CN204097378U - METHYL TRICHLORO SILANE prepares the device of ultra-fine silsesquioxane - Google Patents
METHYL TRICHLORO SILANE prepares the device of ultra-fine silsesquioxane Download PDFInfo
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- CN204097378U CN204097378U CN201420573478.9U CN201420573478U CN204097378U CN 204097378 U CN204097378 U CN 204097378U CN 201420573478 U CN201420573478 U CN 201420573478U CN 204097378 U CN204097378 U CN 204097378U
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- storage tank
- filter
- mixing
- filtrate storage
- mixing filtrate
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Abstract
The utility model relates to a kind of chemical production equipment, particularly relates to the device that METHYL TRICHLORO SILANE prepares ultra-fine silsesquioxane, comprises the first hold-up vessel and is connected with reactor; Reactor is connected with filter, and filter connects water source, provides bath water; The mixing filtrate outlet of filter connects mixing filtrate storage tank, and the wash filtrate outlet of filter connects wash filtrate storage tank; The mixing filtrate outlet ligation still of mixing filtrate storage tank; The outlet of mixing filtrate reservoir bottom connects the second hold-up vessel respectively, and the wash filtrate outlet in wash filtrate storage tank connects filtrate storage tank.This device can obtain ultra-fine silsesquioxane product, continuously alternately discharging and charging, and feed stock conversion is high, and sealing and circulating is little to environmental influence.
Description
Technical field
The utility model relates to a kind of chemical production equipment, particularly relates to the device that METHYL TRICHLORO SILANE prepares ultra-fine silsesquioxane.
Background technology
Organosilicon material is owing to having good physicals, the fields such as aerospace, International Technology, electronic industry, weaving, building, chemical industry that are widely used in play an important role to promotion high-tech industry composition optimizes upgrading, being described as " industrial monosodium glutamate " by image.Organosilicon industry is classified as one of national industry of encouraging and first develop by country.The basic material producing organosilicon material is organosilane monomer, mainly (CH3)
2siCl
2.Mainly adopt the method for methyl chloride and silica flour direct synthesizing methyl-chloro-silane under copper catalyst effect at present both at home and abroad
[3].The method is except generating target product (CH3)
2siCl
2outward, along with generating portion by product: CH
3siCl
3(3-15%), (CH
3)
3siCl (3%), CH
3hSiCl
2(1-3%), (CH
3)
2hSiCl (0.5%), (CH
3)
4si (0.1%), SiCl
4high boiling material (1-6%).Wherein CH
3siCl
3ratio is maximum.At present, because of CH
3siCl
3fully do not developed and caused a large amount of accumulation.Due to CH
3siCl
3belong to hazardous substance and in atmosphere facile hydrolysis produce HCl, bring immense pressure to environment.So CH
3siCl
3process not only become with application bottleneck restrict organosilicon industry development, also certainly will become the key of guiding whole piece industrial chain Sustainable development.
METHYL TRICHLORO SILANE hydrolysis process can be translated into hydrogen chloride gas and silsesquioxane.Hydrogen chloride gas can be used for organosilane monomer production line source as the raw material of synthesis methyl chloride, reduces material cost, reaches recycling economy object.Silsesquioxane can be used for preparing the series of downstream products such as methyl silicate.
Current METHYL TRICHLORO SILANE hydrolysis is prepared silsesquioxane and is taked interval open type method more, and severe operational environment, transformation efficiency is not high." system of methyl siliconic acid produced by a kind of hydrolyzing methyl trichlorosilane " of CN202359049U bulletin can continuous discharging slag, but does not make concrete design to processes such as product filtering separation, washings.The single-phase hydrolysis process of current routine can only obtain the larger silsesquioxane crude product of particle.
Utility model content
For above-mentioned technical problem, the utility model provides the device of the ultra-fine silsesquioxane of complete preparation, and concrete technical scheme is:
METHYL TRICHLORO SILANE prepares the device of ultra-fine silsesquioxane, comprises the first hold-up vessel, reactor, filter, mixing filtrate storage tank, wash filtrate storage tank, the second hold-up vessel;
First hold-up vessel is connected with reactor; Reactor is connected with filter, and filter connects water source, provides bath water;
The mixing filtrate outlet of filter connects mixing filtrate storage tank, and the wash filtrate outlet of filter connects wash filtrate storage tank;
The mixing filtrate outlet ligation still of mixing filtrate storage tank, mixing filtrate enters reactor circulating reaction; Mixing filtrate reservoir bottom outlet connection second hold-up vessel, injects the second hold-up vessel and stores by concentrated hydrochloric acid;
Wash filtrate outlet in wash filtrate storage tank connects mixing filtrate storage tank, wash filtrate recycle.
Optimization design is, described filter comprises the first filter, the second filter; Described mixing filtrate storage tank comprises the first mixing filtrate storage tank, the second mixing filtrate storage tank;
Therefore the device optimized is: METHYL TRICHLORO SILANE prepares the device of ultra-fine silsesquioxane, comprises the first hold-up vessel, reactor, the first filter, the second filter, the first mixing filtrate storage tank, the second mixing filtrate storage tank, wash filtrate storage tank, the second hold-up vessel;
First hold-up vessel is used for depositing tank METHYL TRICHLORO SILANE, and the first hold-up vessel is connected with reactor by the first fresh feed pump;
Polycondensation Reactor and Esterification Reactor portion is connected with the first filter and the second filter respectively, and the first filter and the second filter make solid-liquid separation, washing and silsesquioxane product discharging; First filter is connected water source respectively with the second filter, provides bath water;
First filter is connected the first mixing filtrate storage tank or the second mixing filtrate storage tank with the mixing filtrate outlet in the second filter, the first filter is connected wash filtrate storage tank with the wash filtrate outlet in the second filter;
The mixing filtrate outlet ligation still of the first mixing filtrate storage tank and the second mixing filtrate storage tank, mixing filtrate enters reactor circulating reaction; First mixing filtrate storage tank is connected the second hold-up vessel respectively with the second mixing filtrate reservoir bottom outlet, concentrated hydrochloric acid is injected the second hold-up vessel and stores;
Wash filtrate outlet connection first in wash filtrate storage tank mixes filtrate storage tank or the second mixing filtrate storage tank, wash filtrate recycle.
Scum dredger is arranged at reactor top, the hydrogen chloride gas that absorption reaction produces.
Wherein, reactor reacts under organic phase exists for METHYL TRICHLORO SILANE and sour water.Reactor there is agitator, reactant is fully mixed.
Filter is separated with mixing filtrate by reaction product silsesquioxane; Mixing filtrate storage tank, accepts hydrochloric acid and the organic phase of filter output; Wash filtrate storage tank, the wash filtrate that receiving filtration machine exports.
The METHYL TRICHLORO SILANE that the utility model provides prepares the device of ultra-fine silsesquioxane, can obtain ultra-fine silsesquioxane product and concentrated hydrochloric acid byproduct, and the hydrogen chloride gas of generation is input to the raw material of machine silicon monomer production line source as synthesis methyl chloride; This device can replace discharging and charging continuously, and feed stock conversion is high, and sealing and circulating is little to environmental influence.
Accompanying drawing explanation
Fig. 1 is the utility model system architecture schematic diagram.
Embodiment
Accompanying drawings embodiment of the present utility model.As shown in Figure 1, METHYL TRICHLORO SILANE prepares the device of ultra-fine silsesquioxane, comprise the first hold-up vessel 1, first fresh feed pump 2, reactor 3, agitator 4, scum dredger 5, first transforming valve 6, second transforming valve 7, 3rd transforming valve 8, 4th transforming valve 9, first filter 10, second filter 11, 5th transforming valve 12, 6th transforming valve 13, 7th transforming valve 14, 8th transforming valve 15, first mixing filtrate storage tank 16, second mixing filtrate storage tank 17, wash filtrate storage tank 18, water pump 19, 9th transforming valve 20, tenth transforming valve 21, 11 transforming valve 22, 12 transforming valve 23, second hold-up vessel 24, second fresh feed pump 25, 13 transforming valve 26, 14 transforming valve 27.
First hold-up vessel 1 is for depositing tank METHYL TRICHLORO SILANE, and the METHYL TRICHLORO SILANE in the first hold-up vessel 1 is pumped into the reactor 3 adding organic phase and water by the first fresh feed pump 2, and the agitator 4 on reactor 3 makes each reactant fully mix reaction.
Be connected with the first filter 10 and the second filter 11 with the second transforming valve 7 respectively by the first transforming valve 6 bottom reactor 3, first transforming valve 6 and the second transforming valve 7 control the first filter 10 and the second filter 11 two filters hocket, first filter 10 and the second filter 11 make solid-liquid separation, washing and silsesquioxane product discharging, and when washing and discharging, reactive system does not stop continuous operation.
First filter 10 is connected water source respectively by the 3rd transforming valve 8 with the 4th transforming valve 9 with the second filter 11, provides bath water.
Mixing filtrate in first filter 10 and the second filter 11 enters the first mixing filtrate storage tank 16 or the second mixing filtrate storage tank 17, wash filtrate in first filter 10 and the second filter 11 enters wash filtrate storage tank 18,5th transforming valve 12, the 6th transforming valve 13, the 7th transforming valve 14, the 8th transforming valve 15 control the shunting of mixing filtrate and wash filtrate, and filtration and isolated silsesquioxane product enter drying shed.
First mixing filtrate storage tank 16 and the second mixing filtrate mixed in filtrate storage tank 17 pump into reactor 3 circulating reaction through the second fresh feed pump 25, are controlled the alternate feed of the first mixing filtrate storage tank 16 and the second mixing filtrate storage tank 17 by the 9th transforming valve 20 and the tenth transforming valve 21.
In first mixing filtrate storage tank 16 and the second mixing filtrate storage tank 17, when mixing filtrate bottom hydrogen cloride concentration and reaching about 30%, open the 11 transforming valve the 22 or the 11 transforming valve 23 and concentrated hydrochloric acid is injected the second hold-up vessel 24 and store.
Wash filtrate in wash filtrate storage tank 18 has water pump 19 to add to the first mixing filtrate storage tank 16 or the second mixing filtrate storage tank 17 recycle, and choice of flow direction is controlled by the 13 transforming valve the 26, the 14 transforming valve 27.
The hydrogen chloride gas that reaction produces enters scum dredger 5 by reactor 3 top, reuse after process.
Claims (3)
1. METHYL TRICHLORO SILANE prepares the device of ultra-fine silsesquioxane, it is characterized in that: METHYL TRICHLORO SILANE prepares the device of ultra-fine silsesquioxane, comprise the first hold-up vessel (1), reactor (3), filter, mixing filtrate storage tank, wash filtrate storage tank (18), the second hold-up vessel (24);
First hold-up vessel (1) is connected with reactor (3); Reactor (3) is connected with filter, and filter connects water source, provides bath water;
The mixing filtrate outlet of filter connects mixing filtrate storage tank, and the wash filtrate outlet of filter connects wash filtrate storage tank (18);
Mixing filtrate outlet ligation still (3) of mixing filtrate storage tank, mixing filtrate enters reactor (3) circulating reaction; Mixing filtrate reservoir bottom outlet connection second hold-up vessel, injects the second hold-up vessel and stores by concentrated hydrochloric acid;
Wash filtrate outlet in wash filtrate storage tank (18) connects mixing filtrate storage tank, wash filtrate recycle.
2. METHYL TRICHLORO SILANE according to claim 1 prepares the device of ultra-fine silsesquioxane, it is characterized in that: described filter comprises the first filter (10), the second filter (11); Described mixing filtrate storage tank comprises the first mixing filtrate storage tank (16), the second mixing filtrate storage tank (17);
First hold-up vessel (1) is for depositing tank METHYL TRICHLORO SILANE, and the first hold-up vessel (1) is connected with reactor (3) by the first fresh feed pump (2);
Reactor (3) bottom is connected with the first filter (10) and the second filter (11) respectively, and the first filter (10) and the second filter (11) make solid-liquid separation, washing and silsesquioxane product discharging; First filter (10) is connected water source respectively with the second filter (11), provides bath water;
First filter (10) is connected the first mixing filtrate storage tank (16) or the second mixing filtrate storage tank (17) with the mixing filtrate outlet in the second filter (11), the first filter (10) is connected wash filtrate storage tank (18) with the wash filtrate outlet in the second filter (11);
The mixing filtrate outlet ligation still of the first mixing filtrate storage tank (16) and the second mixing filtrate storage tank (17), mixing filtrate enters reactor (3) circulating reaction; First mixing filtrate storage tank (16) is connected the second hold-up vessel (24) respectively with the second mixing filtrate storage tank (17) outlet at bottom, concentrated hydrochloric acid is injected the second hold-up vessel (24) and stores;
Wash filtrate outlet connection first in wash filtrate storage tank (18) mixes filtrate storage tank (16) or the second mixing filtrate storage tank (17), wash filtrate recycle.
3. METHYL TRICHLORO SILANE according to claim 1 and 2 prepares the device of ultra-fine silsesquioxane, it is characterized in that: scum dredger (5) is arranged at reactor (3) top, the hydrogen chloride gas that absorption reaction produces.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201420573478.9U CN204097378U (en) | 2014-09-29 | 2014-09-29 | METHYL TRICHLORO SILANE prepares the device of ultra-fine silsesquioxane |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201420573478.9U CN204097378U (en) | 2014-09-29 | 2014-09-29 | METHYL TRICHLORO SILANE prepares the device of ultra-fine silsesquioxane |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN204097378U true CN204097378U (en) | 2015-01-14 |
Family
ID=52265823
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201420573478.9U Expired - Fee Related CN204097378U (en) | 2014-09-29 | 2014-09-29 | METHYL TRICHLORO SILANE prepares the device of ultra-fine silsesquioxane |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN204097378U (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106336425A (en) * | 2016-08-24 | 2017-01-18 | 陕西天策新材料科技有限公司 | Continuous production technology for preparing POSS by hydrolytic condensation method and equipment thereof |
-
2014
- 2014-09-29 CN CN201420573478.9U patent/CN204097378U/en not_active Expired - Fee Related
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106336425A (en) * | 2016-08-24 | 2017-01-18 | 陕西天策新材料科技有限公司 | Continuous production technology for preparing POSS by hydrolytic condensation method and equipment thereof |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20150114 Termination date: 20160929 |
|
| CF01 | Termination of patent right due to non-payment of annual fee |