CN108003308A - A kind of modified early strength agent and its synthetic method - Google Patents
A kind of modified early strength agent and its synthetic method Download PDFInfo
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- CN108003308A CN108003308A CN201711009909.3A CN201711009909A CN108003308A CN 108003308 A CN108003308 A CN 108003308A CN 201711009909 A CN201711009909 A CN 201711009909A CN 108003308 A CN108003308 A CN 108003308A
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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
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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
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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
- 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
- C08F283/02—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G on to polycarbonates or saturated polyesters
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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
- C04B2103/00—Function or property of ingredients for mortars, concrete or artificial stone
- C04B2103/10—Accelerators; Activators
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
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Abstract
The present invention relates to concrete admixture field, discloses a kind of modified early strength agent and its synthetic method.In parts by weight, the modification early strength agent of the present invention includes 380~480 parts of 300~350 parts of polypentenol polyoxyethylene ether, 30~50 parts of acrylic acid, 60~80 parts of modified function monomer, 2~4 parts of hydrogen peroxide, 1~1.5 part of reducing agent, 2~2.5 parts of molecular weight regulator, 10~20 parts of sodium hydroxide and water, wherein, modified function monomer includes 30~35 parts of esterdiol in 15~20 parts of acrylamide, 15~25 parts of methallylsulfonic acid sodium and poly epsilon caprolactone.The modification early strength agent of the present invention contains several functions functional group, the early strength of concrete can be improved, accelerate mould turnover, accelerate flow line production, than water-reducing rate, lower air content, the stronger early epistasis energy that conventional early strength agent has higher, due to not containing sulfate, will not cracking.
Description
Technical field
The present invention relates to concrete admixture field, more particularly to a kind of modified early strength agent and its synthetic method.
Background technology
Early strength agent refers to that early strength of concrete, and the additive for not making significant difference to later strength can be improved.It is early strong
The main function of agent is acceleration hydrated cementitious speed, promotes the development of early strength of concrete；Not only there is early powerful, but also tool
There is certain water reducing and strength increasing function.
It is compound that common early strength agent can be divided into strong electrolyte inorganic salts, water soluble organic substance class, organic and inorganic matter
Complex accelerator three classes.Strong electrolyte inorganic salts mainly have chloride salt, Sulfates, Nitrates, and chloride salt effect is good,
Early strength of concrete can be not only improved, also promotees solidifying, antifreezing effect, it is cheap, it is easy to use, but removing blunt of reinforcing steel bar can be made to become rusty
Erosion；And water soluble organic substance class mainly has triisopropanolamine, methanol, ethanol etc., triethanolamine is most commonly used that.Triethanolamine is
Colourless or pale yellow transparent oily liquids, soluble easily in water, general volume is 0.02%~0.05%, has deferred action, generally not
Singly mix, be often used in combination with other early strength agent.Complex accelerator is by compound between various early strength agent components, with early
It is strong compound between agent component and water-reducing agent component, modified effect more more preferable than single early strength agent can be received.But pass through compounding
The early strength agent that mode reaches the early strong purpose of concrete easily makes cement slurry later strength decay and causes steel bar corrosion etc. to be asked
Topic.
The content of the invention
The present invention easily makes cement slurry later strength decline for the early strength agent obtained in the prior art by compounding mode
The shortcomings of subtracting and causing steel bar corrosion, there is provided a kind of modified early strength agent and its synthetic method.
In order to solve the above-mentioned technical problem, the present invention is addressed by following technical proposals：
A kind of modified early strength agent, is made of the raw material of following parts by weight：
Modified function monomer includes 15~20 parts of acrylamide, 15~25 parts of methallylsulfonic acid sodium and poly-epsilon-caprolactone
Glycol 30~35.
Preferably, molecular weight regulator is mercaptopropionic acid or thioacetic acid.The addition of molecular weight regulator is mainly controlled
Molecular weight processed is excessive and causes molecular weight distribution wide, prevents from being crosslinked.
Preferably, reducing agent is sodium formaldehyde sulfoxylate or L-AA.
Preferably, the mass percentage concentration of hydrogen peroxide is 20~40%.
A kind of synthetic method of modified early strength agent, includes the following steps：
(1) isoamyl alcohol polyoxyethylene ether is dissolved in water to obtain isoamyl alcohol polyoxyethylene ether aqueous solution, and dioxygen is water-soluble
Yu Shuizhong obtains hydrogen peroxide solution, acrylic acid and modified function monomer is soluble in water obtains A liquid, molecular weight regulator and reducing agent
It is dissolved in water and obtains B liquid；
(2) isoamyl alcohol polyoxyethylene ether aqueous solution is maintained in 25 DEG C, after adding hydrogen peroxide solution stirring a period of time,
A liquid and B liquid is added dropwise at the same time；
(3) after completion of dropwise addition, after continuing 2~2.5h of stirring at 25 DEG C, with sodium hydroxide solution be neutralized to pH for 6.5~
7.5, obtain modified early strength agent.
Preferably, the time for adding of A liquid is 2.5~3h in step (2), the time for adding of B liquid is 3.5~4h.
The present invention has significant technique effect as a result of above technical scheme：The modification early strength agent of the present invention leads to
Molecular design theory is crossed, introduces modified function monomer from the angle of modified early strength agent synthesis, modified function monomer contains a variety of work(
Energy property functional group, including dihydric alcohol, amide groups, sulfonic group, ester group and double bond etc., can make the steric hindrance of cross-linking system
Effect increase, promotes the condensation of concrete, while the early strength for the concrete for making to the addition of the early strength agent and later strength are all
There is different degrees of raising, and will not Corrosion Reinforcement.
The modification early strength agent of the present invention can improve the early strength of concrete, accelerate mould turnover, accelerate assembly line life
Production, than water-reducing rate, lower air content, the stronger early epistasis energy that conventional early strength agent has higher, due to not containing sulfate,
Therefore will not cracking.
Embodiment
The present invention is described in further detail with embodiment with reference to comparative example.
Comparative example 1
A kind of modified early strength agent, is made of the raw material of following parts by weight：
Modified function monomer includes 67 parts of acrylamide.
Molecular weight regulator is mercaptopropionic acid.The addition of molecular weight regulator mainly controls molecular weight excessive and causes point
Son amount distribution is wide, prevents from being crosslinked.
Reducing agent is sodium formaldehyde sulfoxylate.
The mass percentage concentration of hydrogen peroxide is 30%.
A kind of synthetic method of modified early strength agent, includes the following steps：
(1) isoamyl alcohol polyoxyethylene ether, which is dissolved in 220 parts of water, obtains isoamyl alcohol polyoxyethylene ether aqueous solution, double
Oxygen is water-soluble to obtain hydrogen peroxide solution in 7 parts of water, and acrylic acid and modified function monomer, which are dissolved in 46 parts of water, obtains A liquid, point
The water that son amount conditioning agent and reducing agent are dissolved in 40 parts obtains B liquid；
(2) isoamyl alcohol polyoxyethylene ether aqueous solution is maintained in 25 DEG C, after adding hydrogen peroxide solution stirring a period of time,
A liquid and B liquid is added dropwise at the same time；
The time for adding of A liquid is 3h, and the time for adding of B liquid is 3.5h；
(3) after completion of dropwise addition, after continuing stirring reaction 2h at 25 DEG C, it is 7 to be neutralized to pH with sodium hydroxide solution, is obtained
Colourless modification early strength agent.
Comparative example 2
A kind of modified early strength agent, is made of the raw material of following parts by weight：
Modified function monomer includes 30 parts of 37 parts of acrylamide and methallylsulfonic acid sodium.
Molecular weight regulator is mercaptopropionic acid.The addition of molecular weight regulator mainly controls molecular weight excessive and causes point
Son amount distribution is wide, prevents from being crosslinked.
Reducing agent is sodium formaldehyde sulfoxylate.
The mass percentage concentration of hydrogen peroxide is 30%.
A kind of synthetic method of modified early strength agent, includes the following steps：
(1) isoamyl alcohol polyoxyethylene ether, which is dissolved in 220 parts of water, obtains isoamyl alcohol polyoxyethylene ether aqueous solution, double
Oxygen is water-soluble to obtain hydrogen peroxide solution in 7 parts of water, and acrylic acid and modified function monomer, which are dissolved in 46 parts of water, obtains A liquid, point
The water that son amount conditioning agent and reducing agent are dissolved in 40 parts obtains B liquid；
(2) isoamyl alcohol polyoxyethylene ether aqueous solution is maintained in 25 DEG C, after adding hydrogen peroxide solution stirring a period of time,
A liquid and B liquid is added dropwise at the same time；
The time for adding of A liquid is 3h, and the time for adding of B liquid is 3.5h；
(3) after completion of dropwise addition, after continuing stirring reaction 2h at 25 DEG C, it is 7 to be neutralized to pH with sodium hydroxide solution, is obtained
Colourless modification early strength agent.
Comparative example 3
A kind of modified early strength agent, is made of the raw material of following parts by weight：
Modified function monomer includes 30 parts of 37 parts of acrylamide and poly-epsilon-caprolactone glycol.
Molecular weight regulator is mercaptopropionic acid.The addition of molecular weight regulator mainly controls molecular weight excessive and causes point
Son amount distribution is wide, prevents from being crosslinked.
Reducing agent is sodium formaldehyde sulfoxylate.
The mass percentage concentration of hydrogen peroxide is 30%.
A kind of synthetic method of modified early strength agent, includes the following steps：
(1) isoamyl alcohol polyoxyethylene ether, which is dissolved in 220 parts of water, obtains isoamyl alcohol polyoxyethylene ether aqueous solution, double
Oxygen is water-soluble to obtain hydrogen peroxide solution in 7 parts of water, and acrylic acid and modified function monomer, which are dissolved in 46 parts of water, obtains A liquid, point
The water that son amount conditioning agent and reducing agent are dissolved in 40 parts obtains B liquid；
(2) isoamyl alcohol polyoxyethylene ether aqueous solution is maintained in 25 DEG C, after adding hydrogen peroxide solution stirring a period of time,
A liquid and B liquid is added dropwise at the same time；
The time for adding of A liquid is 3h, and the time for adding of B liquid is 3.5h；
(3) after completion of dropwise addition, after continuing stirring reaction 2h at 25 DEG C, it is 7 to be neutralized to pH with sodium hydroxide solution, is obtained
Colourless modification early strength agent.
Embodiment 1
A kind of modified early strength agent, is made of the raw material of following parts by weight：
Modified function monomer includes 17 parts of acrylamide, 18 parts of methallylsulfonic acid sodium and poly-epsilon-caprolactone glycol 32
Part.
Molecular weight regulator is mercaptopropionic acid.The addition of molecular weight regulator mainly controls molecular weight excessive and causes point
Son amount distribution is wide, prevents from being crosslinked.
Reducing agent is sodium formaldehyde sulfoxylate.
The mass percentage concentration of hydrogen peroxide is 30%.
A kind of synthetic method of modified early strength agent, includes the following steps：
(1) isoamyl alcohol polyoxyethylene ether, which is dissolved in 220 parts of water, obtains isoamyl alcohol polyoxyethylene ether aqueous solution, double
Oxygen is water-soluble to obtain hydrogen peroxide solution in 7 parts of water, and acrylic acid and modified function monomer, which are dissolved in 46 parts of water, obtains A liquid, point
The water that son amount conditioning agent and reducing agent are dissolved in 40 parts obtains B liquid；
(2) isoamyl alcohol polyoxyethylene ether aqueous solution is maintained in 25 DEG C, after adding hydrogen peroxide solution stirring a period of time,
A liquid and B liquid is added dropwise at the same time；
The time for adding of A liquid is 3h, and the time for adding of B liquid is 3.5h；
(3) after completion of dropwise addition, after continuing stirring reaction 2h at 25 DEG C, it is 7 to be neutralized to pH with sodium hydroxide solution, is obtained
Colourless modification early strength agent.
Embodiment 2
A kind of modified early strength agent, including polypentenol polyoxyethylene ether, acrylic acid, modified function monomer, hydrogen peroxide, reduction
Agent, molecular weight regulator, sodium hydroxide and water, are made of the raw material of following parts by weight：
Modified function monomer includes 20 parts of acrylamide, 25 parts of methallylsulfonic acid sodium and poly-epsilon-caprolactone glycol 35
Part.
Molecular weight regulator is mercaptopropionic acid.The addition of molecular weight regulator mainly controls molecular weight excessive and causes point
Son amount distribution is wide, prevents from being crosslinked.
Reducing agent is sodium formaldehyde sulfoxylate.
The mass percentage concentration of hydrogen peroxide is 20%.
A kind of synthetic method of modified early strength agent, includes the following steps：
(1) isoamyl alcohol polyoxyethylene ether, which is dissolved in 230 parts of water, obtains isoamyl alcohol polyoxyethylene ether aqueous solution, double
Oxygen is water-soluble to obtain hydrogen peroxide solution in 16 parts of water, and acrylic acid and modified function monomer, which are dissolved in 70 parts of water, obtains A liquid, point
The water that son amount conditioning agent and reducing agent are dissolved in 46 parts obtains B liquid；
(2) isoamyl alcohol polyoxyethylene ether aqueous solution is maintained in 25 DEG C, after adding hydrogen peroxide solution stirring a period of time,
A liquid and B liquid is added dropwise at the same time；
The time for adding of A liquid is 2.8h, and the time for adding of B liquid is 3.8h；
(3) after completion of dropwise addition, after continuing stirring reaction 2.3h at 25 DEG C, it is 6.5 to be neutralized to pH with sodium hydroxide solution,
Obtain colourless modification early strength agent.
Embodiment 3
A kind of modified early strength agent, including polypentenol polyoxyethylene ether, acrylic acid, modified function monomer, hydrogen peroxide, reduction
Agent, molecular weight regulator, sodium hydroxide and water, are made of the raw material of following parts by weight：
Modified function monomer includes 15 parts of acrylamide, 15 parts of methallylsulfonic acid sodium and poly-epsilon-caprolactone glycol 30
Part.
Molecular weight regulator is thioacetic acid.The addition of molecular weight regulator mainly controls molecular weight excessive and causes point
Son amount distribution is wide, prevents from being crosslinked.
Reducing agent is L-AA.
The mass percentage concentration of hydrogen peroxide is 40%.
A kind of synthetic method of modified early strength agent, includes the following steps：
(1) isoamyl alcohol polyoxyethylene ether, which is dissolved in 200 parts of water, obtains isoamyl alcohol polyoxyethylene ether aqueous solution, double
Oxygen is water-soluble to obtain hydrogen peroxide solution in 3 parts of water, and acrylic acid and modified function monomer, which are dissolved in 40 parts of water, obtains A liquid, point
The water that son amount conditioning agent and reducing agent are dissolved in 35 parts obtains B liquid；
(2) isoamyl alcohol polyoxyethylene ether aqueous solution is maintained in 25 DEG C, after adding hydrogen peroxide solution stirring a period of time,
A liquid and B liquid is added dropwise at the same time；
The time for adding of A liquid is 2.5h, and the time for adding of B liquid is 4h；
(3) after completion of dropwise addition, after continuing stirring reaction 2.5h at 25 DEG C, it is 7.5 to be neutralized to pH with sodium hydroxide solution,
Obtain colourless modification early strength agent.
Embodiment 4
The mechanical property for the modification early strength agent that test comparison example 1-3 and embodiment 1-3 are obtained, test method are marked with reference to country
Quasi- GB/T 50081-2002《Normal concrete mechanical test method》, wherein compression strength using 150mm × 150mm ×
L50mm cube specimens.
Intensity test result (the unit of table 1 comparative example 1-3 and embodiment 1-3：MPa)
From embodiment 1 and comparative example 1-3, with acrylamide or acrylamide and methallylsulfonic acid sodium or third
The compression strength for the modification early strength agent that acrylamide and poly-epsilon-caprolactone glycol obtain for modified function monomer is poor, less than with propylene
The pressure resistance for the modification early strength agent that acid amides, methallylsulfonic acid sodium and poly-epsilon-caprolactone glycol obtain for modified function monomer
Degree, illustrates to have using acrylamide, methallylsulfonic acid sodium and poly-epsilon-caprolactone glycol as modified function monomer preferable
Early strength function：The 1d compression strength of the modification early strength agent of embodiment 1 lifts 23.79%~32.81%, 3d pressure resistances compared with comparative example
Degree 25.77%~30.28%, 7d of lifting compression strength lifts 28.03%~29.15%, 28d compression strength lifting 16.40%
~17.56%.
From embodiment 1-3, the compression strength for the modification early strength agent that embodiment 1 obtains is preferable, is obtained better than embodiment 2-3
The modification early strength agent arrived.
In short, the foregoing is merely presently preferred embodiments of the present invention, all equalizations made according to scope of the present invention patent
Change and modification, should all belong to the covering scope of patent of the present invention.
Claims (6)
1. a kind of modified early strength agent, it is characterised in that be made of the raw material of following parts by weight：
Modified function monomer includes 15~20 parts of acrylamide, 15~25 parts of methallylsulfonic acid sodium and poly-epsilon-caprolactone glycol
30~35 parts.
2. modified early strength agent according to claim 1, it is characterised in that：Molecular weight regulator is mercaptopropionic acid or sulfydryl second
Acid.
3. modified early strength agent according to claim 1, it is characterised in that：Reducing agent is sodium formaldehyde sulfoxylate or L-AA.
4. modified early strength agent according to claim 1, it is characterised in that：The mass percentage concentration of hydrogen peroxide for 20%~
40%.
5. a kind of synthetic method of modified early strength agent according to claim 1, it is characterised in that include the following steps：
(1) isoamyl alcohol polyoxyethylene ether is dissolved in water to obtain isoamyl alcohol polyoxyethylene ether aqueous solution, and hydrogen peroxide is dissolved in water
In obtain hydrogen peroxide solution, acrylic acid and modified function monomer is soluble in water obtains A liquid, molecular weight regulator and reducing agent are dissolved in
Water obtains B liquid；
(2) isoamyl alcohol polyoxyethylene ether aqueous solution is maintained in 25 DEG C, after adding hydrogen peroxide solution stirring a period of time, at the same time
A liquid and B liquid is added dropwise；
(3) after completion of dropwise addition, after continuing 2~2.5h of stirring, it is 6.5~7.5 to be neutralized to pH with sodium hydroxide solution, is modified
Early strength agent.
6. the synthetic method of modified early strength agent according to claim 5, it is characterised in that：In step (2) during the dropwise addition of A liquid
Between be 2.5~3h, the time for adding of B liquid is 3.5~4h.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103693881A (en) * | 2013-12-26 | 2014-04-02 | 四川石达化学股份有限公司 | Polycarboxylic acid water reducer, application and preparation method of polycarboxylic acid water reducer |
| US20150291716A1 (en) * | 2012-12-05 | 2015-10-15 | Sobute New Materials Co., Ltd. | Slump retaining polycarboxylic acid superplasticizer |
| CN106749983A (en) * | 2017-01-23 | 2017-05-31 | 上海高铁化学建材有限公司 | A kind of ultra early-strength polycarboxylate water-reducer and preparation method thereof |
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2017
- 2017-10-25 CN CN201711009909.3A patent/CN108003308A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20150291716A1 (en) * | 2012-12-05 | 2015-10-15 | Sobute New Materials Co., Ltd. | Slump retaining polycarboxylic acid superplasticizer |
| CN103693881A (en) * | 2013-12-26 | 2014-04-02 | 四川石达化学股份有限公司 | Polycarboxylic acid water reducer, application and preparation method of polycarboxylic acid water reducer |
| CN106749983A (en) * | 2017-01-23 | 2017-05-31 | 上海高铁化学建材有限公司 | A kind of ultra early-strength polycarboxylate water-reducer and preparation method thereof |
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| 朱效荣等主编: "《混凝土工作性调整》", 31 May 2016, 中国建材工业出版社 * |
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Application publication date: 20180508 |