CN106749973A - The continuous production device and production method of a kind of polycarboxylate water-reducer - Google Patents
The continuous production device and production method of a kind of polycarboxylate water-reducer Download PDFInfo
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- CN106749973A CN106749973A CN201611120848.3A CN201611120848A CN106749973A CN 106749973 A CN106749973 A CN 106749973A CN 201611120848 A CN201611120848 A CN 201611120848A CN 106749973 A CN106749973 A CN 106749973A
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- pipeline group
- polycarboxylate water
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- 239000003638 chemical reducing agent Substances 0.000 title claims abstract description 46
- 229920005646 polycarboxylate Polymers 0.000 title claims abstract description 40
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 35
- 238000010924 continuous production Methods 0.000 title claims abstract description 21
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 60
- 239000000463 material Substances 0.000 claims abstract description 39
- 238000006116 polymerization reaction Methods 0.000 claims abstract description 34
- 238000006243 chemical reaction Methods 0.000 claims abstract description 32
- 239000007788 liquid Substances 0.000 claims abstract description 30
- 230000000977 initiatory effect Effects 0.000 claims abstract description 27
- 238000000034 method Methods 0.000 claims abstract description 23
- 239000000178 monomer Substances 0.000 claims abstract description 23
- 150000001875 compounds Chemical class 0.000 claims abstract description 22
- 235000011121 sodium hydroxide Nutrition 0.000 claims abstract description 20
- 239000002994 raw material Substances 0.000 claims abstract description 14
- 238000002156 mixing Methods 0.000 claims abstract description 12
- 239000000203 mixture Substances 0.000 claims abstract description 8
- 238000007599 discharging Methods 0.000 claims abstract description 7
- 229920000642 polymer Polymers 0.000 claims abstract description 7
- 238000009413 insulation Methods 0.000 claims abstract description 5
- 239000000243 solution Substances 0.000 claims description 54
- 239000003999 initiator Substances 0.000 claims description 23
- 229920000570 polyether Polymers 0.000 claims description 17
- 239000011259 mixed solution Substances 0.000 claims description 16
- 239000004721 Polyphenylene oxide Substances 0.000 claims description 15
- 239000007864 aqueous solution Substances 0.000 claims description 14
- 238000009938 salting Methods 0.000 claims description 13
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 claims description 8
- 239000002253 acid Substances 0.000 claims description 8
- 238000006386 neutralization reaction Methods 0.000 claims description 8
- 239000003795 chemical substances by application Substances 0.000 claims description 7
- NIXOWILDQLNWCW-UHFFFAOYSA-N acrylic acid group Chemical group C(C=C)(=O)O NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims description 6
- -1 polytetrafluoroethylene Polymers 0.000 claims description 5
- 238000003860 storage Methods 0.000 claims description 5
- 125000003903 2-propenyl group Chemical group [H]C([*])([H])C([H])=C([H])[H] 0.000 claims description 4
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 4
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 4
- DKIDEFUBRARXTE-UHFFFAOYSA-N 3-mercaptopropanoic acid Chemical class OC(=O)CCS DKIDEFUBRARXTE-UHFFFAOYSA-N 0.000 claims description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 3
- LXXNWCFBZHKFPT-UHFFFAOYSA-N Ethyl 2-mercaptopropionate Chemical group CCOC(=O)C(C)S LXXNWCFBZHKFPT-UHFFFAOYSA-N 0.000 claims description 3
- PMNLUUOXGOOLSP-UHFFFAOYSA-N alpha-mercaptopropionic acid Natural products CC(S)C(O)=O PMNLUUOXGOOLSP-UHFFFAOYSA-N 0.000 claims description 3
- SURQXAFEQWPFPV-UHFFFAOYSA-L iron(2+) sulfate heptahydrate Chemical group O.O.O.O.O.O.O.[Fe+2].[O-]S([O-])(=O)=O SURQXAFEQWPFPV-UHFFFAOYSA-L 0.000 claims description 3
- 229910000359 iron(II) sulfate Inorganic materials 0.000 claims description 3
- 239000004033 plastic Substances 0.000 claims description 3
- 229920003023 plastic Polymers 0.000 claims description 3
- 239000002861 polymer material Substances 0.000 claims description 3
- 238000012546 transfer Methods 0.000 claims description 3
- GDSOZVZXVXTJMI-SNAWJCMRSA-N (e)-1-methylbut-1-ene-1,2,4-tricarboxylic acid Chemical compound OC(=O)C(/C)=C(C(O)=O)\CCC(O)=O GDSOZVZXVXTJMI-SNAWJCMRSA-N 0.000 claims description 2
- YZCKVEUIGOORGS-OUBTZVSYSA-N Deuterium Chemical compound [2H] YZCKVEUIGOORGS-OUBTZVSYSA-N 0.000 claims description 2
- 229910001209 Low-carbon steel Inorganic materials 0.000 claims description 2
- 239000011248 coating agent Substances 0.000 claims description 2
- 238000000576 coating method Methods 0.000 claims description 2
- 125000001047 cyclobutenyl group Chemical group C1(=CCC1)* 0.000 claims description 2
- 229910052805 deuterium Inorganic materials 0.000 claims description 2
- 229910052571 earthenware Inorganic materials 0.000 claims description 2
- 239000002320 enamel (paints) Substances 0.000 claims description 2
- 238000005286 illumination Methods 0.000 claims description 2
- 229910052753 mercury Inorganic materials 0.000 claims description 2
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 claims description 2
- 229920000056 polyoxyethylene ether Polymers 0.000 claims description 2
- 229940051841 polyoxyethylene ether Drugs 0.000 claims description 2
- 150000003839 salts Chemical class 0.000 claims description 2
- 239000010935 stainless steel Substances 0.000 claims description 2
- 229910001220 stainless steel Inorganic materials 0.000 claims description 2
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 claims description 2
- 229920002554 vinyl polymer Polymers 0.000 claims description 2
- 229910052724 xenon Inorganic materials 0.000 claims description 2
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 claims description 2
- BKOOMYPCSUNDGP-UHFFFAOYSA-N 2-methylbut-2-ene Chemical compound CC=C(C)C BKOOMYPCSUNDGP-UHFFFAOYSA-N 0.000 claims 1
- ZZZCUOFIHGPKAK-UHFFFAOYSA-N D-erythro-ascorbic acid Natural products OCC1OC(=O)C(O)=C1O ZZZCUOFIHGPKAK-UHFFFAOYSA-N 0.000 claims 1
- 229930003268 Vitamin C Natural products 0.000 claims 1
- MWQBWSPPTQGZII-UHFFFAOYSA-N ethoxy(phenyl)phosphinic acid Chemical compound CCOP(O)(=O)C1=CC=CC=C1 MWQBWSPPTQGZII-UHFFFAOYSA-N 0.000 claims 1
- 235000019154 vitamin C Nutrition 0.000 claims 1
- 239000011718 vitamin C Substances 0.000 claims 1
- 238000010923 batch production Methods 0.000 abstract description 4
- 238000005265 energy consumption Methods 0.000 abstract description 4
- 230000000052 comparative effect Effects 0.000 description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 11
- 239000004568 cement Substances 0.000 description 8
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 6
- 230000015572 biosynthetic process Effects 0.000 description 6
- 238000003786 synthesis reaction Methods 0.000 description 6
- 150000007513 acids Chemical class 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 5
- 239000000047 product Substances 0.000 description 5
- 230000009466 transformation Effects 0.000 description 5
- 206010054949 Metaplasia Diseases 0.000 description 4
- 230000032683 aging Effects 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 230000015689 metaplastic ossification Effects 0.000 description 4
- 238000003756 stirring Methods 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 3
- 229960005070 ascorbic acid Drugs 0.000 description 3
- 235000010323 ascorbic acid Nutrition 0.000 description 3
- 239000011668 ascorbic acid Substances 0.000 description 3
- 229910052757 nitrogen Inorganic materials 0.000 description 3
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 description 2
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 2
- 238000007334 copolymerization reaction Methods 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 230000018109 developmental process Effects 0.000 description 2
- 230000003467 diminishing effect Effects 0.000 description 2
- 239000012153 distilled water Substances 0.000 description 2
- 239000002002 slurry Substances 0.000 description 2
- 150000003384 small molecules Chemical class 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- AUHZEENZYGFFBQ-UHFFFAOYSA-N 1,3,5-trimethylbenzene Chemical class CC1=CC(C)=CC(C)=C1 AUHZEENZYGFFBQ-UHFFFAOYSA-N 0.000 description 1
- 229920003171 Poly (ethylene oxide) Polymers 0.000 description 1
- 239000002202 Polyethylene glycol Substances 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- IAQRGUVFOMOMEM-UHFFFAOYSA-N butene Natural products CC=CC IAQRGUVFOMOMEM-UHFFFAOYSA-N 0.000 description 1
- 125000002843 carboxylic acid group Chemical group 0.000 description 1
- 230000008602 contraction Effects 0.000 description 1
- 239000012895 dilution Substances 0.000 description 1
- 238000010790 dilution Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 150000002170 ethers Chemical class 0.000 description 1
- HOCOIDRZLNGZMV-UHFFFAOYSA-N ethoxy(oxido)phosphanium Chemical compound CCO[PH2]=O HOCOIDRZLNGZMV-UHFFFAOYSA-N 0.000 description 1
- 230000007717 exclusion Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000004744 fabric Substances 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 238000001764 infiltration Methods 0.000 description 1
- 230000008595 infiltration Effects 0.000 description 1
- 238000009434 installation Methods 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 229920001223 polyethylene glycol Polymers 0.000 description 1
- 238000010926 purge Methods 0.000 description 1
- 239000012925 reference material Substances 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- VWDWKYIASSYTQR-UHFFFAOYSA-N sodium nitrate Inorganic materials [Na+].[O-][N+]([O-])=O VWDWKYIASSYTQR-UHFFFAOYSA-N 0.000 description 1
- 239000002689 soil Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- PXQLVRUNWNTZOS-UHFFFAOYSA-N sulfanyl Chemical class [SH] PXQLVRUNWNTZOS-UHFFFAOYSA-N 0.000 description 1
- 239000013589 supplement Substances 0.000 description 1
- 238000011282 treatment Methods 0.000 description 1
- 238000010792 warming Methods 0.000 description 1
- 239000003643 water by type Substances 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
- C08F2/01—Processes of polymerisation characterised by special features of the polymerisation apparatus used
-
- 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 discloses the continuous production device and production method of a kind of polycarboxylate water-reducer.Continuous production method of the present invention includes：Stock blend stage, solution A, solution B and solution C enter pipeline group by flowmeter and pump of getting the raw materials ready；Compound initiating stage, solution D and monomer E enter pipeline group through magnetic drive pump, flowmeter together with early stage batch mixing, and carry out the ultraviolet compound initiation polymerization of normal temperature；Normal temperature holding stage, early stage material carries out normal temperature insulation by pipeline group, and polymerization is fully carried out；Discharging stage is neutralized, liquid caustic soda solution F enters pipeline group through magnetic drive pump, flowmeter together with early stage polymer, and neutralized rear discharging finally obtains polycarboxylate water-reducer.The technological process of production of the present invention is simple, is greatly improved production efficiency and production capacity, reduces investment of production equipment and energy consumption；And the conversion ratio of polymerization is substantially increased, the batch production mode of polycarboxylate water-reducer is veritably transformed into continuous prodution mode.
Description
Technical field
The present invention relates to technical field of concrete additives, more particularly to a kind of ultraviolet compound initiation of use normal temperature serialization
Production equipment produces the method and technology of polycarboxylate water-reducer.
Background technology
In recent years, with the development of concrete technology, the application of high performance water reducing agent of polyocarboxy acid is constantly popularized, with its volume
Low, water-reducing rate is high, function of slump protection is excellent, contraction is low, energy-conserving and environment-protective many advantages, such as, gradually obtained in numerous engineerings extensively should
With.Polycarboxylic acids molecule is typically by the unsaturated small molecule containing carboxylic acid group, the unsaturated macromolecular containing polyethylene oxide base and contains
The Comblike polymers compound of the unsaturated small molecule copolymerization of other functional groups.Not only performance is excellent for polycarboxylate water-reducer
It is different, and produce and use with environmental protection characteristic, harmful substance contents are few, are acknowledged as concrete admixture development from now on
Direction.
The synthesis of current polycarboxylate water-reducer is substantially and is carried out in specific reactor or similar containers, using big
Monomeric polyether bottoming, is added dropwise initiator, acrylic acid or protects collapse monomer and functional monomer etc. in a certain temperature conditions
Material, and this several activated monomer is carried out copolymerization, synthesize structure difference or the different polycarboxylate water-reducer product of function.
Polycarboxylate water-reducer manufacturer is generally produced using the polymerization production device of batch (-type) both at home and abroad at present.It is general this
Polymerization production device includes polymerization reaction kettle, and multiple dropping tanks are connected with by pipeline respectively outside polymerization reaction kettle, material from
Constantly being added drop-wise in dropping tank carries out polymerisation in reactor.A kind of polycarboxylic acids is described in Chinese patent CN204395957U
Water reducer high efficiency reactor, its reactor inside is provided with Multi-stage stirring bar and stirring vane, and stirring vane layering cloth
Put, every layer of blade can be stirred to the polycarboxylic acids solution in reactor, it is to avoid upper and lower solution shape is different, mixed effect
It is all fine with reaction effect.A kind of polymerisation for producing polycarboxylate water-reducer is described in Chinese patent CN204768671U
Kettle, temperature system is provided with its reactor, and the temperature system includes system for detecting temperature, the outside temperature inside polymerization reaction kettle
Degree control system, the program temperature modulation component of periphery.Wherein polymerization reaction kettle can according to reaction different phase the need for carry
For suitable reaction temperature, and then reaction efficiency is improved, increase product yield.
But the device of this batch (-type) and mode of production structure are complex, reaction kettle body and corresponding pipeline are taken up space
Larger, the production time is more long, it is necessary to temperature-controlling system strictly controls temperature, energy consumption is larger, and each batch for low production efficiency
Polycarboxylate water-reducer performance differ, it would be highly desirable to improve.It is badly in need of a kind of large-scale continuous production device of research and development and method at present
To solve the above problems.Described in Chinese patent CN102942659A a kind of for pipe reaction device production polycarboxylic acids diminishing
The interval metaplasia of polycarboxylate water-reducer is produced and becomes approximate continuous metaplasia and produce by the method for agent, the method, the raw material that will configure with
Auxiliary material is added after being polymerized in pipe reaction device, and product enters aging in storage tank and neutralizes.The method changes reactor
It is pipe reaction device, improves production scale and efficiency, but the later stage stills need to be carried out in storage tank aging in batches or manages
Formula reaction unit discharge outlet neutralize could obtain polycarboxylate water-reducer, be not a complete continuous prodution work
Skill, the production capacity of large-scale production is limited using neutralization ageing can.Also, the tube type apparatus that the method is provided are single pipeline,
It is unfavorable for maintenance and installation.For the problem in above-mentioned patent, Chinese patent CN103537241A is improved it, there is provided
A kind of single channel pipe reaction device for producing polycarboxylate water-reducer, including the process that feeds intake, insulating process and neutralization dilution,
Total overall reaction process is carried out in single channel reaction tube, and the reaction unit in each stage is completely or partially in thermostat
In, reaction terminates rear polycarboxylate water-reducer and is discharged from discharging opening, without carrying out other subsequent treatments.Production technology is simplified, greatly
Improve production efficiency and production capacity greatly.But above-mentioned patent does not pay close attention to the conversion ratio of the polymerizate in polymerization process, with interval
The polycarboxylic acids transformation efficiency more than 90% that metaplasia is produced is compared, the transformation efficiency of polymerizate also only 60~75%, above-mentioned in addition
Two kinds of duct type process units are required for completely or partially being immersed in constant temperature waters, and energy consumption is larger.
The content of the invention
The purpose of the present invention is to solve the shortcomings of the prior art, there is provided a kind of normal temperature for producing polycarboxylate water-reducer is ultraviolet
The compound continuous production device for triggering and method.Mainly solve the technical problem of following three aspect：(1) polycarboxylate water-reducer connects
Continuous metaplasia needs separately to match somebody with somebody ageing can or reactor during producing；(2) polycarboxylate water-reducer continuous production device needs whole
Or part is immersed in thermostat, equipment is complicated, not easy-maintaining；(3) polycarboxylate water-reducer continuous prodution polymerization conversion effect
The relatively low problem of rate.
In order to realize foregoing invention purpose, the technical solution adopted in the present invention is as follows：
A kind of continuous production device of polycarboxylate water-reducer, including material serialization is flowed through and a series of for what is reacted
The pipeline group and relevant apparatus of series connection, and the serial pipe group can flow through different phase and be divided into four ranks according to material
Section：
Wherein, the first stage is the stock blend stage, including flowmeter, get the raw materials ready pump and pipeline group, and wherein material is passed through successively
Excessively stream gauge and pump of getting the raw materials ready enter pipeline group；
Second stage is to be combined initiating stage, including the ultraviolet light inlayed in magnetic drive pump, flowmeter, pipeline group and pipeline group
Light source, the new material for adding, i.e., the material that the material that second stage enters is obtained through the reaction of magnetic drive pump, flowmeter and first stage
Enter pipeline group together, and carry out ultraviolet compound initiation of normal temperature and be polymerized；
Phase III is normal temperature holding stage, including pipeline group, mass flow surge tank and centrifugal pump, second stage reaction
The material for obtaining carries out normal temperature insulation polymerization by pipeline group, and subsequently into mass flow surge tank, the tank is used to enter the 4th
The regulation of the mass flow in stage, next stage is entered by centrifugal pump；
Fourth stage is to neutralize discharging stage, including magnetic drive pump, flowmeter and pipeline group, the material warp that fourth stage enters
Enter pipeline group together with the material that magnetic drive pump, flowmeter are obtained with phase III reaction, discharged after neutralized batch mixing；
The pipeline group is a series of serial pipes；The inwall of all pipeline groups is equipped with spoiler, wherein flow-disturbing
Plate and material flow through direction in 90 °~150 °.
The cross-section of pipeline shape can be circle, ellipticity, ovate, rectangular-shaped, star-like shape or flat type shape.
The material of the pipeline group be plastic tube, the inwall coating stainless steel tube of polytetrafluoroethylene (PTFE), inwall enamel coating it is low
Carbon steel pipe or earthenware；
The pipeline group can be connected in any form according to actual space mounting；
The length of the pipeline group needs to be selected according to the extent of polymerization of material, generally 200~500 meters, pipe
The diameter of road group is generally 0.05~0.08 meter；The length ratio of the pipeline group of the four-stage is followed successively by 1：5~9：1~2：1
~2.
The pipeline group, can be with linear pattern connection or closely folded form connection according to actual space mounting.
A kind of continuous production method of polycarboxylate water-reducer, whole production process is as follows：
(1) polyether macromonomer solution A, Fe are prepared respectively2+Salting liquid B, H2O2Aqueous solution C, ascorbic acid-chain-transferring agent-
Ultraviolet initiator mixed solution D, activated monomer E, liquid caustic soda solution F, and transfer them to storage tank to be fed；
Wherein polyether macromonomer solution A, Fe2+Salting liquid B and H2O2Aqueous solution C is pumped into the pipeline of first stage successively
Batch mixing is carried out in group, is not stopped in the pipeline group of second stage；
(2) activated monomer E, ascorbic acid-chain-transferring agent-ultraviolet initiator mixed solution D are added second in batches
In the compound initiation polymerization pipeline group in stage, and the material obtained with first stage reaction carries out polymerisation；
(3) polymerizate enters the normal temperature utilidor group of phase III after, and polymerization is fully carried out；
(4) last polymer material is neutralized and discharged with liquid caustic soda solution F in the neutralization discharge pipe group of fourth stage,
Finally obtain the polycarboxylate water-reducer.
According to technique needs, batch mixing in the first stage pipeline group initiating terminal of getting the raw materials ready is provided with charging aperture, for polyethers is big
Monomer solution A, Fe2+Salting liquid B and H2O2Aqueous solution C is pumped into pipeline group successively；
Several charging apertures for being in diverse location are provided with the compound initiation pipeline group of second stage, for by activity
Monomer E, ascorbic acid-chain-transferring agent-ultraviolet initiator mixed solution D add the compound initiation of second stage to be polymerized in batches
In pipeline group, the quantity of the wherein charging aperture of second stage is generally 3~8, and the inlet amount of each charging aperture is equal；
The charging aperture of liquid caustic soda solution F is provided with the neutralization discharge pipe initiating terminal of fourth stage.
The pipeline group inwall of the compound initiating stage of the second stage has been uniformly distributed several ultraviolet sources, wherein second
The pipeline group initiating terminal in stage sets first ultraviolet source, sets a ultraviolet source every 2 meters afterwards；Ultraviolet light is by following
Light source is produced：Mercury lamp, xenon lamp, deuterium lamp, ultraviolet LED lamp, illumination are the ultraviolet light that wavelength is 295~400nm, and light source power is 20
~500w.
The raw material need to be configured to certain density specification solution：Wherein polyether macromonomer solution A mass concentration is 60%,
Fe2+Salting liquid B mass concentrations are 0.1%, H2O2Aqueous solution C mass concentrations be 5%, ascorbic acid solution mass concentration be 1~
1.5%, chain-transferring agent concentration of polymer solution is 1~1.5%, and ultraviolet initiator concentration of polymer solution is 1~1.5%, liquid caustic soda
Solution F mass concentrations are 35%；
Wherein ascorbic acid-chain-transferring agent-ultraviolet initiator mixed solution D be by above-mentioned mass concentration in the range of it is anti-
Bad hematic acid solution, three kinds of solution of chain-transferring agent solution and ultraviolet initiator solution mix composition with arbitrary proportion.
The material has certain feed rate into pipeline：Wherein polyether macromonomer solution A feed rate be 100~
500kg/h, Fe2+Salting liquid B feed rates are 1.2~5.5kg/h, H2O2Aqueous solution C feed rates are 1.5~8kg/h, anti-bad
Hematic acid-chain-transferring agent-ultraviolet initiator mixed solution D feed rates are 50~250kg/h, and activated monomer E feed rates are
10.5~35kg/h, liquid caustic soda solution F feed rate are 11~36kg/h.
The polyether macromonomer A is selected from allyl polyethenoxy ether, methyl allyl polyoxyethylene ether, cyclobutenyl polyoxy second
It is any one in alkene ether, methyl butene base APEO, vinyl APEO, hydroxyl butyl vinyl APEO
Kind；Wherein the weight average molecular weight of polyether macromonomer A is 1000~5000；
The Fe2+Salt B is green vitriol；
The activated monomer E is acrylic acid；
The ultraviolet initiator is two (2,4,6- trimethylbenzoyls)-phenyl phosphine oxides, 2,4,6- trimethylbenzenes
Any one in Fonnylphenyl phosphinic acid ethyl ester；
The chain-transferring agent is 2 mercaptopropionic acid, 3- mercaptopropionic acids, 2- mercaprols, 3- mercaprols, TGA, mercapto
Any one in base ethanol；
The liquid caustic soda solution F is sodium hydroxide solution.
Beneficial effects of the present invention are as follows：
The production equipment of the ultraviolet compound initiation production polycarboxylate water-reducer of normal temperature that the present invention is provided, mainly using pipeline group
It is sequentially connected in series and forms, technological process is simple, be greatly improved production efficiency and production capacity, reduces investment of production equipment and production energy
Consumption；It is combined using normal temperature and triggers polymerization, without infiltration in thermostat, ultraviolet initiation polymerization also substantially increases poly- pipeline group
The conversion ratio of conjunction, is veritably transformed into continuous prodution mode by the batch production mode of polycarboxylate water-reducer.
Brief description of the drawings
Fig. 1 is the structural representation of the continuous production device of the ultraviolet compound initiation of normal temperature of the invention.
Specific mark in Fig. 1 is respectively：11,22,42 flowmeters, 12 are got the raw materials ready pump, 13,23,31,43 pipeline groups, and 14 disturb
Stream plate, 21,41 magnetic drive pumps, 24 ultraviolet sources, 32 mass flow surge tanks, 33 centrifugal pumps.
Specific embodiment
The present invention is specifically described below in conjunction with specific embodiment, to be best understood from the content of the invention,
But the content of embodiment is not intended to limit the protection domain of the invention.
The weight average molecular weight and polymerisation conversion of polycarboxylate water-reducer described in embodiment are using high productivity computing instrument
(GPC) it is measured.Wherein splitter is using two gel chromatographic columnses series connection of Shodex SB806+803,40 DEG C of column temperature, flowing
It is mutually 0.1M NaNO3The aqueous solution, flow velocity is 1.0ml/min, and sample size is the aqueous solution of 20 μ l 0.5%；Detector：Shodex
RI-71 type differential refraction detectors；Standard curve making uses polyethylene glycol GPC reference materials (Sigma-Aldrich, molecular weight
1010000,478000,263000,118000,44700,18600,6690,1960,628,232).
The continuous production device of polycarboxylate water-reducer of the present invention, including material serialization is flowed through and for reaction
The pipeline group and relevant apparatus of a series of series connection；And the serial pipe group can flow through different phase and be divided into four according to material
Part, wherein, the first stage is the stock blend stage, including flowmeter 11, gets the raw materials ready pump 12 and pipeline group 13, wherein material successively
Enter pipeline group 13 by flowmeter 11 and pump 12 of getting the raw materials ready, the inwall of pipeline group 13 is provided with spoiler 14, the pipe of following several stages
Road group is as the stage structures；Second stage is to be combined initiating stage, including magnetic drive pump 21, flowmeter 22, the and of pipeline group 23
The ultraviolet source 24 inlayed in pipeline group, material enters pipeline group 23 through magnetic drive pump 21, flowmeter 22 together with early stage batch mixing,
And carry out the ultraviolet compound initiation polymerization of normal temperature；Phase III is normal temperature holding stage, including pipeline group 31, mass flow surge tank
32 and centrifugal pump 33, the material of reaction carries out normal temperature insulation by pipeline group 31, and polymerization is fully carried out, and is buffered into mass flow
Tank, the tank is used for the regulation of later stage mass flow, and next stage is entered by centrifugal pump 33；Fourth stage is to neutralize discharging rank
Section, including magnetic drive pump 41, flowmeter 42 and pipeline group 43, the material that fourth stage enters through magnetic drive pump 41, flowmeter 42 with it is preceding
Phase polymer enters pipeline group 43 together, is discharged after neutralized batch mixing.
Whole production process is as follows：Certain density polyether macromonomer solution A, Fe are prepared respectively2+Salting liquid B,
H2O2Aqueous solution C, ascorbic acid-chain-transferring agent-ultraviolet initiator mixed solution D, activated monomer E, liquid caustic soda solution F, and by its
It is transferred in storage tank to be fed；Wherein polyether macromonomer solution A, Fe2+Salting liquid B and H2O2Aqueous solution C is in the first stage
Batch mixing is carried out in batch mixing pipeline group, is not stopped in the pipeline group of second stage；By activated monomer E, ascorbic acid-chain tra nsfer
Agent-ultraviolet initiator mixed solution D is sequentially added in the compound initiation polymerization pipeline group of second stage in batches, and with first
The batch mixing in stage carries out polymerisation；Polymerizate enters the normal temperature utilidor group of phase III afterwards, and polymerization is fully carried out；
Last polymer material carries out neutralization discharging with liquid caustic soda solution F in the neutralization discharge pipe group of fourth stage, finally obtains poly- carboxylic
Sour water reducer.
The compound activated monomer E for triggering polymerization stage, ascorbic acid-chain-transferring agent-ultraviolet initiator mixed solution D are needed
To feed successively in batches simultaneously, so meet serialization kinetics of polymerization reaction so that polymerization conversion efficiency tends to maximum, when
The situation of feeding quantity can also be so adjusted according to actual conditions, to obtain required structure and performance；Other charge door therein
Quantity and the distance between charge door, poly- carboxylic can equally be adjusted with this according to actual process increase in demand or reduction
The structure and performance of acid.
Embodiment 1
The pipeline group that the present embodiment is used is 200 meters, a diameter of 0.05 meter of plastic tube, the pipeline of four-stage for length
Length ratio is 1：5：1：1, wherein the uv power of compound initiation polymerization stage is 20w, the charging aperture in the stage is 3, and
And the charging aperture in the stage by equidistantly distributing, i.e. the charging aperture of second stage is evenly distributed in the pipeline group of second stage,
1st charging aperture is distributed 1 charging aperture every 25 meters afterwards in the starting end of second stage, the end of second stage do not set into
Material mouth.
Required raw material is configured to specification solution：The allyl polyethenoxy ether (Mw=1000) of 60% mass concentration,
The H of the copperas solution of 0.1% mass concentration, 5% mass concentration2O2Solution, 1% mass concentration ascorbic acid solution, 1%
Mass concentration 2 mercaptopropionic acid, the mixed solution of 1% mass concentration two (2,4,6- trimethylbenzoyls)-phenyl phosphine oxide,
35% mass sodium hydroxide solution.Wherein polyether macromonomer solution A feed rate is 100kg/h, Fe2+Salting liquid B feed rates
It is 1.2kg/h, hydrogen peroxide solution C feed rates are 1.5kg/h, ascorbic acid-chain-transferring agent-ultraviolet initiator mixed solution
D feed rates are 50kg/h, and activated monomer E feed rates are 10.5kg/h, and liquid caustic soda solution F feed rates are 11kg/h.Wherein
Compound initiating stage has 3 charging apertures, and the feed rate of each charging aperture is made up of two parts, Part I be ascorbic acid-
The feed rate 50/3=16.66kg/h of chain-transferring agent-ultraviolet initiator mixed solution D, Part II is that activated monomer E enters
Stream amount 10.5/3=3.5kg/h.Be uniformly added into above-mentioned material in pipeline group by control charging rate, while ultraviolet light is opened,
Carry out continuous prodution.When insufficient raw material, supplement in time.
The detailed synthesis condition and production equipment parameter of the embodiment are listed in Tables 1 and 2.
Embodiment 2~10
Embodiment 2~10 uses identical production equipment with embodiment 1, and production technology is identical, simply synthesis condition and life
Produce device parameter different, detailed synthesis condition and production equipment parameter are listed in Tables 1 and 2.
Comparative example 1~2
Comparative example 1~2 corresponds to embodiment 1~2 respectively, is simply combined and triggers the ultraviolet source of polymerization stage to be not switched on.
Detailed synthesis condition and production equipment parameter are listed in Tables 1 and 2.
Comparative example 3
The polycarboxylate water-reducer prepared using batch reactor, equipped with thermometer, agitator, dropping funel and nitrogen
In the 1L glass round bottom flask of conduit, add 185.0g distilled water, 275.5g allyl polyethenoxy ethers and be with 3.4g concentration
30% hydrogen peroxide, stirs rising temperature for dissolving, and purge round-bottomed flask, the oxygen in exclusion system with nitrogen.Under nitrogen protection,
40 DEG C are warming up to, then 54.0g acrylic acid, 1.26g 3- mercaptopropionic acids and 100.0g water are mixed and is made uniform monomer
The aqueous solution, it is at the uniform velocity dropped in round-bottomed flask, and time for adding is 3h.Simultaneously be at the uniform velocity added dropwise by 160.0g distilled water with
The initiator solution of 0.92g ascorbic acid, time for adding is 3.5h.Continue constant temperature insulation 2h after complete soln completion of dropping, so
After be cooled to 40 DEG C or so, add NaOH to be neutralized to pH=7.0 or so, obtain polycarboxylate water-reducer.
Synthesis condition in the embodiment of table 1 and comparative example
Production equipment parameter in the embodiment of table 2 and comparative example
Application Example
Embodiment 1~10 and comparative example 1~3 are carried out into performance comparison, according to GB8076-2008《Concrete admixture》's
Relevant regulations carry out the measure of flowing degree of net paste of cement and concrete water-reducing ratio.Entered using high productivity computing instrument (GPC) simultaneously
The weight average molecular weight and polymerization conversion efficiency of row determination sample.Wherein flowing degree of net paste of cement test, using south of the River little Ye fields
The cement of 52.5P. II, weighs cement 300g, and amount of water is 87g, and water reducer solid volume is the 0.12% of cement weight, and test is just
Paste flowing degree after beginning fluidity and 60min；Concrete water-reducing ratio experiment is carried out under 25 DEG C of environment, and testing cement is used
The cement of south of the River little Ye fields 52.5P. II, fixed water reducer solid volume is the 0.2% of cement weight, and adjustment water consumption makes newly to mix mixed
Solidifying soil initial slump is 21.0 ± 1cm.Above-mentioned experimental result is shown in Table 3.
The performance comparison of the embodiment of table 3 and comparative example
From the point of view of result of the test, water reducer prepared by comparative example 1~10 and comparative example 1~3, it can be seen that：
(1) 95% is all reached using the ultraviolet compound sample transformation efficiency for triggering the embodiment 1~10 being polymerized to obtain of normal temperature
More than, the transformation efficiency of the product for illustrating that continuous prodution can be obviously improved using the production equipment and process；
(2) under conditions of ultraviolet source is not switched on, the sample transformation efficiency of comparative example 1~2, net slurry and diminishing are forthright
Corresponding embodiment 1~2 all can be accordingly less than, illustrates that uv-light polymerization can trigger polymerization efficiency with service hoisting normal temperature, it is bright
Aobvious lifting properties of product；(3) the sample phase of the sample of the embodiment 1~10 of continuous prodution and the comparative example 3 of batch production
Than polymerization conversion efficiency, net slurry and water-reducing rate performance are all suitable, can reach the performance requirement of batch production.
Claims (10)
1. a kind of continuous production device of polycarboxylate water-reducer, it is characterised in that flowed through including material serialization and for anti-
The pipeline group and relevant apparatus of a series of series connection answered, and the serial pipe group can flow through different phase division according to material
Into four-stage：
Wherein, the first stage is the stock blend stage, including flowmeter（11）, pump of getting the raw materials ready（12）And pipeline group（13）, wherein thing
Material sequentially passes through flowmeter（11）With pump of getting the raw materials ready（12）Into pipeline group（13）；
Second stage is to be combined initiating stage, including magnetic drive pump（21）, flowmeter（22）, pipeline group（23）Inlayed with pipeline group
Ultraviolet source（24）, the new material for adding, i.e., the material that second stage enters is through magnetic drive pump（21）, flowmeter（22）With
The material that one elementary reaction is obtained enters pipeline group together（23）, and carry out the ultraviolet compound initiation polymerization of normal temperature；
Phase III is normal temperature holding stage, including pipeline group（31）, mass flow surge tank（32）And centrifugal pump（33）, second
The material that elementary reaction is obtained is by pipeline group（31）Normal temperature insulation polymerization is carried out, subsequently into mass flow surge tank（32）,
The tank is used for the regulation of the mass flow for entering fourth stage, by centrifugal pump（33）Into next stage；
Fourth stage is to neutralize discharging stage, including magnetic drive pump（41）, flowmeter（42）And pipeline group（43）, fourth stage entrance
Material through magnetic drive pump（41）, flowmeter（42）Enter pipeline group together with the material obtained with phase III reaction（43）, in
Discharged with after batch mixing；
The pipeline group is a series of serial pipes；The inwall of all pipeline groups is equipped with spoiler（14）, wherein flow-disturbing
Plate and material flow through direction in 90 ° ~ 150 °.
2. a kind of continuous production device of polycarboxylate water-reducer according to claim 1, it is characterised in that the pipeline
Shape of cross section can be circle, ellipticity, ovate, rectangular-shaped, star-like shape or flat type shape.
3. a kind of continuous production device of polycarboxylate water-reducer according to claim 2, it is characterised in that the pipeline
The material of group is plastic tube, stainless steel tube, the low carbon steel pipe or earthenware of inwall enamel coating of inwall coating polytetrafluoroethylene (PTFE)；
The pipeline group can be connected in any form according to actual space mounting；
The length of the pipeline group is 200 ~ 500 meters, a diameter of 0.05 ~ 0.08 meter；The length of the pipeline group of the four-stage
Than being followed successively by 1：5~9：1~2：1~2.
4. a kind of continuous production device of polycarboxylate water-reducer according to claim 3, it is characterised in that the pipeline
Group, can be with linear pattern connection or closely folded form connection according to actual space mounting.
5. a kind of usage right requires the continuous prodution of the polycarboxylate water-reducer of continuous production device described in 1 to 4 any one
Method, it is characterised in that production process is as follows：
（1）Polyether macromonomer solution A, Fe are prepared respectively2+Salting liquid B, H2O2Aqueous solution C, ascorbic acid-chain-transferring agent-ultraviolet light
Initiator mixed solution D, activated monomer E, liquid caustic soda solution F, and transfer them to storage tank to be fed；
Wherein polyether macromonomer solution A, Fe2+Salting liquid B and H2O2Aqueous solution C is pumped into the pipeline group of first stage successively
Batch mixing is carried out, is not stopped in the pipeline group of second stage；
（2）Activated monomer E, ascorbic acid-chain-transferring agent-ultraviolet initiator mixed solution D are added into second stage in batches
Compound initiation polymerization pipeline group in, and carry out polymerisation with the material that obtains of first stage reaction；
（3）Polymerizate enters the normal temperature utilidor group of phase III afterwards, and polymerization is fully carried out；
（4）Last polymer material is neutralized and discharged with liquid caustic soda solution F in the neutralization discharge pipe group of fourth stage, finally
Obtain the polycarboxylate water-reducer.
6. the continuous production method of a kind of polycarboxylate water-reducer according to claim 5, it is characterised in that in the first rank
The batch mixing pipeline group initiating terminal of getting the raw materials ready of section is provided with charging aperture, for by polyether macromonomer solution A, Fe2+Salting liquid B and H2O2It is water-soluble
Liquid C is pumped into pipeline group successively（13）In；
Several charging apertures for being in diverse location are provided with the compound initiation pipeline group of second stage, for by activated monomer
E, ascorbic acid-chain-transferring agent-ultraviolet initiator mixed solution D add pipeline group in batches（23）In, wherein second stage
Charging aperture quantity be 3 ~ 8, the inlet amount of each charging aperture is equal；
The charging aperture of liquid caustic soda solution F is provided with the neutralization discharge pipe initiating terminal of fourth stage.
7. the continuous production method of a kind of polycarboxylate water-reducer according to claim 6, it is characterised in that described second
The pipeline group inwall of stage compound initiating stage has been uniformly distributed several ultraviolet sources, wherein the pipeline group starting of second stage
End sets first ultraviolet source, sets a ultraviolet source every 2 meters afterwards；Ultraviolet light is produced by following light source：Mercury lamp, xenon
Lamp, deuterium lamp, ultraviolet LED lamp, illumination are that wavelength is the ultraviolet light of 295 ~ 400nm, and light source power is 20 ~ 500w.
8. a kind of continuous production method of polycarboxylate water-reducer according to claim 7, it is characterised in that the polyethers
Large monomer solution A mass concentrations are 60%, Fe2+Salting liquid B mass concentrations are 0.1%, H2O2Aqueous solution C mass concentrations are 5%, are resisted
Bad hematic acid concentration of polymer solution is 1 ~ 1.5%, and chain-transferring agent concentration of polymer solution is 1 ~ 1.5%, ultraviolet initiator solution quality
Concentration is 1 ~ 1.5%, and liquid caustic soda solution F mass concentrations are 35%；
Wherein ascorbic acid-chain-transferring agent-ultraviolet initiator mixed solution D is by the Vitamin C in the range of above-mentioned mass concentration
Acid solution, three kinds of solution of chain-transferring agent solution and ultraviolet initiator solution mix composition with arbitrary proportion.
9. the continuous production method of a kind of polycarboxylate water-reducer according to right wants 8, it is characterised in that the material enters
The feed rate for entering pipeline is respectively：Wherein polyether macromonomer solution A feed rate is 100 ~ 500 kg/h, Fe2+Salting liquid B enters
Stream amount is 1.2 ~ 5.5 kg/h, H2O2Aqueous solution C feed rates are 1.5 ~ 8 kg/h, ascorbic acid-chain-transferring agent-ultraviolet light
Initiator mixed solution D feed rates are 50 ~ 250 kg/h, and activated monomer E feed rates are 10.5 ~ 35 kg/h, liquid caustic soda solution
F feed rates are 11 ~ 36kg/h.
10. the continuous production method of a kind of polycarboxylate water-reducer according to claim 9, it is characterised in that described poly-
Ether polymeric monomer A is selected from allyl polyethenoxy ether, methyl allyl polyoxyethylene ether, cyclobutenyl APEO, methyl butene
Any one in base APEO, vinyl APEO, hydroxyl butyl vinyl APEO；The wherein big list of polyethers
The weight average molecular weight of body A is 1000 ~ 5000；
The Fe2+Salt B is green vitriol；
The activated monomer E is acrylic acid；
The ultraviolet initiator is two（2,4,6- trimethylbenzoyls）- phenyl phosphine oxide, 2,4,6- trimethylbenzoyls
Any one in base phenyl-phosphonic acid ethyl ester；
The chain-transferring agent is 2 mercaptopropionic acid, 3- mercaptopropionic acids, 2- mercaprols, 3- mercaprols, TGA, sulfydryl second
Any one in alcohol；
The liquid caustic soda solution F is sodium hydroxide solution.
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