CN108440721A - A kind of production method of high-performance water reducing agent - Google Patents
A kind of production method of high-performance water reducing agent Download PDFInfo
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- CN108440721A CN108440721A CN201810390035.9A CN201810390035A CN108440721A CN 108440721 A CN108440721 A CN 108440721A CN 201810390035 A CN201810390035 A CN 201810390035A CN 108440721 A CN108440721 A CN 108440721A
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- Prior art keywords
- reducing agent
- mother liquor
- production method
- water reducing
- polycarboxylic acids
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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
- C04B24/2688—Copolymers containing at least three different monomers
- C04B24/2694—Copolymers containing at least three different monomers 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
- 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
- C08F220/04—Acids; Metal salts or ammonium salts thereof
- C08F220/06—Acrylic acid; Methacrylic acid; Metal salts or ammonium salts thereof
-
- 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
- C08F220/12—Esters of monohydric alcohols or phenols
- C08F220/14—Methyl esters, e.g. methyl (meth)acrylate
-
- 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)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Polyethers (AREA)
Abstract
The present invention provides a kind of production method of high-performance water reducing agent comprising following steps：S1, ethylene oxide, propylene oxide, methallyl alcohol the first intermediate product of acquisition are provided；S2, ethylene oxide, propylene oxide, prenol the second intermediate product of acquisition are provided；S3, modified polyether intermediate is obtained；S4, offer acrylic acid, methyl acrylate etc., by above-mentioned each component hybrid reaction, obtain the first polycarboxylic acids mother liquor；S5, the second polycarboxylic acids mother liquor is obtained；S6, the modified polyether intermediate is added separately in the first polycarboxylic acids mother liquor and the second polycarboxylic acids mother liquor, the product of acquisition is mixed, mother liquor intermediate is obtained；S7, water, colophonium pyrolytic polymer air entraining agent, sodium gluconate are provided, each component and mother liquor intermediate compounding is obtained to the water-reducing agent of the present invention.Water-reducing agent provided by the invention can reduce the water being added in concrete construction, be conducive to the setting time for shortening concrete, and improve the intensity of concrete.
Description
Technical field
The present invention relates to a kind of concrete additive technical field more particularly to a kind of producers of high-performance water reducing agent
Method.
Background technology
Concrete is the construction material that the realm of building construction often needs to use.During practice of construction, in order to enable
Each component is sufficiently mixed in concrete, is needed concrete being stirred with a certain amount of water and is mixed.Due to concrete middle reaches
The water of amorph is less, therefore usually requires the more water of addition and mixed.It is coagulated however, excessive water is added and increases concrete
Solid time.Therefore, in view of the above-mentioned problems, it is necessary to propose further solution.
Invention content
It is existing in the prior art to overcome the purpose of the present invention is to provide a kind of production method of high-performance water reducing agent
It is insufficient.
For achieving the above object, the present invention provides a kind of production method of high-performance water reducing agent comprising following step
Suddenly：
S1, ethylene oxide, propylene oxide, methallyl alcohol are provided, three's hybrid reaction is obtained into the first intermediate product；
S2, ethylene oxide, propylene oxide, prenol are provided, three's hybrid reaction is obtained into the second intermediate product；
S3, the first intermediate product and the second intermediate product are mixed, obtains modified polyether intermediate；
S4, acrylic acid, methyl acrylate, butyl acrylate, methyl methacrylate, mercaptoethanol, rongalite, dimension are provided
Above-mentioned each component hybrid reaction is obtained the first polycarboxylic acids mother liquor by C；
S5, acrylic acid, thioacetic acid, rongalite, Victoria C are provided, by above-mentioned each component hybrid reaction, obtains the second polycarboxylic acids
Mother liquor；
S6, the modified polyether intermediate is added separately to the first polycarboxylic acids mother liquor and the second polycarboxylic acids mother liquor
In, the product of acquisition is mixed, mother liquor intermediate is obtained；
S7, water, colophonium pyrolytic polymer air entraining agent, sodium gluconate are provided, each component and mother liquor intermediate compounding is obtained this
The water-reducing agent of invention.
The improvement of the production method of high-performance water reducing agent as the present invention, in the step S1, the ethylene oxide, ring
Ethylene Oxide, methallyl alcohol weight ratio be 1-5:2-3:4-6.
The improvement of the production method of high-performance water reducing agent as the present invention, in the step S2, the ethylene oxide, ring
Ethylene Oxide, prenol weight ratio be 2-5:4-5:3-6.
The improvement of the production method of high-performance water reducing agent as the present invention, in the step S4, the acrylic acid, propylene
Sour methyl esters, butyl acrylate, methyl methacrylate, mercaptoethanol, rongalite, Victoria C weight ratio be 1-1.2：2-3：2.3-
3.2：1.3-1.8：1.2-2.2：0.8-1.5：0.5-0.8.
The improvement of the production method of high-performance water reducing agent as the present invention, in the step S5, the acrylic acid, sulfydryl
Acetic acid, rongalite, Victoria C weight ratio be 0.8-1.2：1.5-2.5：2.3-3.5：2.2-2.5.
The improvement of the production method of high-performance water reducing agent as the present invention, in the rapid S7, the water, the rosin hot polymerization that provide
Object air entraining agent, sodium gluconate weight ratio be 2.3-3.5：1.8-2.6：3.5-4.2.
The improvement of the production method of high-performance water reducing agent as the present invention, in the step S7, in each component and mother liquor
Before intermediate compounding, polycarboxylic acids pulvis also is added in phase mother liquor intermediate.
Compared with prior art, the beneficial effects of the invention are as follows：The production method of the high-performance water reducing agent of the present invention provides
Water-reducing agent can reduce the water being added in concrete construction, be conducive to the setting time for shortening concrete, and improve
The intensity of concrete.
Specific implementation mode
With reference to specific embodiment, the present invention is described in detail, but it should explanation, these embodiment party
Formula is not limitation of the present invention, and those of ordinary skill in the art are according to function, method or knot made by these embodiments
Equivalent transformation on structure or replacement, all belong to the scope of protection of the present invention within.
The present invention provides a kind of production method of high-performance water reducing agent comprising following steps：
S1, ethylene oxide, propylene oxide, methallyl alcohol are provided, three's hybrid reaction is obtained into the first intermediate product.
Wherein, the ethylene oxide, propylene oxide, methallyl alcohol weight ratio be 1-5:2-3:4-6.Specifically, institute
The first intermediate product is stated to be prepared as follows：
It is passed through nitrogen displacement 5min in a kettle, reduces oxygen content in container, is then pumped into the methallyl alcohol of metering
Reaction starting liquid is prepared with a certain amount of catalyst (KOH), stirring system is opened, is warming up to 95 DEG C -105 DEG C, is passed through a small amount of
Ethylene oxide and propylene oxide initiation reaction.After waiting for induction period, it is continuously passed through the mixture of ethylene oxide and propylene oxide,
So that kettle internal pressure power is maintained at 0.2-0.35MPa confined reactions, controlling reaction temperature is at 90-110 DEG C.Time control is passed through in 2-
3 hours, it is warming up to 110 DEG C after the reaction was complete, opens vacuum dehydration 1 hour (vacuum degree is more than -0.098MPa), vacuum dehydration master
If using liquid (water) be evaporated in vacuo the when of becoming steam need absorb heat, utilize water evaporation heat absorption principle.Very
Ethylene oxide and propylene oxide reaction are added after sky dehydration, reaction temperature control at 110 DEG C, ethylene oxide and propylene oxide
Feed time was controlled at 3-5 hours, waited for that pressure is down in kettle<0.03MPa and when maintaining certain numerical value, can be considered as reaction knot
Beam keeps temperature, carries out vacuum dehydration 1 hour again (vacuum degree is more than -0.098MPa).100 DEG C are cooled to hereinafter, being added few
Amount oxalic acid is neutralized to subacidity, adds a small amount of hydrogen peroxide and bleaches half an hour in 60-80 DEG C, after be cooled to 50-60 DEG C and go out
Material.Finished fluid is pumped into slice material feeding jar through discharging pump, and material feeding jar makes material be maintained at 60 DEG C by way of indirectly heat, to protect
Semi-finished product form is demonstrate,proved, is handled convenient for follow-up workshop section.
S2, ethylene oxide, propylene oxide, prenol are provided, three's hybrid reaction is obtained into the second intermediate product.
Wherein, the ethylene oxide, propylene oxide, prenol weight ratio be 2-5:4-5:3-6.Specifically, described
Second intermediate product is prepared as follows：
Be passed through in a kettle nitrogen displacement 5min, reduce container in oxygen content, be then pumped into metering prenol and
A certain amount of catalyst (KOH) prepares reaction starting liquid, opens stirring system, is warming up to 95 DEG C -105 DEG C, is passed through a small amount of ring
Oxidative ethane and propylene oxide initiation reaction.After waiting for induction period, it is continuously passed through the mixture of ethylene oxide and propylene oxide, is made
It obtains kettle internal pressure power and is maintained at 0.2-0.35MPa confined reactions, controlling reaction temperature is at 90-110 DEG C.Time control is passed through in 2-3
Hour, 115 DEG C are warming up to after the reaction was complete, opens vacuum dehydration 1 hour (vacuum degree is more than -0.098MPa).Then it adds
Ethylene oxide and propylene oxide reaction, at 110 DEG C, the feed time control of ethylene oxide and propylene oxide exists for reaction temperature control
3-5 hours, wait for that pressure is down in kettle<0.03MPa and when maintaining certain numerical value, can be considered as reaction and terminate to keep temperature, then
Secondary progress vacuum dehydration 1 hour.It is cooled to 100 DEG C and is neutralized to subacidity hereinafter, a small amount of oxalic acid is added, add a small amount of hydrogen peroxide
In 60-80 DEG C bleach half an hour, after be cooled to 50-60 DEG C of discharging.Finished fluid is pumped into slice material feeding jar, feeding through discharging pump
Tank makes material be maintained at 60 DEG C by way of indirectly heat, to ensure in the form of semi-finished product, is handled convenient for follow-up workshop section.
S3, the first intermediate product and the second intermediate product are mixed, obtains modified polyether intermediate.
S4, acrylic acid, methyl acrylate, butyl acrylate, methyl methacrylate, mercaptoethanol, rongalite, dimension are provided
Above-mentioned each component hybrid reaction is obtained the first polycarboxylic acids mother liquor by C.
Wherein, the acrylic acid, methyl acrylate, butyl acrylate, methyl methacrylate, mercaptoethanol, rongalite,
The weight ratio of Victoria C is 1-1.2：2-3：2.3-3.2：1.3-1.8：1.2-2.2：0.8-1.5：0.5-0.8.
S5, acrylic acid, thioacetic acid, rongalite, Victoria C are provided, by above-mentioned each component hybrid reaction, obtains the second polycarboxylic acids
Mother liquor.
Wherein, the acrylic acid, thioacetic acid, rongalite, Victoria C weight ratio be 0.8-1.2：1.5-2.5：2.3-3.5：
2.2-2.5。
S6, the modified polyether intermediate is added separately to the first polycarboxylic acids mother liquor and the second polycarboxylic acids mother liquor
In, the product of acquisition is mixed, mother liquor intermediate is obtained.
S7, water, colophonium pyrolytic polymer air entraining agent, sodium gluconate are provided, each component and mother liquor intermediate compounding is obtained this
The water-reducing agent of invention.
Wherein, the water that provides, colophonium pyrolytic polymer air entraining agent, sodium gluconate weight ratio be 2.3-3.5：1.8-2.6：
3.5-4.2.In addition, before each component and mother liquor intermediate compounding, polycarboxylic acids pulvis also is added in phase mother liquor intermediate.
In conclusion the water-reducing agent that the production method of the high-performance water reducing agent of the present invention provides can reduce concrete construction
The water being added in the process is conducive to the setting time for shortening concrete, and improves the intensity of concrete.
It is obvious to a person skilled in the art that invention is not limited to the details of the above exemplary embodiments, Er Qie
In the case of without departing substantially from spirit or essential attributes of the invention, the present invention can be realized in other specific forms.Therefore, no matter
From the point of view of which point, the present embodiments are to be considered as illustrative and not restrictive, and the scope of the present invention is by appended power
Profit requires rather than above description limits, it is intended that all by what is fallen within the meaning and scope of the equivalent requirements of the claims
Variation is included within the present invention.
In addition, it should be understood that although this specification is described in terms of embodiments, but not each embodiment is only wrapped
Containing an independent technical solution, this description of the specification is merely for the sake of clarity, and those skilled in the art should
It considers the specification as a whole, the technical solutions in the various embodiments may also be suitably combined, forms those skilled in the art
The other embodiment being appreciated that.
Claims (7)
1. a kind of production method of high-performance water reducing agent, which is characterized in that the production method of the high-performance water reducing agent includes such as
Lower step：
S1, ethylene oxide, propylene oxide, methallyl alcohol are provided, three's hybrid reaction is obtained into the first intermediate product；
S2, ethylene oxide, propylene oxide, prenol are provided, three's hybrid reaction is obtained into the second intermediate product；
S3, the first intermediate product and the second intermediate product are mixed, obtains modified polyether intermediate；
S4, acrylic acid, methyl acrylate, butyl acrylate, methyl methacrylate, mercaptoethanol, rongalite, Victoria C are provided, it will
Above-mentioned each component hybrid reaction obtains the first polycarboxylic acids mother liquor；
S5, acrylic acid, thioacetic acid, rongalite, Victoria C are provided, by above-mentioned each component hybrid reaction, it is female obtains the second polycarboxylic acids
Liquid；
S6, the modified polyether intermediate is added separately in the first polycarboxylic acids mother liquor and the second polycarboxylic acids mother liquor, it will
The product of acquisition mixes, and obtains mother liquor intermediate；
S7, water, colophonium pyrolytic polymer air entraining agent, sodium gluconate are provided, each component and mother liquor intermediate compounding is obtained into the present invention
Water-reducing agent.
2. the production method of high-performance water reducing agent according to claim 1, which is characterized in that described in the step S1
Ethylene oxide, propylene oxide, methallyl alcohol weight ratio be 1-5:2-3:4-6.
3. the production method of high-performance water reducing agent according to claim 1, which is characterized in that described in the step S2
Ethylene oxide, propylene oxide, prenol weight ratio be 2-5:4-5:3-6.
4. the production method of high-performance water reducing agent according to claim 1, which is characterized in that described in the step S4
Acrylic acid, methyl acrylate, butyl acrylate, methyl methacrylate, mercaptoethanol, rongalite, Victoria C weight ratio be 1-
1.2：2-3：2.3-3.2：1.3-1.8：1.2-2.2：0.8-1.5：0.5-0.8.
5. the production method of high-performance water reducing agent according to claim 1, which is characterized in that described in the step S5
Acrylic acid, thioacetic acid, rongalite, Victoria C weight ratio be 0.8-1.2：1.5-2.5：2.3-3.5：2.2-2.5.
6. the production method of high-performance water reducing agent according to claim 1, which is characterized in that in the rapid S7, provide
Water, colophonium pyrolytic polymer air entraining agent, sodium gluconate weight ratio be 2.3-3.5：1.8-2.6：3.5-4.2.
7. the production method of high-performance water reducing agent according to claim 1, which is characterized in that in the step S7, each
Polycarboxylic acids pulvis also is added in phase mother liquor intermediate with before mother liquor intermediate compounding in component.
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| CN201810390035.9A CN108440721A (en) | 2018-04-27 | 2018-04-27 | A kind of production method of high-performance water reducing agent |
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| CN104177561A (en) * | 2014-07-30 | 2014-12-03 | 广东红墙新材料股份有限公司 | Polycarboxylate water reducing agent with slow-release property and mud resistance as well as preparation method and application of polycarboxylate water reducing agent |
| CN104292397A (en) * | 2014-09-23 | 2015-01-21 | 江苏奥莱特新材料有限公司 | Method for preparing special functional polycarboxylate water reducer for PHC pipe pile |
| CN105198265A (en) * | 2015-10-14 | 2015-12-30 | 广东红墙新材料股份有限公司 | Preparation method of pipe pile |
| CN105294952A (en) * | 2015-11-24 | 2016-02-03 | 南京红宝丽醇胺化学有限公司 | Preparation method of polycarboxylic water-reducing agent |
| CN105906753A (en) * | 2016-05-31 | 2016-08-31 | 江苏中铁奥莱特新材料有限公司 | Preparation method of polycarboxylate superplasticizer |
| CN107057053A (en) * | 2017-05-17 | 2017-08-18 | 浙江凯德化工有限公司 | A kind of preparation method of water reducer monomer |
| CN107903565A (en) * | 2017-11-29 | 2018-04-13 | 浙江大东吴集团建设新材料有限公司 | A kind of high performance polycarboxylate water-reducer and preparation method thereof |
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2018
- 2018-04-27 CN CN201810390035.9A patent/CN108440721A/en active Pending
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104177561A (en) * | 2014-07-30 | 2014-12-03 | 广东红墙新材料股份有限公司 | Polycarboxylate water reducing agent with slow-release property and mud resistance as well as preparation method and application of polycarboxylate water reducing agent |
| CN104292397A (en) * | 2014-09-23 | 2015-01-21 | 江苏奥莱特新材料有限公司 | Method for preparing special functional polycarboxylate water reducer for PHC pipe pile |
| CN105198265A (en) * | 2015-10-14 | 2015-12-30 | 广东红墙新材料股份有限公司 | Preparation method of pipe pile |
| CN105294952A (en) * | 2015-11-24 | 2016-02-03 | 南京红宝丽醇胺化学有限公司 | Preparation method of polycarboxylic water-reducing agent |
| CN105906753A (en) * | 2016-05-31 | 2016-08-31 | 江苏中铁奥莱特新材料有限公司 | Preparation method of polycarboxylate superplasticizer |
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Application publication date: 20180824 |