CN110183479A - A kind of system and technique of the hydrolysis of low pressure dimethyldichlorosilane - Google Patents
A kind of system and technique of the hydrolysis of low pressure dimethyldichlorosilane Download PDFInfo
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- CN110183479A CN110183479A CN201910522412.4A CN201910522412A CN110183479A CN 110183479 A CN110183479 A CN 110183479A CN 201910522412 A CN201910522412 A CN 201910522412A CN 110183479 A CN110183479 A CN 110183479A
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- hydrolysis
- analytic tower
- dimethyldichlorosilane
- separator
- low pressure
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- 238000006460 hydrolysis reaction Methods 0.000 title claims abstract description 85
- 230000007062 hydrolysis Effects 0.000 title claims abstract description 84
- LIKFHECYJZWXFJ-UHFFFAOYSA-N dimethyldichlorosilane Chemical compound C[Si](C)(Cl)Cl LIKFHECYJZWXFJ-UHFFFAOYSA-N 0.000 title claims abstract description 41
- 238000000034 method Methods 0.000 title claims abstract description 30
- 230000008676 import Effects 0.000 claims abstract description 26
- 239000012528 membrane Substances 0.000 claims abstract description 19
- 239000007788 liquid Substances 0.000 claims abstract description 17
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 17
- 239000012071 phase Substances 0.000 claims abstract description 16
- 239000007791 liquid phase Substances 0.000 claims abstract description 12
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 75
- 238000006243 chemical reaction Methods 0.000 claims description 36
- 229910000041 hydrogen chloride Inorganic materials 0.000 claims description 33
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 claims description 33
- 239000007789 gas Substances 0.000 claims description 21
- 239000002253 acid Substances 0.000 claims description 13
- 239000007792 gaseous phase Substances 0.000 claims description 9
- 239000000463 material Substances 0.000 claims description 9
- 239000011344 liquid material Substances 0.000 claims description 6
- 238000009833 condensation Methods 0.000 claims description 5
- 230000005494 condensation Effects 0.000 claims description 5
- 239000000945 filler Substances 0.000 claims description 4
- 238000009434 installation Methods 0.000 claims description 3
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 claims description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 2
- 230000008859 change Effects 0.000 claims description 2
- 239000000460 chlorine Substances 0.000 claims description 2
- 229910052801 chlorine Inorganic materials 0.000 claims description 2
- 239000001257 hydrogen Substances 0.000 claims description 2
- 229910052739 hydrogen Inorganic materials 0.000 claims description 2
- 150000003839 salts Chemical class 0.000 claims 1
- 239000000413 hydrolysate Substances 0.000 description 20
- 239000000047 product Substances 0.000 description 18
- 239000003921 oil Substances 0.000 description 10
- 239000000243 solution Substances 0.000 description 10
- 229920006395 saturated elastomer Polymers 0.000 description 8
- 230000000052 comparative effect Effects 0.000 description 7
- 238000005903 acid hydrolysis reaction Methods 0.000 description 6
- 230000008569 process Effects 0.000 description 6
- 238000000926 separation method Methods 0.000 description 5
- 238000000746 purification Methods 0.000 description 4
- 230000003068 static effect Effects 0.000 description 4
- 238000005406 washing Methods 0.000 description 4
- 238000003556 assay Methods 0.000 description 3
- 239000007795 chemical reaction product Substances 0.000 description 3
- 238000004458 analytical method Methods 0.000 description 2
- 230000007423 decrease Effects 0.000 description 2
- 230000007812 deficiency Effects 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000013589 supplement Substances 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- 150000001335 aliphatic alkanes Chemical class 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 239000013505 freshwater Substances 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 230000008439 repair process Effects 0.000 description 1
- 230000011218 segmentation Effects 0.000 description 1
- 239000007787 solid 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
- C07F7/0836—Compounds with one or more Si-OH or Si-O-metal linkage
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
Abstract
Present disclose provides the systems and technique of a kind of hydrolysis of low pressure dimethyldichlorosilane, the system includes hydrolysis reactor, circulating pump, Analytic Tower, separator, the import of the outlet connection Analytic Tower of the hydrolysis reactor, the liquid-phase outlet of the Analytic Tower connects separator import, the separator water phase outlet connection pump inlet, the circulating-pump outlet connects hydrolysis reactor import, the feed-line of the pipeline connection dimethyldichlorosilane between circulating pump and hydrolysis reactor；The Analytic Tower includes distributing disc and at membrane module, the distributing disc is set to the upper position inside falling liquid film Analytic Tower, liquid distributing hole is provided on the distributing disc, the lower section that distributing disc is set at membrane module is described to be composed of at membrane module several groups " people " font plate；The tubular structure that the separator is vertically arranged, bottom are exported equipped with water phase, and top is equipped with oil and mutually exports.
Description
Technical field
This disclosure relates to a kind of system and technique of the hydrolysis of low pressure dimethyldichlorosilane.
Background technique
Here statement only provides background information related with the disclosure, without necessarily constituting the prior art.
Currently, there are two types of domestic the sector dimethyldichlorosilane hydrolysis process, one is azeotropic acid hydrolysis, the technique side
The hydrolysate quality that method obtains is relatively good, but it is larger to consume energy, and the oil-containing spent acid of by-product is more intractable, this process base
This is no longer used in the industry.Another method is saturated acid hydrolysis (frequently referred to " Concentrated acid hydrolysis "), and the disclosed invention people grinds
Study carefully discovery, this method is since reaction pressure is relatively higher, acid concentration is higher, so there are dimethyldichlorosilane reaction is endless
Entirely, the situation that end group chlorinity is high, hydrolysate viscosity is high, acid value is higher, so that the setting of subsequent purification washing system is more multiple
Miscellaneous, process is relatively long, increases investment and operating cost.
Summary of the invention
In order to solve the deficiencies in the prior art, purpose of this disclosure is to provide a kind of hydrolysis of low pressure dimethyldichlorosilane
The preferable hydrolysate product of quality can be obtained in system and technique, the technique；Meanwhile greatly reducing the folder of output hydrogen chloride gas
Band oil mass, alleviates the influence to follow-up system.Because this technique hydrolysis reaction pressure reduces, system equipment, pipeline integral load
Decline, solid circulating rate decline, largely reduces construction cost and operating cost.
To achieve the goals above, the technical solution of the disclosure are as follows:
On the one hand, the system of a kind of low pressure dimethyldichlorosilane hydrolysis, including hydrolysis reactor, circulating pump, Analytic Tower,
Separator, the import of the outlet connection Analytic Tower of the hydrolysis reactor, the liquid-phase outlet of the Analytic Tower connect separator into
Mouthful, separator water phase outlet connection pump inlet, the circulating-pump outlet connects hydrolysis reactor import, circulating pump with
The feed-line of pipeline connection dimethyldichlorosilane between hydrolysis reactor；
The Analytic Tower includes distributing disc and at membrane module, and the distributing disc is set to the middle and upper part inside falling liquid film Analytic Tower
Position, is provided with liquid distributing hole on the distributing disc, the lower section that distributing disc is set at membrane module, it is described at membrane module by several
Group " people " font plate is composed, and gaseous phase outlet is opened up at the top of Analytic Tower, and parsing tower bottom opens up liquid-phase outlet；
The tubular structure that the separator is vertically arranged, bottom are exported equipped with water phase, and top is equipped with oil and mutually exports.
Firstly, circulating pump is arranged in the disclosure between hydrolysis reactor and separator, the hydrochloric acid in separator is delivered to
In hydrolysis reactor, the effect of the circulating pump are as follows: 1. provide part reaction pressure to hydrolysis reactor, to make the hydrolysis
It can continue to carry out, 2. are pre-mixed the reaction water of recycle acid and supplement sufficiently, mention for dimethyldichlorosilane hydrolysis
The moisture needed for reaction.
Secondly, Analytic Tower is arranged in the disclosure, the material after hydrolysis flows into the conjunction of " people " font board group after entering Analytic Tower
Membrane module make generate hydrogen chloride gas escape in time, it is therefore prevented that gas film behavior, be more conducive to hydrolysis forward direction progress,
To further increase the reaction yield of product.
Circulating pump is arranged in hydrolysis reactor import in third, the disclosure, exports setting Analytic Tower, the group in hydrolysis reactor
Closing setting can make dimethyldichlorosilane reaction more complete, effectively increase the conversion ratio of dimethyldichlorosilane, and make
The acidity value for obtaining product substantially reduces, and (acidity value of common saturated acid hydrolysis prods is generally 3% lower than 1.2% for acidity value
More than).
On the other hand, the technique of a kind of low pressure dimethyldichlorosilane hydrolysis, provides above system, and circulating pump is by separator
In hydrochloric acid extraction after be pre-mixed with dimethyldichlorosilane after be delivered in hydrolysis reactor and carry out a hydrolysis,
Material after hydrolysis enters Analytic Tower, and material forms liquid film at membrane module Analytic Tower, the hydrogen chloride analysis in liquid film
The reaction of secondary water solution is carried out after out, the liquid material after reacting in Analytic Tower enters separator, and the liquid material of separator is divided into
Two layers, lower layer is aqueous layer, and upper layer is oily phase layer, and aqueous layer is hydrochloric acid, and oily phase layer is product, and reaction pressure control is 50kPa
Hereinafter, the control of the temperature of hydrolysis reactor and Analytic Tower is 30~50 DEG C.
It chemically examines and demonstrate,proves through actual industrial, the technique of the disclosure can not only reduce reaction pressure, and can greatly improve production
Product yield, yield is higher than 99.9%, while can also substantially reduce the acidity value of product, makes first order reaction hydrolysis product acid angle value
Reach 1.2% or less.
The disclosure has the beneficial effect that
1. the hydrolysate chain length that the system and technique of the disclosure obtain is uniform, product category is more concentrated, impurity is few, matter
Amount is preferable.
2. hydrogen chloride gas can be removed in time by the system and technique of the disclosure, be conducive to dimethyldichlorosilane water
Solution reaction, keeps the reaction more complete, conversion yields increase.Meanwhile (especially end group chlorine contains the reduction of hydrolysate chloride ion-containing
Amount), so that the acidity value for controlling product is significantly less than the acidity value of traditional saturated acid hydrolysis prods.
3. the purification and washing system flow of the hydrolysate of disclosure technique shortens, and the load and energy of subsequent cracking technology
Consumption substantially reduces.
4. the product yield of disclosure technique is higher than 99.9%, product hydrolysis product per ton consumes raw material dimethyl dichloro silicon
The amount of alkane is already close to theoretical value.
Detailed description of the invention
The Figure of description for constituting a part of this disclosure is used to provide further understanding of the disclosure, and the disclosure is shown
Meaning property embodiment and its explanation do not constitute the improper restriction to the disclosure for explaining the disclosure.
Fig. 1 is the structural schematic diagram for the system that the low pressure dimethyldichlorosilane of the embodiment of the present disclosure 1 hydrolyzes；
Wherein, 1, circulating pump, 2, hydrolysis reactor, 3, Analytic Tower, 4, condenser, 5, drier, 6, demister, 7, separation
Device, 8, compressor pump.
Specific embodiment
It is noted that described further below be all exemplary, it is intended to provide further instruction to the disclosure.Unless another
It indicates, all technical and scientific terms used herein has usual with disclosure person of an ordinary skill in the technical field
The identical meanings of understanding.
It should be noted that term used herein above is merely to describe specific embodiment, and be not intended to restricted root
According to the illustrative embodiments of the disclosure.As used herein, unless the context clearly indicates otherwise, otherwise singular
Also it is intended to include plural form, additionally, it should be understood that, when in the present specification using term "comprising" and/or " packet
Include " when, indicate existing characteristics, step, operation, device, component and/or their combination.
Existing dimethyldichlorosilane, which is hydrolyzed, in view of existing saturated acid reacts incomplete, end group chlorinity height, hydrolysate
The deficiencies of viscosity is high, acid value is high, in order to solve technical problem as above, the present disclosure proposes a kind of low pressure dimethyldichlorosilanes
The system and technique of hydrolysis.
In a kind of exemplary embodiment of the disclosure, a kind of system of low pressure dimethyldichlorosilane hydrolysis, packet are provided
Include hydrolysis reactor, circulating pump, Analytic Tower, separator, the import of the outlet connection Analytic Tower of the hydrolysis reactor, the solution
The liquid-phase outlet for analysing tower connects separator import, the separator water phase outlet connection pump inlet, the circulating-pump outlet
Hydrolysis reactor import is connected, the feed-line of the pipeline connection dimethyldichlorosilane between circulating pump and hydrolysis reactor；
The Analytic Tower includes distributing disc and at membrane module, and the distributing disc is set to the middle and upper part inside falling liquid film Analytic Tower
Position, is provided with liquid distributing hole on the distributing disc, the lower section that distributing disc is set at membrane module, it is described at membrane module by several
Group " people " font plate is composed；
The tubular structure that the separator is vertically arranged, bottom are exported equipped with water phase, and top is equipped with oil and mutually exports.
Firstly, circulating pump is arranged in the disclosure between hydrolysis reactor and separator, the hydrochloric acid in separator is delivered to
In hydrolysis reactor, the effect of the circulating pump are as follows: 1. provide part reaction pressure to hydrolysis reactor, to make the hydrolysis
It can continue to carry out, 2. are pre-mixed the reaction water of recycle acid and supplement sufficiently, mention for dimethyldichlorosilane hydrolysis
The moisture needed for reaction.
Secondly, Analytic Tower is arranged in the disclosure, the material after hydrolysis flows into the conjunction of " people " font board group after entering Analytic Tower
Membrane module make generate hydrogen chloride gas escape in time, it is therefore prevented that gas film behavior, be more conducive to hydrolysis forward direction progress,
To further increase the reaction yield of product.
Circulating pump is arranged in hydrolysis reactor import in third, the disclosure, exports setting Analytic Tower, the group in hydrolysis reactor
Closing setting can make dimethyldichlorosilane reaction more complete, effectively increase the conversion ratio of dimethyldichlorosilane, and make
The acidity value for obtaining product substantially reduces, and (acidity value of common saturated acid hydrolysis prods is generally 3% lower than 1.2% for acidity value
More than).
The Analytic Tower that the disclosure uses is detailed in the Chinese patent application No. is CN201520127801.4.
In one or more embodiments of the embodiment, including hydrogen chloride purifying device, the hydrogen chloride purifying device
Import connection Analytic Tower gaseous phase outlet.
In the series embodiment, the import of the liquid-phase outlet connection separator of the hydrogen chloride purifying device.It can will divide
From hydrochloric acid and be chlorinated partial hydrolysate that hydrogen takes away Collection utilization again.
In the series embodiment, the hydrogen chloride purifying device includes condenser.
In the series embodiment, the hydrogen chloride purifying device includes drier.
In the series embodiment, the hydrogen chloride purifying device includes demister.
In the series embodiment, the hydrogen chloride purifying device includes being sequentially connected condenser, drying according to gas flow
Device, demister, the gaseous phase outlet of the import connection Analytic Tower of condenser, the gaseous phase outlet of the import connection condenser of drier,
The gaseous phase outlet of the import connection drier of demister；The liquid-phase outlet of condenser, the liquid-phase outlet of drier, demister liquid
Mutually outlet is all connected with the import of separator.
In the series embodiment, including compressor pump, the gas of the import connection hydrogen chloride purifying device of the compressor pump
Mutually export.It is convenient to provide hydrogen chloride gas use for user.
The structure of hydrolysis reactor is similar to static mixer, in order to increase residence time of the material in hydrolysis reactor,
Filler is added in hydrolysis reactor.In one or more embodiments of the embodiment, the hydrolysis reactor is tubulose knot
Structure, the interior several hybrid blades of installation of the tubular structure, and filler is filled in tubular structure.
In the series embodiment, card is arranged at the both ends of tubular structure, and the card is vertical with the axis of tubular structure, institute
Stating card is the plate structure for opening up several through-holes.
The another embodiment of the disclosure provides a kind of technique of low pressure dimethyldichlorosilane hydrolysis, provides
System is stated, circulating pump is delivered to hydrolysis after being pre-mixed after extracting the hydrochloric acid in separator out with dimethyldichlorosilane
A hydrolysis is carried out in device, the material after hydrolysis enters Analytic Tower, and material is formed Analytic Tower at membrane module
Liquid film, the hydrogen chloride in liquid film carry out the reaction of secondary water solution after being precipitated, the liquid material after reacting in Analytic Tower enters separator,
The liquid material of separator is divided into two layers, and lower layer is aqueous layer, and upper layer is oily phase layer, and aqueous layer is hydrochloric acid, and oily phase layer is product,
Reaction pressure control is 50kPa hereinafter, the control of the temperature of hydrolysis reactor and Analytic Tower is 30~50 DEG C.
It chemically examines and demonstrate,proves through actual industrial, the technique of the disclosure can not only reduce reaction pressure, and can greatly improve production
Product yield, yield is higher than 99.9%, while can also substantially reduce the acidity value of product, makes first order reaction hydrolysis product acid angle value
Reach 1.2% or less.
In one or more embodiments of the embodiment, the quality that the hydrochloric acid extracted out to separator adds water to adjust hydrochloric acid is dense
Degree is 33~35%.
In one or more embodiments of the embodiment, hydrogen chloride gas that Analytic Tower is precipitated by condensation, it is dry and/
Or demisting processing.When Analytic Tower be precipitated hydrogen chloride gas successively by condensation, drying and demisting processing after, can be by hydrogen chloride
The oil content of gas is reduced to 5ppm or less.
The hydrolysis of separator separation is generated to be purified into subsequent purification and washing system.
Reaction pressure described in the disclosure is gauge pressure.Gauge pressure refer to total absolute pressure be more than ambient atmospheric pressure number or
Certain point is higher by the part pressure of atmospheric pressure in liquid.
In order to enable those skilled in the art can clearly understand the technical solution of the disclosure, below with reference to tool
The technical solution of the disclosure is described in detail in the embodiment and comparative example of body.
Embodiment 1
A kind of system of low pressure dimethyldichlorosilane hydrolysis, as shown in Figure 1, including circulating pump 1, hydrolysis reactor 2, solution
Analyse tower 3, condenser 4, drier 5, demister 6, separator 7 and compressor pump 8.
Hydrolysis reactor 2, hydrolysis reactor are tubular structure, several hybrid blades of installation in the tubular structure, and are managed
Filler is filled in shape structure.Card is arranged at the both ends of tubular structure, and the card is vertical with the axis of tubular structure, the card
For the plate structure for opening up several through-holes.
Hydrochloric acid solution does the carrier reacted, enters after being mixed in pipeline with dimethyldichlorosilane by the pressurization of circulating pump 1
Hydrolysis reactor 2 quickly mixes in hydrolysis reactor 2, after hydrolysis reactor 2 enters Analytic Tower 3, flows into " people " font board group
Close at membrane module, so that reaction solution is formed several liquid films in film forming segmentation, further hydrogen chloride gas is precipitated in reaction completely,
Produce hydrolysate oil phase.Hydrolysate oil and 3 tower bottom of hydrochloric acid mixed solution self-analytic data tower enter separator 7,7 top hydrolysate of separator
Enter subsequent purification washing system after oily mutually spilling；Lower part hydrochloric acid recycles after being supplemented quantitative fresh water.Hydrogen chloride gas
Enter condenser 4 by releasing at the top of Analytic Tower 3, gas enters back into drier 5 after condensation portion sour water, and hydrogen chloride gas is freezed
It is dry, then pass through demister 6, makes to control in 5ppm into the drop amount containing band in the hydrogen chloride gas of compressor pump 8 hereinafter, dry
User's use is delivered to after hydrogen chloride gas after dry is pressurized.
Specific process parameter are as follows:
Diformazan inlet amount is 1 l/h, and hydrochloric acid circulation measures 5 ls/h, concentration of hydrochloric acid 35%.Test reaction process
The control of middle pressure is in 50kPa or so, and reaction temperature control is at 45 DEG C or so, reaction product oil mutually residence time 3 in the separator
Minute or so, static 5 minutes after separation, it is 54:46, acidity content in hydrolysate that assay, which measures hydrolysate loop wire ratio, at this time
For 0.3% (saturated acid hydrolyzes generally 3% or more).
Embodiment 2
The system of the present embodiment is same as Example 1.
Specific process parameter are as follows:
Diformazan inlet amount is 1 l/h, and hydrochloric acid circulation measures 3 ls/h, concentration of hydrochloric acid 35%.Test reaction process
The control of middle pressure is in 50KPa or so, and reaction temperature control is at 45 DEG C or so, reaction product oil mutually residence time 3 in the separator
Minute or so, static 5 minutes after separation, it is 51:49, acidity content in hydrolysate that assay, which measures hydrolysate loop wire ratio, at this time
For 0.5% (saturated acid hydrolyzes generally 3% or more).
Embodiment 3
The system of the present embodiment is same as Example 1.
Specific process parameter are as follows:
Diformazan inlet amount is 1 l/h, and hydrochloric acid circulation measures 5 ls/h, concentration of hydrochloric acid 33%.Test reaction process
The control of middle pressure is in 30KPa or so, and reaction temperature control is at 45 DEG C or so, reaction product oil mutually residence time 3 in the separator
Minute or so, static 5 minutes after separation, it is 58:42, acidity content in hydrolysate that assay, which measures hydrolysate loop wire ratio, at this time
For 0.65% (saturated acid hydrolyzes generally 3% or more).
Comparative example 1
The system of this comparative example is identical as the system of embodiment 1, and difference is: being not provided with Analytic Tower 3.
It is produced according to the technological parameter of embodiment 1, acidity content is 3.2% in hydrolysate at this time.
Comparative example 2
The system of this comparative example is identical as the system of embodiment 1, and difference is: being not provided with circulating pump 2.
It is produced according to the technological parameter of embodiment 1, acidity content is 3.6% in hydrolysate at this time.
Comparative example 3
The system of this comparative example is identical as the system of embodiment 1, and difference is: Analytic Tower 3 is not configured to membrane module.
It is produced according to the technological parameter of embodiment 1, acidity content is 4.2% in hydrolysate at this time.
The foregoing is merely preferred embodiment of the present disclosure, are not limited to the disclosure, for the skill of this field
For art personnel, the disclosure can have various modifications and variations.It is all within the spirit and principle of the disclosure, it is made any to repair
Change, equivalent replacement, improvement etc., should be included within the protection scope of the disclosure.
Claims (10)
1. a kind of system of low pressure dimethyldichlorosilane hydrolysis, characterized in that including hydrolysis reactor, circulating pump, Analytic Tower,
Separator, the import of the outlet connection Analytic Tower of the hydrolysis reactor, the liquid-phase outlet of the Analytic Tower connect separator into
Mouthful, separator water phase outlet connection pump inlet, the circulating-pump outlet connects hydrolysis reactor import, circulating pump with
The feed-line of pipeline connection dimethyldichlorosilane between hydrolysis reactor；
The Analytic Tower includes distributing disc and at membrane module, and the distributing disc is set to the upper position inside falling liquid film Analytic Tower,
Be provided with liquid distributing hole on the distributing disc, the lower section that distributing disc is set at membrane module, it is described at membrane module by several groups
" people " font plate is composed；
The tubular structure that the separator is vertically arranged, bottom are exported equipped with water phase, and top is equipped with oil and mutually exports.
2. the system of low pressure dimethyldichlorosilane hydrolysis as described in claim 1, characterized in that purify and fill including hydrogen chloride
It sets, the gaseous phase outlet of the import connection Analytic Tower of the hydrogen chloride purifying device.
3. the system of low pressure dimethyldichlorosilane hydrolysis as claimed in claim 2, characterized in that the hydrogen chloride purifying dress
The import for the liquid-phase outlet connection separator set.
4. the system of low pressure dimethyldichlorosilane hydrolysis as claimed in claim 2, characterized in that the hydrogen chloride purifying dress
It sets including condenser；
Or, the hydrogen chloride purifying device includes drier；
Or, the hydrogen chloride purifying device includes demister.
5. the system of low pressure dimethyldichlorosilane hydrolysis as claimed in claim 2, characterized in that the hydrogen chloride purifying dress
Setting according to gas flow includes being sequentially connected condenser, drier, demister, and the gas phase of the import connection Analytic Tower of condenser goes out
Mouthful, the gaseous phase outlet of the import connection condenser of drier, the gaseous phase outlet of the import connection drier of demister；Condenser
Liquid-phase outlet, the liquid-phase outlet of drier, demister liquid-phase outlet be all connected with the import of separator.
6. the system of low pressure dimethyldichlorosilane hydrolysis as claimed in claim 2, characterized in that including compressor pump, institute
State the gaseous phase outlet of the import connection hydrogen chloride purifying device of compressor pump.
7. the system of low pressure dimethyldichlorosilane as claimed in claim 2 hydrolysis, characterized in that the hydrolysis reactor is
Tubular structure, the interior several hybrid blades of installation of the tubular structure, and filler is filled in tubular structure；
Preferably, card is arranged at the both ends of tubular structure, and the card is vertical with the axis of tubular structure, and the card is to open up
The plate structure of several through-holes.
8. a kind of technique of low pressure dimethyldichlorosilane hydrolysis, characterized in that provide that claim 1~7 is any described to be
System, circulating pump are delivered in hydrolysis reactor after being pre-mixed after extracting the hydrochloric acid in separator out with dimethyldichlorosilane
A hydrolysis is carried out, the material after hydrolysis enters Analytic Tower, and material forms liquid film at membrane module Analytic Tower,
Hydrogen chloride in liquid film carries out the reaction of secondary water solution after being precipitated, the liquid material after reacting in Analytic Tower enters separator, separates
The liquid material of device is divided into two layers, and lower layer is aqueous layer, and upper layer is oily phase layer, and aqueous layer is hydrochloric acid, and oily phase layer is product, reaction
Pressure control is 50kPa hereinafter, the control of the temperature of hydrolysis reactor and Analytic Tower is 30~50 DEG C.
9. the technique of low pressure dimethyldichlorosilane hydrolysis as claimed in claim 8, characterized in that the salt extracted out to separator
The mass concentration that acid plus water adjust hydrochloric acid is 33~35%.
10. the technique of low pressure dimethyldichlorosilane hydrolysis as claimed in claim 8, characterized in that the chlorine that Analytic Tower is precipitated
Change hydrogen by condensation, the processing of dry and/or demisting；Preferably, Analytic Tower be precipitated hydrogen chloride gas successively by condensation,
The processing of dry and demisting.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910522412.4A CN110183479B (en) | 2019-06-17 | 2019-06-17 | System and process for hydrolyzing low-pressure dimethyldichlorosilane |
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| CN201910522412.4A CN110183479B (en) | 2019-06-17 | 2019-06-17 | System and process for hydrolyzing low-pressure dimethyldichlorosilane |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113996256A (en) * | 2021-11-12 | 2022-02-01 | 新疆晶硕新材料有限公司 | Method and device for treating dimethyl dichlorosilane hydrolysate |
| CN114085381A (en) * | 2021-11-29 | 2022-02-25 | 内蒙古恒星化学有限公司 | Gas-phase dimethyl dichlorosilane hydrolysis process |
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| CN113996256A (en) * | 2021-11-12 | 2022-02-01 | 新疆晶硕新材料有限公司 | Method and device for treating dimethyl dichlorosilane hydrolysate |
| CN113996256B (en) * | 2021-11-12 | 2023-11-14 | 新疆晶硕新材料有限公司 | Method and device for treating dimethyl dichlorosilane hydrolysate |
| CN114085381A (en) * | 2021-11-29 | 2022-02-25 | 内蒙古恒星化学有限公司 | Gas-phase dimethyl dichlorosilane hydrolysis process |
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