CN110105479A - A kind of low consumption environment-friendly type water phase suspension chliorinated polyvinyl chloride preparation method - Google Patents
A kind of low consumption environment-friendly type water phase suspension chliorinated polyvinyl chloride preparation method Download PDFInfo
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- CN110105479A CN110105479A CN201910493366.XA CN201910493366A CN110105479A CN 110105479 A CN110105479 A CN 110105479A CN 201910493366 A CN201910493366 A CN 201910493366A CN 110105479 A CN110105479 A CN 110105479A
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- polyvinyl chloride
- chlorine
- chlorination tank
- hydrochloric acid
- preparation
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- 239000004800 polyvinyl chloride Substances 0.000 title claims abstract description 49
- 229920000915 polyvinyl chloride Polymers 0.000 title claims abstract description 48
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 32
- 238000002360 preparation method Methods 0.000 title claims abstract description 27
- 239000000725 suspension Substances 0.000 title claims abstract description 25
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 73
- 238000005660 chlorination reaction Methods 0.000 claims abstract description 63
- 239000000460 chlorine Substances 0.000 claims abstract description 56
- 229910052801 chlorine Inorganic materials 0.000 claims abstract description 56
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 claims abstract description 55
- 238000000034 method Methods 0.000 claims abstract description 41
- 239000007788 liquid Substances 0.000 claims abstract description 19
- 238000004519 manufacturing process Methods 0.000 claims abstract description 15
- 238000005406 washing Methods 0.000 claims abstract description 14
- 239000004801 Chlorinated PVC Substances 0.000 claims abstract description 7
- 229920000457 chlorinated polyvinyl chloride Polymers 0.000 claims abstract description 7
- 238000001035 drying Methods 0.000 claims abstract description 7
- 239000007787 solid Substances 0.000 claims abstract description 7
- 230000018044 dehydration Effects 0.000 claims abstract description 6
- 238000006297 dehydration reaction Methods 0.000 claims abstract description 6
- 239000002002 slurry Substances 0.000 claims abstract description 5
- 238000010792 warming Methods 0.000 claims description 17
- 230000008569 process Effects 0.000 claims description 13
- 239000007789 gas Substances 0.000 claims description 10
- 239000003999 initiator Substances 0.000 claims description 10
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 8
- 239000002270 dispersing agent Substances 0.000 claims description 7
- 229910000041 hydrogen chloride Inorganic materials 0.000 claims description 7
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 claims description 7
- 238000005119 centrifugation Methods 0.000 claims description 6
- 238000006243 chemical reaction Methods 0.000 claims description 6
- 150000003839 salts Chemical class 0.000 claims description 6
- 238000013021 overheating Methods 0.000 claims description 5
- OMPJBNCRMGITSC-UHFFFAOYSA-N Benzoylperoxide Chemical group C=1C=CC=CC=1C(=O)OOC(=O)C1=CC=CC=C1 OMPJBNCRMGITSC-UHFFFAOYSA-N 0.000 claims description 4
- 235000019400 benzoyl peroxide Nutrition 0.000 claims description 4
- 238000001816 cooling Methods 0.000 claims description 4
- 239000000377 silicon dioxide Substances 0.000 claims description 4
- 238000004065 wastewater treatment Methods 0.000 claims description 4
- 150000001336 alkenes Chemical class 0.000 claims description 3
- 239000000498 cooling water Substances 0.000 claims description 3
- 238000010612 desalination reaction Methods 0.000 claims description 3
- 239000012299 nitrogen atmosphere Substances 0.000 claims description 3
- 239000002351 wastewater Substances 0.000 claims description 3
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 2
- 239000003795 chemical substances by application Substances 0.000 claims description 2
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 2
- WBLXMRIMSGHSAC-UHFFFAOYSA-N [Cl].[Cl] Chemical compound [Cl].[Cl] WBLXMRIMSGHSAC-UHFFFAOYSA-N 0.000 claims 1
- 239000011347 resin Substances 0.000 abstract description 20
- 229920005989 resin Polymers 0.000 abstract description 20
- 239000012071 phase Substances 0.000 abstract description 17
- 239000000047 product Substances 0.000 abstract description 13
- 239000006227 byproduct Substances 0.000 abstract description 5
- 238000005260 corrosion Methods 0.000 abstract description 4
- 230000007797 corrosion Effects 0.000 abstract description 4
- 238000003912 environmental pollution Methods 0.000 abstract description 3
- 239000007791 liquid phase Substances 0.000 abstract description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 16
- 229910052757 nitrogen Inorganic materials 0.000 description 8
- 239000002253 acid Substances 0.000 description 5
- 239000000243 solution Substances 0.000 description 5
- 238000004458 analytical method Methods 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 238000006386 neutralization reaction Methods 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 238000006467 substitution reaction Methods 0.000 description 3
- BZHJMEDXRYGGRV-UHFFFAOYSA-N Vinyl chloride Chemical compound ClC=C BZHJMEDXRYGGRV-UHFFFAOYSA-N 0.000 description 2
- 239000003513 alkali Substances 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 230000006837 decompression Effects 0.000 description 2
- 210000003298 dental enamel Anatomy 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 238000011010 flushing procedure Methods 0.000 description 2
- 239000004615 ingredient Substances 0.000 description 2
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 238000006116 polymerization reaction Methods 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 238000005979 thermal decomposition reaction Methods 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- FFBHFFJDDLITSX-UHFFFAOYSA-N benzyl N-[2-hydroxy-4-(3-oxomorpholin-4-yl)phenyl]carbamate Chemical compound OC1=C(NC(=O)OCC2=CC=CC=C2)C=CC(=C1)N1CCOCC1=O FFBHFFJDDLITSX-UHFFFAOYSA-N 0.000 description 1
- 239000012267 brine Substances 0.000 description 1
- 125000001309 chloro group Chemical group Cl* 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 229920006351 engineering plastic Polymers 0.000 description 1
- 239000003063 flame retardant Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 238000005272 metallurgy Methods 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 230000009965 odorless effect Effects 0.000 description 1
- 239000007800 oxidant agent Substances 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 238000004806 packaging method and process Methods 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000012797 qualification Methods 0.000 description 1
- 150000003254 radicals Chemical class 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- HPALAKNZSZLMCH-UHFFFAOYSA-M sodium;chloride;hydrate Chemical compound O.[Na+].[Cl-] HPALAKNZSZLMCH-UHFFFAOYSA-M 0.000 description 1
- 230000009967 tasteless effect Effects 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- 238000009941 weaving Methods 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
- C08F8/00—Chemical modification by after-treatment
- C08F8/18—Introducing halogen atoms or halogen-containing groups
- C08F8/20—Halogenation
- C08F8/22—Halogenation by reaction with free halogens
Landscapes
- Chemical & Material Sciences (AREA)
- General Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)
Abstract
The embodiment of the invention discloses a kind of low consumption environment-friendly type water phase suspension chliorinated polyvinyl chloride preparation methods, the method is using desalted water or resolving hydrochloric acid liquid as suspension, polyvinyl chloride is suspended in liquid phase with the solid content not higher than 30%, by controlling the logical chlorine speed and chlorination reaction temperature of chlorination reaction four-stage, the chlorine being passed through no more than 20% theoretical chlorine dosage makes the chlorinty of resin to 66~70%.Chliorinated polyvinyl chloride slurry removes hydrochloric acid by centrifuge, hydrochloric acid obtains resolving hydrochloric acid liquid fully recovering in suspension preparation after deep resolution system, thick chlorinated polyvinyl chloride resin is neutralized, washing, centrifugal dehydration, drying, obtain heat-resisting height, performance it is stable be suitable for manufacturing tubing and pipe fitting resin corrosion-resistant, resistant to high temperature.The problem of preparation method is poor to solve product heat resistance in the existing method for preparing chliorinated polyvinyl chloride, high production cost, environmental pollution and by-product dilute hydrochloric acid can not be handled.
Description
Technical field
The present invention relates to chemical preparation techniques fields, and in particular to a kind of low consumption environment-friendly type water phase suspension chlorinated polyvinyl chloride second
Alkene preparation method.
Background technique
Chliorinated polyvinyl chloride is made by polyvinyl chloride (PVC) resin is chlorination modified, is a kind of model engineering plastic.The production
Product are white or faint yellow tasteless, odorless, nontoxic loose particles or powder.Polyvinyl chloride resin after superchlorination, strand arrangement
Scrambling increases, and polarity increases, and increases the dissolubility of resin, and chemical stability increases, to improve the heat-resisting of material
The performance of the corrosion of property and acid and alkali resistance, salt, oxidant etc..Improve the mechanical performance of the heat distortion temperature of resin, chlorinity
Generally 65%~72% (WT), vicat softening temperature are increased to 90-125 DEG C by 72-82 DEG C, and maximum operation (service) temperature is up to 110
DEG C, long-term use temperature is 95 DEG C.
CPVC is its corrosion resistance, heat resistance, solubility, fire-retardant other than many excellent performances for having PVC concurrently
Property, mechanical strength etc. are greatly improved than PVC, thus CPVC be it is a kind of have a extensive future, function admirable it is novel
Material, is widely used in the fields such as building, chemical industry, metallurgy, shipbuilding, electric appliance, weaving, and application prospect is very wide.
Currently, the method for preparing chliorinated polyvinyl chloride mainly has solvent method, gas solid method, water phase suspension etc..Solvent method
The shortcomings that be production product heat resistance it is poor, high production cost, there are also environmental pollutions；The shortcomings that gas solid method is resin chlorination
Unevenly, heat-resistant stability difference etc..Though the product heat resistance of water phase suspension production is good, cost is also low, traditional production
It is had the following problems in technique:
1, two sections, three sections of chlorination techniques are used substantially, lead to chlorine speed and temperature, pressure control not fine enough, the tree of output
Rouge molecule branch and chain rupture are excessive, and resin heat resistance and stability are poor；
2, a large amount of concentration of by-product is that 10~15% hydrochloric acid can not be disposed in water phase suspension production.
Thus, it is desirable to new preparation method is improved or proposed to the preparation method of existing chliorinated polyvinyl chloride, with gram
Take the above problem of the prior art.
Summary of the invention
The embodiment of the present invention is designed to provide a kind of low consumption environment-friendly type water phase suspension chliorinated polyvinyl chloride preparation side
Method, to poor, the high production cost that solves product heat resistance in the existing method for preparing chliorinated polyvinyl chloride, environmental pollution, with
And by-product dilute hydrochloric acid the problem of can not handling.
To achieve the above object, the embodiment of the present invention provides a kind of low consumption environment-friendly type water phase suspension chliorinated polyvinyl chloride system
Preparation Method, the method includes the following steps:
(1) in batching kettle, the desalination water slurry for the polyvinyl chloride that solid content is 20~30wt% is prepared, is then moved to
In chlorination tank；
(2) initiator is added in chlorination tank and dispersing agent is warming up to 70~80 DEG C and is passed through chlorine in nitrogen atmosphere,
Polyvinyl chloride based on 1500Kg maintains logical 2~4Kg/min of chlorine speed, chlorination tank tail gas valve is closed after 6~8 minutes；
(3) by chlorination tank persistently overheating to 105 DEG C, logical 2~9Kg/min of chlorine speed is adjusted in the process, controls chlorination
0.05~0.30Mpa of kettle pressure；
(4) from chlorination tank collect chlorinty be 66~70% high heat resistance stability chliorinated polyvinyl chloride, through depickling from
Hydrochloric acid in chliorinated polyvinyl chloride coarse fodder is completely separated out by scheming；
(5) it is poly- to obtain chlorination for neutralized, washing, centrifugal dehydration, drying by the chliorinated polyvinyl chloride coarse fodder in step (4)
Vinyl chloride finished product.
Further, in step (2), the quality based on polyvinyl chloride, the additional amount of initiator is 0.01~1.5wt%,
The additional amount of dispersing agent is 0.05~5wt%.
Further, the initiator is selected from dibenzoyl peroxide.
Further, the dispersing agent is selected from polyvinyl alcohol or silica solution.
Further, in step (3), the persistently overheating of chlorination tank includes following process:
Chlorination tank is warming up to 90~96 DEG C, adjusts and leads to 2~5Kg/min of chlorine speed, and control chlorination tank pressure 0.05~
0.1Mpa；
Chlorination tank is warming up to 96~100 DEG C, adjusts and leads to 3~8Kg/min of chlorine speed, and control chlorination tank pressure 0.1~
0.13Mpa；
Chlorination tank is warming up to 100~102 DEG C, adjusts and leads to 3~7Kg/min of chlorine speed, and control chlorination tank pressure 0.13~
0.18Mpa；And
Chlorination tank is warming up to 102~105 DEG C, adjusts and leads to 2~6Kg/min of chlorine speed, and control chlorination tank pressure 0.18~
0.30Mpa。
Further, step (3) further includes, and when be passed through that amount of chlorine is theoretical chlorine dosage 105~115%, stops logical
Chlorine is depressured chlorination tank fast cooling using collet cooling water, chlorination tank exhaust valve, row is opened when chlorination tank pressure is to 0.1Mpa
Put the remaining chlorine for not participating in reaction.
Further, the hydrochloric acid isolated in step (4) removes hydrogen chloride gas after storing up, into hydrochloric acid depth resolution system
Body obtains resolving hydrochloric acid liquid.
Further, the concentration of hydrogen chloride is 0~1.2wt% in the resolving hydrochloric acid liquid.
Further, in step (1), in addition to initial suspension is using desalted water, the suspension of remaining production period is all made of
The resolving hydrochloric acid liquid is prepared.
Further, it in step (5), neutralizes and the less salt waste water of water-washing step generation is discharged after wastewater treatment；Centrifugation
The mother liquid coming that step generates is back to water-washing step.
Wherein, above-mentioned neutralization, washing, centrifugal dehydration, drying process and etc. be to those skilled in the art
Well-known technique, therefore not carefully state.
For the method for the present invention using desalted water or resolving hydrochloric acid liquid as suspension, polyvinyl chloride is outstanding with the solid content not higher than 30%
Float in liquid phase, by controlling the logical chlorine speed and chlorination reaction temperature of chlorination reaction four-stage, is passed through no more than 20% reason
Make the chlorinty of resin to 66~70% by the chlorine of chlorine dosage.Chliorinated polyvinyl chloride slurry removes hydrochloric acid, salt by centrifuge
Acid obtains resolving hydrochloric acid liquid fully recovering in suspension preparation after parsing deeply, thick chlorinated polyvinyl chloride resin is neutralized, washing,
Centrifugal dehydration, drying, obtain heat-resisting high, performance it is stable be suitable for manufacturing tubing and pipe fitting resin corrosion-resistant, resistant to high temperature.
The control of low consumption environment-friendly type water phase suspesion process described in the method for the present invention is stablized, easy to operate, removes original suspension
For liquid using outside desalted water, normal production period is all made of the resolving hydrochloric acid liquid after parsing deeply, and it is raw to greatly reduce traditional water phase method
The consumption of the desalted water of production. art, at the same also solve traditional water phase method production in generate a large amount of concentration be 10~15% hydrochloric acid without
The problem of method utilizes.
The technical solution of the embodiment of the present invention has the advantages that
1, the present invention is using the logical chlorine of control chlorination reaction four-stage and the technical process of temperature control process: in logical chlorine first
Stage leads to chlorine using low speed, avoids resin in the presence of a large amount of initiators, and excessive free radical occurs in resin surface
Excessive chlorination substitution reaction, resin surface form the area Gao Hanlv；Second stage improves temperature, increases logical chlorine dose, and resin is drawing
So that chlorine is penetrated into resin under the action of hair agent and substitution reaction occurs；Phase III control chlorination tank temperature remains a constant speed on steadily
It rises, slightly subtracts logical chlorine dose, resin continues to keep efficient chlorine substitution reaction when initiator is used up；Fourth stage improves reaction again
Temperature further increases resin chlorinty close to its softening temperature, guarantees the chlorination uniformity of resin from inside and outside, increases tree
The heat-resistant stability of rouge.
2, the hydrochloric acid purposes of 10~15wt% of by-product of traditional water phase method is very narrow, traditional substantially without customer demand
Method of disposal can consume a large amount of neutralizer, while generate a large amount of brine wastes.The side that the method for the present invention uses hydrochloric acid to parse deeply
Legal system obtains the resolving hydrochloric acid liquid of 0~1.2wt%, is entirely used for preparing PVC suspension.The use of desalted water can be greatly reduced in this way
Amount, moreover it is possible to obtain widely used hydrogen chloride gas (such as chlor-alkali enterprises are as the raw material for producing vinyl chloride), this method is from basic
On solve the handling problems of conventional method by-product diluted acid.
3, the method that water phase suspension provided in an embodiment of the present invention prepares chliorinated polyvinyl chloride, technology controlling and process are stablized, behaviour
Make simplicity, the chliorinated polyvinyl chloride properties of product of low consumption environmental protection, preparation are stablized, widely used.
Detailed description of the invention
It, below will be to embodiment party in order to illustrate more clearly of embodiments of the present invention or technical solution in the prior art
Formula or attached drawing needed to be used in the description of the prior art are briefly described.It should be evident that the accompanying drawings in the following description is only
It is merely exemplary, it for those of ordinary skill in the art, without creative efforts, can also basis
The attached drawing of offer, which is extended, obtains other implementation attached drawings.
Structure depicted in this specification, ratio, size etc., only to cooperate the revealed content of specification, for
Those skilled in the art understands and reads, and is not intended to limit the invention enforceable qualifications, therefore does not have technical
Essential meaning, the modification of any structure, the change of proportionate relationship or the adjustment of size are not influencing the function of the invention that can be generated
Under effect and the purpose that can reach, should all still it fall in the range of disclosed technology contents obtain and can cover.
Fig. 1 is the technique of low consumption environment-friendly type water phase suspension chliorinated polyvinyl chloride preparation method provided in an embodiment of the present invention
Flow diagram.
Wherein appended drawing reference are as follows:
1, ingredient；2, chlorination；3, it is centrifuged depickling；4, it neutralizes；5, it washes；6, it is centrifuged；7, dry；8, it packs；9, acid tank；
10, hydrochloric acid parses deeply；11, downstream user；12, wastewater treatment.
Specific embodiment
Embodiments of the present invention are illustrated by particular specific embodiment below, those skilled in the art can be by this explanation
Content disclosed by book is understood other advantages and efficacy of the present invention easily, it is clear that described embodiment is the present invention one
Section Example, instead of all the embodiments.Based on the embodiments of the present invention, those of ordinary skill in the art are not doing
Every other embodiment obtained under the premise of creative work out, shall fall within the protection scope of the present invention.
Embodiment 1
As shown in Figure 1, it is shown that low consumption environment-friendly type water phase suspension chlorinated polyvinyl chloride second provided by one embodiment of the present invention
The process flow diagram of alkene preparation method.
The process flow of the preparation method specifically includes:
(1) in batching kettle, the desalination water slurry for the polyvinyl chloride that solid content is 20~30wt% is prepared, ingredient is carried out
Process 1, then moves in chlorination tank；
(2) initiator is added in chlorination tank and dispersing agent is warming up to 70~80 DEG C and is passed through chlorine in nitrogen atmosphere,
Polyvinyl chloride based on 1500Kg maintains logical 2~4Kg/min of chlorine speed, chlorination tank tail gas valve is closed after 6~8 minutes；
(3) by chlorination tank persistently overheating to 105 DEG C, logical 2~9Kg/min of chlorine speed is adjusted in the process, controls chlorination
Kettle 0.05~0.30Mpa of pressure carries out chlorination process 2；
(4) from chlorination tank collect chlorinty be 66~70% high heat resistance stability chliorinated polyvinyl chloride, through depickling from
Hydrochloric acid in chliorinated polyvinyl chloride coarse fodder is completely separated out by scheming, carries out centrifugation deacidification 3；
(5) neutralized 4, washing 5, centrifugal dehydration 6, dry 7 and packaging 8 by chliorinated polyvinyl chloride coarse fodder in step (4),
Obtain chliorinated polyvinyl chloride finished product；
(6) hydrochloric acid isolated in step (4) removes hydrogen chloride gas into hydrochloric acid depth resolution system after acid tank 9 is stored up
Body carries out hydrochloric acid depth resolving 10, obtains resolving hydrochloric acid liquid, which is completely used for the suspension of configuration step (1)
Liquid；The hydrogen chloride gas of acquisition is used for downstream user 11；
(7) it in step (5), neutralizes the less salt waste water that 4 generate with 5 steps of washing and is discharged after wastewater treatment 12；It is centrifuged 6 steps
Suddenly the mother liquid coming generated is back to 5 steps of washing.
Embodiment 2
In the enamel chlorination tank of 12500L, the Corvic of the 1500Kg degree of polymerization 1000 and taking off for 8500Kg is added
Salt water, initiator amount are the 0.3wt% of polyvinyl chloride dosage, that is, the dibenzoyl peroxide of 4.5Kg concentration 75wt% is added,
After adding the silica solution of 4Kg concentration 30wt%, chlorination tank is passed through nitrogen, and nitrogen flushing catches up with oxygen 30 minutes, while collet hot water liter
Temperature closes nitrogen to 80 DEG C, is passed through the chlorine that flow is 2Kg/min, and logical chlorine closes chlorination tank exhaust valve, temperature after catching up with nitrogen 8 minutes
90~96 DEG C of control is led to 2~5Kg/min of chlorine speed control and is maintained 120 minutes, is warming up to 96~100 DEG C, and logical chlorine speed 3 is adjusted
~8Kg/min is kept for 90 minutes, is warming up to 100~102 DEG C, is adjusted logical 3~6Kg/min of chlorine speed, is kept for 60 minutes, heating
To 102~105 DEG C, logical 2~6Kg/min of chlorine speed is adjusted, is kept for 45 minutes, always logical chlorine dose is the 110 of theoretical chlorine dosage at this time
~115%, stop logical chlorine, reaction pressure reaches 0.3Mpa at this time；Fast cooling decompression is forced by collet cooling water simultaneously, instead
When temperature being answered to be down to 90 DEG C, exhaust valve is opened, is then discharged, through being centrifuged depickling, neutralization, washing, centrifugation, drying, obtains chlorination
Polyvinyl chloride product, the analysis indexes such as chlorinty, thermal decomposition temperature are shown in Table 1.
1 embodiment 2 of table obtains the analysis of chliorinated polyvinyl chloride properties of product
Embodiment 3
In the enamel chlorination tank of 12500L, the Corvic of the 1500Kg degree of polymerization 1000 and the chlorine of 8500Kg is added
Change hydrogen concentration 1.2wt% resolving hydrochloric acid liquid, initiator amount is the 0.3wt% of polyvinyl chloride dosage, i.e. addition 4.5Kg concentration
The dibenzoyl peroxide of 75wt%, after adding the silica solution of 4Kg concentration 30wt%, chlorination tank is passed through nitrogen, and oxygen is caught up in nitrogen flushing
30 minutes, while collet is warming up to 80 DEG C with hot water, closes nitrogen, is passed through the chlorine that flow is 2Kg/min, logical chlorine catches up with nitrogen 8 minutes
Chlorination tank exhaust valve is closed afterwards, and temperature controls 90~96 DEG C, leads to 2~5Kg/min of chlorine speed control and maintains 120 minutes, is warming up to
96~100 DEG C, adjust logical 3~8Kg/min of chlorine speed, kept for 90 minutes, be warming up to 100~102 DEG C, adjust logical chlorine speed 3~
6Kg/min is kept for 60 minutes, is warming up to 102~105 DEG C, is adjusted and is led to 2~6Kg/min of chlorine speed, holding 45 minutes, always at this time
Logical chlorine dose is the 110~115% of theoretical chlorine dosage, stops logical chlorine, reaction pressure reaches 0.3Mpa at this time；It is cold by collet simultaneously
But water force fast cooling decompression, when reaction temperature is down to 90 DEG C, open exhaust valve, then discharge, through centrifugation depickling, neutralization,
Washing, centrifugation, drying, obtain chliorinated polyvinyl chloride product, the analysis indexes such as chlorinty, thermal decomposition temperature are shown in Table 2.
2 embodiment 3 of table obtains the analysis of chliorinated polyvinyl chloride properties of product
The method that the water phase suspension that the above embodiment of the present invention provides prepares chliorinated polyvinyl chloride, technology controlling and process are stablized,
Easy to operate, the chliorinated polyvinyl chloride properties of product of low consumption environmental protection, preparation are stablized, and performance parameter fully meets every reference mark
Standard, it is widely used.
Although above having used general explanation and specific embodiment, the present invention is described in detail, at this
On the basis of invention, it can be made some modifications or improvements, this will be apparent to those skilled in the art.Therefore,
These modifications or improvements without departing from theon the basis of the spirit of the present invention are fallen within the scope of the claimed invention.
Claims (10)
1. a kind of low consumption environment-friendly type water phase suspension chliorinated polyvinyl chloride preparation method, which is characterized in that the method includes under
Column step:
(1) in batching kettle, the desalination water slurry for the polyvinyl chloride that solid content is 20~30wt% is prepared, chlorination is then moved to
In kettle；
(2) initiator is added in chlorination tank and dispersing agent is warming up to 70~80 DEG C and is passed through chlorine, be based in nitrogen atmosphere
The polyvinyl chloride of 1500Kg maintains logical 2~4Kg/min of chlorine speed, chlorination tank tail gas valve is closed after 6~8 minutes；
(3) by chlorination tank persistently overheating to 105 DEG C, logical 2~9Kg/min of chlorine speed is adjusted in the process, controls chlorination tank pressure
0.05~0.30Mpa of power；
(4) the high heat resistance stability chliorinated polyvinyl chloride that chlorinty is 66~70% is collected from chlorination tank, through depickling centrifuge
Hydrochloric acid in chliorinated polyvinyl chloride coarse fodder is completely separated out；
(5) neutralized, washing, centrifugal dehydration, drying by the chliorinated polyvinyl chloride coarse fodder in step (4), obtains chlorinated polyvinyl chloride second
Alkene finished product.
2. preparation method according to claim 1, which is characterized in that in step (2), the quality based on polyvinyl chloride is drawn
The additional amount for sending out agent is 0.01~1.5wt%, and the additional amount of dispersing agent is 0.05~5wt%.
3. preparation method according to claim 2, which is characterized in that the initiator is selected from dibenzoyl peroxide.
4. preparation method according to claim 2, which is characterized in that the dispersing agent is selected from polyvinyl alcohol or silica solution.
5. preparation method according to claim 1, which is characterized in that in step (3), under the persistently overheating of chlorination tank includes
Column process:
Chlorination tank is warming up to 90~96 DEG C, adjusts logical 2~5Kg/min of chlorine speed, controls 0.05~0.1Mpa of chlorination tank pressure；
Chlorination tank is warming up to 96~100 DEG C, adjusts logical 3~8Kg/min of chlorine speed, controls 0.1~0.13Mpa of chlorination tank pressure；
Chlorination tank is warming up to 100~102 DEG C, adjusts and leads to 3~7Kg/min of chlorine speed, and control chlorination tank pressure 0.13~
0.18Mpa；And
Chlorination tank is warming up to 102~105 DEG C, adjusts and leads to 2~6Kg/min of chlorine speed, and control chlorination tank pressure 0.18~
0.30Mpa。
6. preparation method according to claim 5, which is characterized in that step (3) further includes, and is theoretical when being passed through amount of chlorine
Chlorine dosage 105~115% when, stop logical chlorine, chlorination tank fast cooling be depressured using collet cooling water, chlorination tank pressure is extremely
Chlorination tank exhaust valve is opened when 0.1Mpa, the remaining chlorine of reaction is not participated in discharge.
7. preparation method according to claim 1, which is characterized in that the hydrochloric acid isolated in step (4) after storing up, into
Enter hydrochloric acid depth resolution system removing hydrogen chloride gas, obtains resolving hydrochloric acid liquid.
8. preparation method according to claim 7, which is characterized in that the concentration of hydrogen chloride is 0 in the resolving hydrochloric acid liquid
~1.2wt%.
9. preparation method according to claim 7, which is characterized in that in step (1), except initial suspension uses desalted water
Outside, the suspension of remaining production period is all made of the resolving hydrochloric acid liquid and prepares.
10. preparation method according to claim 1, which is characterized in that in step (5), neutralize and water-washing step generation
Less salt waste water is discharged after wastewater treatment；The mother liquid coming that centrifugation step generates is back to water-washing step.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH1129613A (en) * | 1997-07-10 | 1999-02-02 | Tokuyama Sekisui Ind Corp | Production of chlorinated vinyl chloride-based resin |
| CN1974615A (en) * | 2006-12-20 | 2007-06-06 | 上海氯碱化工股份有限公司 | Prepn process of chlorinated polyvinyl chloride resin |
| CN101486778A (en) * | 2009-02-16 | 2009-07-22 | 上海氯碱化工股份有限公司 | Preparation of chlorinated polyvinyl chloride resin for pipe fittings |
| CN104017115A (en) * | 2014-05-29 | 2014-09-03 | 南皮县至信化工有限公司 | Preparation method for chlorinated polyvinyl chloride |
| CN104231130A (en) * | 2013-06-09 | 2014-12-24 | 上海氯碱化工股份有限公司 | Chlorinated polyvinyl chloride resin and preparation method and application |
-
2019
- 2019-06-06 CN CN201910493366.XA patent/CN110105479B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH1129613A (en) * | 1997-07-10 | 1999-02-02 | Tokuyama Sekisui Ind Corp | Production of chlorinated vinyl chloride-based resin |
| CN1974615A (en) * | 2006-12-20 | 2007-06-06 | 上海氯碱化工股份有限公司 | Prepn process of chlorinated polyvinyl chloride resin |
| CN101486778A (en) * | 2009-02-16 | 2009-07-22 | 上海氯碱化工股份有限公司 | Preparation of chlorinated polyvinyl chloride resin for pipe fittings |
| CN104231130A (en) * | 2013-06-09 | 2014-12-24 | 上海氯碱化工股份有限公司 | Chlorinated polyvinyl chloride resin and preparation method and application |
| CN104017115A (en) * | 2014-05-29 | 2014-09-03 | 南皮县至信化工有限公司 | Preparation method for chlorinated polyvinyl chloride |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111704686A (en) * | 2020-07-23 | 2020-09-25 | 上海宝钱化工有限公司 | Preparation method of high chlorinated polyethylene |
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