CN106632884A - Method for preparing polycarboxylate superplasticizer - Google Patents
Method for preparing polycarboxylate superplasticizer Download PDFInfo
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- CN106632884A CN106632884A CN201610924544.6A CN201610924544A CN106632884A CN 106632884 A CN106632884 A CN 106632884A CN 201610924544 A CN201610924544 A CN 201610924544A CN 106632884 A CN106632884 A CN 106632884A
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- polyoxyethylene ether
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- polycarboxylate water
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- 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
- 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
- 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)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Ceramic Engineering (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
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Abstract
The invention relates to a method for preparing a polycarboxylate superplasticizer. The method comprises the following steps: dissolving isopentenol polyoxyethylene ether in running water so as to form a polyether solution with the mass concentration of 40-55%; adding an active aid, uniformly stirring, and adding an oxidant; dropwise adding acrylic acid aqueous solution and a mixed aqueous solution of a chain transfer agent and a reducing agent; regulating the pH value of the system, wherein the molar ratio of the isopentenol polyoxyethylene ether to the acrylic acid is 1:(3.1-7), the addition amount of the active aid accounts for 1-5% of the mass of the isopentenol polyoxyethylene ether, the addition amount of the chain transfer agent accounts for 0.05-1.5% of the mass of the isopentenol polyoxyethylene ether, the addition amount of the oxidant accounts for 1-3% of the mass of the isopentenol polyoxyethylene ether, and the addition amount of the reducing agent accounts for 0.06-0.8% of the mass of the isopentenol polyoxyethylene ether. The method disclosed by the invention is simple in process, convenient to operate, low in cost and suitable for normal temperature production, and the defects of the preparation method of the existing polycarboxylate superplasticizer are overcome.
Description
Technical field
The present invention relates to a kind of preparation method of polycarboxylate water-reducer, more particularly to a kind of to be synthesized using running water low temperature
The method of polycarboxylate water-reducer.
Background technology
Poly carboxylic acid series water reducer is containing carboxyl graft copolymer in molecule, with the spy that polyoxyethylene forms " pectination "
Different molecular structure, it has the advantages that volume is low, water-reducing rate is high, does not isolate, slump-retaining energy is good, is after calcium lignosulfonate, naphthalene system
The third generation high-performance water reducing agent grown up after ordinary water-reducing agent, high efficiency water reducing agent for representative.With China's water conservancy, bridge
The rise of the infrastructure such as beam, nuclear power, tunnel, railway, poly carboxylic acid series water reducer is more and more applied.
At present the polyethers raw material of production polycarboxylate water-reducer is mainly methoxypolyethylene glycol methacrylate, pi-allyl and gathers
Oxyethylene group ether, methyl allyl polyoxyethylene ether, isopentene group alcohol polyoxyethylene ether.With constantly sending out for polyethers technology
Exhibition, in recent years the synthetic technology level of polycarboxylate water-reducer is obviously improved, and its industrialized production is synthesized by the initial step of esters two
Method technique ethers one-step synthesis till now, reaction temperature is by 40-80 DEG C of high temperature production development till now 20-40 DEG C
Ordinary temperature production.But, in the winter time, because Central China's temperature is often less than 10 DEG C, when carrying out ordinary temperature production using existing technique,
A small amount of steam or boiler heating are remained a need for, it is absolute without thermal source production in order to realize, energy resource consumption is reduced, need further
Reduce the reaction temperature of poly carboxylic acid series water reducer synthesis.
In order to reduce the reaction temperature of poly carboxylic acid series water reducer synthesis, domestic and international researcher has carried out substantial amounts of research work
Make, the way for generally adopting is reacted with redox system low temperature softening water or low temperature segmentation.
A kind of preparation method of low temperature and high concentration polycarboxylate water-reducer, " persulfuric acid are disclosed in patent CN104371074
Under ammonium-sulfate iron " redox system, using softened water, (or iso-amylene is claimed by methyl thiazolinyl APEO at 0-15 DEG C
Alcohol APEO, TPEG) and two kinds of water miscible monomers of acrylic acid carry out the method that the segmentation of single tank is added dropwise and prepare high concentration
Polycarboxylate water-reducer.This kind of method needs first carry out water sofening treatment, and reacts segmentation and carry out, complex process and course of reaction
It is difficult to control to.
In patent CN105418856A, when the temperature of reaction system is in 0-10 DEG C, 10-20 DEG C, 20-30 DEG C, 30-40
DEG C, within the scope of the different temperature such as 40-50 DEG C when using different factory formulas and technique synthesis polycarboxylate water-reducer.Method behaviour
Make complicated, be unfavorable for continuation steady production.
In patent 104356316A, methenamine is adopted for cleanser, prepare polycarboxylic acids using running water at normal temperatures
Water reducer.This method is not suitable for the low temperature synthesis of winter water reducer, and needs to add cleanser in course of reaction, increased
Cost.
As can be seen here, the preparation method of above-mentioned existing polycarboxylate water-reducer has obviously still suffered from inconvenience and defect, and urgently
Wait to be further improved.How a kind of process is simple, easy to operate, low cost and suitable for ordinary temperature production are founded
The preparation method of new, polycarboxylate water-reducer, real category current industry pole needs improved target.
The content of the invention
The technical problem to be solved in the present invention is to provide a kind of preparation method of polycarboxylate water-reducer so as to process is simple,
Easy to operate, low cost and suitable for ordinary temperature production, so as to overcome the shortcomings of the preparation method of existing polycarboxylate water-reducer.
To solve above-mentioned technical problem, a kind of preparation method of polycarboxylate water-reducer of the invention is comprised the following steps：A. will
Isopentenol polyoxyethylene ether is dissolved in running water and forms polyether solutions of the mass concentration for 40-55%；B. activity is added to help
Agent, is stirring evenly and then adding into oxidant；C. acrylic acid aqueous solution and chain-transferring agent, the mixed aqueous solution of reducing agent is added dropwise；D. adjust
Section system pH；Wherein, isopentenol polyoxyethylene ether and acrylic acid mol ratio are 1:3.1-7, the addition of coagent
The 1-5% of isopentenol polyoxyethylene ether quality is accounted for, the addition of chain-transferring agent accounts for isopentenol polyoxyethylene ether quality
0.05-1.5%, the addition of oxidant accounts for the 1-3% of isopentenol polyoxyethylene ether quality, and the addition of reducing agent accounts for isoamyl
The 0.06-0.8% of enol APEO quality.
Used as a modification of the present invention, described coagent is methacrylic acid, accounts for isopentenol polyoxyethylene ether
The 1-5% of quality.
Described step C is specially：Start simultaneously at dropwise addition acrylic acid aqueous solution and chain-transferring agent, the mixing of reducing agent are water-soluble
Liquid, is added dropwise duration and is respectively 3 hours and 3.5 hours.
Described chain-transferring agent is thio-alcohol water-soluble chain transfer agent.
Described thio-alcohol water-soluble chain transfer agent is the one kind in TGA, mercaptopropionic acid or mercaptoethanol.
Also include step E after described step D, as needed, the regulation that adds water is to required solids content.
Described oxidant is the mixing of one or more in hydrogen peroxide, ammonium persulfate, sodium peroxydisulfate.
Described reducing agent is the mixing of one or more in ascorbic acid, sodium sulfite, sodium formaldehyde sulfoxylate, ferrous sulfate.
The molecular weight of described isopentenol polyoxyethylene ether is 2000-3000.
Described step D is using the aqueous solution regulation system pH value of NaOH to 6-8.
After such design, the present invention at least has advantages below：
1st, the present invention adopts the redox initiation system of hydrogen peroxide-ascorbic acid, and adds in bed material homemade
Coagent, reduces reaction temperature, even if need not heat that under the room temperature of 0-3 DEG C of Central China radical polymerization can also be made
Close reaction to be normally carried out, realize industrialized production, reaction is easily controlled, simple production process, can produce without thermal source, reduce
Production cycle, three-waste free discharge is more environmentally friendly, and use range is wider；
2nd, it is not high to water quality requirement, without the need for deionized water, using ordinary tap water, technique and production equipment are simplified, save
About the energy, reduces production cost, and cost performance is high；
3rd, synthesize water reducer for low temperature running water and invent, but be equally applicable to tap water at normal temperature polycarboxylate water-reducer
Production, for the ambient stable production under Various Seasonal different temperatures technical guarantee is provided.
Specific embodiment
The preparation method of polycarboxylate water-reducer of the present invention is mainly comprised the following steps：
First, isopentenol polyoxyethylene ether is dissolved in into formation mass concentration in running water molten for the polyethers of 40-55%
Liquid.Isopentenol polyoxyethylene ether with molecular weight as 2000-3000 used in the present invention is advisable.
Secondly, coagent is added, is stirring evenly and then adding into oxidant.Wherein, coagent of the present invention is excellent
Methacrylic acid is selected, addition is 1-5% with the mass ratio of isopentenol polyoxyethylene ether.In the self-control coagent of the present invention
In.Oxidant can adopt the mixing of one or more in hydrogen peroxide, ammonium persulfate, sodium peroxydisulfate, the addition of oxidant
Account for the 1-3% of isopentenol polyoxyethylene ether quality.
Again, acrylic acid aqueous solution and chain-transferring agent, the mixed aqueous solution of reducing agent is added dropwise.Specifically, start simultaneously at
Acrylic acid aqueous solution and chain-transferring agent, the mixed aqueous solution of reducing agent is added dropwise.
Wherein, acrylic acid and the mol ratio of isopentenol polyoxyethylene ether are 3.1-7:1, it is a length of during the dropwise addition of its aqueous solution
3 hours.Chain-transferring agent can be using the thio-alcohol water-soluble chain transfer agents such as TGA, mercaptopropionic acid or mercaptoethanol, addition
It is 0.05-1.5% with the mass ratio of isopentenol polyoxyethylene ether.Reducing agent can using ascorbic acid, sodium sulfite, hang it is white
The mixing of one or more in block, ferrous sulfate, addition is 0.06- with the mass ratio of isopentenol polyoxyethylene ether
0.8%.A length of 3.5 hours when chain-transferring agent, the dropwise addition of the mixed aqueous solution of reducing agent.
Afterwards, regulation system pH value, for example, using the aqueous solution regulation system pH value of NaOH to 6-8.
Finally, can also as needed, the regulation that adds water is to required solids content.
It is given below it is several specifically prepare example, be beneficial to and technical scheme be expanded on further.
Embodiment 1
The common running water of 271kg is added in reactor, under agitation, the isoamyl that molecular weight is 2400 is added
Enol APEO (TPEG) 250kg, adds until completely dissolved coagent methacrylic acid 12.5kg.Stir
Afterwards, add 28% hydrogen peroxide 7.4kg, it is 3 DEG C that stirring measures bed material temperature after 10 minutes, start to be added dropwise 40.2kg acrylic acid with
What the aqueous solution acrylic acid and 2.0kg ascorbic acid, 3.75kg TGAs and 50kg running water that 80kg running water is prepared was prepared
Mixed solution, is added dropwise duration and is respectively 3 hours and 3.5 hours, after completion of dropping, is incubated 1 hour, after question response is finished, adopts
It is 7 that 32% sodium hydroxide solution adjusts the pH value of product, and the product of gained is the polycarboxylic acids of ultralow temperature running water production and subtracts
Aqua.
Embodiment 2
The common running water of 820Kg is added in reactor, under agitation, the isoamyl that molecular weight is 2000 is added
Enol APEO 550kg, adds until completely dissolved methacrylic acid 16kg.After stirring, 28% hydrogen peroxide is added
8.25kg, it is 10 DEG C that bed material temperature is measured after stirring 10 minutes, starts to be added dropwise 89.5kg acrylic acid with the preparation of 175kg running water
The mixed solution that aqueous solution acrylic acid and 1.92kg ascorbic acid, 4.4kg TGAs and 115kg running water are prepared, during dropwise addition
It is long to be respectively 3 hours and 3.5 hours, after completion of dropping, 1 hour is incubated, after question response is finished, the NaOH using 32% is molten
It is 6 that liquid adjusts the pH value of product, and the product of gained is the polycarboxylate water-reducer of low temperature running water production.
Embodiment 3
The common running water of 614Kg is added in reactor, under agitation, the isoamyl that molecular weight is 3000 is added
Enol APEO 750kg, adds until completely dissolved methacrylic acid 7.5kg.After stirring, 28% hydrogen peroxide is added
8.8kg, it is 17 DEG C that stirring measures bed material temperature after 10 minutes, starts that the water that 120kg acrylic acid is prepared with 175kg running water is added dropwise
The mixed solution that Solution Propylene acid and 0.5kg ascorbic acid, 0.38kg TGAs and 120kg running water are prepared, is added dropwise duration
Respectively 3 hours and 3.5 hours, after completion of dropping, 1 hour is incubated, after question response is finished, using 32% sodium hydroxide solution
The pH value for adjusting product is 7, and the product of gained is the polycarboxylate water-reducer of tap water at normal temperature production.
Embodiment 4
The common running water of 400Kg is added in reactor, under agitation, the isoamyl that molecular weight is 2400 is added
Enol APEO 400kg, adds until completely dissolved methacrylic acid 8.0kg.After stirring, 28% hydrogen peroxide is added
7.2kg, it is 12 DEG C that bed material temperature is measured after stirring 10 minutes, starts to be added dropwise 37.5kg acrylic acid with the preparation of 175kg running water
The mixed solution that aqueous solution acrylic acid and 1.6kg ascorbic acid, 2.4kg TGAs and 120kg running water are prepared, is added dropwise duration
Respectively 3 hours and 3.5 hours, after completion of dropping, 1 hour is incubated, after question response is finished, using 32% sodium hydroxide solution
The pH value for adjusting product is 7, and the product of gained is the polycarboxylate water-reducer of tap water at normal temperature production.
Embodiment 5
The common running water of 900Kg is added in reactor, under agitation, the isoamyl that molecular weight is 2400 is added
Enol APEO 600kg, adds until completely dissolved methacrylic acid 7.2kg.After stirring, 28% hydrogen peroxide is added
16.8kg, it is 20 DEG C that bed material temperature is measured after stirring 10 minutes, starts to be added dropwise 57.6kg acrylic acid with the preparation of 175kg running water
The mixed solution that aqueous solution acrylic acid and 3.6kg ascorbic acid, 7.2kg TGAs and 115kg running water are prepared, is added dropwise duration
Respectively 3 hours and 3.5 hours, after completion of dropping, 1 hour is incubated, after question response is finished, using 32% sodium hydroxide solution
The pH value for adjusting product is 8, and the product of gained is the polycarboxylate water-reducer of low temperature running water production.
Effect assessment：
1. paste flowing degree evaluation
According to《Methods for testing uniformity of concrete admixture》(GB/t8077-2012) carry out：W/C=0.29, additive
The solid volume of folding is 0.2%, and the product determined prepared by the above embodiment of the present invention is limited with Wuhan Growth hormone secretagogue building materials science and technology share
HGC type water reducers (prior art products) of company's ordinary temperature production carries out paste flowing degree contrasting detection under identical volume, inspection
Survey result as shown in table 1 below：
Table 1：Performance test results
Only it is most representational index to starch to water reducer application performance, by the test data of table 1, it can be seen that
Under identical volume, the present invention prepared by polycarboxylate water-reducer initial paste flowing degree equivalent to or better than prior art produce
Product；Fluidity after 60mim is also preferable, therefore, after technical solution of the present invention, process is simple, reaction controllability is good, is suitable for
Scope is wide, and the application performance of market similar-type products can be also reached in the case where energy consumption is little, even better.
2. concrete evaluation
By GB 8076-2008《Concrete admixture》The match ratio test concrete performance of regulation.Prepare in this experiment
C30 grade concretes, wherein cement are the new PO42.5 of China, and flyash is II grade of ash, and sand (contains for the middle sand that modulus of fineness is 2.8
Mud amount 3.5%), stone is the continuous grading of 5-25mm, and water reducer volume is the 1.0% of gel rubber material consumption.Enter by match ratio
Row experiment：Cement:Flyash：Breeze：Sand：Stone：Water：Additive=220:70:70:787:1043:170:5.76 (unit：
Kg)；Test result is as follows：
Table 2：Concrete performance examination result
The test data of table 2 shows that the polycarboxylate water-reducer of the present invention is compared with the similar-type products of market, and water-reducing rate is suitable,
The concrete function of slump protection of 1 hour is basically identical or slightly good.
Therefore, after using technical solution of the present invention, embodiment process is simple is easy to operate, and reaction is gentle easily-controllable, in low temperature
And normal temperature it is apyrogenic in the case of the product that obtains can reach the application performance of market similar-type products, even more excellent, explanation
The polycarboxylate water-reducer function admirable of the present invention, there is good practical value.
The above, is only presently preferred embodiments of the present invention, and any pro forma restriction is not made to the present invention, this
Art personnel make a little simple modification, equivalent variations or modification using the technology contents of the disclosure above, all fall within this
In bright protection domain.
Claims (10)
1. a kind of preparation method of polycarboxylate water-reducer, it is characterised in that comprise the following steps：
A. isopentenol polyoxyethylene ether is dissolved in running water and forms polyether solutions of the mass concentration for 40-55%；
B. coagent is added, oxidant is stirring evenly and then adding into；
C. acrylic acid aqueous solution and chain-transferring agent, the mixed aqueous solution of reducing agent is added dropwise；
D. regulation system pH value；
Wherein, isopentenol polyoxyethylene ether and acrylic acid mol ratio are 1:3.1-7,
The addition of coagent accounts for the 1-5% of isopentenol polyoxyethylene ether quality,
The addition of chain-transferring agent accounts for the 0.05-1.5% of isopentenol polyoxyethylene ether quality,
The addition of oxidant accounts for the 1-3% of isopentenol polyoxyethylene ether quality,
The addition of reducing agent accounts for the 0.06-0.8% of isopentenol polyoxyethylene ether quality.
2. a kind of preparation method of polycarboxylate water-reducer according to claim 1, it is characterised in that described coagent
For methacrylic acid.
3. the preparation method of a kind of polycarboxylate water-reducer according to claim 1, it is characterised in that described step C is concrete
For：Dropwise addition acrylic acid aqueous solution and chain-transferring agent, the mixed aqueous solution of reducing agent are started simultaneously at, duration is added dropwise and is respectively 3 hours
With 3.5 hours.
4. a kind of preparation method of polycarboxylate water-reducer according to claim 1, it is characterised in that described chain-transferring agent
For thio-alcohol water-soluble chain transfer agent.
5. a kind of preparation method of polycarboxylate water-reducer according to claim 4, it is characterised in that described thio-alcohol water
Dissolubility chain-transferring agent is the one kind in TGA, mercaptopropionic acid or mercaptoethanol.
6. the preparation method of a kind of polycarboxylate water-reducer according to claim 1, it is characterised in that after described step D
Also include step E, as needed, the regulation that adds water is to required solids content.
7. the preparation method of a kind of polycarboxylate water-reducer according to claim 1, it is characterised in that described oxidant is
The mixing of one or more in hydrogen peroxide, ammonium persulfate, sodium peroxydisulfate.
8. the preparation method of a kind of polycarboxylate water-reducer according to claim 1, it is characterised in that described reducing agent is
The mixing of one or more in ascorbic acid, sodium sulfite, sodium formaldehyde sulfoxylate, ferrous sulfate.
9. a kind of preparation method of polycarboxylate water-reducer according to claim 1, it is characterised in that described prenol
The molecular weight of APEO is 2000-3000.
10. the preparation method of a kind of polycarboxylate water-reducer according to claim 1, it is characterised in that described step D is adopted
With the aqueous solution regulation system pH value of NaOH to 6-8.
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| CN109020362A (en) * | 2018-07-26 | 2018-12-18 | 上海石化安东混凝土有限公司 | Ultra-retardation concrete and preparation method thereof |
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