CN109796488A - A kind of preparation method and its preparation facilities of dimethoxydiphenylsilane - Google Patents
A kind of preparation method and its preparation facilities of dimethoxydiphenylsilane Download PDFInfo
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- CN109796488A CN109796488A CN201910230342.5A CN201910230342A CN109796488A CN 109796488 A CN109796488 A CN 109796488A CN 201910230342 A CN201910230342 A CN 201910230342A CN 109796488 A CN109796488 A CN 109796488A
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Abstract
The invention discloses a kind of preparation methods of dimethoxydiphenylsilane, it has the advantages that method is simple but high-efficient, high income, its key points of the technical solution are that diphenyl dichlorosilane monomer is delivered to esterification tower top after the metering of the second spinner flowmeter by monomer feed pump the following steps are included: methanol is delivered to esterification column bottom by methanol feed pump after the metering of the first rotor flowmeter；Methanol and diphenyl dichlorosilane monomer carry out adverse current esterification in esterification column；The hydrogen chloride gas produced after esterification at the top of esterification column by being discharged, it generates dimethoxydiphenylsilane crude product and stays in esterification column bottom, and rectifying column is pumped to through centre and carries out rectifying separation, dimethoxydiphenylsilane qualified products are obtained at the top of rectifying column after rectifying, rectifier bottoms obtain high-boiling components, and the present invention is suitable for chemical technology field.
Description
Technical field
The invention belongs to chemical technology fields, refer in particular to a kind of preparation method of dimethoxydiphenylsilane.
Background technique
Dimethoxydiphenylsilane is mainly used in propylene polymerization, plays the catalyst for improving isotacticity.Hexichol
Base dimethoxysilane is reacted to obtain by diphenyl dichlorosilane and methanol esterification, and reaction equation is (C6H5)2SiCl2+
2CH3OH====(C6H5)2Si(OCH3)2+2HCl.Existing preparation method is more many and diverse, low efficiency and yield bottom, such as
If the hydrogen chloride gas that reaction generates is discharged not in time, it is easy to generate side reaction with other reactants, and produce by-product, therefore
It needs for hydrogen chloride gas to be discharged in time, but needs to add other substances and carry out neutralization reaction, so that reaction system is more
Complexity, and cost improves.
Summary of the invention
The object of the present invention is to provide a kind of preparation method of dimethoxydiphenylsilane, but effects simple with method
The advantages of rate height, high income.
The object of the present invention is achieved like this: a kind of preparation method of dimethoxydiphenylsilane, it is characterised in that:
The following steps are included:
Methanol is delivered to esterification column bottom, diphenyl dichlorosilane list after the metering of the first rotor flowmeter by methanol feed pump
Body is delivered to esterification tower top after the metering of the second spinner flowmeter by monomer feed pump；Methanol and diphenyl dichlorosilane monomer exist
Adverse current esterification is carried out in esterification column；The hydrogen chloride gas produced after esterification generates hexichol by being discharged at the top of esterification column
Base dimethoxysilane crude product stays in esterification column bottom, and is pumped to rectifying column through centre and carries out rectifying separation, rectifying column after rectifying
Top obtains dimethoxydiphenylsilane qualified products, and rectifier bottoms obtain high-boiling components.
The present invention is further arranged to: temperature control exists in 70~85 DEG C, tower top temperature control in the esterification column tower body
40~55 DEG C.
The present invention is further arranged to: the high-boiling components of bottom are handled through decolorization filtering after the rectifying column rectifying separation.
The present invention is further arranged to: the hydrogen chloride tail gas being discharged at the top of esterification column in the esterification is through falling film absorption
The hydrochloric acid of concentration 31% is made.
A kind of preparation facilities of dimethoxydiphenylsilane, it is characterised in that: include:
Methanol storage tank: for storing methanol feedstock,
Monomer storage tank: for storing diphenyl dichlorosilane monomer,
Esterification column: for carrying out adverse current esterification,
Rectifying column: the dimethoxydiphenylsilane crude product for will generate after esterification carries out rectifying separation；
It is connected between methanol storage tank and the tower bottom of esterification column by being equipped with methanol feed pump and the first rotor flowmeter, monomer
Be connected between storage tank and the tower top of esterification column by being equipped with monomer feed pump and the second spinner flowmeter, esterification column and rectifying column it
Between pass through intermediate pump be connected to.
The present invention is further arranged to: the tower top of esterification column is also connected with falling-film absorber.
The present invention is further arranged to: the esterification column includes sequentially connected tower top, tower body and tower bottom, and tower top is equipped with
Enterprising material mouth, upper gas outlet and temperature survey mouth, tower body is interior to be equipped with the first reaction zone from top to bottom set gradually, the second reaction
Area and third reaction zone, the first sieve plate that the first reaction zone is equipped with several vertical installations and is arranged two-by-two, two adjacent first sieves
Flow-guiding channel is formed between plate, is equipped with several horizontally disposed second sieve plates in second reaction zone, if being equipped in third reaction zone
Filler stem, tower bottom are equipped with lower feed inlet and lower discharge port, and heating tube is equipped in tower body, and tower top is equipped with cooling spacer.
The present invention is further arranged to: being connected with condenser and return tank, the top of return tank on the upper gas outlet in turn
Portion is connected to falling-film absorber, and the bottom of return tank is connected to the second reaction zone of esterification column.
The present invention is further arranged to: the flow-guiding channel is equipped with setting bracket, and setting bracket includes several with first
The horizontally disposed filter of sieve plate, filter are equipped with non-woven fabrics, and have water conservancy diversion gap between filter and non-woven fabrics.
The present invention is further arranged to: second sieve plate is that double-layer structure includes upper plate body and lower body, upper plate body
With sieve pore is equipped on lower body, the sieve pore of upper plate body and the sieve pore of lower body shift to install, between upper plate body and lower body
Spacing is 0.8-1.2mm.
It has the advantage that this preparation method step is simple by using above-mentioned technical proposal, does not need in reaction system
The new substance of middle addition goes to neutralize hydrogen chloride, and the by-product obtained after preparing can also be utilized effectively, and utility value is high；
First reaction zone realizes pre-reaction, and hydrogen chloride gas is discharged in fast speed, and second reaction zone realizes that it is sufficiently reacted, third reaction
Area realizes further reaction to remaining a small amount of not aitiogenic diphenyl dichlorosilane liquid, passes through the first reaction zone, the
The combination of two reaction zones and third reaction zone, esterification is abundant, and hydrogen chloride can be discharged with methanol gas floating upward quickly, reduces
The possibility of side reaction is generated, furthermore this esterification tower structure simplifies, and can reduce esterification tower height degree, manufacturing cost is low, easy to maintain.
Detailed description of the invention
Fig. 1 is structural schematic diagram of the invention；
Fig. 2 is the structural schematic diagram of esterification column in the present invention；
Fig. 3 is the portion the A enlarged structure schematic diagram of Fig. 2 of the present invention；
Fig. 4 is the portion the B enlarged structure schematic diagram of Fig. 2 of the present invention；
Fig. 5 is preparation flow block diagram of the invention；
Appended drawing reference in figure are as follows: 1, methanol storage tank；2, monomer storage tank；3, esterification column；31, enterprising material mouth；32, upper outlet
Mouthful；33, temperature survey mouth；34, lower feed inlet；35, lower discharge port；36, heating tube；37, cool down spacer；310, the first reaction
Area；320, second reaction zone；330, third reaction zone；311, the first sieve plate；312, setting bracket；313, filter；314, nonwoven
Cloth；315, water conservancy diversion gap；316, positioning protrusion；317, card needle；321, the second sieve plate；322, upper plate body；323, lower body；331,
Filler；4, rectifying column；5, falling-film absorber；6, condenser；7, return tank.
Specific embodiment
With specific embodiment, the invention will be further described with reference to the accompanying drawing, referring to Fig. 1-5:
A kind of preparation method of dimethoxydiphenylsilane, it is characterised in that: the following steps are included:
Methanol is delivered to 3 bottom of esterification column, diphenyl dichlorosilane after the metering of the first rotor flowmeter by methanol feed pump
Monomer is delivered to esterification column 3 after the metering of the second spinner flowmeter by monomer feed pump and pushes up；Methanol and diphenyl dichlorosilane list
Body carries out adverse current esterification in esterification column 3；The hydrogen chloride gas produced after esterification is raw by being discharged at the top of esterification column 3
3 bottom of esterification column is stayed at dimethoxydiphenylsilane crude product, and is pumped to rectifying column 4 through centre and carries out rectifying separation, rectifying
Dimethoxydiphenylsilane qualified products are obtained at the top of rectifying column 4 afterwards, 4 bottom of rectifying column obtains high-boiling components.
At 70~85 DEG C, 3 tower top temperature of esterification column is controlled at 40~55 DEG C for temperature control in 3 tower body of esterification column.
The high-boiling components of bottom are made poly- diphenylmethyl oxysilane, are through decolorization filtering after 4 rectifying of the rectifying column separation
The good constitution controller of high-temperature silicon disulfide rubber, as by-product sale.
The salt of concentration 31% is made through falling film absorption for the hydrogen chloride tail gas being discharged at the top of esterification column 3 in the esterification
Acid, the hydrochloric acid of concentration 31% can be pumped to storage in hydrochloric acid tank, and hydrochloric acid can be pumped to reaction kettle, then in stirring shape
The aluminium hydroxide that metering is added under state carries out temperature reaction, and reaction temperature is controlled at 80~100 DEG C；Reaction is produced after reaction
Object sucks crystallization kettle, is put into centrifuge after vacuum crystallization and is centrifuged, and obtains alchlor finished product, and mother liquor returns to crystallization kettle
It is recycled, continues crystallization with reaction solution mixing and produce crystal aluminum chloride.
This preparation method step is simple, does not need to add new substance in the reaction system and goes to neutralize hydrogen chloride, and prepares
The by-product obtained afterwards can also be utilized effectively, and utility value is high.
A kind of preparation facilities of dimethoxydiphenylsilane, comprising:
Methanol storage tank 1: for storing methanol feedstock,
Monomer storage tank 2: for storing diphenyl dichlorosilane monomer,
Esterification column 3: for carrying out adverse current esterification,
Rectifying column 4: the dimethoxydiphenylsilane crude product for will generate after esterification carries out rectifying separation；
It is connected between methanol storage tank 1 and the tower bottom of esterification column 3 by being equipped with methanol feed pump and the first rotor flowmeter, it is single
It is connected between body storage tank 2 and the tower top of esterification column 3 by being equipped with monomer feed pump and the second spinner flowmeter, esterification column 3 and essence
It evaporates and is connected between tower 4 by intermediate pump.
The tower top of esterification column 3 is also connected with falling-film absorber 5, for recycling hydrochloric acid.
The esterification column 3 includes sequentially connected tower top, tower body and tower bottom, and tower top is equipped with enterprising material mouth 31, upper outlet
Mouth 32 and temperature survey mouth 33, tower body is interior to be equipped with the first reaction zone 310,320 and of second reaction zone from top to bottom set gradually
Third reaction zone 330, the first reaction zone 310 are equipped with several vertical installations and the first sieve plates 311 for being arranged two-by-two, and two adjacent the
Flow-guiding channel is formed between one sieve plate 311, is equipped with several horizontally disposed second sieve plates 321 in second reaction zone 320, third is anti-
If answering and being equipped with filler stem 331 in area 330, tower bottom is equipped with lower feed inlet 34 and lower discharge port 35, is equipped with heating tube 36 in tower body,
Tower top is equipped with cooling spacer 37.
Heating tube 36 makes its control at 70-85 DEG C, column bottom temperature also controls for being internally heated to esterification column 3
Between 70-85 DEG C, it is convenient for methanol gasifying, realizes the adverse current esterification of methanol gas and diphenyl dichlorosilane liquid, cooling
Spacer 37 cools down to tower top by cooling water, makes its control at 40-55 DEG C, so that methanol enters for connecting cooling water
It can liquefy and flow back in tower body again when 3 top of esterification column.
It is connected with condenser 6 and return tank 7, the top of return tank 7 and falling-film absorber 5 on the upper gas outlet 32 in turn
Connection, the bottom of return tank 7 is connected to the second reaction zone 320 of esterification column 3.
The hydrogen chloride that reaction generates is discharged by upper gas outlet 32, return tank 7 is flowed to after the cooling of condenser 6, due to chlorination
Other gases such as methanol may be had in hydrogen discharge process, therefore other materials can liquefy again after condensation, and pass through
Return tank 7 collect after be back in esterification column 3, react again again, both can ensure that the purity of hydrogen chloride gas, also facilitate for
The control of raw material usage amount.
The flow-guiding channel is equipped with setting bracket 312, and setting bracket 312 is set including several with 311 level of the first sieve plate
The filter 313 set, filter 313 are equipped with non-woven fabrics 314, and have water conservancy diversion gap 315 between filter 313 and non-woven fabrics 314.
The installation grillage for fixing the first sieve plate 311 is additionally provided in first reaction zone 310, setting bracket further includes fixing
Bracket on installation grillage, filter 313 is connected with bracket, and filter 313 can be flexible material, and the surface of filter 313 can be with
Setting positioning protrusion 316 and card needle 317, non-woven fabrics 314 are fixed on card needle 317, and non-woven fabrics 314 is supported with positioning protrusion 316,
So that having water conservancy diversion gap 315 between filter 313 and non-woven fabrics 314, setting bracket 312 is only intended to play non-woven fabrics 314
Fixed function, non-woven fabrics 314 are made of fiber filament, have good gas permeability, and diphenyl dichlorosilane liquid is in non-woven fabrics
Flowing on 314 is slower, and methanol gas can realize lateral or vertical Xiang Liudong with opposite non-woven fabrics 314, is convenient for diphenyl two
Coming into full contact between chlorosilane liquid produced and methanol gas improves reaction probabilities, improves the yield of product, water conservancy diversion gap 315
Spacing controls within 2mm, it is ensured that can improve reactivity and improve gas permeability.
It includes upper plate body 322 and lower body 323 that second sieve plate 321, which is double-layer structure, upper plate body 322 and lower body
Sieve pore is equipped on 323, the sieve pore of upper plate body 322 and the sieve pore of lower body 323 shift to install, upper plate body 322 and lower body 323
Between spacing be 0.8-1.2mm.
Since the spacing between upper plate body 322 and lower body 323 is smaller, liquid is between upper plate body 322 and lower body 323
Liquid film layer easy to form, when gasification of methanol increases in the amount of 3 tower bottom of esterification column, gasification of methanol can break through the entrance of liquid film layer
First reaction zone 310, and the sieve pore of the sieve pore and lower body 323 due to upper plate body 322 shifts to install, i.e., is not directly to be connected to,
So the type of flow of the gasification of methanol in the second sieve plate 321 is bottom horizontal flow sheet, gas liquid interfacial area is substantially increased, is strengthened
Reaction probabilities improve the yield of product；Spacing between two group of second sieve plate 321 can be larger, and gas is accelerated to float；Through multiple
Test obtains, when the spacing between upper plate body 322 and lower body 323 is less than 0.8, and as spacing reduces, between liquid
Body or gas fluidity are gradually reduced, and reaction rate is excessively slow, and the hydrogen chloride gas for reacting generation is not easy to float, when upper plate body 322
Spacing between lower body 323 is greater than 1.2mm, and as spacing increases, and the contact of gas and liquid declines, reaction probabilities drop
It is low, therefore the spacing between upper plate body 322 and lower body 323 is controlled in 0.8-1.2mm, and its preferred value is 1mm.
Filler 331 in third reaction zone 330 can be several spherical ceramic beads, heap poststack, between gap for liquid
It flows down and gas floats, so that can further realize adverse current between gas-liquid generates esterification.
The advantages of first reaction zone 310 is: due to the setting of non-woven fabrics 314, liquid can be along the lower infiltration of non-woven fabrics 314, stream
Speed is more slow, but can sufficiently react with floating methanol gas, and the hydrogen sulfide gas generated can then pass through water conservancy diversion gap 315
Quickly through and be discharged；The advantages of second reaction zone 320, is: it can be come into full contact between gas-liquid, reaction probabilities greatly improve,
Esterification effect is optimal；The advantages of third reaction zone 330, is: due to filler 331 be it is spherical, between good permeability, liquid
The percolation flow velocity of body is fast, and liquid can globally flow, and flow meter area is big, it is easier to gas-liquid counter current is realized between methanol gas
Esterification.
First reaction zone 310 realizes pre-reaction, and hydrogen chloride gas is discharged in fast speed, and second reaction zone 320 realizes that it is filled
Dividing reaction, not aitiogenic diphenyl dichlorosilane liquid realizes further reaction to 330 pairs of residues of third reaction zone on a small quantity,
By the combination of the first reaction zone 310, second reaction zone 320 and third reaction zone 330, esterification is abundant, and hydrogen chloride can
It is discharged with methanol gas floating upward quickly, reduces the possibility for generating side reaction, furthermore 3 structure of this esterification column simplifies, and can reduce esterification
3 height of tower, manufacturing cost is low, and easy to maintain, the yield of dimethoxydiphenylsilane reaches 97% or more after rectifying.
The index of correlation of dimethoxydiphenylsilane made from this preparation method and preparation facilities are as follows:
Appearance: colourless transparent liquid；
Content: >=97%；
Density at a temperature of 20 DEG C: 1.06-1.1g/cm3；
Index of refraction: 1.535-1.545 ηD 20。
Above-described embodiment is only presently preferred embodiments of the present invention, is not limited the scope of the invention according to this, therefore: it is all according to
The equivalence changes that structure of the invention, shape, principle are done, should all be covered by within protection scope of the present invention.
Claims (10)
1. a kind of preparation method of dimethoxydiphenylsilane, it is characterised in that: the following steps are included:
Methanol is delivered to esterification column (3) bottom, diphenyl dichlorosilane list after the metering of the first rotor flowmeter by methanol feed pump
Body is delivered to esterification column (3) top by monomer feed pump after the metering of the second spinner flowmeter；Methanol and diphenyl dichlorosilane list
Body carries out adverse current esterification in esterification column；The hydrogen chloride gas produced after esterification is raw by being discharged at the top of esterification column (3)
Esterification column (3) bottom is stayed at dimethoxydiphenylsilane crude product, and is pumped to rectifying column (4) through centre and carries out rectifying separation,
Dimethoxydiphenylsilane qualified products are obtained at the top of rectifying column (4) after rectifying, rectifying column (4) bottom obtains high-boiling components.
2. a kind of preparation method of dimethoxydiphenylsilane according to claim 1, it is characterised in that: the esterification
Temperature control is in 70~85 DEG C, tower top temperature control at 40~55 DEG C in tower (3) tower body.
3. a kind of preparation method of dimethoxydiphenylsilane according to claim 1, it is characterised in that: the rectifying
The high-boiling components of bottom are handled through decolorization filtering after tower (4) rectifying separation.
4. a kind of preparation method of dimethoxydiphenylsilane according to claim 1, it is characterised in that: the esterification
The hydrochloric acid of concentration 31% is made through falling film absorption for the hydrogen chloride tail gas being discharged at the top of esterification column (3) in reaction.
5. a kind of preparation facilities suitable for any one dimethoxydiphenylsilane described in right 1-4, it is characterised in that: packet
It includes:
Methanol storage tank (1): for storing methanol feedstock,
Monomer storage tank (2): for storing diphenyl dichlorosilane monomer,
Esterification column (3): for carrying out adverse current esterification,
Rectifying column (4): the dimethoxydiphenylsilane crude product for will generate after esterification carries out rectifying separation；
It is connected between methanol storage tank (1) and the tower bottom of esterification column (3) by being equipped with methanol feed pump and the first rotor flowmeter, it is single
It is connected between body storage tank (2) and the tower top of esterification column (3) by being equipped with monomer feed pump and the second spinner flowmeter, esterification column
(3) it is connected between rectifying column (4) by intermediate pump.
6. a kind of preparation facilities of dimethoxydiphenylsilane according to claim 5, it is characterised in that: esterification column (3)
Tower top be also connected with falling-film absorber (5).
7. a kind of preparation facilities of dimethoxydiphenylsilane according to claim 5, it is characterised in that: the esterification column
It (3) include sequentially connected tower top, tower body and tower bottom, tower top is equipped with enterprising material mouth (31), upper gas outlet (32) and temperature and surveys
It measures mouth (33), it is anti-that the first reaction zone (310), second reaction zone (320) and the third from top to bottom set gradually is equipped in tower body
It answers area (330), the first reaction zone (310) is equipped with several vertical installations and the first sieve plates (311) for being arranged two-by-two, and two adjacent the
Flow-guiding channel is formed between one sieve plate (311), and several horizontally disposed second sieve plates (321) are equipped in second reaction zone (320),
For third reaction zone (330) if interior be equipped with filler stem (331), tower bottom is equipped with lower feed inlet (34) and lower discharge port (35), tower body
Interior to be equipped with heating tube (36), tower top is equipped with cooling spacer (37).
8. a kind of preparation facilities of dimethoxydiphenylsilane according to claim 6, it is characterised in that: the upper outlet
Condenser (6) and return tank (7) are connected in turn on mouth (32), and the top of return tank (7) is connected to falling-film absorber (5), is returned
The bottom of stream tank (7) is connected to the second reaction zone (320) of esterification column (3).
9. a kind of preparation facilities of dimethoxydiphenylsilane according to claim 5, it is characterised in that: the water conservancy diversion is logical
Road is equipped with setting bracket (312), and setting bracket (312) includes several and the first sieve plate (311) horizontally disposed filter
(313), filter (313) is equipped with non-woven fabrics (314), and has water conservancy diversion gap between filter (313) and non-woven fabrics (314)
(315)。
10. a kind of preparation facilities of dimethoxydiphenylsilane according to claim 5, it is characterised in that: described second
It includes upper plate body (322) and lower body (323) that sieve plate (321), which is double-layer structure, on upper plate body (322) and lower body (323)
It is equipped with sieve pore, the sieve pore of upper plate body (322) and the sieve pore of lower body (323) shift to install, upper plate body (322) and lower body
(323) spacing between is 0.8-1.2mm.
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| CN201910230342.5A CN109796488B (en) | 2019-03-26 | 2019-03-26 | Preparation method and preparation device of diphenyldimethoxysilane |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113387978A (en) * | 2021-06-11 | 2021-09-14 | 江西蓝星星火有机硅有限公司 | Method for preparing diphenyl dimethoxysilane by continuous alcoholysis method |
| CN113980277A (en) * | 2020-07-27 | 2022-01-28 | 新特能源股份有限公司 | Phenyl hydroxyl silicone oil, phenyl hydrogen-containing silicone oil, and preparation methods and preparation devices thereof |
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| CN101348497A (en) * | 2008-08-29 | 2009-01-21 | 仙桃市蓝天化工有限责任公司 | Preparation technique of methyl trimethoxysilane |
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| CN101004012A (en) * | 2003-12-09 | 2007-07-25 | 邱则有 | A hollow shuttering component in use for filling in concrete |
| CN101348497A (en) * | 2008-08-29 | 2009-01-21 | 仙桃市蓝天化工有限责任公司 | Preparation technique of methyl trimethoxysilane |
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| CN113980277A (en) * | 2020-07-27 | 2022-01-28 | 新特能源股份有限公司 | Phenyl hydroxyl silicone oil, phenyl hydrogen-containing silicone oil, and preparation methods and preparation devices thereof |
| CN113387978A (en) * | 2021-06-11 | 2021-09-14 | 江西蓝星星火有机硅有限公司 | Method for preparing diphenyl dimethoxysilane by continuous alcoholysis method |
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