CN105820298A - Photo-initiation type polycarboxylic acid water reducing agent and preparation method thereof - Google Patents
Photo-initiation type polycarboxylic acid water reducing agent and preparation method thereof Download PDFInfo
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- CN105820298A CN105820298A CN201610225940.XA CN201610225940A CN105820298A CN 105820298 A CN105820298 A CN 105820298A CN 201610225940 A CN201610225940 A CN 201610225940A CN 105820298 A CN105820298 A CN 105820298A
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- Prior art keywords
- light
- reducer
- polycarboxylate water
- light trigger
- type polycarboxylate
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- 239000003638 chemical reducing agent Substances 0.000 title claims abstract description 28
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 28
- 238000002360 preparation method Methods 0.000 title abstract description 9
- 239000002253 acid Substances 0.000 title abstract 3
- 238000006243 chemical reaction Methods 0.000 claims abstract description 23
- 230000032683 aging Effects 0.000 claims abstract description 13
- 238000000034 method Methods 0.000 claims abstract description 10
- 229920000570 polyether Polymers 0.000 claims abstract description 9
- 239000004721 Polyphenylene oxide Substances 0.000 claims abstract description 8
- 239000000178 monomer Substances 0.000 claims abstract 4
- 229920005646 polycarboxylate Polymers 0.000 claims description 21
- 239000008367 deionised water Substances 0.000 claims description 19
- 229910021641 deionized water Inorganic materials 0.000 claims description 19
- 229920000056 polyoxyethylene ether Polymers 0.000 claims description 19
- 229940051841 polyoxyethylene ether Drugs 0.000 claims description 19
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims description 16
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 15
- DKIDEFUBRARXTE-UHFFFAOYSA-N 3-mercaptopropanoic acid Chemical compound OC(=O)CCS DKIDEFUBRARXTE-UHFFFAOYSA-N 0.000 claims description 14
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 claims description 13
- QVDTXNVYSHVCGW-ONEGZZNKSA-N isopentenol Chemical compound CC(C)\C=C\O QVDTXNVYSHVCGW-ONEGZZNKSA-N 0.000 claims description 13
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 12
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 10
- OMIGHNLMNHATMP-UHFFFAOYSA-N 2-hydroxyethyl prop-2-enoate Chemical compound OCCOC(=O)C=C OMIGHNLMNHATMP-UHFFFAOYSA-N 0.000 claims description 9
- FPYJFEHAWHCUMM-UHFFFAOYSA-N maleic anhydride Chemical compound O=C1OC(=O)C=C1 FPYJFEHAWHCUMM-UHFFFAOYSA-N 0.000 claims description 9
- 125000003903 2-propenyl group Chemical group [H]C([*])([H])C([H])=C([H])[H] 0.000 claims description 6
- HRPVXLWXLXDGHG-UHFFFAOYSA-N Acrylamide Chemical compound NC(=O)C=C HRPVXLWXLXDGHG-UHFFFAOYSA-N 0.000 claims description 6
- CERQOIWHTDAKMF-UHFFFAOYSA-N Methacrylic acid Chemical compound CC(=C)C(O)=O CERQOIWHTDAKMF-UHFFFAOYSA-N 0.000 claims description 6
- DNJIEGIFACGWOD-UHFFFAOYSA-N ethyl mercaptane Natural products CCS DNJIEGIFACGWOD-UHFFFAOYSA-N 0.000 claims description 6
- DGVVWUTYPXICAM-UHFFFAOYSA-N β‐Mercaptoethanol Chemical compound OCCS DGVVWUTYPXICAM-UHFFFAOYSA-N 0.000 claims description 6
- QZPSOSOOLFHYRR-UHFFFAOYSA-N 3-hydroxypropyl prop-2-enoate Chemical compound OCCCOC(=O)C=C QZPSOSOOLFHYRR-UHFFFAOYSA-N 0.000 claims description 5
- 239000003513 alkali Substances 0.000 claims description 4
- 150000001875 compounds Chemical class 0.000 claims description 4
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical compound OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 claims description 3
- 239000003795 chemical substances by application Substances 0.000 claims description 3
- 239000002994 raw material Substances 0.000 claims description 2
- 235000003642 hunger Nutrition 0.000 claims 1
- 238000004519 manufacturing process Methods 0.000 abstract description 8
- 239000000203 mixture Substances 0.000 abstract description 5
- 238000005265 energy consumption Methods 0.000 abstract description 3
- 239000003607 modifier Substances 0.000 abstract 1
- 230000003472 neutralizing effect Effects 0.000 abstract 1
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 15
- 238000003756 stirring Methods 0.000 description 15
- 239000013068 control sample Substances 0.000 description 12
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 description 5
- 229960005070 ascorbic acid Drugs 0.000 description 5
- 239000000463 material Substances 0.000 description 5
- 230000003287 optical effect Effects 0.000 description 5
- GGZZISOUXJHYOY-UHFFFAOYSA-N 8-amino-4-hydroxynaphthalene-2-sulfonic acid Chemical compound C1=C(S(O)(=O)=O)C=C2C(N)=CC=CC2=C1O GGZZISOUXJHYOY-UHFFFAOYSA-N 0.000 description 4
- 230000000630 rising effect Effects 0.000 description 4
- 235000011121 sodium hydroxide Nutrition 0.000 description 4
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 3
- 238000011161 development Methods 0.000 description 3
- 230000018109 developmental process Effects 0.000 description 3
- 230000000977 initiatory effect Effects 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 238000007254 oxidation reaction Methods 0.000 description 3
- 150000003254 radicals Chemical class 0.000 description 3
- HZAXFHJVJLSVMW-UHFFFAOYSA-N 2-Aminoethan-1-ol Chemical compound NCCO HZAXFHJVJLSVMW-UHFFFAOYSA-N 0.000 description 2
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 2
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 2
- 238000007334 copolymerization reaction Methods 0.000 description 2
- BPMFZUMJYQTVII-UHFFFAOYSA-N guanidinoacetic acid Chemical compound NC(=N)NCC(O)=O BPMFZUMJYQTVII-UHFFFAOYSA-N 0.000 description 2
- 239000003999 initiator Substances 0.000 description 2
- 229910052700 potassium Inorganic materials 0.000 description 2
- 239000011591 potassium Substances 0.000 description 2
- 239000012966 redox initiator Substances 0.000 description 2
- 239000000523 sample Substances 0.000 description 2
- 229910052708 sodium Inorganic materials 0.000 description 2
- 239000011734 sodium Substances 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- BKOOMYPCSUNDGP-UHFFFAOYSA-N 2-methylbut-2-ene Chemical group CC=C(C)C BKOOMYPCSUNDGP-UHFFFAOYSA-N 0.000 description 1
- AMULJSVDIHMAOX-UHFFFAOYSA-N 3-hydroxypropyl prop-2-enoate;prop-2-enoic acid Chemical compound OC(=O)C=C.OCCCOC(=O)C=C AMULJSVDIHMAOX-UHFFFAOYSA-N 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- OFOBLEOULBTSOW-UHFFFAOYSA-N Propanedioic acid Natural products OC(=O)CC(O)=O OFOBLEOULBTSOW-UHFFFAOYSA-N 0.000 description 1
- 150000008065 acid anhydrides Chemical class 0.000 description 1
- 230000004913 activation Effects 0.000 description 1
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium peroxydisulfate Substances [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 description 1
- VAZSKTXWXKYQJF-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)OOS([O-])=O VAZSKTXWXKYQJF-UHFFFAOYSA-N 0.000 description 1
- 229910001870 ammonium persulfate Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 150000001732 carboxylic acid derivatives Chemical class 0.000 description 1
- 150000001735 carboxylic acids Chemical class 0.000 description 1
- 239000004568 cement Substances 0.000 description 1
- 230000008602 contraction Effects 0.000 description 1
- 238000004132 cross linking Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 1
- VZCYOOQTPOCHFL-UPHRSURJSA-N maleic acid Chemical compound OC(=O)\C=C/C(O)=O VZCYOOQTPOCHFL-UPHRSURJSA-N 0.000 description 1
- 239000011976 maleic acid Substances 0.000 description 1
- 239000007800 oxidant agent Substances 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 150000002978 peroxides Chemical class 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- PXQLVRUNWNTZOS-UHFFFAOYSA-N sulfanyl Chemical class [SH] PXQLVRUNWNTZOS-UHFFFAOYSA-N 0.000 description 1
- 238000010189 synthetic method Methods 0.000 description 1
- 238000004227 thermal cracking Methods 0.000 description 1
- VZCYOOQTPOCHFL-UHFFFAOYSA-N trans-butenedioic acid Natural products OC(=O)C=CC(O)=O VZCYOOQTPOCHFL-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- 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
- C04B24/2641—Polyacrylates; Polymethacrylates
- C04B24/2647—Polyacrylates; Polymethacrylates 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
- C08F2/00—Processes of polymerisation
- C08F2/46—Polymerisation initiated by wave energy or particle radiation
- C08F2/48—Polymerisation initiated by wave energy or particle radiation by ultraviolet or visible light
-
- 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
Abstract
The invention relates to a photo-initiation type polycarboxylic acid water reducing agent and a preparation method thereof. The preparation method comprises the following steps: dissolving the following components into water in parts by weight: 72 to 90 parts of a big polyether monomer, 10 to 27 parts of an unsaturated poly-monomer, 0.2 to 0.9 part of a molecular weight modifier and 0.3 to 1.0 part of a photoinitiator, so as to obtain a mixed monomer solution; continuously performing ultraviolet irradiation on the mixture in a photo-initiation reactor, then performing aging reaction in a reaction kettle for 0.2 to 2 h, and neutralizing to reach the PH of 6.5 to 7.5 so as to obtain a finished product. The preparation method can be carried out under room temperature, and even low temperature, so that the energy consumption is low; the reaction is fast, and the production efficiency is high; the whole reaction process is short in time. The process method is simple and is easy to operate, and the production efficiency of the polycarboxylic acid water reducing agent can be greatly improved, so that the product has higher market competitiveness.
Description
Technical field
The present invention relates to a kind of cement concrete poly carboxylic acid series water reducer and preparation method thereof, be related specifically to one
Plant light-initiated type polycarboxylate water-reducer and preparation method thereof.
Technical background
Polycarboxylate water-reducer is low with its volume, water-reducing rate is high, the mobility of fresh concrete and retentivity good, low
The performance that contraction, environmental friendliness etc. are excellent, it has also become studied in recent years or even from now on and the emphasis of application and development.
The research and development of domestic polycarboxylate water-reducer and production application all achieve bigger development, and product is also by relatively
Single progressively moves towards multi items, multifunction, multi-level development.
Polycarboxylate water-reducer product in the market mainly uses thermal cracking and the oxidoreduction of peroxide
System discharges free radical, the activity of the reaction of initiation reaction system.CN00127294.2 describes a kind of poly-
Carboxylic acids graft type high-performance water reducing agent and synthetic method thereof, it is with Ammonium persulfate. as initiator, at 90 DEG C
Copolymerization and obtain.CN101215120A describes the preparation method of a kind of polycarboxylate dehydragent, and reaction uses
Initiation method is redox initiation, and initiator has Oxidizing and Reducing Agents to constitute, copolymerization by the way of dropping
Obtain product.Document report is all by heat or to add reducing agent as exciting agent, complex manufacturing, reaction
With duration, production efficiency is low, and energy consumption is high.
Summary of the invention
The invention aims to improve the deficiencies in the prior art and provide light-initiated type polycarboxylate water-reducer,
Present invention also offers the preparation method of above-mentioned light-initiated type polycarboxylate water-reducer, the method room temperature, simplicity, fast
Speed, instead of the redox system initiator system as reaction using light trigger, and efficiency of initiation is improved,
Can effectively improve the production efficiency of polycarboxylate water-reducer product.
The technical scheme is that a kind of light-initiated type polycarboxylate water-reducer, it is characterised in that its raw material components
And the mass parts of each component is respectively as follows:
Polyether macromonomer: 72-90 part；
Unsaturated comonomer: 10-27 part；
Molecular weight regulator: 0.2-0.9 part；
Light trigger: 0.3-1.0 part.
The most above-mentioned polyether macromonomer is allyl polyethenoxy ether, metering system polyoxyethylene ether or iso-amylene
One or more in polyoxyethylenated alcohol；The molecular weight of polyether macromonomer is 1200-5000.
The most above-mentioned unsaturated comonomer is acrylic acid, methacrylic acid, acrylamide, maleic acid
One or more in acid anhydride, 2-(Acryloyloxy)ethanol or Hydroxypropyl acrylate.
The most above-mentioned molecular weight regulator is the one in TGA, mercaptopropionic acid or mercaptoethanol or two
Kind.
The most above-mentioned light trigger is water-soluble light trigger, including light trigger-184, light trigger
-1105, light trigger-DETX, light trigger-2959, light trigger-QTX or light trigger-HBP.
Present invention also offers the method preparing above-mentioned light-initiated type polycarboxylate water-reducer, its concrete steps are such as
Under:
(1) according to proportioning weigh polyether macromonomer, unsaturated comonomer, light trigger, molecular weight regulator and
Deionized water, puts in reactor, dissolves, obtain compound；
(2) compound is in Photoinitiated reactions device, by continuous print ultraviolet light irradiate after, the most aging instead
Answering 0.2-2h, add alkali being neutralized to PH is 6.5-7.5, obtains light-initiated type polycarboxylate water-reducer.
The mass concentration of the most preparation-obtained light-initiated type polycarboxylate water-reducer is 30-70%.
Wave-length coverage 150-600nm of the most above-mentioned ultraviolet light, the intensity of ultraviolet light is 10-20mj/cm2；
Ultraviolet light irradiation time is 3-10 minute.
The most above-mentioned alkali is sodium hydroxide, potassium hydroxide or triethanolamine.
Beneficial effect:
Prior art is all by heat or to add reducing agent as exciting agent, and the present invention is by uviol lamp light emission
Ultraviolet photon, thus cause polymerization crosslinking and graft reaction, there is the advantage of following several respects in it: 1, produces
Free radical speed is fast；2, free radical is evenly distributed in the solution, obtains molecular weight distribution narrower, and is prone to control
System；3, without Dropping feeder, production technology is simple；4, the reaction used time is short, improves production efficiency；5, draw
Sending out activation energy low, energy consumption is low, meets the policy of energy-saving and emission-reduction.
Detailed description of the invention
Below by embodiment, technical solution of the present invention is described in further detail.
Embodiment 1
Isopentenol polyoxyethylene ether (molecular weight 2400): 85 parts
Acrylic acid: 13 parts
Mercaptopropionic acid: 0.6 part
Light trigger-2959:0.7 part
Deionized water: 60 parts
At room temperature, water, isopentenol polyoxyethylene ether, acrylic acid, mercaptopropionic acid, light trigger-2959,
Add in Photoinitiated reactions still, stirring and dissolving, mix homogeneously；Opening ultra violet lamp, optical frequency is at 275-350nm
Consecutive variations, light intensity 15mj/cm2, irradiate 5min, aging 1 hour, hydro-oxidation sodium was neutralized to pH=6.5,
Being product, mass concentration concentration is 60%.
Control sample 1
Isopentenol polyoxyethylene ether (molecular weight 2400): 85 parts
Acrylic acid: 13 parts
Mercaptopropionic acid: 0.6 part
Hydrogen peroxide: 0.84 part
Vitamin c: 0.25 part
Deionized water: 60 parts
In four-hole bottle, add isopentenol polyoxyethylene ether and deionized water, start to stir rising temperature for dissolving.Temperature
Reach 50 DEG C, add H2O2, after stirring 10min, start in flask, drip mercaptopropionic acid, Vc molten
Liquid M and acrylic acid solution N, was added dropwise to complete respectively within 3.5h and the 3h time.After M material adds,
At 60 DEG C of aging 1h.Reaction terminates, and treats that temperature is down to less than 40 DEG C, and the liquid caustic soda adding sodium hydroxide is adjusted to
PH value is 6.5, obtains control sample 1.
Embodiment 2
Allyl polyethenoxy ether (molecular weight 1200): 72 parts
Acrylic acid: 15 parts
Maleic anhydride: 12 parts
TGA: 0.7 part
Light trigger-QTX:0.4 part
Deionized water: 35 parts
At room temperature, deionized water, allyl polyethenoxy ether, acrylic acid, maleic anhydride, sulfydryl
Acetic acid, light trigger-QTX, add in Photoinitiated reactions still, stirring and dissolving, mix homogeneously；Open ultraviolet
Light irradiation, optical frequency is at 200-400nm consecutive variations, 20mj/cm2, irradiate 4min, aging 2 hours, add
Potassium hydroxide is neutralized to pH=7, is product, and mass concentration is 70%.
Control sample 2
Allyl polyethenoxy ether (molecular weight 1200): 70 parts
Acrylic acid: 15 parts
Maleic anhydride: 12 parts
TGA: 0.7 part
Hydrogen peroxide: 1.1 parts
Vitamin c: 0.42 part
Deionized water: 35 parts
In four-hole bottle, add allyl polyethenoxy ether, maleic anhydride and deionized water, start stirring and rise
Temperature is dissolved.Temperature reaches 60 DEG C, adds H2O2, after stirring 10min, start to drip mercapto in flask
Guanidine-acetic acid, Vc solution M and acrylic acid solution N, be added dropwise to complete respectively within 3.5h and the 3h time.
After M material adds, at 65 DEG C of aging 1h.Reaction terminates, and treats that temperature is down to less than 40 DEG C, adds hydroxide
It is 7 that potassium is adjusted to pH value, obtains control sample 2.
Embodiment 3
Methyl allyl polyoxyethylene ether (molecular weight 2900): 80
Methacrylic acid: 8
2-(Acryloyloxy)ethanol: 12
Mercaptopropionic acid: 0.4
Light trigger-HBP:0.6
Deionized water: 100
At 5 DEG C, deionized water, methyl allyl polyoxyethylene ether, methacrylic acid, acrylic acid hydroxyl
Ethyl ester, mercaptopropionic acid, light trigger-HBP, add in Photoinitiated reactions still, stirring and dissolving, mix homogeneously；
Opening ultra violet lamp, optical frequency is at 350-550nm consecutive variations, 12mj/cm2, irradiation 8min, aging 0.5
Hour, hydro-oxidation sodium is neutralized to pH=7.5, is product, and its mass concentration is 50%.
Control sample 3
Methyl allyl polyoxyethylene ether (molecular weight 2900): 80
Methacrylic acid: 8
2-(Acryloyloxy)ethanol: 12
Mercaptopropionic acid: 0.4
Hydrogen peroxide: 0.4 part
Vitamin c: 0.12 part
Deionized water: 100
In four-hole bottle, add methyl allyl polyoxyethylene ether and deionized water, start to stir rising temperature for dissolving.Temperature
Degree reaches 35 DEG C, adds H2O2, after stirring 10min, start to drip mercaptopropionic acid, Vc in flask
Solution M and methacrylic acid, 2-(Acryloyloxy)ethanol solution N, dripped respectively within 3.5h and the 3h time
Add.After M material adds, at 48 DEG C of aging 1h.Reaction terminates, and treats that temperature is down to less than 40 DEG C, adds
Enter sodium hydroxide being adjusted to pH value is 7.5, obtains control sample 3.
Embodiment 4
Isopentenol polyoxyethylene ether (molecular weight 5000): 87
Acrylamide: 3
Maleic anhydride: 13
Mercaptoethanol: 0.8
Light trigger-184:1.0
Deionized water: 150
At room temperature, deionized water, isopentenol polyoxyethylene ether, acrylamide, maleic anhydride,
Mercaptoethanol, light trigger-184, add in Photoinitiated reactions still, stirring and dissolving, mix homogeneously；Open purple
Outer light irradiation, optical frequency is at 200-325nm consecutive variations, 10mj/cm2, irradiation 9min, aging 1 hour,
Add triethanolamine and be neutralized to pH=6.8, be product, its mass concentration 40%.
Control sample 4
Isopentenol polyoxyethylene ether (molecular weight 5000): 87
Acrylamide: 3
Maleic anhydride: 13
Mercaptoethanol: 0.8
Hydrogen peroxide: 0.4 part
Vitamin c: 0.12 part
Deionized water: 150
In four-hole bottle, add isopentenol polyoxyethylene ether, maleic anhydride and deionized water, start stirring
Rising temperature for dissolving.Temperature reaches 50 DEG C, adds H2O2, after stirring 10min, start to drip in flask
Mercaptoethanol, Vc solution M and acrylamide solution N, dripped respectively within 3.5h and the 3h time
Become.After M material adds, at 60 DEG C of aging 1h.Reaction terminates, and treats that temperature is down to less than 40 DEG C, adds three
It is 6.8 that ethanolamine is adjusted to pH value, obtains control sample 4.
Embodiment 5
Isopentenol polyoxyethylene ether (molecular weight 1200): 75
Acrylic acid: 4
2-(Acryloyloxy)ethanol: 9.5
Hydroxypropyl acrylate: 11.5
Mercaptopropionic acid: 0.7
Light trigger-DETX:0.75
Water: 82
At 10 DEG C, water, isopentenol polyoxyethylene ether, acrylic acid, 2-(Acryloyloxy)ethanol, acrylic acid
Hydroxypropyl acrylate, mercaptopropionic acid, light trigger-DETX, add in Photoinitiated reactions still, stirring and dissolving, and mixing is all
Even；Opening ultra violet lamp, optical frequency is at 300-500nm consecutive variations, 13.5mj/cm2, irradiate 5min,
Aging 2 hours, hydro-oxidation potassium was neutralized to pH=7.5, is product, its mass concentration 55%.
Control sample 5
Isopentenol polyoxyethylene ether (molecular weight 1200): 75
Acrylic acid: 6
2-(Acryloyloxy)ethanol: 10.5
Hydroxypropyl acrylate: 12.5
Mercaptopropionic acid: 0.7
Hydrogen peroxide: 0.4 part
Vitamin c: 0.12 part
Deionized water: 82
In four-hole bottle, add isopentenol polyoxyethylene ether and deionized water, start to stir rising temperature for dissolving.Temperature
Reach 40 DEG C, add H2O2, after stirring 10min, start in flask, drip mercaptopropionic acid, Vc molten
Liquid M and acrylic acid, 2-(Acryloyloxy)ethanol, Hydroxypropyl acrylate solution N, respectively when 3.5h and 3h
In be added dropwise to complete.After M material adds, at 50 DEG C of aging 1h.Reaction terminates, treat temperature be down to 40 DEG C with
Under, add potassium hydroxide being adjusted to pH value is 7.5, obtains control sample 5.
Paste flowing degree is tested: with reference to GB8077-2000 " Methods for testing uniformity of concrete admixture ", right
Embodiment 1 carries out paste flowing degree test, W/C to embodiment 5 gained sample and control sample 1 to control sample 5
It is 0.29.
The paste flowing degree of the different sample of table 1 and gradual loss
Claims (9)
1. a light-initiated type polycarboxylate water-reducer, it is characterised in that its raw material components and the mass parts of each component
It is respectively as follows:
Polyether macromonomer: 72-90 part；
Unsaturated comonomer: 10-27 part；
Molecular weight regulator: 0.2-0.9 part；
Light trigger: 0.3-1.0 part.
Light-initiated type polycarboxylate water-reducer the most according to claim 1, it is characterised in that described polyethers
Polymeric monomer is in allyl polyethenoxy ether, metering system polyoxyethylene ether or isopentenol polyoxyethylene ether
Plant or multiple；The molecular weight of polyether macromonomer is 1200-5000.
Light-initiated type polycarboxylate water-reducer the most according to claim 1, it is characterised in that described insatiable hunger
With comonomer be acrylic acid, methacrylic acid, acrylamide, maleic anhydride, 2-(Acryloyloxy)ethanol or
One or more in Hydroxypropyl acrylate.
Light-initiated type polycarboxylate water-reducer the most according to claim 1, it is characterised in that described molecule
Amount regulator is one or both in TGA, mercaptopropionic acid or mercaptoethanol.
Light-initiated type polycarboxylate water-reducer the most according to claim 1, it is characterised in that described light draws
Send out agent be water-soluble light trigger, including light trigger-184, light trigger-1105, light trigger-DETX,
Light trigger-2959, light trigger-QTX or light trigger-HBP.
6. the method preparing light-initiated type polycarboxylate water-reducer as claimed in claim 1, its concrete steps
As follows:
(1) according to proportioning weigh polyether macromonomer, unsaturated comonomer, light trigger, molecular weight regulator and
Deionized water, puts in reactor, dissolves, obtain compound；
(2) compound is in Photoinitiated reactions device, by continuous print ultraviolet light irradiate after, the most aging instead
Answering 0.2-2h, add alkali being neutralized to PH is 6.5-7.5, obtains light-initiated type polycarboxylate water-reducer.
Method the most according to claim 1, it is characterised in that the quality of light-initiated type polycarboxylate water-reducer
Concentration is 30-70%.
Method the most according to claim 1, it is characterised in that the wave-length coverage of described ultraviolet light
150-600nm, the intensity of ultraviolet light is 10-20mj/cm2；Ultraviolet light irradiation time is 3-10 minute.
Method the most according to claim 1, it is characterised in that described alkali is sodium hydroxide, hydroxide
Potassium or triethanolamine.
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| CN107759742A (en) * | 2016-08-15 | 2018-03-06 | 上海东大化学有限公司 | A kind of polycarboxylate water-reducer and preparation method thereof and application method |
| CN108084363A (en) * | 2017-12-28 | 2018-05-29 | 科之杰新材料集团有限公司 | A kind of preparation method of reinforcing type polycarboxylic acid water-reducing agent |
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| CN107759742A (en) * | 2016-08-15 | 2018-03-06 | 上海东大化学有限公司 | A kind of polycarboxylate water-reducer and preparation method thereof and application method |
| CN107759742B (en) * | 2016-08-15 | 2019-10-01 | 上海东大化学有限公司 | A kind of polycarboxylate water-reducer and preparation method thereof and application method |
| CN106317402A (en) * | 2016-08-19 | 2017-01-11 | 浙江皇马科技股份有限公司 | Polyether monomer and preparation method and application thereof |
| CN107226890A (en) * | 2017-07-14 | 2017-10-03 | 安徽中铁工程材料科技有限公司 | A kind of uv-light polymerization method of high-performance water reducing agent |
| CN108084363A (en) * | 2017-12-28 | 2018-05-29 | 科之杰新材料集团有限公司 | A kind of preparation method of reinforcing type polycarboxylic acid water-reducing agent |
| WO2019128690A1 (en) * | 2017-12-28 | 2019-07-04 | 科之杰新材料集团有限公司 | Preparation method for high slump-retention polycarboxylic acid water reducing agent |
| CN108283911A (en) * | 2018-01-24 | 2018-07-17 | 咸阳师范学院 | Oil emulsion high molecular surfactant and preparation method thereof |
| CN112708046A (en) * | 2019-12-23 | 2021-04-27 | 科之杰新材料集团有限公司 | Ether super-early-strength polycarboxylate superplasticizer and preparation method thereof |
| CN112708046B (en) * | 2019-12-23 | 2022-10-28 | 科之杰新材料集团有限公司 | Ether super-early-strength polycarboxylate superplasticizer and preparation method thereof |
| CN112708049A (en) * | 2020-08-24 | 2021-04-27 | 重庆建研科之杰建材有限公司 | Concrete slump retaining agent and preparation method thereof |
| CN116943565A (en) * | 2023-09-20 | 2023-10-27 | 山西虎邦新型建材有限公司 | Polycarboxylate water reducing agent automated production control system |
| CN116943565B (en) * | 2023-09-20 | 2023-12-19 | 山西虎邦新型建材有限公司 | Polycarboxylate water reducing agent automated production control system |
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Inventor after: Qian Shanshan Inventor after: Huang Chunman Inventor after: Jiang Haidong Inventor after: Wang Gaoming Inventor after: Hu Yangcheng Inventor after: Zheng Chunyang Inventor after: Guo Zhaolai Inventor before: Zhang Ling Inventor before: Qian Shanshan Inventor before: Ding Bei Inventor before: Wang Yi Inventor before: Jiang Haidong Inventor before: Zheng Chunyang |
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Application publication date: 20160803 |