CN103804610B - A kind of preparation method of the high-performance polycarboxylic acids water reducing agent of technique without thermal source - Google Patents
A kind of preparation method of the high-performance polycarboxylic acids water reducing agent of technique without thermal source Download PDFInfo
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- CN103804610B CN103804610B CN201410050035.6A CN201410050035A CN103804610B CN 103804610 B CN103804610 B CN 103804610B CN 201410050035 A CN201410050035 A CN 201410050035A CN 103804610 B CN103804610 B CN 103804610B
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Abstract
The invention discloses the preparation method of the high-performance polycarboxylic acids water reducing agent of a kind of technique without thermal source, comprise the following steps: 1) a certain proportion of unsaturated APEO and water are joined in reactor, stirring makes it dissolve；2) at 5 ~ 30 DEG C, disposably add aqueous oxidizing agent solution, and stir；3) dripping the accelerator of proper proportion and the mixed solution of chain-transferring agent and comonomer respectively, 2 4h drip off, and after completion of dropwise addition, cure 1.5 hours, finally, add alkaline conditioner so that it is neutralize, i.e. obtain described polycarboxylate water-reducer.Preparation method technique of the present invention is simple, and the water reducer low-dosage preparing can have high dispersive property.And use without thermal source technique, decrease the step of heating so that producing easier, cost is lower, more friendly to environment, decreases the consumption to the energy.
Description
Technical field
The invention belongs to the technical field of construction material, particularly relate to the preparation method of the high-performance polycarboxylic acids water reducing agent of a kind of technique without thermal source.
Background technology
As concrete develops to the direction of high performance and multifunction, it is desirable to concrete has high workability, high intensity, a high-durability, and can meet in many application in particular cases.Have ultra-dispersed performance super plasticizer oneself become one of indispensable component in high performance concrete.
In recent years, as country is to further paying attention to of energy-saving and emission-reduction and promoting rapidly of low-carbon economy theory, scientific worker is also concerned with how to reduce its consumption to the energy while striving and improve cement water reducing agent performance.Particularly enterprise, is striving to find the product of low energy consumption, is possible not only to cost-effective, and the trouble that the examination & approval that can reduce boiler bring.
On the other hand, the process producing polycarboxylate water-reducer at present uses the mode of heating mostly, such as uses steam heating, heat-conducting oil heating etc., all can cause environmental pollution.
Content of the invention
The technical problem to be solved is to provide the preparation method of the high-performance polycarboxylic acids water reducing agent of a kind of technique without thermal source, it can overcome problem and shortage present in prior art and production, use without thermal source technique, the high-performance water reducing agent with low-dosage, high water reducing rate, low slump loss can be synthesized.
For solving above-mentioned technical problem, the technical solution of the present invention is:
The preparation method of the high-performance polycarboxylic acids water reducing agent of a kind of technique without thermal source, comprises the following steps:
1) joining in reactor by a certain proportion of unsaturated APEO and water, stirring makes it dissolve；
2) at 5 ~ 30 DEG C, disposably add aqueous oxidizing agent solution, and stir；
3) drip the accelerator (reducing agent) of proper proportion and the mixed solution of chain-transferring agent and comonomer respectively, after completion of dropwise addition, cure 1.5 hours, finally, add alkaline conditioner so that it is neutralize, i.e. obtain described polycarboxylate water-reducer.
The raw-material mass fraction of above-mentioned reaction is:
Unsaturated APEO: 100-250；
The consumption of water: the consumption of the unsaturated APEO of 1.0-2.0 times；
Comonomer: 10-50；
Oxidant: 0.1-5；
Accelerator: 0.1-5；
Chain-transferring agent: 0.1-5；
Alkaline conditioner: 10-40.
Described unsaturated APEO is allyl polyethenoxy ether, methyl allyl polyoxyethylene ether or isopentene group APEO.
Described oxidant is hydrogen peroxide, persulfate or water-soluble azo class oxidant.
Described persulfate is potassium peroxydisulfate, sodium peroxydisulfate or ammonium persulfate.
Described water-soluble azo class oxidant is azo diisobutyl amidine hydrochloride, azo two isobutyl imidazoline hydrochloride or azo dicyano valeric acid.
Described accelerator is sodium hypophosphite, L-AA, sodium hydrogensulfite, ferrous sulfate, sodium thiosulfate, sodium formaldehyde sulfoxylate or maleficent acid.
Described chain-transferring agent is 2-TGA, 3-mercaptopropionic acid, methylpropene sodium sulfonate, mercapto succinic acid or 2 mercapto ethanol.
Described comonomer is 2 kinds in acrylic acid, methacrylic acid, itaconic acid, maleic acid, crotonic acid, citric acid, methyl acrylate, ethyl acrylate, butyl acrylate, vinylacetate, hydroxy-ethyl acrylate or hydroxypropyl acrylate or two or more combination.
Described alkaline conditioner is NaOH, Strong oxdiative potassium, calcium hydroxide, ammoniacal liquor, sodium metasilicate or monoethanolamine, and the addition of this alkaline conditioner is 6-7 to make the pH value of solution.
Using after such scheme, the present invention has following effective effect:
1. preparation method of the present invention uses one-step synthesis method, condition is easily controlled, stable performance, production does not needs heating, it is the technique of a kind of environmental protection, it is easy to industrialized production, technique is simple, mainly uses highly active oxidant, and carries out copolyreaction by introducing multiple monomer, its molecular structure is comb-type structure, main chain contains polar group, side chain contains the become space obstacle of polyethylene oxide base segment, be conducive to improving the dispersiveness of cement and dispersiveness holding capacity, embody low-dosage polymolecularity, the advantage such as high-collapse-retentivity.
2. preparation method of the present invention uses the redox system trigger monomer of low-activation energy to carry out copolymerization, it is polymerizable at normal temperatures, suitable reaction temperature is in the range of 5 ~ 30 DEG C, it is achieved that the industrialized production without thermal source of product, simplifies production equipment, the production cost reducing, and the redox system efficiency of initiation of low-activation energy is high, improve reactivity, reduce the residual quantity of monomer, the conversion ratio making product is high, and is effectively controlled the generation of high temperature secondary reaction.Therefore, the product obtaining has higher dispersive property.
In a word, present invention employs without thermal source technique, decrease the step of heating so that producing easier, cost is lower, more friendly to environment, decreases the consumption to the energy.
Detailed description of the invention
Below in conjunction with specific embodiment, the invention will be further described.Following number refers both to mass fraction.
Embodiment
1
1) joining in reactor by the allyl polyethenoxy ether of 100 parts and the water of 150 parts, stirring makes it dissolve；
2) at 5 ~ 30 DEG C, the disposable ammonium persulfate (also can substitute with sodium peroxydisulfate or potassium peroxydisulfate) adding 2 parts, stirs half an hour；
3) methyl acrylate (this methyl acrylate also can be by ethyl acrylate or the butyl acrylate replacement) mixed solution of the sodium hypophosphite of 2 parts and 2-TGA (this 2-TGA also can be substituted by the 3-mercaptopropionic acid) mixed solution of 1 part and the acrylic acid (this acrylic acid also can be substituted by methacrylic acid or itaconic acid) of 10 parts and 5 parts is dripped respectively, 3h drips off, cure 1.5 hours, finally, add sodium hydroxide solution (the also available hydrogen potassium oxide of 20 parts, calcium hydroxide, ammoniacal liquor, sodium metasilicate or monoethanolamine substitute), make it neutralize, i.e. can get high-performance poly carboxylic acid mother liquor.
Embodiment
2
1) joining in reactor by the methyl allyl polyoxyethylene ether of 150 parts and the water of 225 parts, stirring makes it dissolve；
2) at 5 ~ 30 DEG C, the disposable hydrogen peroxide adding 3 parts, stirs half an hour；
3) hydroxy-ethyl acrylate (this hydroxy-ethyl acrylate also can be substituted by the hydroxypropyl acrylate) mixed solution of the sodium hydrogensulfite (this sodium hydrogensulfite also can be substituted by sodium formaldehyde sulfoxylate) of 1 part and the mercapto succinic acid mixed solution of 1 part and the maleic acid of 30 parts and 5 parts is dripped respectively, 2h drips off, cure 1.5 hours, finally, add the sodium hydroxide solution of 30 parts, make it neutralize, i.e. can get high-performance poly carboxylic acid mother liquor.
Embodiment
3
1) joining in reactor by the isopentene group APEO of 200 parts and the water of 300 parts, stirring makes it dissolve；
2) at 5 ~ 30 DEG C, the disposable azo two isobutyl imidazoline hydrochloride (azo diisobutyl amidine hydrochloride or azo dicyano valeric acid also can be used to substitute) adding 0.5 part, stirs half an hour；
3) the hydroxy-ethyl acrylate mixed solution of the sodium thiosulfate (this sodium thiosulfate also can be substituted by L-AA or ferrous sulfate) of 1 part and the mercapto succinic acid mixed solution of 1 part and the crotonic acid of 30 parts and 5 parts is dripped respectively, 2h drips off, cure 1.5 hours, finally, add the sodium hydroxide solution of 35 parts, make it neutralize, i.e. can get high-performance poly carboxylic acid mother liquor.
Embodiment
4
1) joining in reactor by the methyl allyl polyoxyethylene ether of 250 parts and the water of 375 parts, stirring makes it dissolve；
2) at 5 ~ 30 DEG C, the disposable ammonium persulfate adding 2.5 parts, stirs half an hour；
3) the vinylacetate mixed solution of the maleficent acid of 1.2 parts and 2 mercapto ethanol (this 2 mercapto ethanol also can be substituted by the methylpropene sodium sulfonate) mixed solution of 1 part and the citric acid of 50 parts and 5 parts is dripped respectively, 4h drips off, cure 1.5 hours, finally, add the sodium hydroxide solution of 40 parts, make it neutralize, i.e. can get high-performance poly carboxylic acid mother liquor.
Comparative example
1
1) methyl allyl polyoxyethylene ether of 200 parts and the water of 200 parts are joined in reactor, open mixer, and temperature is risen to 60 DEG C；
2) dripping 3 parts of hydrogen peroxide solutions, the 3-mercaptopropionic acid mixed solution of the L-AA of 1 part and 1 part and the acrylic acid solution of 25 parts respectively, 3h drips off, cure 1 hour, finally, add the sodium hydroxide solution of 20 parts, make it neutralize, i.e. can get high-performance poly carboxylic acid mother liquor.
Embodiment 1 ~ 4 and comparative example 1 being synthesized the sample obtaining, using standard cement, volume presses cement quality 0.3%, according to GB 8076-2008 " concrete admixture ", survey its concrete water-reducing ratio, the slump and through when slump-loss.Concrete mix is: cement 360kg/m3, sand 803kg/m3, stone 982 kg/m3, the slump controls at 210 ± 10mm, and acquired results is as shown in table 1.
| Sample | Comparative example 1 | Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 |
| Water-reducing rate/% | 28 | 32 | 34 | 33 | 35 |
| Slump T0 | 200 | 210 | 215 | 210 | 220 |
| Through when slump T1h | 150 | 195 | 200 | 205 | 205 |
| 28d compressive strength rate/%, is not less than | 125 | 140 | 145 | 140 | 145 |
The above, be only presently preferred embodiments of the present invention, not impose any restrictions the technical scope of the present invention, therefore the change that in every case claim under this invention and specification are done or modification, all should belong to patent of the present invention within the scope of cover.
Claims (8)
1. the preparation method of the high-performance polycarboxylic acids water reducing agent without thermal source technique, it is characterised in that comprise the following steps:
1) it by mass fraction is:
Unsaturated APEO: 100-250；
The consumption of water: the consumption of the unsaturated APEO of 1.0-2.0 times；
Comonomer: 10-50；
Oxidant: 0.1-5；
Accelerator: 0.1-5；
Chain-transferring agent: 0.1-5；
Alkaline conditioner: 10-40
Reaction raw material join in reactor, stirring make it dissolve；
2) at 5 ~ 30 DEG C, disposably add aqueous oxidizing agent solution, and stir；Described oxidant is hydrogen peroxide, persulfate or water-soluble azo class oxidant；
3) dripping the accelerator of proper proportion and the mixed solution of chain-transferring agent and comonomer respectively, 2-4h drips off, and after completion of dropwise addition, cures 1.5 hours, finally, adds alkaline conditioner so that it is neutralize, i.e. obtain described polycarboxylate water-reducer.
2. the preparation method of the high-performance polycarboxylic acids water reducing agent of a kind of technique without thermal source according to claim 1, it is characterized in that: in step 1), described unsaturated APEO is allyl polyethenoxy ether, methyl allyl polyoxyethylene ether or isopentene group APEO.
3. the preparation method of the high-performance polycarboxylic acids water reducing agent of a kind of technique without thermal source according to claim 1, it is characterised in that: described step 2) in persulfate be potassium peroxydisulfate, sodium peroxydisulfate or ammonium persulfate.
4. the preparation method of the high-performance polycarboxylic acids water reducing agent of a kind of technique without thermal source according to claim 1, it is characterised in that: described step 2) in water-soluble azo class oxidant be azo diisobutyl amidine hydrochloride, azo two isobutyl imidazoline hydrochloride or azo dicyano valeric acid.
5. the preparation method of the high-performance polycarboxylic acids water reducing agent of a kind of technique without thermal source according to claim 1, it is characterized in that: in step 3), described accelerator is sodium hypophosphite, L-AA, sodium hydrogensulfite, ferrous sulfate, sodium thiosulfate, sodium formaldehyde sulfoxylate or maleficent acid.
6. the preparation method of the high-performance polycarboxylic acids water reducing agent of a kind of technique without thermal source according to claim 1, it is characterized in that: in step 3), described chain-transferring agent is 2-TGA, 3-mercaptopropionic acid, methylpropene sodium sulfonate, mercapto succinic acid or 2 mercapto ethanol.
7. the preparation method of the high-performance polycarboxylic acids water reducing agent of a kind of technique without thermal source according to claim 1, it is characterized in that: in step 3), described comonomer is 2 kinds in acrylic acid, methacrylic acid, itaconic acid, maleic acid, crotonic acid, citric acid, methyl acrylate, ethyl acrylate, butyl acrylate, vinylacetate, hydroxy-ethyl acrylate or hydroxypropyl acrylate or two or more combination.
8. the preparation method of the high-performance polycarboxylic acids water reducing agent of a kind of technique without thermal source according to claim 1, it is characterized in that: in step 3), described alkaline conditioner is NaOH, potassium hydroxide, calcium hydroxide, ammoniacal liquor, sodium metasilicate or monoethanolamine, and the addition of this alkaline conditioner is to make the pH value of solution be 6-7.
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