CN108299489A - A kind of vinyl tributyl ketoximyl silane continuous reaction system - Google Patents
A kind of vinyl tributyl ketoximyl silane continuous reaction system Download PDFInfo
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- CN108299489A CN108299489A CN201810138622.9A CN201810138622A CN108299489A CN 108299489 A CN108299489 A CN 108299489A CN 201810138622 A CN201810138622 A CN 201810138622A CN 108299489 A CN108299489 A CN 108299489A
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- Prior art keywords
- reaction
- pipe type
- bundle pipe
- cooling water
- bundle
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- 238000006243 chemical reaction Methods 0.000 title claims abstract description 130
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 title claims abstract description 24
- 229910000077 silane Inorganic materials 0.000 title claims abstract description 24
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 title claims abstract description 20
- 229920002554 vinyl polymer Polymers 0.000 title claims abstract description 20
- 238000007599 discharging Methods 0.000 claims abstract description 23
- 239000000463 material Substances 0.000 claims description 89
- 239000000498 cooling water Substances 0.000 claims description 37
- FSEUPUDHEBLWJY-HWKANZROSA-N diacetylmonoxime Chemical compound CC(=O)C(\C)=N\O FSEUPUDHEBLWJY-HWKANZROSA-N 0.000 claims description 25
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 claims description 24
- 238000000605 extraction Methods 0.000 claims description 20
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 20
- GQIUQDDJKHLHTB-UHFFFAOYSA-N trichloro(ethenyl)silane Chemical compound Cl[Si](Cl)(Cl)C=C GQIUQDDJKHLHTB-UHFFFAOYSA-N 0.000 claims description 19
- 239000005050 vinyl trichlorosilane Substances 0.000 claims description 19
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 18
- 229910052802 copper Inorganic materials 0.000 claims description 18
- 239000010949 copper Substances 0.000 claims description 18
- 239000002994 raw material Substances 0.000 claims description 18
- 210000005239 tubule Anatomy 0.000 claims description 18
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 16
- 230000008602 contraction Effects 0.000 claims description 14
- 238000002156 mixing Methods 0.000 claims description 13
- 235000019270 ammonium chloride Nutrition 0.000 claims description 12
- 125000004836 hexamethylene group Chemical group [H]C([H])([*:2])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[*:1] 0.000 claims description 10
- ZWEHNKRNPOVVGH-UHFFFAOYSA-N 2-Butanone Chemical compound CCC(C)=O ZWEHNKRNPOVVGH-UHFFFAOYSA-N 0.000 claims description 8
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 claims description 8
- 229910021529 ammonia Inorganic materials 0.000 claims description 8
- 239000000284 extract Substances 0.000 claims description 8
- 230000007062 hydrolysis Effects 0.000 claims description 8
- 238000006460 hydrolysis reaction Methods 0.000 claims description 8
- 239000007787 solid Substances 0.000 claims description 8
- 239000002904 solvent Substances 0.000 claims description 8
- 239000003921 oil Substances 0.000 claims description 5
- 235000019198 oils Nutrition 0.000 claims description 5
- WHIVNJATOVLWBW-PLNGDYQASA-N (nz)-n-butan-2-ylidenehydroxylamine Chemical compound CC\C(C)=N/O WHIVNJATOVLWBW-PLNGDYQASA-N 0.000 claims description 4
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 claims description 4
- 239000005977 Ethylene Substances 0.000 claims description 4
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 4
- 238000005915 ammonolysis reaction Methods 0.000 claims description 4
- 230000008859 change Effects 0.000 claims description 4
- 238000002425 crystallisation Methods 0.000 claims description 4
- 230000008025 crystallization Effects 0.000 claims description 4
- 239000007788 liquid Substances 0.000 claims description 4
- 238000006386 neutralization reaction Methods 0.000 claims description 4
- 125000005646 oximino group Chemical group 0.000 claims description 4
- 230000001376 precipitating effect Effects 0.000 claims description 4
- 238000004062 sedimentation Methods 0.000 claims description 4
- 238000000926 separation method Methods 0.000 claims description 4
- 238000003756 stirring Methods 0.000 claims description 4
- 239000008157 edible vegetable oil Substances 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 3
- 238000001816 cooling Methods 0.000 claims 1
- 238000004519 manufacturing process Methods 0.000 abstract description 10
- 238000005265 energy consumption Methods 0.000 abstract description 2
- 239000002184 metal Substances 0.000 description 6
- 229910052751 metal Inorganic materials 0.000 description 6
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 5
- 239000010439 graphite Substances 0.000 description 5
- 229910002804 graphite Inorganic materials 0.000 description 5
- 238000000034 method Methods 0.000 description 5
- 229920003023 plastic Polymers 0.000 description 5
- 239000004033 plastic Substances 0.000 description 5
- 239000000919 ceramic Substances 0.000 description 3
- 230000007797 corrosion Effects 0.000 description 3
- 238000005260 corrosion Methods 0.000 description 3
- 238000010586 diagram Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- XDTMQSROBMDMFD-UHFFFAOYSA-N Cyclohexane Chemical compound C1CCCCC1 XDTMQSROBMDMFD-UHFFFAOYSA-N 0.000 description 1
- -1 and groove Substances 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000007689 inspection Methods 0.000 description 1
- 238000002955 isolation Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 1
- 238000012805 post-processing Methods 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 230000036632 reaction speed Effects 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F7/00—Compounds containing elements of Groups 4 or 14 of the Periodic Table
- C07F7/02—Silicon compounds
- C07F7/08—Compounds having one or more C—Si linkages
- C07F7/0834—Compounds having one or more O-Si linkage
- C07F7/0892—Compounds with a Si-O-N linkage
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/24—Stationary reactors without moving elements inside
- B01J19/2415—Tubular reactors
- B01J19/242—Tubular reactors in series
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Silicon Compounds (AREA)
Abstract
A kind of vinyl tributyl ketoximyl silane continuous reaction system, including premix tank, bundle pipe type reactor, the bundle pipe type reactor includes reaction feeder, discharging collection chamber and at least one bundle pipe type reaction module, the reaction feeder is located at the top of bundle pipe type reaction module, and bundle pipe type reaction module bottom is provided with discharging collection chamber；The bundle pipe type reaction module constitutes bundle pipe type reaction module combination application after connecting up and down with other bundle pipe type reaction module.The present invention has the advantages that temperature precise control, safe and reliable, floor space is small, management is simplified；Using bundle pipe type reactor, temperature precise control, safe and reliable reactor continuous feeding and discharging is, it can be achieved that accurate dosing under DCS controls, labor intensity of operating staff substantially reduce；Compared to existing autoclave batch reactor production efficiency height, low energy consumption.
Description
Technical field
The present invention relates to chemical reactor technical field, especially a kind of vinyl tributyl ketoximyl silane continuous reaction
System.
Background technology
The tank reactor of intermittently operated, be all reactants are primary before operation be added, with the progress of reaction,
Temperature in the kettle, concentration and reaction speed all change over time, always until being reached scheduled conversion ratio discharging.Currently,
Batch still due to its is simple in structure, easy to operate, flexibility is big by extensive use, but the charging of batch still, discharging, inspection
And non-cutting time needed for cleaning equipment etc. is long, causes labor intensity high, low production efficiency cannot be satisfied prior art requirement, because
This urgent need develops a set of continuous reaction technique to solve prior art deficiency.
Invention content
The purpose of the present invention is in view of the shortcomings of the prior art, providing a kind of vinyl tributyl ketoximyl silane continuous reaction
System, to solve the problems, such as above-mentioned background technology.
To solve prior art problem, the technical solution adopted by the present invention is：A kind of vinyl tributyl ketoximyl silane company
Continuousization reaction system, it is characterized in that the reaction system includes premix tank, bundle pipe type reactor, the bundle pipe type reaction
Device includes that reaction feeder, discharging collection chamber and at least one bundle pipe type reaction module, the reaction feeder are located at boundling
Pipe reaction module top, bundle pipe type reaction module bottom are provided with discharging collection chamber；
The first raw material mouth and the second raw material mouth are equipped at the top of the premix tank, the first raw material mouth connects with diacetylmonoxime mother tube
It connects, the second raw material mouth is connect with hexamethylene mother tube；
The reaction feeder is mainly made of upper cavity, the lower chamber for being located at upper cavity bottom, is equipped at the top of the upper cavity
Third raw material mouth, third raw material mouth are connect with vinyl trichlorosilane feed pipe, and the side of the lower chamber is equipped with mixed material
Feed inlet；
The premix tank bottom is exported equipped with mixed material, and the mixed material outlet is fed by discharge nozzle and mixed material
Mouth connection；
The bundle pipe type reaction module includes material main body, and reducing materail tube, the change are axially arranged in the material main body
Diameter materail tube has expansion segment and contraction section, and cooling water pipe is additionally provided in the material main body；
The lower chamber lower shaft is to multiple water conservancy diversion tubules are provided with, and water conservancy diversion tubule upper end passes through at the top of lower chamber and upper cavity
Connection, water conservancy diversion tubule lower end stretches in reducing materail tube；
The discharging collection chamber bottom is equipped with reaction mass discharge port, and the reaction mass discharge port passes through reaction mass discharge nozzle
It is connect with curing kettle top entry, the curing bottom portion is exported equipped with reaction material, and the reaction material outlet is connect with drainage conduit.
Preferably, the upper cavity bottom is equipped with plush copper, groove, the lower chamber bottom are equipped at the top of the lower chamber
Equipped with plush copper, groove is equipped at the top of the material main body, the material main body bottom is equipped with plush copper, the discharging collection chamber top
Equipped with groove；Upper cavity bottom plush copper is adapted with lower chamber top groove, lower chamber bottom plush copper and base material sheet
Body top groove is adapted, and material main body bottom plush copper is adapted with discharging collection chamber top groove.
Preferably, being radially provided with cooling water pipe in the material main body, one side of the material main body is equipped with cooling water
Distributor box, material main body the other side are equipped with cooling water collection box, and the cooling water distributor box is equipped with cooling water inlet, cooling
Water collector is equipped with cooling water outlet, and the one end of the cooling water pipe is connect with cooling water distributor box, and cooling water pipe is another
End is connect with cooling water collection box.
Preferably, the reducing materail tube expansion segment diameter 6~40mm, 3~20mm of the contraction section diameter, the receipts
10~1000mm of contracting segment length；
Preferably, a diameter of 8~12mm of reducing materail tube expansion segment；The reducing materail tube contraction section a diameter of 4~
6mm, the contraction segment length are 200~500mm.
Preferably, 0.5~2mm of interior diameter at the water conservancy diversion tubule lower part outlet.
Preferably, interior diameter is 0.8~1mm at the water conservancy diversion tubule lower part outlet.
Preferably, the reducing materail tube entrance and exit is expansion segment, water conservancy diversion tubule lower end extends to reducing
The inlet of first contraction section of materail tube.
Collect preferably, the bundle pipe type reaction module is constituted after connecting up and down with other bundle pipe type reaction module
Beam tube type reaction module combination application.
A kind of vinyl tributyl ketoximyl silane continuous reaction technique, steps are as follows for reaction process：
A. by diacetylmonoxime and hexamethylene according to mass ratio 1：0.5~5 proportioning after mass flowmenter continuous metering respectively by flowing
Enter premix tank, mixed material is obtained after uniform stirring mixing in blending tank；
B. by the mixed material waited until in step A by being sent into bundle pipe type reactor after mass flowmenter continuous metering；Simultaneously
Vinyl trichlorosilane according to diacetylmonoxime mass ratio 1：Vinyl trichlorosilane is passed through mass flow by 0.1~0.3 proportioning
With being pumped into bundle pipe type reactor after meter continuous metering；
C. after mixed material is mixed and reacted rapidly with vinyl trichlorosilane, reaction material, reaction temperature control 20~60 are obtained
℃；
D. the obtained reaction material in step C is delivered into curing kettle, the reaction material then gone out from curing kettle is layered as edible vegetable oil
Layer and oximate layer；
E. the boiled oil layer in step D enters to neutralize in kettle with ammonia and neutralize, and sedimentation separation is chloride solid and mixing after neutralization
Liquid, chloride solid enter after precipitating in extraction kettle；Mixed liquor is detached by rectifying column, and high-purity ethylene base three is obtained in tower reactor
Butanone oximino silane finished product；
F. the solvent also isolated at the top of rectifying column in step E enters extraction kettle, and rectifier light component material is back to boundling
Tubular reactor；
G. oximate layer is squeezed by pump in extraction kettle in step D, and the solvent that extraction kettle includes extract returns to after metering
In bundle pipe type reactor；Butanone oxime hydrochloride in extraction kettle after extractant extracts removes hydrolysis kettle, then logical by hydrolysis
It is layered after entering ammonia ammonolysis, is divided into diacetylmonoxime layer and ammonium chloride solution layer；
H. diacetylmonoxime layer recycles after being dehydrated rectifying in step G, then is back to bundle pipe type reactor reaction；
I. ammonium chloride solution layer is dried to obtain ammonium chloride after evaporative crystallization in step G.
Preferably, diacetylmonoxime and hexamethylene are according to mass ratio 1 in the step A：1~2 quality proportioning.
Preferably, diacetylmonoxime and vinyl trichlorosilane are according to mass ratio 1 in the step B：0.27~0.29 matches
Than.
Preferably, reaction temperature is divided into two sections of controls, 25~30 DEG C of leading portion, 35~40 DEG C of back segment in the step C.
In bundle pipe type reaction module, one reaction mass directly enters from materail tube opening, and another strand of material is by anti-
The water conservancy diversion tubule of feeder is answered to send to the minor diameter of materail tube part, two strands of materials form fierce turbulent flow and mix rapidly simultaneously herein
Reaction；Feeder realizes the two kinds of easily isolation of vigorous reaction material before the reaction, and realizes two kinds of easily plays in reaction
Strong reaction mass evenly distributes, and avoids quality, safety accident that the uneven hybrid reaction of reaction mass causes.
Heat of reaction is transferred to rapidly cooling water by base material, and takes bundle pipe type reaction module out of by cooling water, to protect
Reaction temperature is demonstrate,proved to stablize in control range.
The present invention has the advantages that temperature precise control, safe and reliable, floor space is small, management is simplified；Using bundle pipes
Formula reactor, temperature precise control, safe and reliable reactor continuous feeding and discharging operate, it can be achieved that the lower accurate dosing of DCS controls
Personnel labor intensity substantially reduces；Compared to existing autoclave batch reactor production efficiency height, low energy consumption, and products obtained therefrom quality
It is more stable.
Description of the drawings
Fig. 1 is the structural schematic diagram of the present invention；
Fig. 2 is the structural schematic diagram of bundle pipe type reactor in Fig. 1.
Specific implementation mode
To facilitate the understanding of the present invention, below with reference to relevant drawings to invention is more fully described.In attached drawing
Give the present invention preferred embodiment.But the present invention can realize in different forms, however it is not limited to be retouched herein
The embodiment stated.It is opposite, purpose of providing these embodiments is make it is more thorough and comprehensive to the disclosure.
A kind of vinyl tributyl ketoximyl silane continuous reaction system, including premix tank 6, bundle pipe type reactor 7,
Kettle 8 is cured, is connect with diacetylmonoxime mother tube 62 by the first raw material mouth 61 at the top of the premix tank, at the top of the premix tank
It is additionally provided with the second raw material mouth 63, the second raw material mouth 63 is connect with hexamethylene mother tube 64；The premix tank bottom is equipped with
Material outlet 65, the material outlet are connect by discharge nozzle 66 with bundle pipe type reactor head second charging aperture 17；It is described
Bundle pipe type reactor includes reaction feeder 1, discharging collection chamber 5 and at least one bundle pipe type reaction module 2；Reaction charging
Device 1 is located at 2 top of bundle pipe type reaction module, and bundle pipe type reaction module bottom is provided with discharging collection chamber 5.Bundle pipes
Formula reaction module constitutes bundle pipe type reaction module combination application after connecting up and down with other bundle pipe type reaction module.It is described
Reaction feeder includes upper cavity 11, lower chamber 15, water conservancy diversion tubule 16, and third raw material mouth 12 is equipped at the top of upper cavity, and third is former
Material mouth 12 is connect with vinyl trichlorosilane feed pipe 71.The upper cavity bottom is equipped with plush copper 13, is set at the top of the lower chamber
Fluted 14, upper cavity bottom plush copper is adapted with lower chamber top groove.The side of the lower chamber is equipped with second charging aperture
17, it is equipped with more longitudinally disposed water conservancy diversion tubules 16 in the lower chamber, 18 interior diameters 0.5 at the water conservancy diversion tubule lower part outlet
~2mm, preferred a diameter of 0.8~1mm, the lower chamber bottom is equipped with plush copper.
The bundle pipe type reaction module 2 includes cooling water distributor box 3, cooling water pipe 36, material main body 21, reducing material
Pipe 4, cooling water collection box 33,21 1 side of the material main body are equipped with cooling water distributor box 3,21 other side of the material main body
Portion be equipped with cooling water collection box 33, the cooling water distributor box be equipped with cooling water inlet 31, the cooling water distributor box with it is cold
But 36 end of water pipe connects, and the more cooling water pipes being laterally arranged are equipped in the material main body, are also set in the material main body
There are multiple longitudinally disposed reducing materail tubes 4, the reducing materail tube to be equipped with expansion segment 37 and contraction section 42, reducing materail tube enters
Mouth and outlet are expansion segment, and water conservancy diversion tubule lower end extends to the inlet of first contraction section of reducing materail tube.Expansion segment
Locate 6~40mm of diameter, preferred a diameter of 8~12mm.3~20mm of diameter at the contraction section, preferred a diameter of 4~6mm.
Contraction 10~the 1000mm of segment length, preferred segment length of shrinking is 200~500mm.Cooling water collection box and cooling water pipe
End connects, and groove is equipped at the top of the material main body, and lower chamber bottom plush copper is adapted with material main body top groove.It is described
Material main body bottom is equipped with plush copper, and groove, material main body bottom plush copper and discharging collection chamber are equipped at the top of the discharging collection chamber
Top groove is adapted.5 bottom of discharging collection chamber is equipped with reaction material discharge port 51.The reaction material discharge port passes through reaction
Material discharge nozzle 52 is connect with curing 8 top entry 81 of kettle, and the curing bottom portion is equipped with reaction material and exports 82, and the reaction material goes out
Mouth 82 is connect with drainage conduit 83.
Feeder 1 is reacted using metal, plastics, ceramics, graphite manufacture, preferably corrosion resistant metal, polytetrafluoroethylplastic plastic
Manufacture；Bundle pipe type reaction module 2 is manufactured using metal, ceramics, graphite, plastic manufacturing, preferably graphite and corrosion resistant metal, into
One step preferably uses graphite to manufacture；The discharging use of collection chamber 5 metal, plastics, ceramics, graphite manufacture, preferably corrosion resistant metal gather
Ptfe plastic manufactures.
Its operation principle is that vinyl trichlorosilane material enters the upper cavity of reaction feeder by third raw material mouth 12
Interior, in premix tank after evenly mixing, mixed material is entered by second charging aperture 17 to react for diacetylmonoxime, hexamethylene raw material
In the lower chamber of feeder, diacetylmonoxime, cyclohexane mixtures material at reducing materail tube and water conservancy diversion tubule outlet at bottom by flowing out
Vinyl trichlorosilane material fast reaction, since fast reaction will produce high temperature, reaction while, will be more by cooling water pipe
Remaining heat is taken out of.It after the completion of reducing material inner reaction tube, drops down onto in discharging collection chamber, is discharged by reaction material outlet ripe
Change and handled in kettle, the reaction material come out from curing kettle is handled with postprocessing working procedures are pumped into.Bundle pipe type reaction module 2 can
According to actual production increase in demand or reduction, to have saved production space.
Embodiment 1
A kind of vinyl tributyl ketoximyl silane continuous reaction technique, steps are as follows for reaction process：
A. by diacetylmonoxime and hexamethylene according to mass ratio 1：2 proportioning is premixed by being flowed into after mass flowmenter continuous metering respectively
Tank is closed, mixed material is obtained after uniform stirring mixing in blending tank；
B. by the mixed material waited until in step A by being sent into bundle pipe type reactor after mass flowmenter continuous metering；Simultaneously
Vinyl trichlorosilane according to diacetylmonoxime mass ratio 1：0.26 proportioning connects vinyl trichlorosilane by mass flowmenter
With being pumped into bundle pipe type reactor after continuous metering；
C. after mixed material is mixed and reacted rapidly with vinyl trichlorosilane, reaction material, reaction temperature leading portion control 25 are obtained
DEG C, reaction temperature back segment controls 40 DEG C；
D. the obtained reaction material in step C is delivered into curing kettle 8, the reaction material then gone out from curing kettle 8 is layered as clearly
Oil reservoir and oximate layer；
E. the boiled oil layer in step D enters to neutralize in kettle with ammonia and neutralize, and sedimentation separation is chloride solid and mixing after neutralization
Liquid, chloride solid enter after precipitating in extraction kettle；Mixed liquor is detached by rectifying column, and high-purity ethylene base three is obtained in tower reactor
Butanone oximino silane finished product；
F. the solvent also isolated at the top of rectifying column in step E enters extraction kettle, and rectifier light component material is back to boundling
Tubular reactor；
G. oximate layer is squeezed by pump in extraction kettle in step D, and the solvent that extraction kettle includes extract returns to after metering
In bundle pipe type reactor；Butanone oxime hydrochloride in extraction kettle after extractant extracts removes hydrolysis kettle, then logical by hydrolysis
It is layered after entering ammonia ammonolysis, is divided into diacetylmonoxime layer and ammonium chloride solution layer；
H. diacetylmonoxime layer recycles after being dehydrated rectifying in step G, then is back to bundle pipe type reactor reaction；
I. ammonium chloride solution layer is dried to obtain ammonium chloride after evaporative crystallization in step G.
Embodiment 2
A kind of vinyl tributyl ketoximyl silane continuous reaction technique, steps are as follows for reaction process：
A. by diacetylmonoxime and hexamethylene according to mass ratio 1：1 proportioning is premixed by being flowed into after mass flowmenter continuous metering respectively
Tank is closed, mixed material is obtained after uniform stirring mixing in blending tank；
B. by the mixed material waited until in step A by being sent into bundle pipe type reactor after mass flowmenter continuous metering；Simultaneously
Vinyl trichlorosilane according to diacetylmonoxime mass ratio 1：0.29 proportioning connects vinyl trichlorosilane by mass flowmenter
With being pumped into bundle pipe type reactor after continuous metering；
C. after mixed material is mixed and reacted rapidly with vinyl trichlorosilane, reaction material, reaction temperature leading portion control 30 are obtained
DEG C, reaction temperature back segment controls 35 DEG C；
D. the obtained reaction material in step C is delivered into curing kettle, the reaction material then gone out from curing kettle is layered as edible vegetable oil
Layer and oximate layer；
E. the boiled oil layer in step D enters to neutralize in kettle with ammonia and neutralize, and sedimentation separation is chloride solid and mixing after neutralization
Liquid, chloride solid enter after precipitating in extraction kettle；Mixed liquor is detached by rectifying column, and high-purity ethylene base three is obtained in tower reactor
Butanone oximino silane finished product；
F. the solvent also isolated at the top of rectifying column in step E enters extraction kettle, and rectifier light component material is back to boundling
Tubular reactor；
G. oximate layer is squeezed by pump in extraction kettle in step D, and the solvent that extraction kettle includes extract returns to after metering
In bundle pipe type reactor；Butanone oxime hydrochloride in extraction kettle after extractant extracts removes hydrolysis kettle, then logical by hydrolysis
It is layered after entering ammonia ammonolysis, is divided into diacetylmonoxime layer and ammonium chloride solution layer；
H. diacetylmonoxime layer recycles after being dehydrated rectifying in step G, then is back to bundle pipe type reactor reaction；
I. ammonium chloride solution layer is dried to obtain ammonium chloride after evaporative crystallization in step G.
Embodiment of the present invention is only the description carried out to the preferred embodiment of the present invention, not to the present invention
Conception and scope is defined, and not departing from the present invention relates under the premise of thought, engineers and technicians are to this hair in this field
The various modifications and improvement that bright technical solution is made should all fall into protection scope of the present invention, the claimed skill of the present invention
It uses, has all been recorded in detail in the claims in art.
Claims (10)
1. a kind of vinyl tributyl ketoximyl silane continuous reaction system, it is characterized in that the reaction system includes premixing
Tank, bundle pipe type reactor, the bundle pipe type reactor include reaction feeder, discharging collection chamber and at least one bundle pipes
Formula reaction module, the reaction feeder are located at the top of bundle pipe type reaction module, and bundle pipe type reaction module bottom is set
It is equipped with discharging collection chamber；
The first raw material mouth and the second raw material mouth are equipped at the top of the premix tank, the first raw material mouth connects with diacetylmonoxime mother tube
It connects, the second raw material mouth is connect with hexamethylene mother tube；
The reaction feeder is mainly made of upper cavity, the lower chamber for being located at upper cavity bottom, is equipped at the top of the upper cavity
Third raw material mouth, third raw material mouth are connect with vinyl trichlorosilane feed pipe, and the side of the lower chamber is equipped with mixed material
Feed inlet；
The premix tank bottom is exported equipped with mixed material, and the mixed material outlet is fed by discharge nozzle and mixed material
Mouth connection；
The bundle pipe type reaction module includes material main body, and reducing materail tube, the change are axially arranged in the material main body
Diameter materail tube has expansion segment and contraction section, and cooling water pipe is additionally provided in the material main body；
The lower chamber lower shaft is to multiple water conservancy diversion tubules are provided with, and water conservancy diversion tubule upper end passes through at the top of lower chamber and upper cavity
Connection, water conservancy diversion tubule lower end stretches in reducing materail tube；
The discharging collection chamber bottom is equipped with reaction mass discharge port, and the reaction mass discharge port passes through reaction mass discharge nozzle
It is connect with curing kettle top entry, the curing bottom portion is exported equipped with reaction material, and the reaction material outlet is connect with drainage conduit.
2. a kind of vinyl tributyl ketoximyl silane continuous reaction system according to claim 1, it is characterised in that institute
It states upper cavity bottom and is equipped with plush copper, groove is equipped at the top of the lower chamber, the lower chamber bottom is equipped with plush copper, the base material sheet
Groove is equipped at the top of body, the material main body bottom is equipped with plush copper, groove is equipped at the top of the discharging collection chamber；The upper cavity
Bottom plush copper is adapted with lower chamber top groove, and lower chamber bottom plush copper is adapted with material main body top groove, institute
Material main body bottom plush copper is stated to be adapted with discharging collection chamber top groove.
3. a kind of vinyl tributyl ketoximyl silane continuous reaction system according to claim 1, it is characterised in that institute
It states and is radially provided with cooling water pipe in material main body, one side of the material main body is equipped with cooling water distributor box, and material main body is another
Side is equipped with cooling water collection box, and the cooling water distributor box is equipped with cooling water inlet, and cooling water collection box is equipped with cooling
The one end of water out, the cooling water pipe is connect with cooling water distributor box, cooling water pipe the other end and cooling water collection box
Connection.
4. a kind of vinyl tributyl ketoximyl silane continuous reaction system according to claim 1, it is characterised in that institute
State reducing materail tube expansion segment 6~40mm of diameter, the preferably a diameter of 8~12mm of reducing materail tube expansion segment；The contraction section is straight
3~20mm of diameter, the preferably a diameter of 4~6mm of reducing materail tube contraction section；Contraction 10~the 1000mm of segment length, preferably shrinks
Segment length is 200~500mm.
5. a kind of vinyl tributyl ketoximyl silane continuous reaction system according to claim 1, it is characterised in that institute
0.5~2mm of interior diameter at water conservancy diversion tubule lower part outlet is stated, interior diameter is 0.8~1mm preferably at water conservancy diversion tubule lower part outlet.
6. a kind of vinyl tributyl ketoximyl silane continuous reaction system according to claim 1, it is characterised in that institute
The entrance and exit for stating reducing materail tube is expansion segment, and water conservancy diversion tubule lower end extends to first contraction section of reducing materail tube
Inlet.
7. a kind of vinyl tributyl ketoximyl silane continuous reaction system according to claim 1, it is characterised in that institute
Composition bundle pipe type reaction module after bundle pipe type reaction module is connected up and down with other bundle pipe type reaction module is stated to combine
Using.
8. a kind of reaction process using vinyl tributyl ketoximyl silane continuous reaction system described in claim 1, work
Steps are as follows for skill：
A. by diacetylmonoxime and hexamethylene according to mass ratio 1：0.5~5 proportioning after mass flowmenter continuous metering respectively by flowing
Enter premix tank, mixed material is obtained after uniform stirring mixing in blending tank；
B. by the mixed material waited until in step A by being sent into bundle pipe type reactor after mass flowmenter continuous metering；Simultaneously
Vinyl trichlorosilane according to diacetylmonoxime mass ratio 1：Vinyl trichlorosilane is passed through mass flow by 0.1~0.3 proportioning
With being pumped into bundle pipe type reactor after meter continuous metering；
C. after mixed material is mixed and reacted rapidly with vinyl trichlorosilane, reaction material, reaction temperature control 20~60 are obtained
℃；
D. the obtained reaction material in step C is delivered into curing kettle, the reaction material then gone out from curing kettle is layered as edible vegetable oil
Layer and oximate layer；
E. the boiled oil layer in step D enters to neutralize in kettle with ammonia and neutralize, and sedimentation separation is chloride solid and mixing after neutralization
Liquid, chloride solid enter after precipitating in extraction kettle；Mixed liquor is detached by rectifying column, and high-purity ethylene base three is obtained in tower reactor
Butanone oximino silane finished product；
F. the solvent also isolated at the top of rectifying column in step E enters extraction kettle, and rectifier light component material is back to boundling
Tubular reactor；
G. oximate layer is squeezed by pump in extraction kettle in step D, and the solvent that extraction kettle includes extract returns to after metering
In bundle pipe type reactor；Butanone oxime hydrochloride in extraction kettle after extractant extracts removes hydrolysis kettle, then logical by hydrolysis
It is layered after entering ammonia ammonolysis, is divided into diacetylmonoxime layer and ammonium chloride solution layer；
H. diacetylmonoxime layer recycles after being dehydrated rectifying in step G, then is back to bundle pipe type reactor reaction；
I. ammonium chloride solution layer is dried to obtain ammonium chloride after evaporative crystallization in step G.
9. a kind of reaction process of vinyl tributyl ketoximyl silane continuous reaction system according to claim 8,
It is characterized in that diacetylmonoxime and hexamethylene are according to mass ratio 1 in the step A：1~2 quality proportioning；Diacetylmonoxime in the step B
With vinyl trichlorosilane according to mass ratio 1：0.27~0.29 proportioning.
10. a kind of reaction process of vinyl tributyl ketoximyl silane continuous reaction system according to claim 8,
It is characterized in that in the step C that reaction temperature is divided into two sections of controls, 25~30 DEG C of leading portion, 35~40 DEG C of back segment.
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| CN115193353A (en) * | 2022-06-28 | 2022-10-18 | 四川花语精细化工有限公司 | Production device and process of dodecyl trimethyl ammonium chloride |
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