polyocarboxy acid；PH value is preferable in 6 ranges: when pH value is lower than 4, polymer is muddy,
Its paste flowing degree, concrete slump completely without；When pH value is higher than 9, under paste flowing degree, concrete slump start
Drop；Good with the compatibility of various cement, the slump-retaining of concrete can be good, extends the construction time of concrete；Volume is low,
Water-reducing rate is high, shrinks small；Increase substantially early stage, the later strength of concrete；Chloride ion content is low, alkali content is low, is conducive to
The durability of concrete, production process is pollution-free, is free of formaldehyde, is a kind of green product.
Embodiment 2
A kind of manufacturing method of high performance water reducing agent of polyocarboxy acid, includes the following steps:
Step 1: raw material prepare: isopentene group polyoxyethylene ether, hydrogen peroxide, initiator, acrylic acid, acrylic acid hydroxyl second
Ester, hydroxy methyl methacrylate, 2- acrylamide-2-methylpro panesulfonic acid AMPS, chain-transferring agent, piece alkali, deionized water；Cause
Agent is for one of benzoyl peroxide, persulfate, potassium peroxydisulfate, reducing agent sodium hydrogensulfite, azodiisobutyronitrile or extremely
It is two kinds few；
Step 2: mixing heating: deionized water and isopentene group polyoxyethylene ether are added in reaction kettle, and heats up to it
To 55 DEG C:
Step 3: hydrogen peroxide addition: hydrogen peroxide is added in the mixed liquor of step 2；
Step 4: acrylic acid, hydroxy-ethyl acrylate, methyl uniformly polymerization reaction: are added dropwise into the mixed liquor of step 3
Acrylate, 2- acrylamide-2-methylpro panesulfonic acid AMPS, chain-transferring agent and water mixed liquor, be added dropwise it is time-consuming≤
3.5h is added initiator, and stirs after completion of dropwise addition, keep the temperature at 60 DEG C；
Step 5: neutralization reaction: by the polymer of step 4 be cooled to 50 DEG C hereinafter, while stirring be added piece alkali, adjust
PH value 6.5, can be obtained high performance water reducing agent of polyocarboxy acid；PH value is preferable in 6.5 ranges: when pH value is lower than 4, polymer is muddy
It is turbid, paste flowing degree, concrete slump completely without；When pH value is higher than 9, paste flowing degree, concrete slump start
Decline；Good with the compatibility of various cement, the slump-retaining of concrete can be good, extends the construction time of concrete；Volume
Low, water-reducing rate is high, shrinks small；Increase substantially early stage, the later strength of concrete；Chloride ion content is low, alkali content is low, favorably
In the durability of concrete, production process is pollution-free, is free of formaldehyde, is a kind of green product.
Embodiment 3
A kind of manufacturing method of high performance water reducing agent of polyocarboxy acid, includes the following steps:
Step 1: raw material prepare: isopentene group polyoxyethylene ether, hydrogen peroxide, initiator, acrylic acid, acrylic acid hydroxyl second
Ester, hydroxy methyl methacrylate, 2- acrylamide-2-methylpro panesulfonic acid AMPS, chain-transferring agent, piece alkali, deionized water；Cause
Agent is for one of benzoyl peroxide, persulfate, potassium peroxydisulfate, reducing agent sodium hydrogensulfite, azodiisobutyronitrile or extremely
It is two kinds few；
Step 2: mixing heating: deionized water and isopentene group polyoxyethylene ether are added in reaction kettle, and heats up to it
To 55 DEG C:
Step 3: hydrogen peroxide addition: hydrogen peroxide is added in the mixed liquor of step 2；
Step 4: acrylic acid, hydroxy-ethyl acrylate, methyl uniformly polymerization reaction: are added dropwise into the mixed liquor of step 3
Acrylate, 2- acrylamide-2-methylpro panesulfonic acid AMPS, chain-transferring agent and water mixed liquor, be added dropwise it is time-consuming≤
3.5h is added initiator, and stirs after completion of dropwise addition, keep the temperature at 62 DEG C；
Step 5: neutralization reaction: by the polymer of step 4 be cooled to 50 DEG C hereinafter, while stirring be added piece alkali, adjust
PH value 7, can be obtained high performance water reducing agent of polyocarboxy acid；PH value is preferable in 7 ranges: when pH value is lower than 4, polymer is muddy,
Its paste flowing degree, concrete slump completely without；When pH value is higher than 9, under paste flowing degree, concrete slump start
Drop；Good with the compatibility of various cement, the slump-retaining of concrete can be good, extends the construction time of concrete；Volume is low,
Water-reducing rate is high, shrinks small；Increase substantially early stage, the later strength of concrete；Chloride ion content is low, alkali content is low, is conducive to
The durability of concrete, production process is pollution-free, is free of formaldehyde, is a kind of green product.
It although an embodiment of the present invention has been shown and described, for the ordinary skill in the art, can be with
A variety of variations, modification, replacement can be carried out to these embodiments without departing from the principles and spirit of the present invention by understanding
And modification, the scope of the present invention is defined by the appended.
Claims (5)
1. a kind of manufacturing method of high performance water reducing agent of polyocarboxy acid, which comprises the steps of:
Step 1: raw material prepare: isopentene group polyoxyethylene ether, hydrogen peroxide, initiator, acrylic acid, hydroxy-ethyl acrylate, first
Base acrylate, 2- acrylamide-2-methylpro panesulfonic acid AMPS, chain-transferring agent, piece alkali, deionized water；
Step 2: mixing heating: deionized water and isopentene group polyoxyethylene ether are added in reaction kettle, and heats up to it:
Step 3: hydrogen peroxide addition: hydrogen peroxide is added in the mixed liquor of step 2；
Step 4: acrylic acid, hydroxy-ethyl acrylate, metering system uniformly polymerization reaction: are added dropwise into the mixed liquor of step 3
Sour hydroxyl methyl esters, 2- acrylamide-2-methylpro panesulfonic acid AMPS, chain-transferring agent and water mixed liquor, after completion of dropwise addition be added draw
Agent is sent out, and is stirred, is kept the temperature；
Step 5: neutralization reaction: the polymer of step 4 is cooled down, and piece alkali is added while stirring, is adjusted pH value, be can be obtained poly-
Carboxylic acid high-performance water reducing agent.
2. a kind of manufacturing method of high performance water reducing agent of polyocarboxy acid according to claim 1, it is characterised in that: the initiation
Agent is for one of benzoyl peroxide, persulfate, potassium peroxydisulfate, reducing agent sodium hydrogensulfite, azodiisobutyronitrile or extremely
It is two kinds few.
3. a kind of manufacturing method of high performance water reducing agent of polyocarboxy acid according to claim 1, it is characterised in that: the step
In two, deionized water and isopentene group polyoxyethylene ether are added in reaction kettle, and 55 DEG C are warming up to it.
4. a kind of manufacturing method of high performance water reducing agent of polyocarboxy acid according to claim 1, it is characterised in that: the step
Dropwise addition time-consuming≤3.5h in four, the temperature of heat preservation are 58-62 DEG C.
5. a kind of manufacturing method of high performance water reducing agent of polyocarboxy acid according to claim 1, it is characterised in that: the step
In five, polymer be cooled to 50 DEG C hereinafter, while stirring be added piece alkali, adjust pH value 6-7.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201811257835.XA CN109485801A (en) | 2018-10-26 | 2018-10-26 | A kind of manufacturing method of high performance water reducing agent of polyocarboxy acid |
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| CN201811257835.XA CN109485801A (en) | 2018-10-26 | 2018-10-26 | A kind of manufacturing method of high performance water reducing agent of polyocarboxy acid |
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101538134A (en) * | 2009-04-14 | 2009-09-23 | 大连市建筑科学研究设计院股份有限公司 | Polyether class polycarboxylic acid high-efficiency water reducing agent and preparation method thereof |
| CN104692700A (en) * | 2015-02-11 | 2015-06-10 | 四川恒泽建材有限公司 | Slow-release slump-retaining type polycarboxylic acid high-performance water reducing agent and preparation method thereof |
-
2018
- 2018-10-26 CN CN201811257835.XA patent/CN109485801A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101538134A (en) * | 2009-04-14 | 2009-09-23 | 大连市建筑科学研究设计院股份有限公司 | Polyether class polycarboxylic acid high-efficiency water reducing agent and preparation method thereof |
| CN104692700A (en) * | 2015-02-11 | 2015-06-10 | 四川恒泽建材有限公司 | Slow-release slump-retaining type polycarboxylic acid high-performance water reducing agent and preparation method thereof |
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Application publication date: 20190319 |