CN109107325A - Methylchlorosilane emptying end gas recovery method and recyclable device - Google Patents
Methylchlorosilane emptying end gas recovery method and recyclable device Download PDFInfo
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- CN109107325A CN109107325A CN201811036740.5A CN201811036740A CN109107325A CN 109107325 A CN109107325 A CN 109107325A CN 201811036740 A CN201811036740 A CN 201811036740A CN 109107325 A CN109107325 A CN 109107325A
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- boiling components
- end gas
- methylchlorosilane
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/002—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by condensation
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D45/00—Separating dispersed particles from gases or vapours by gravity, inertia, or centrifugal forces
- B01D45/12—Separating dispersed particles from gases or vapours by gravity, inertia, or centrifugal forces by centrifugal forces
- B01D45/16—Separating dispersed particles from gases or vapours by gravity, inertia, or centrifugal forces by centrifugal forces generated by the winding course of the gas stream, the centrifugal forces being generated solely or partly by mechanical means, e.g. fixed swirl vanes
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/14—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by absorption
- B01D53/18—Absorbing units; Liquid distributors therefor
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2258/00—Sources of waste gases
- B01D2258/02—Other waste gases
Abstract
The present invention relates to chemical technology field, a kind of methylchlorosilane emptying end gas recovery method and recyclable device are disclosed；Methylchlorosilane emptying end gas recovery method includes: the high-boiling components for recycling and generating in methylchlorosilane synthetic reaction；Condense high-boiling components；First emptying end gas is passed through condensed high-boiling components；Condensed high-boiling components absorb the first emptying end gas.Methylchlorosilane emptying end gas recyclable device includes: emptying end gas conveying mechanism, the first condensing mechanism and reaction kettle, and reaction kettle one end is connected to the first condensing mechanism, and the reaction kettle other end is connected to emptying end gas conveying mechanism.The present invention is by recycling the high-boiling components generated in methylchlorosilane synthetic reaction；The first emptying end gas is absorbed by condensed high-boiling components, the recovery yield of monomer in emptying end gas is promoted to 80%, the generation of waste oil is reduced, solves problem of the prior art.
Description
Technical field
The present invention relates to chemical technology fields, more particularly to a kind of methylchlorosilane emptying end gas recovery method and return
Receiving apparatus.
Background technique
Currently, generalling use chloromethanes both at home and abroad in organosilicon production with silicon powder and synthesizing work by heterogeneous catalytic reaction
Skill produces (CH3)2SiCl2, abbreviation direct method.In direct synthesis (CH3)2SiCl2Industrial production in, organosilicon synthesis
(CH3)2SiCl2Equal products can carry a large amount of raw material silicon powder and catalyst copper powder and some by-products secretly.
Organic silicon monomer emptying end gas treatment process is relatively simple at this stage, increases a heat exchange after emptying end gas
Device, using heat exchanger recovery section organic silicon monomer emptying end gas, emptying end gas cannot recycle completely.Emptying in the prior art
Recovery yield of monomer in tail gas only has 30%, and the rate of recovery is low, and unrecovered emptying end gas can generate waste oil and waste acid water, therefore,
Recovery yield of monomer is low to lead to the wasting of resources, and waste oil and spent acid water be easy to cause greatly environmental pollution.
Summary of the invention
The purpose of the present invention is to solve the above problem, provide a kind of methylchlorosilane emptying end gas recovery method with
And recyclable device.
To achieve the above object, in a first aspect, the present invention provides a kind of methylchlorosilane emptying end gas recovery method, packet
It includes:
The high-boiling components generated in recycling methylchlorosilane synthetic reaction, high-boiling components refer to that boiling point is more than 70.2 DEG C of liquid phase by-product
Object；
Condense the high-boiling components；
First emptying end gas is passed through the condensed high-boiling components；
The condensed high-boiling components absorb first emptying end gas.
Optionally, above-mentioned methylchlorosilane emptying end gas recovery method, further includes: have first emptying to absorption
The high-boiling components of tail gas are parsed, are separated.
Optionally, above-mentioned methylchlorosilane emptying end gas recovery method, the high-boiling components are to contain Si-O-Si key
Or/and Si-CH2The mixture of-Si key or/and Si-Si bond compound.
Optionally, above-mentioned methylchlorosilane emptying end gas recovery method, the method tool of the condensation high-boiling components
Body are as follows:
Cool down at least through condensed in two stages to the high-boiling components.
Optionally, above-mentioned methylchlorosilane emptying end gas recovery method, level-one condensation using recirculated water as refrigerant,
Flow velocity of the recirculated water in heat exchanger is controlled, primary temperature reducing is carried out to the high-boiling components by the heat exchanger；
B-grade condensation, as refrigerant, is controlled flow velocity of the ethylene glycol in the heat exchanger, passes through institute using ethylene glycol
It states heat exchanger and second level cooling is carried out to the high-boiling components.
Second aspect, the present invention provides a kind of recyclable devices for the recycling of methylchlorosilane emptying end gas, comprising: puts
Empty tail gas conveying mechanism, the first condensing mechanism and reaction kettle, described reaction kettle one end is connected to first condensing mechanism, described
The reaction kettle other end is connected to the emptying end gas conveying mechanism；
The emptying end gas conveying mechanism is for inputting the first emptying end gas into the reaction kettle；
First condensing mechanism is for condensing high-boiling components；
The reaction kettle carries out absorbing reaction to first emptying end gas for condensed high-boiling components.
Optionally, the above-mentioned recyclable device for the recycling of methylchlorosilane emptying end gas, further includes: be connected to described anti-
Answer the monomer rectifying mechanism of kettle；
The monomer rectifying mechanism is used to have the high-boiling components of first emptying end gas to be parsed absorption, divide
From.
Optionally, the above-mentioned recyclable device for the recycling of methylchlorosilane emptying end gas, comprising: collecting mechanism and power
Mechanism, described collecting mechanism one end are connected to the reaction kettle, and the collecting mechanism other end is connected to the power mechanism one
End, the power mechanism other end are connected to the monomer rectifying mechanism；
The collecting mechanism is used to receive the high-boiling components for absorbing and having first emptying end gas；
The power mechanism is used to have the high-boiling components of first emptying end gas to be passed through the monomer rectifying absorption
Mechanism.
Optionally, the above-mentioned recyclable device for the recycling of methylchlorosilane emptying end gas, the first condensing mechanism packet
First-stage condenser and secondary condenser are included, described secondary condenser one end is connected to the first-stage condenser, the B-grade condensation
The device other end is connected to the reaction kettle；
The first-stage condenser is used to carry out primary temperature reducing to the high-boiling components；
The secondary condenser is used to carry out second level cooling to the high-boiling components.
Optionally, the above-mentioned recyclable device for the recycling of methylchlorosilane emptying end gas, further includes: cold with described first
The high-boiling components conveying mechanism that solidifying mechanism is connected, the high-boiling components conveying mechanism are used to convey into first condensing mechanism high
Boil object.
Compared with prior art, present invention has an advantage that
The present invention provides a kind of methylchlorosilane emptying end gas recovery methods, by recycling methylchlorosilane synthetic reaction
The high-boiling components of middle generation；The first emptying end gas is absorbed by condensed high-boiling components, the monomer in emptying end gas is returned
Yield is promoted to 80%, reduces the generation of waste oil, solves problem of the prior art.
Detailed description of the invention
The drawings described herein are used to provide a further understanding of the present invention, constitutes a part of the invention, this hair
Bright illustrative embodiments and their description are used to explain the present invention, and are not constituted improper limitations of the present invention.In the accompanying drawings:
Fig. 1 is the flow chart of organic silicon monomer synthetic method；
Fig. 2 is the flow chart of methylchlorosilane emptying end gas recovery method；
Fig. 3 is the stream for the method that S02 separates the principal product and by-product that generate in methylchlorosilane synthetic reaction
Cheng Tu；
Fig. 4 is the structural schematic diagram of methylchlorosilane emptying end gas recyclable device；
Fig. 5 is the structural block diagram of the synthesis system synthesized for organic silicon monomer；
Fig. 6 is crude monomer tower, the structural block diagram for taking off high tower, high boiling tower and monomer rectifying mechanism；
The components in the drawings are labeled as follows:
The recyclable device 1 of methylchlorosilane emptying end gas recycling, emptying end gas conveying mechanism 11 are vented surge tank 111, the
One condensing mechanism 12, first-stage condenser 121, secondary condenser 122, reaction kettle 13, monomer rectifying mechanism 14 take off low tower 141, and one
First tower 142 gently divides tower 143, hydrogeneous tower 144, azeotrope column 145, front three tower 146, collecting mechanism 15, power mechanism 16, methyl chloride
Silane synthesizer 2, fluidized bed 21, cyclone separator 22, the first recovering mechanism 23, the second recovering mechanism 24, scrubbing tower 25, slightly
Monomer tower 26 takes off high tower 27, high boiling tower 28, chloromethanes tower 29, the second condensing mechanism 30, high-boiling components conveying mechanism 31.
Specific embodiment
To make the object, technical solutions and advantages of the present invention clearer, below in conjunction with the specific embodiment of the invention and
Technical solution of the present invention is clearly and completely described in corresponding attached drawing.Obviously, described embodiment is only 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.
Multiple embodiments of the invention will be disclosed with schema below, as clearly stated, the details in many practices
It will be explained in the following description.It should be appreciated, however, that the details in these practices is not applied to limit the present invention.Also
It is to say, in some embodiments of the invention, the details in these practices is non-essential.In addition, for the sake of simplifying schema,
Some known usual structures and component will be painted it in the drawings in simply illustrative mode.
The description for being such as related to " first ", " second " in the present invention is used for description purposes only, and not especially censures order
Or the meaning of cis-position, also non-limiting the present invention, the component described just for the sake of difference with same technique term or behaviour
Make, be not understood to indicate or imply its relative importance or implicitly indicate the quantity of indicated technical characteristic.
" first " is defined as a result, the feature of " second " can explicitly or implicitly include at least one of the features.
As shown in Figure 1, a kind of organic silicon monomer synthetic method, comprising:
S01, using silicon powder, chloromethanes as reactant, copper powder carries out methylchlorosilane synthetic reaction as catalyst,
High-boiling components refer to that boiling point is more than 70.2 DEG C of liquid phase by-product；
S02 separates the principal product methylchlorosilane and by-product that generate in methylchlorosilane synthetic reaction, main product
Object methylchlorosilane and by-product are referred to as thick methylchlorosilane；
The first emptying end gas isolated from the by-product is carried out methyl chloride silicon with the high-boiling components isolated by S03
The reaction of alkane emptying end gas recovery method.
Recovery yield of monomer in emptying end gas in the prior art only has 30%, and the rate of recovery is low, unrecovered emptying end gas
Waste oil and waste acid water can be generated, therefore, to solve the above-mentioned problems, as shown in Fig. 2, the present invention provides involved in a kind of S03
The methylchlorosilane emptying end gas recovery method arrived, comprising:
S031 recycles the high-boiling components generated in methylchlorosilane synthetic reaction；
S032 condenses high-boiling components；
First emptying end gas is passed through condensed high-boiling components by S033；
S034, condensed high-boiling components absorb the first emptying end gas.
The present invention absorbs the first emptying end gas by condensed high-boiling components, by the MONOMER RECOVERY in emptying end gas
Rate is promoted to 80%, reduces the generation of waste oil, solves problem of the prior art.
In order to there is the high-boiling components of emptying end gas to carry out resource circulation utilization, therefore the application to absorption further include: S035 is right
Absorption has the high-boiling components of the first emptying end gas to be parsed, separated.The application goes out various of monomer by S035 Desorption separation, then
The monomer isolated is recycled.
The high-boiling components of the application frequently with contain Si-O-Si key or/and Si-CH2- Si key or/and Si-Si bond compound
Mixture.
Due to carrying out primary condensation to the more demanding of refrigerant to high-boiling components, the S032 of the application condenses high-boiling components
Method frequently with: cool down at least through condensed in two stages to high-boiling components.
From the aspect of economy and operation readiness, the application is frequently with B-grade condensation.If using B-grade condensation to height
Boiling object cools down, then the level-one condensation of the application using recirculated water as refrigerant, flow velocity of the control loop water in heat exchanger,
Primary temperature reducing is carried out to high-boiling components by heat exchanger；The application is frequently with 25 DEG C of recirculated waters as refrigerant, and flow control is in 10m3/
H, using tubular heat exchanger, high-boiling components are down to 28 DEG C from 100 DEG C by level-one condensation；B-grade condensation is using ethylene glycol as cold
Matchmaker controls flow velocity of the ethylene glycol in heat exchanger, carries out second level cooling to high-boiling components by heat exchanger.The application is frequently with -8 DEG C
Ethylene glycol is as refrigerant, and flow control is in 10m3/ h, using tubular heat exchanger, high-boiling components are down to 3 from 28 DEG C by B-grade condensation
℃.The present invention is easier uniformly to condense high-boiling components by condensation stage by stage, and operation is more easier, and refrigerant is easier to obtain
?.
In order to enable the high-boiling components cycle applications in methylchlorosilane synthetic reaction into above-mentioned reaction, and can have
Effect ground separates principal product and by-product, and separates to the multiple compounds in by-product, realizes resource again
It utilizes, as shown in figure 3, being separated in the application S02 to the principal product and by-product that are generated in methylchlorosilane synthetic reaction
Method frequently with following method, specifically:
S021 carries out cyclonic separation to the thick methylchlorosilane generated in methylchlorosilane synthetic reaction, obtains outlet respectively
Mutually thick methylchlorosilane and the thick copper silicon powder of solid phase；
The solid phase copper silicon powder isolated is vented by S022, obtains the first emptying end gas and solid phase essence copper silicon powder；
S023 flows back the solid phase essence copper silicon powder isolated, and solid phase essence copper silicon powder is as methylchlorosilane synthetic reaction
Reactant；
S024 washs the thick methylchlorosilane of gas phase, isolates screenings；
S025, respectively be isolated by from the thick methylchlorosilane of gas phase for isolating screenings smart methylchlorosilane, crude monomer and
The thick chloromethanes of gas phase；
S026 isolates high-boiling components from crude monomer；
S027, the first emptying end gas and high-boiling components carry out the reaction of above-mentioned methylchlorosilane emptying end gas recovery method；
S028 is vented the thick chloromethanes of gas phase, isolates smart chloromethanes, carries out to the second emptying end gas of discharge cold
It is solidifying.
Solid phase essence copper silicon powder, smart methylchlorosilane, essence has been effectively separated by the reaction of S021-S028 in the present invention
Chloromethanes, high-boiling components and various of monomer realize the recycling of resource, design more scientific.
Above-mentioned machine silicon monomer synthetic method is described in detail below by citing and association reaction chemical formula, this act
The reaction process control of example is as follows: 270~320 DEG C of temperature, 0.31~0.33MPa of pressure, the size controlling of silicon powder 130~
180um, gas velocity are controlled in 2800~3500m3/ h, bed height control between 0.1MPa~0.140MPa；
S01 carries out methylchlorosilane synthetic reaction, reaction using silicon powder, chloromethanes and catalyst copper powder as reactant
Chemical formula includes:
Main reaction:
Side reaction includes:Deng；
Therefore, the product of methylchlorosilane synthetic reaction includes: Trichloromethyl silane, dimethyldichlorosilane, front three
One chlorosilane of base, tetramethylsilane, the hydrogeneous dichlorosilane of monomethyl, the hydrogeneous chlorosilane of dimethyl, high-boiling components and low-boiling-point substance etc. are high
Boiling object is the mixture containing Si-O-Si key or/and Si-CH2-Si key or/and Si-Si bond compound, mainly includes trimethyl
Trichlorine disilane and dimethyl tetrachloro disilane.Since silico briquette surface is easy to produce oxide layer, copper contains oxygen element in catalyst,
Therefore oxygen element is brought into silicon powder and copper powder, oxygen element participates in complicated chemical reaction in methylchlorosilane synthetic reaction,
And then the compound containing Si-O-Si key in high-boiling components；Low-boiling-point substance refers to that boiling point is lower than 40 DEG C of liquid phase by-product, mainly includes four
Methyl-monosilane, isopentane, trichlorosilane, chloromethanes, dimethyl are containing silicane hydroxide etc..
Trichloromethyl silane, dimethyldichlorosilane, tri-methyl-chlorosilane, tetramethylsilane, monomethyl in product
The hydrogeneous chlorosilane of hydrogeneous dichlorosilane, dimethyl is gas phase；And since reactant reaction is incomplete, have solid phase silicon
Powder and copper powder are mixed in product.
S02 separates the principal product methylchlorosilane and by-product that generate in methylchlorosilane synthetic reaction, main product
Object methylchlorosilane and by-product are referred to as thick methylchlorosilane, specifically include:
S021 carries out cyclonic separation to the thick methylchlorosilane generated in methylchlorosilane synthetic reaction, obtains outlet respectively
Mutually thick methylchlorosilane and the thick copper silicon powder of solid phase；
The solid phase copper silicon powder isolated is vented by S022, obtains the first emptying end gas and solid phase essence copper silicon powder；First
Emptying end gas ingredient, content are as follows:
One first emptying end gas ingredient of table and content
| Ingredient | Content (%) |
| Chloromethanes | 2.08 |
| Tetramethylsilane | 0.37 |
| 3- methylpentane | 0.04 |
| Butylene | 0.01 |
| The hydrogeneous chlorosilane of dimethyl | 0.05 |
| The hydrogeneous dichlorosilane of monomethyl | 0.25 |
| Silicon tetrachloride | 0.11 |
| The hydrogeneous chlorosilane of trimethyl | 6.55 |
| 2,3- neohexene | 0.02 |
| The hydrogeneous trichlorosilane of monomethyl | 8.65 |
| The hydrogeneous dichlorosilane of dimethyl | 70.10 |
| High-boiling components | 11.77 |
| It is total | 100.00 |
S023 flows back the solid phase essence copper silicon powder isolated, and solid phase essence copper silicon powder is as methylchlorosilane synthetic reaction
Reactant；
S024 washs the thick methylchlorosilane of gas phase, isolates screenings；
S025, respectively be isolated by from the thick methylchlorosilane of gas phase for isolating screenings smart methylchlorosilane, crude monomer and
The thick chloromethanes of gas phase；
S026 isolates high-boiling components from crude monomer；
Crude monomer ingredient specifically includes that the hydrogeneous chlorosilane of high-boiling components, dimethyl, the hydrogeneous dichlorosilane of monomethyl, tetrachloro
The hydrogeneous chlorosilane of SiClx, trimethyl, the hydrogeneous trichlorosilane of monomethyl, the hydrogeneous dichlorosilane of dimethyl and low-boiling-point substance, crude monomer
Into de- high tower, high-boiling components and the hydrogeneous dichlorosilane of a small amount of dimethyl are isolated from de- high tower, the mixture isolated enters
High boiling tower respectively is isolated by high-boiling components and the hydrogeneous dichlorosilane of dimethyl from high boiling tower, and it is anti-that high-boiling components execute S031-S035
It answers, the hydrogeneous dichlorosilane of dimethyl is back to de- high tower and continues separation reaction；
S027, the first emptying end gas and high-boiling components carry out the anti-of above-mentioned methylchlorosilane emptying end gas recovery method S03
The step of answering, specially executing S031-S035
S031 recycles the high-boiling components generated in methylchlorosilane synthetic reaction；
S032 condenses high-boiling components；
First emptying end gas is passed through condensed high-boiling components by S033；
S034, condensed high-boiling components absorb the first emptying end gas；
The reflux of unabsorbed first emptying end gas executes S024, unabsorbed first emptying end gas ingredient and contains measurer
Body is as follows:
The unabsorbed first emptying end gas ingredient of table two and content
It is unabsorbed after showing that the first emptying end gas is absorbed by high-boiling components by the way that table one and table two to be compared
Emptying end gas content is 20.08%, is compared with the first emptying end gas total content 100.00%, the recycling of the first emptying end gas
Rate reaches 80%, compared with 30% rate of recovery recycled in the prior art by heat exchanger to the first emptying end gas, uses
The first emptying end gas rate of recovery of emptying end gas recovery method of the invention has been significantly improved, and reduces waste oil
It generates.
S035 has the high-boiling components of the first emptying end gas to be parsed, separated absorption, and the application passes through S035 Desorption separation
Then various of monomer out recycles the monomer isolated, specifically:
The application frequently with by eight tower distillation technologies by Trichloromethyl silane, dimethyldichlorosilane, trimethyl one
The hydrogeneous chlorosilane of the hydrogeneous dichlorosilane of chlorosilane, tetramethylsilane, monomethyl, dimethyl, high-boiling components, low-boiling-point substance are from monomer rectifying
Desorption separation comes out one by one in mechanism, and the plant downstream that the substance desorbed enters our factory utilizes.Such as: monomethyl trichlorine silicon
Alkane is for making white carbon black；Dimethyldichlorosilane is for making raw rubber after hydrolyzing；Tri-methyl-chlorosilane is hydrogeneous for making
Closure agent etc.；High-boiling components a part is used for high boiling cracking, and a part continues on for emptying end gas recycling, realizes the circulation benefit of resource
With, it economizes on resources, it is economic and environment-friendly.
S028 is vented the thick chloromethanes of gas phase, isolates smart chloromethanes, carries out to the second emptying end gas of discharge cold
It is solidifying.
Recovery yield of monomer in emptying end gas in the prior art only has 30%, and the rate of recovery is low, unrecovered emptying end gas
Waste oil and waste acid water can be generated, therefore, to solve the above-mentioned problems, as shown in figure 4, the present invention provides one kind to be used for methyl chloride
The recyclable device 1 of silane emptying end gas recycling, comprising: emptying end gas conveying mechanism 11, the first condensing mechanism 12 and reaction kettle 13,
13 one end of reaction kettle is connected to the first condensing mechanism 12, and 13 other end of reaction kettle is connected to emptying end gas conveying mechanism 11；Emptying
Tail gas conveying mechanism 11 is for inputting the first emptying end gas into reaction kettle 13；First condensing mechanism 12 is for condensing high-boiling components；
Reaction kettle 13 carries out absorbing reaction to the first emptying end gas for condensed high-boiling components.The reaction kettle 13 of the application is frequently with suction
Tower is received, absorption tower is frequently with packed absorber.
In order to there is the high-boiling components of emptying end gas to carry out resource circulation utilization to absorption, as shown in figure 4, therefore the application also wraps
It includes: being connected to the monomer rectifying mechanism 14 of reaction kettle 13；The height that monomer rectifying mechanism 14 is used to have the first emptying end gas to absorption
Boiling object is parsed, is separated.
As shown in figure 4, the application further include: collecting mechanism 15 and power mechanism 16,15 one end of collecting mechanism are connected to instead
Kettle 13 is answered, 15 other end of collecting mechanism is connected to 16 one end of power mechanism, and 16 other end of power mechanism is connected to monomer rectifying machine
Structure 14；Collecting mechanism 15 is used to receive the high-boiling components for absorbing and having the first emptying end gas；Power mechanism 16 has first for that will absorb
The high-boiling components of emptying end gas are passed through monomer rectifying mechanism 14.
Due to carrying out primary condensation to the more demanding of refrigerant to high-boiling components, the first condensing mechanism 12 of the application is often
Using B-grade condensation, as shown in Figure 4, comprising: first-stage condenser 121 and secondary condenser 122,122 one end of secondary condenser connect
It is connected to first-stage condenser 121,122 other end of secondary condenser is connected to reaction kettle 13；First-stage condenser 121 is used for high-boiling components
Carry out primary temperature reducing；Secondary condenser 122 is used to carry out second level cooling to high-boiling components.
As shown in figure 5, a kind of synthesis system for organic silicon monomer synthesis, comprising: 2 He of methylchlorosilane synthesizer
Above-mentioned methylchlorosilane emptying end gas recyclable device 1, methylchlorosilane synthesizer 2 be used for methylchlorosilane emptying end gas
The recyclable device 1 of recycling is connected；Methylchlorosilane synthesizer 2 is for methylchlorosilane synthetic reaction and to the thick of generation
Methylchlorosilane is separated, and obtains smart methylchlorosilane.
In order to enable the high-boiling components cycle applications in methylchlorosilane synthetic reaction into above-mentioned reaction, and can have
Effect ground separates principal product and by-product, and separates to the multiple compounds in by-product, realizes resource again
It utilizes, as shown in figure 5, the methylchlorosilane synthesizer 2 of the application includes: fluidized bed 21, the recycling of cyclone separator 22, first
Mechanism 23, the second recovering mechanism 24, scrubbing tower 25, crude monomer tower 26, de- high tower 27, high boiling tower 28, chloromethanes tower 29 and second
Condensing mechanism 30；Fluidized bed 21 is connected with cyclone separator 22, fluidized bed 21 for silicon powder, chloromethanes and catalyst copper powder into
Row methylchlorosilane synthetic reaction；22 one end of cyclone separator is connected with scrubbing tower 25, the other end respectively with the first recycling machine
Structure 23, the second recovering mechanism 24 are connected, and cyclone separator 22 is used for the thick methyl generated in methylchlorosilane synthetic reaction
Chlorosilane carries out cyclonic separation, obtains the thick methylchlorosilane of gas phase and the thick copper silicon powder of solid phase respectively；First recovering mechanism 23 1
End, 24 one end of the second recovering mechanism are connected with fluidized bed 21, and 23 other end of the first recovering mechanism, the second recovering mechanism 24 are another
One end is connected with reaction kettle 13；One of first recovering mechanism 23 and the second recovering mechanism 24 are for recycling solid phase copper silicon
Solid phase copper silicon powder is flowed back to fluidized bed 21, the first recycling machine for pressurizeing by powder, the first recovering mechanism 23 and the second recovering mechanism 24
The first emptying end gas that structure 23 and the second recovering mechanism 24 are used to be discharged is transported to reaction kettle 13；Scrubbing tower 25 and crude monomer
Tower 26 is connected, and scrubbing tower 25 isolates screenings for washing to the thick methylchlorosilane of gas phase；26 one end of crude monomer tower with
Chloromethanes tower 30 is connected, and 26 other end of crude monomer tower is connected with de- high tower 27, and crude monomer tower 26 is used for isolating screenings
Thick methylchlorosilane separated, respectively be isolated by smart methylchlorosilane, crude monomer and the thick chloromethanes of gas phase；De- high tower 27 with
Monomer rectifying mechanism 14 is connected, and for de- high tower 27 for separating to crude monomer, separation obtains high-boiling components, and high-boiling components are defeated
It send to the first condensing mechanism 12, the crude monomer for isolating high-boiling components is delivered to monomer rectifying mechanism 14；Monomer rectifying mechanism 14
For being parsed, being separated to the crude monomer for absorbing the high-boiling components for having the first emptying end gas and isolating high-boiling components, obtain more
Kind monomer；Chloromethanes tower 29 is connected with the second condensing mechanism 30, and chloromethanes tower 28 is used to separate the thick chloromethanes of gas phase,
Isolate smart chloromethanes；Second condensing mechanism 30 is for condensing the second emptying end gas.Why the application devises
One recovering mechanism 23 and the second recovering mechanism 24 are because the thick copper silicon powder isolated of cyclone separator 22 enters the without pressurization
One recovering mechanism 23 or the second recovering mechanism 24 once pressurization will can not achieve the purpose for collecting thick copper silicon powder, and pass through first
The copper silicon powder that recovering mechanism 23 or the second recovering mechanism 24 are isolated, which needs to pressurize, can just flow back into fluidized bed 21, flow back to speed more
Fastly, therefore a recovering mechanism will be unable to realize and be collected simultaneously, separate thick copper silicon powder, and using the smart copper silicon powder isolated as conjunction
At the function of reaction raw materials；Therefore the application is more scientific；Concrete operations are as follows: when the solid phase splicing of the first recovering mechanism 23 is arrived
When 15t or more or when 24 solid phase of the second recovering mechanism is lower than 5t, the first recovering mechanism 23 and the second recovering mechanism 24 are carried out
Switching, pressurization feed supplement need to add to pressure 0.7MPa, and pressure release splicing needs to let out pressure to 0.1MPa or less.
Since the first recovering mechanism 23 and the second recovering mechanism 24 are intermittent emptying, and emptying end gas amount when being vented
Greatly, reaction kettle 3 is easy to appear dry plate phenomenon, and as shown in Figure 4 and Figure 5, therefore the emptying end gas conveying mechanism 11 of the application often wraps
Include: blowdown piping and emptying surge tank 111, blowdown piping one end is connected to the first recovering mechanism 23 and the second recovering mechanism
On 24, emptying surge tank 111 is connected between blowdown piping and the first condensing mechanism 12, and emptying surge tank 111 makes emptying end gas
It can uniformly input in reaction kettle 3, solve the problems, such as that reaction kettle 3 dry plate occurs because gas velocity is excessive.
Due to containing a small amount of impurity from the high-boiling components that de- high tower 27 comes out, in order to be purified to high-boiling components, such as Fig. 5 institute
Show, the methylchlorosilane synthesizer 2 of the application further includes high boiling tower 28, and de- 27 one end of high tower is connect with high boiling tower 28, takes off height
The tower other end is connected with monomer rectifying mechanism 14, and 28 one end of high boiling tower passes through high-boiling components conveying mechanism 31 and the first condensing mechanism
12 connections, the high-boiling components conveying mechanism 31 of the application often select high-boiling components delivery pump, and de- high tower 27 is for dividing crude monomer
From separation obtains thick high-boiling components and various of monomer mixture, and thick high-boiling components are passed through high boiling tower 28, various of monomer mixture is led to
Enter monomer rectifying mechanism 14, smart high-boiling components are delivered to the first condensing mechanism 12 for isolating smart high-boiling components by high boiling tower 28.
As shown in fig. 6, monomer rectifying mechanism 14 include: take off low tower 141, a first tower 142, gently divide tower 143, hydrogeneous tower 144,
Azeotrope column 145, front three tower 146, monomer rectifying mechanism 14 and de- high tower 27, high boiling tower 28 constitute eight tower distillation technologies；Take off low tower
141 one end are connect with de- high tower 27, are taken off low 141 other end of tower and are connect with a first tower 142；Gently divide 143 one end of tower and takes off low tower 141
Connection, gently divides 143 other end of tower to connect with hydrogeneous tower 144；145 one end of azeotrope column is connect with hydrogeneous tower 144, and azeotrope column 145 is another
One end is connect with front three tower 146, and front three tower 146 is connect with de- high tower 27.Monomer rectifying mechanism 14 is by Trichloromethyl silane, two
The hydrogeneous chlorosilane of the hydrogeneous dichlorosilane of dimethyl dichlorosilane (DMCS), tri-methyl-chlorosilane, tetramethylsilane, monomethyl, dimethyl, height
Object, the low-boiling-point substance Desorption separation one by one from monomer rectifying mechanism 14 are boiled, the plant downstream benefit that the substance obtained enters our factory is desorbed
With.
Above-described specific example of the invention, to the purpose of the present invention, technical scheme and beneficial effects carried out into
One step is described in detail, it should be understood that the above is only a specific embodiment of the present invention, is not limited to this hair
Bright, all within the spirits and principles of the present invention, any modification, equivalent substitution, improvement and etc. done should be included in the present invention
Protection scope within.
Claims (10)
1. a kind of methylchlorosilane emptying end gas recovery method characterized by comprising
The high-boiling components generated in recycling methylchlorosilane synthetic reaction, high-boiling components refer to that boiling point is more than 70.2 DEG C of liquid phase by-product；
Condense the high-boiling components；
First emptying end gas is passed through the condensed high-boiling components；
The condensed high-boiling components absorb first emptying end gas.
2. methylchlorosilane emptying end gas recovery method according to claim 1, which is characterized in that further include: to absorption
There are the high-boiling components of first emptying end gas to be parsed, separated.
3. methylchlorosilane emptying end gas recovery method according to claim 1 or 2, which is characterized in that the high-boiling components
To contain Si-O-Si key or/and Si-CH2The mixture of-Si key or/and Si-Si bond compound.
4. methylchlorosilane emptying end gas recovery method according to claim 1 or 2, which is characterized in that the condensation institute
The method for stating high-boiling components specifically:
Cool down at least through condensed in two stages to the high-boiling components.
5. methylchlorosilane emptying end gas recovery method according to claim 4, which is characterized in that level-one condensation, which uses, to follow
Ring water controls flow velocity of the recirculated water in heat exchanger as refrigerant, is carried out just by the heat exchanger to the high-boiling components
Grade cooling；
B-grade condensation, as refrigerant, is controlled flow velocity of the ethylene glycol in the heat exchanger, is changed by described using ethylene glycol
Hot device carries out second level cooling to the high-boiling components.
6. a kind of recyclable device for the recycling of methylchlorosilane emptying end gas described in claim 1-5 any one, special
Sign is, comprising: emptying end gas conveying mechanism, the first condensing mechanism and reaction kettle, described reaction kettle one end are connected to described
One condensing mechanism, the reaction kettle other end are connected to the emptying end gas conveying mechanism；
The emptying end gas conveying mechanism is for inputting the first emptying end gas into the reaction kettle；
First condensing mechanism is for condensing high-boiling components；
The reaction kettle carries out absorbing reaction to first emptying end gas for condensed high-boiling components.
7. the recyclable device according to claim 6 for the recycling of methylchlorosilane emptying end gas, which is characterized in that also wrap
It includes: being connected to the monomer rectifying mechanism of the reaction kettle；
The monomer rectifying mechanism is used to have the high-boiling components of first emptying end gas to be parsed, separated absorption.
8. the recyclable device according to claim 7 for the recycling of methylchlorosilane emptying end gas, which is characterized in that packet
Include: collecting mechanism and power mechanism, described collecting mechanism one end are connected to the reaction kettle, the collecting mechanism other end connection
In described power mechanism one end, the power mechanism other end is connected to the monomer rectifying mechanism；
The collecting mechanism is used to receive the high-boiling components for absorbing and having first emptying end gas；
The power mechanism is used to absorb the high-boiling components for having first emptying end gas and is passed through the monomer rectifying mechanism.
9. the recyclable device described according to claim 6 or 7 or 8 for the recycling of methylchlorosilane emptying end gas, feature exist
In first condensing mechanism includes first-stage condenser and secondary condenser, and described secondary condenser one end is connected to described one
Grade condenser, the secondary condenser other end are connected to the reaction kettle；
The first-stage condenser is used to carry out primary temperature reducing to the high-boiling components；
The secondary condenser is used to carry out second level cooling to the high-boiling components.
10. the recyclable device described according to claim 6 or 7 or 8 for the recycling of methylchlorosilane emptying end gas, feature exist
In, further includes: the high-boiling components conveying mechanism being connected with first condensing mechanism, the high-boiling components conveying mechanism are used for institute
It states and conveys high-boiling components in the first condensing mechanism；
The reaction kettle is absorption tower.
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Effective date of registration: 20230731 Address after: Room 202, 2 / F, 530 Yashan West Road, gangang District, Jiaxing City, Zhejiang Province, 314201 Patentee after: Hesheng silicon (Jiaxing) Co.,Ltd. Address before: 314201 No. 530 Yashan Road, Zhapu Town, Jiaxing City, Zhejiang Province Patentee before: HOSHINE SILICON INDUSTRY CO.,LTD. |