CN106279565A - A kind of two excitation system produces solid polycarboxylic acid water reducing agent and preparation method thereof - Google Patents
A kind of two excitation system produces solid polycarboxylic acid water reducing agent and preparation method thereof Download PDFInfo
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- CN106279565A CN106279565A CN201610728042.6A CN201610728042A CN106279565A CN 106279565 A CN106279565 A CN 106279565A CN 201610728042 A CN201610728042 A CN 201610728042A CN 106279565 A CN106279565 A CN 106279565A
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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
- C04B24/2605—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds 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
- 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
- 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
- C08F2/02—Polymerisation in bulk
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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
- C08F4/00—Polymerisation catalysts
- C08F4/40—Redox systems
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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)
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- Polymers & Plastics (AREA)
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Abstract
The invention discloses a kind of two excitation system and produce solid polycarboxylic acid water reducing agent and preparation method thereof, be to use oxidoreduction to excite two kinds of free radical polymerization process of system and polymerisation in bulk to produce solid polycarboxylic acid water reducing agent.The solid polycarboxylic acid water reducing agent that this technique produces is to carry out the polymerization of molecule, grafting and the solid polycarboxylic acid water reducing agent with the combed molecular structure identical with conventional liq polycarboxylate water-reducer that formed under initiator and chain-transferring agent effect with unsaturated carboxylic acid and unsaturation polyethenoxy ether class polymeric monomer.Owing to this process uses two excitation technique, molecular structure is flexible, the product of different performance can be obtained by introducing different group, to concrete ground material strong adaptability, without any volatile solvent in the solid polycarboxylic acid water reducing agent prepared, product can prepare lamellar or powdery solid polycarboxylate water-reducer by condensation microtomy or mechanical activation comminution, in use can be configured to the aqueous solution of various concentration, there is saving cost of transportation, characteristic easy to use, and the solid polycarboxylic acid water reducing agent of powdery can be directly used in the preparation of dry powder and mortar, there is extraordinary market application foreground.
Description
Technical field
The present invention relates to chemical building material field, be related specifically to a kind of two excitation system produce solid polycarboxylic acid water reducing agent and
Its preparation method.
Background technology
Poly carboxylic acid series water reducer is as component important in modern concrete, and the suitability to improving concrete plays important
Effect, polycarboxylate water-reducer keeps directly improving concrete by adjust that concrete mixes and stirs period water-reducing rate or the slump
Performance, is widely used in concrete works field, is the high-performance water reducing agent of a new generation.But polycarboxylic acids diminishing at present
Agent is many to be existed with liquid, there is the problem that cost of transportation is high, in certain journey for outlet or long-distance transportation as admittedly calculated by folding
Limit the range of application of water reducer on degree, and along with the development of dry powder and mortar, market is also badly in need of a kind of high-quality solid
Body polycarboxylate water-reducer.
Patent CN102372828A (date of publication: 2012.03.14) reports the side of a kind of synthesis of solid polycarboxylate water-reducer
Method.The technical scheme of this patent is to use the monomer containing unsaturated group to react at organic solvent, adds after the completion of reaction
Alkaline matter neutralizes and prepares polycarboxylate water-reducer through centrifuging treatment, then by obtained polycarboxylate water-reducer through overdrying
Dry process obtains solid polycarboxylic acid water reducing agent.One solid polycarboxylic acid water reducing agent of the present invention uses low temperature regime to be prepared from, and keeps away
Exempt from polycarboxylate water-reducer to crosslink because of high temperature spray-drying, destroyed the structure of polycarboxylate water-reducer, thus prepare performance
The most superior solid polycarboxylic acid water reducing agent.But this patent of invention first will through centrifuging treatment, after through dried
Just can form solid polycarboxylic acid water reducing agent, production cost is high, and needs to use a large amount of heat energy in dry run, is unfavorable for joint
Can environmental protection.
Patent CN100366565C (date of publication: 2008.02.06) reports the preparation side of a kind of powder polycarboxylic acids water reducing agent
Method, it is that by nebulizer, polycarboxylate water-reducer solution is formed droplet, is injected into hothouse, enters the hot-air of hothouse
Air-flow is identical with flow direction of material, and hothouse inlet temperature is 120-200 DEG C, and leaving air temp is 50-110 DEG C, drying, sedimentation and
Obtain powder polycarboxylic acids water reducing agent.Although this technique solves subproblem, such as material glues and side reaction easily occurs under wall, high temperature
Etc. problem, but inevitably use spray drying method must bring high energy consumption, and in being spray-dried link high temperature to poly-
Carboxylic acid molecules can produce partial cross-linked, damages polycarboxylic acids molecular structure, affects using effect.
Patent CN104628969A (date of publication: 2015.05.20) reports a kind of slow-release solid poly carboxylic acid series water reducer
Preparation method, the carboxylic acids minor comonomer containing unsaturated double-bond is carried out pre-place first with amine organic molecule by this patent
Reason；Then above-mentioned pretreated unsaturated acrylic compounds minor comonomer and unsaturated polyoxyethylene ether polymeric monomer are added heat fusing
After, the unsaturated esters minor comonomer of dropping under initiator and chain-transferring agent effect, course of reaction is placed in anhydrous organic solvent-free
Environment is prepared by bulk polymerization.The present invention is by utilizing the method for polymerisation in bulk to prepare in anhydrous solvent-free environment
Slow-release solid poly carboxylic acid series water reducer have that technique is simple, easily controllable, save cost of transportation and environment friendly and pollution-free etc. excellent
Point, it is achieved that slowly discharge in concrete, keeps the purpose that the slump 3～4h is not lost, and market application foreground is extensive.But
This patent of invention in course of reaction with anhydrous organic solvent as dispersion, first have to face the recycling of solvent
Problem, it is contemplated that whether the change of each organic component impacts product during recycling, secondly, to recovery
The operation of device to tighten control, and prevents solvent volatilization, leakage to environment.
The solid polycarboxylic acid water reducing agent announced at present is many using organic solvent as dispersant, and solvent content is carried out by the later stage again
Separate, reclaim, or with spray-dried forms, primary liquid polycarboxylate water-reducer is carried out process of dusting.But, both the above is normal
All there is deficiency to a certain extent in the solid polycarboxylic acid water reducing agent that produces seen, as using organic solvent as dispersant, first has to
After considering organic solvent portion recovery, whether component changes, and whether recycling impacts product quality, and secondly, polycarboxylic acids subtracts
Water preparation is as a kind of surfactant, and environment also can be caused secondary pollution by solvent residual in solid water reducer.As passed through
Spray dried form carries out the production of powder polycarboxylic acids water reducing agent, and in production process, energy consumption strengthens, and is unfavorable for energy-conserving and environment-protective, and
During high temperature dusts, also can destroy polycarboxylate water-reducer molecular structure, affect product serviceability.
Summary of the invention
The technical problem to be solved in the present invention is to provide a kind of two excitation system and produces solid polycarboxylic acid water reducing agent
And preparation method thereof, use oxidation-reduction to excite two kinds of free radical polymerization process of system and polymerisation in bulk to produce solid polycarboxylic acids
Water reducer.
The present invention solves above-mentioned technical problem and the technical scheme is that a kind of two excitation system produces solid polycarboxylic acids and subtracts
Water preparation, it is characterised in that: it is made up of following component and percentage by weight: unsaturated polyethenoxy ether class polymeric monomer 75-90%, no
Saturated carboxylic acid 15-20%, chain-transferring agent 0.5-1.5%, polymerisation in bulk initiator 0.1-0.3%, oxidant 0.05-0.3%, also
Former dose of 0.01-0.2%.
Further technical scheme is, described unsaturated polyethenoxy ether class polymeric monomer is methallyl alcohol polyoxyethylene
One in ether (HPEG), isopentenol polyoxyethylene ether (TPEG), allyl alcohol polyethenoxy ether (APEG).
Further technical scheme is, described unsaturated polyethenoxy ether class polymeric monomer mean molecule quantity is 2400-
4000。
Further technical scheme is, described unsaturated carboxylic acid is acrylic acid, methacrylic acid, maleic anhydride, clothing health
One or more in acid.
Further technical scheme is, described chain-transferring agent is mercaptopropionic acid, TGA, methacrylic sulfonic acid
One or more in sodium, mercaptoethanol.
Further technical scheme is, described polymerisation in bulk initiator is azo diisopropylamidinateand oxazoline hydrochlorate
(VA-044), dibenzoyl peroxide, azodiisobutyronitrile, 2,2'-Azobis(2,4-dimethylvaleronitrile), peroxy dicarbonate diethyl ester
(EHP), the one in tert-butyl hydroperoxide, cumyl peroxide, the peroxidating trimethylacetic acid tert-butyl ester.
Further technical scheme is, described oxidant be the one in Ammonium persulfate., potassium peroxydisulfate, hydrogen peroxide or
Several.
Further technical scheme is, described reducing agent be sodium sulfite, sodium thiosulfate, L-AA,
One or more in ferrous sulfate, oxalic acid, glucose, sodium hypophosphite.
Further technical scheme is, described a kind of two excitation system produces the preparation side of solid polycarboxylic acid water reducing agent
Method, comprises the following steps:
(1) the unsaturated polyethenoxy ether class polymeric monomer of above-mentioned percentage by weight is put in reactor, be warming up to 60-
80 DEG C, stir standby after polymeric monomer is fully melted.
(2) stirring containing unsaturated carboxylic acid, chain-transferring agent, the mixed liquor of reducing agent by above-mentioned percentage by weight
After, it is designated as A liquid, standby.
(3) polymerisation in bulk initiator, the oxidant of above-mentioned weight face proportion by subtraction are rendered in reactor successively, throw in every time
Interval stirring 5-20 minute.
(4) keep reactor temperature at 60-80 DEG C, at the uniform velocity drip the A liquid of preparation, time for adding control in step (2)
System was at 2-4 hour.
(5) A drop is incubated aging 1-3 hour stopped reaction, blowing after adding.
(6) treat that product temperature is down to 20-40 DEG C, described solid polycarboxylic acid water reducing agent.
Use produced by technique scheme and have the beneficial effects that: the solid polycarboxylic acid water reducing agent that this method produces be with
Unsaturated carboxylic acid and unsaturated polyethenoxy ether class polymeric monomer carry out the polymerization of molecule under initiator and chain-transferring agent effect, connect
Branch and the solid polycarboxylic acid water reducing agent with the combed molecular structure identical with conventional liq polycarboxylate water-reducer that formed.Due to
Use two excitation system, the scion grafting group of polycarboxylate water-reducer molecule can be adjusted flexibly so that it is equal to the cement of different brands
There is the preferable suitability.Have that technique is simple, production cost is low, the free of contamination feature of safety and environmental protection, the solid polycarboxylic acids of production
Water reducer is not only suitable with existing liquid polycarboxylate water-reducer performance, and can be substantially reduced by the solid calculating of folding and transport into
This.The biggest impetus is served for expanding the range of application of polycarboxylate water-reducer.The present invention uses the freedom of two excitation
Base polymerization, does not use any organic solvent in production process, it is to avoid solvent volatilization causes environmental pollution；Two excitation free radical
Polymerization can adjust polycarboxylate water-reducer molecular structure easily, to the cement of different brands and concrete admixture and aggregate tool
There is good adaptability, overcome polycarboxylate water-reducer use difference geographically；Later stage section or atomization process need not adopt
Dry with dusting, energy-saving and cost-reducing, save and produce and use cost, polycarboxylate water-reducer is expanded range of application and serves the biggest
Impetus.It it is a kind of production method safe and environment-friendly, efficient.
Detailed description of the invention
Below the technical scheme in the embodiment of the present invention is clearly and completely described, it is clear that described embodiment
It is only a part of embodiment of the present invention rather than whole embodiments.Based on the embodiment in the present invention, the common skill in this area
The every other embodiment that art personnel are obtained under not making creative work premise, broadly falls into the model of present invention protection
Enclose.
Elaborate a lot of detail in the following description so that fully understanding the present invention, but the present invention is all right
Using other to be different from alternate manner described here to implement, those skilled in the art can be without prejudice to intension of the present invention
In the case of do similar popularization, therefore the present invention is not limited by following public specific embodiment.
Embodiment 1
1. take HPEG2400:180g, put in reactor, be warming up to 65 DEG C, after fully melting, open stirring, and
Keep current still temperature.
2. methacrylic acid: 25g, mercaptopropionic acid: 1g, glucose: 0.2g, stirs, and is designated as A liquid.
Adding potassium peroxydisulfate: 1.2g, 2,2'-Azobis(2,4-dimethylvaleronitrile): 0.2g the most successively in reactor, after feeding intake, interval is stirred every time
Mix 15 minutes.
The A liquid that the most at the uniform velocity 2. dropping step prepares, it is desirable to time for adding 3 hours.
5. after A liquid adds dropping, insulation aging reaction 1 hour.
6. after aging reaction, blowing, when product is cooled to 20-40 DEG C, solid polycarboxylic acid water reducing agent can be obtained.
Embodiment 2
1. take HPEG3000:200g, put in reactor, be warming up to 75 DEG C, after fully melting, open stirring, and
Keep current still temperature.
2. methacrylic acid: 5g, acrylic acid: 35g, mercaptopropionic acid: 1.5g, methylpropene sodium sulfonate: 0.8g, ortho phosphorous acid
Sodium: 0.1g, stirs, and is designated as A liquid.
Adding potassium peroxydisulfate: 1.2g, dibenzoyl peroxide: 1g the most successively in reactor, after feeding intake, interval is stirred every time
Mix 15 minutes.
The A liquid that the most at the uniform velocity 2. dropping step prepares, it is desirable to time for adding 2.5 hours.
5. after A liquid adds dropping, insulation aging reaction 2 hours.
6. after aging reaction, blowing, when product is cooled to 20-40 DEG C, solid polycarboxylic acid water reducing agent can be obtained.
Embodiment 3
1. take TPEG3000:200g, put in reactor, be warming up to 80 DEG C, after fully melting, open stirring, and
Keep current still temperature.
2. methacrylic acid: 20g, acrylic acid: 15g, TGA: 1.2g, sodium hypophosphite: 0.2g, is sufficiently stirred for all
Even, it is designated as A liquid.
In reactor, add potassium peroxydisulfate: 1g, azodiisobutyronitrile: 1g the most successively, after feeding intake, be spaced stirring 15 every time
Minute.
The A liquid that the most at the uniform velocity 2. dropping step prepares, it is desirable to time for adding 1.5 hours.
5. after A liquid adds dropping, insulation aging reaction 1 hour.
6. after aging reaction, blowing, when product is cooled to 20-40 DEG C, solid polycarboxylic acid water reducing agent can be obtained.
Embodiment 4
1. take HPEG3000:200g, put in reactor, be warming up to 70 DEG C, after fully melting, open stirring, and
Keep current still temperature.
2. acrylic acid: 25g, maleic anhydride: 1g, TGA: 0.6g, methylpropene sodium sulfonate: 0.2g, ortho phosphorous acid
Sodium: 0.3g, stirs, and is designated as A liquid.
Hydrogen peroxide: 2.0g, azodiisobutyronitrile: 1.5g, interval stirring after every time feeding intake is added the most successively in reactor
15 minutes.
The A liquid that the most at the uniform velocity 2. dropping step prepares, it is desirable to time for adding 2.5 hours.
5. after A liquid adds dropping, insulation aging reaction 2 hours.
6. after aging reaction, blowing, when product is cooled to 20-40 DEG C, solid polycarboxylic acid water reducing agent can be obtained.
Embodiment 5
1. take HPEG3000:220g, put in reactor, be warming up to 70 DEG C, after fully melting, open stirring, and
Keep current still temperature.
2. acrylic acid: 25g, methacrylic acid: 15g mercaptopropionic acid: 1.2g, mercaptopropionic acid: 1.5g, L-AA:
0.5g, stirs, and is designated as A liquid.
Adding Ammonium persulfate.: 0.9g, 2,2'-Azobis(2,4-dimethylvaleronitrile): 1.0g the most successively in reactor, after feeding intake, interval is stirred every time
Mix 15 minutes.
The A liquid that the most at the uniform velocity 2. dropping step prepares, it is desirable to time for adding 2.0 hours.
5. after A liquid adds dropping, insulation aging reaction 1 hour.
6. after aging reaction, blowing, when product is cooled to 20-40 DEG C, solid polycarboxylic acid water reducing agent can be obtained.
Implementation result
Below by corresponding experiment, the solid polycarboxylic acid water reducing agent prepared in checking above-described embodiment 1-5, take respectively
Stating the prepared solid polycarboxylic acid water reducing agent of experimental example and be configured to the aqueous solution of 10%, reference numeral is 1#-5#, takes liquid mother liquor and joins
Making the aqueous solution of 10%, as comparative example, reference numeral is 0#.
1, flowing degree of net paste of cement
This effects two excitation solid polycarboxylic acid water reducing agent solution mobility action effect to different cement, experiment is surveyed
Determine each embodiment paste flowing degree to different cement types under the solid volume of identical folding.According to " GBT8077-2000 coagulation
Soil additive homogeneity test method ", detect flowing degree of net paste of cement, W/C=0.29, water reducer volume is the solid volume of folding, knot
Fruit is shown in Table 1.
Table 1 flowing degree of net paste of cement is tested
From table 1 data analysis, the solid polycarboxylic acid water reducing agent of the inventive method synthesis is to the different adaptability of cement, dispersions
Power all shows excellence.
2, concrete flowability energy result
This experiment uses east, Ji cement PO.42.5 to test, and checking the various embodiments described above are at identical concrete mix
In divergence and slump holding capacity.
Table 2 concrete mix
Table 3 concrete flowability energy result
From table 3 data analysis, the solid polycarboxylic acid water reducing agent of the inventive method synthesis, all can show in concrete system
Go out excellent mobility with slump-retaining.
Claims (9)
1. a two excitation system produces solid polycarboxylic acid water reducing agent, it is characterised in that: the present invention is by following component and weight hundred
Proportion by subtraction forms: unsaturated polyethenoxy ether class polymeric monomer 75-90%, unsaturated carboxylic acid 15-20%, chain-transferring agent 0.5-1.5%,
Polymerisation in bulk initiator 0.1-0.3%, oxidant 0.05-0.3%, reducing agent 0.01-0.2%.
A kind of two excitation system the most according to claim 1 produces solid polycarboxylic acid water reducing agent, it is characterised in that: described not
Saturated polyethenoxy ether class polymeric monomer be methyl allyl alcohol polyoxyethylene ether (HPEG), isopentenol polyoxyethylene ether (TPEG),
One in allyl alcohol polyethenoxy ether (APEG).
A kind of two excitation system the most according to claim 2 produces solid polycarboxylic acid water reducing agent, it is characterised in that: described insatiable hunger
It is 2400-4000 with polyethenoxy ether class polymeric monomer mean molecule quantity.
A kind of two excitation system the most according to claim 1 produces solid polycarboxylic acid water reducing agent, it is characterised in that: described not
Saturated carboxylic acid is one or more in acrylic acid, methacrylic acid, maleic anhydride, itaconic acid.
A kind of two excitation system the most according to claim 1 produces solid polycarboxylic acid water reducing agent, it is characterised in that: described
Chain-transferring agent is one or more in mercaptopropionic acid, TGA, methylpropene sodium sulfonate, mercaptoethanol.
A kind of two excitation system the most according to claim 1 produces solid polycarboxylic acid water reducing agent, it is characterised in that: described
Polymerisation in bulk initiator be azo diisopropylamidinateand oxazoline hydrochlorate (VA-044), dibenzoyl peroxide, azodiisobutyronitrile,
2,2'-Azobis(2,4-dimethylvaleronitrile), peroxy dicarbonate diethyl ester (EHP), tert-butyl hydroperoxide, cumyl peroxide, peroxidating
One in the trimethylacetic acid tert-butyl ester.
A kind of two excitation system the most according to claim 1 produces solid polycarboxylic acid water reducing agent, it is characterised in that: described
Oxidant is one or more in Ammonium persulfate., potassium peroxydisulfate, hydrogen peroxide.
A kind of two excitation system the most according to claim 1 produces solid polycarboxylic acid water reducing agent, it is characterised in that: described
Reducing agent is in sodium sulfite, sodium thiosulfate, L-AA, ferrous sulfate, oxalic acid, glucose, sodium hypophosphite
One or more.
9. produce solid polycarboxylic acid water reducing agent according to a kind of two excitation system described in claim 1-8 any one claim
Preparation method, it is characterised in that comprise the steps:
(1) the unsaturated polyethenoxy ether class polymeric monomer of above-mentioned percentage by weight is put in reactor, be warming up to 60-80
DEG C, stir standby after polymeric monomer is fully melted；
(2) by after the stirring containing unsaturated carboxylic acid, chain-transferring agent, the mixed liquor of reducing agent of above-mentioned percentage by weight,
It is designated as A liquid, standby；
(3) polymerisation in bulk initiator, the oxidant of above-mentioned weight face proportion by subtraction are rendered in reactor successively, throw in interval every time
Stir 5-20 minute；
(4) keeping reactor temperature at 60-80 DEG C, at the uniform velocity drip the A liquid of preparation in step (2), time for adding controls
2-4 hour；
(5) A drop is incubated aging 1-3 hour stopped reaction, blowing after adding；
(6) treat that product temperature is down to 20-40 DEG C, described solid polycarboxylic acid water reducing agent.
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| CN108707211A (en) * | 2018-07-09 | 2018-10-26 | 山西佳维新材料股份有限公司 | A kind of collapse protection type solid polycarboxylic acid water reducing agent and preparation method thereof |
| CN108821633A (en) * | 2018-07-09 | 2018-11-16 | 山西佳维新材料股份有限公司 | A kind of water reducing type solid polycarboxylic acid water reducing agent and preparation method thereof |
| CN108948289A (en) * | 2018-07-27 | 2018-12-07 | 刘翠芬 | A kind of modified polycarboxylic acid water-reducing agent pulvis and its synthesis preparation method |
| CN109437644A (en) * | 2018-12-03 | 2019-03-08 | 苏州市兴邦化学建材有限公司 | A kind of synthetic method improving polycarboxylate water-reducer cement adaptability |
| CN109942222A (en) * | 2019-03-27 | 2019-06-28 | 山西佳维新材料股份有限公司 | A kind of preparation method of solid early strength polycarboxylic acid high performance dehydragent |
| CN110240676A (en) * | 2019-04-10 | 2019-09-17 | 武汉理工大学 | A kind of preparation method of solid polycarboxylic acid water reducing agent |
| CN110642997A (en) * | 2019-10-18 | 2020-01-03 | 山东银泰化学技术有限公司 | High-adaptability powdery polycarboxylate superplasticizer and preparation method thereof |
| CN110713575A (en) * | 2019-11-07 | 2020-01-21 | 湖南铭煌科技发展有限公司 | Synthesis method of water-reducing solid polycarboxylate superplasticizer |
| CN113354108A (en) * | 2021-05-12 | 2021-09-07 | 深圳市点石源水处理技术有限公司 | Modified S-carboxyethyl thiosuccinic acid and preparation method and application thereof |
| US11597859B2 (en) | 2020-01-24 | 2023-03-07 | Oatey Co. | Solvent cement formulations having extended shelf life |
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