CN109796488B - Preparation method and preparation device of diphenyldimethoxysilane - Google Patents
Preparation method and preparation device of diphenyldimethoxysilane Download PDFInfo
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- CN109796488B CN109796488B CN201910230342.5A CN201910230342A CN109796488B CN 109796488 B CN109796488 B CN 109796488B CN 201910230342 A CN201910230342 A CN 201910230342A CN 109796488 B CN109796488 B CN 109796488B
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Abstract
The invention discloses a preparation method of diphenyldimethoxysilane, which has the advantages of simple method, high efficiency and high yield, and the technical scheme is characterized by comprising the following steps: the methyl alcohol is metered by a methyl alcohol feed pump through a first rotor flowmeter and then is conveyed to the bottom of the esterification tower, and the diphenyl dichlorosilane monomer is metered by a monomer feed pump through a second rotor flowmeter and then is conveyed to the top of the esterification tower; carrying out counter-current esterification reaction on methanol and a diphenyl dichlorosilane monomer in an esterification tower; the hydrogen chloride gas produced after the esterification reaction is discharged from the top of the esterification tower, the generated crude diphenyldimethoxysilane is left at the bottom of the esterification tower and is sent to a rectifying tower for rectification and separation through an intermediate pump, the qualified diphenyldimethoxysilane product is obtained at the top of the rectifying tower after rectification, and the high-boiling-point substance is obtained at the bottom of the rectifying tower.
Description
Technical Field
The invention belongs to the technical field of chemical industry, and particularly relates to a preparation method of diphenyldimethoxysilane.
Background
The diphenyldimethoxysilane is mainly used in propylene polymerization reaction and plays a role of a catalyst for improving isotacticity. The diphenyldimethoxysilane is obtained by esterification reaction of diphenyldichlorosilane and methanol, and the reaction equation is (C)6H5)2SiCl2+2CH3OH＝＝＝＝(C6H5)2Si(OCH3)2+2 HCl. The existing preparation method is relatively complex, low in efficiency and low in yield, for example, hydrogen chloride gas generated by reaction is easily subjected to side reaction with other reactants if not discharged in time, and byproducts are produced, so that the hydrogen chloride gas needs to be discharged in time, but other substances need to be added for neutralization reaction, so that the reaction system is more complex, and the cost is increased.
Disclosure of Invention
The invention aims to provide a preparation method of diphenyldimethoxysilane, which has the advantages of simple method, high efficiency and high yield.
The purpose of the invention is realized as follows: a preparation method of diphenyldimethoxysilane is characterized by comprising the following steps: the method comprises the following steps:
the methyl alcohol is metered by a methyl alcohol feed pump through a first rotor flowmeter and then is conveyed to the bottom of the esterification tower, and the diphenyl dichlorosilane monomer is metered by a monomer feed pump through a second rotor flowmeter and then is conveyed to the top of the esterification tower; carrying out counter-current esterification reaction on methanol and a diphenyl dichlorosilane monomer in an esterification tower; discharging hydrogen chloride gas produced after the esterification reaction from the top of the esterification tower, remaining the generated crude diphenyldimethoxysilane at the bottom of the esterification tower, pumping the crude diphenyldimethoxysilane to a rectifying tower for rectification and separation through an intermediate pump, obtaining a qualified diphenyldimethoxysilane product at the top of the rectifying tower after rectification, and obtaining a high-boiling-point substance at the bottom of the rectifying tower.
The invention is further configured to: the temperature in the esterification tower body is controlled to be 70-85 ℃, and the temperature at the top of the esterification tower is controlled to be 40-55 ℃.
The invention is further configured to: and (3) decoloring and filtering the high-boiling-point substances at the bottom after rectification and separation in the rectifying tower.
The invention is further configured to: the hydrogen chloride tail gas discharged from the top of the esterification tower in the esterification reaction is absorbed by falling film to prepare hydrochloric acid with the concentration of 31%.
A preparation device of diphenyldimethoxysilane is characterized in that: the method comprises the following steps:
a methanol storage tank: is used for storing the methanol raw material,
a monomer storage tank: is used for storing the diphenyl dichlorosilane monomer,
an esterification tower: is used for carrying out the counter-current esterification reaction,
a rectifying tower: used for rectifying and separating the crude diphenyldimethoxysilane product generated after the esterification reaction;
the methanol storage tank is communicated with the bottom of the esterification tower through a methanol feeding pump and a first rotor flowmeter, the monomer storage tank is communicated with the top of the esterification tower through a monomer feeding pump and a second rotor flowmeter, and the esterification tower is communicated with the rectifying tower through an intermediate pump.
The invention is further configured to: the top of the esterification tower is also connected with a falling film absorber.
The invention is further configured to: the esterification tower is including the top of the tower that connects gradually, the body of the tower and the bottom of the tower, be equipped with the last feed inlet on the top of the tower, go up gas outlet and temperature measurement mouth, be equipped with the first reaction zone that from top to bottom sets gradually in the body of the tower, second reaction zone and third reaction zone, be equipped with the first sieve of a plurality of vertical installations and two liang of settings on the first reaction zone, form the water conservancy diversion passageway between the double-phase adjacent first sieve, be equipped with the second sieve that a plurality of levels set up in the second reaction zone, be equipped with a plurality of fillers in the third reaction zone, be equipped with feed inlet and bottom discharge mouth down on the tower bottom, be equipped.
The invention is further configured to: the upper gas outlet is sequentially connected with a condenser and a reflux tank, the top of the reflux tank is communicated with the falling film absorber, and the bottom of the reflux tank is communicated with the second reaction zone of the esterification tower.
The invention is further configured to: the water conservancy diversion passageway is last to be equipped with design support, and design support includes a plurality of and first sieve level setting separate the net, separates to be equipped with the non-woven fabrics on the net, and separates to have the water conservancy diversion clearance between net and the non-woven fabrics.
The invention is further configured to: the second sieve plate is of a double-layer structure and comprises an upper plate body and a lower plate body, sieve holes are formed in the upper plate body and the lower plate body, the sieve holes in the upper plate body and the sieve holes in the lower plate body are arranged in a staggered mode, and the distance between the upper plate body and the lower plate body is 0.8-1.2 mm.
By adopting the technical scheme, the method has the following advantages: the preparation method has simple steps, does not need to add new substances in a reaction system to neutralize hydrogen chloride, can effectively utilize the by-products obtained after preparation, and has high utilization value; the first reaction zone realizes pre-reaction, hydrogen chloride gas is discharged quickly, the second reaction zone realizes full reaction, the third reaction zone realizes further reaction on the residual small amount of diphenyl dichlorosilane liquid which does not generate reaction, esterification reaction is full through the combination of the first reaction zone, the second reaction zone and the third reaction zone, and hydrogen chloride can be discharged along with methanol gas quickly in an upward floating mode, so that the possibility of generating side reaction is reduced.
Drawings
FIG. 1 is a schematic structural view of the present invention;
FIG. 2 is a schematic view of the structure of an esterification column in the present invention;
FIG. 3 is an enlarged view of portion A of FIG. 2 according to the present invention;
FIG. 4 is an enlarged view of the portion B of FIG. 2 according to the present invention;
FIG. 5 is a block diagram of a manufacturing process of the present invention;
the reference numbers in the figures are: 1. a methanol storage tank; 2. a monomer storage tank; 3. an esterification tower; 31. an upper feed inlet; 32. an upper air outlet; 33. a temperature measurement port; 34. a lower feed inlet; 35. a lower discharge hole; 36. heating a tube; 37. a cooling spacer sleeve; 310. a first reaction zone; 320. a second reaction zone; 330. a third reaction zone; 311. a first screen deck; 312. shaping the bracket; 313. separating the net; 314. non-woven fabrics; 315. a flow guide gap; 316. positioning the projection; 317. clamping a needle; 321. a second screen deck; 322. an upper plate body; 323. a lower plate body; 331. a filler; 4. a rectifying tower; 5. a falling film absorber; 6. a condenser; 7. and (7) refluxing the tank.
Detailed Description
The invention is further described in the following with specific embodiments in conjunction with the accompanying drawings, see fig. 1-5:
a preparation method of diphenyldimethoxysilane is characterized by comprising the following steps: the method comprises the following steps:
the methanol is metered by a first rotor flowmeter through a methanol feed pump and then is conveyed to the bottom of the esterification tower 3, and the diphenyl dichlorosilane monomer is metered by a second rotor flowmeter through a monomer feed pump and then is conveyed to the top of the esterification tower 3; carrying out counter-current esterification reaction on methanol and a diphenyl dichlorosilane monomer in an esterification tower 3; and (3) discharging hydrogen chloride gas produced after the esterification reaction from the top of the esterification tower 3, remaining the generated crude diphenyldimethoxysilane at the bottom of the esterification tower 3, pumping the crude diphenyldimethoxysilane to a rectifying tower 4 for rectification and separation through an intermediate pump, obtaining a qualified product of the diphenyldimethoxysilane at the top of the rectifying tower 4 after rectification, and obtaining a high-boiling-point substance at the bottom of the rectifying tower 4.
The temperature in the tower body of the esterification tower 3 is controlled to be 70-85 ℃, and the temperature at the top of the esterification tower 3 is controlled to be 40-55 ℃.
And the high-boiling residue at the bottom after rectification and separation in the rectifying tower 4 is decolorized and filtered to prepare poly diphenyl methoxy silane, which is a good structural control agent for high-temperature vulcanized silicone rubber and is sold as a byproduct.
Hydrogen chloride tail gas discharged from the top of an esterification tower 3 in the esterification reaction is absorbed by a falling film to prepare hydrochloric acid with the concentration of 31%, the hydrochloric acid with the concentration of 31% can be pumped into a hydrochloric acid storage tank for storage, the hydrochloric acid can be pumped into a reaction kettle, and then metered aluminum hydroxide is added under the stirring state for heating reaction, wherein the reaction temperature is controlled to be 80-100 ℃; after the reaction is finished, the reaction product is sucked into a crystallization kettle, after vacuum crystallization, the crystallization product is put into a centrifuge for centrifugal separation to obtain a finished product of aluminum trichloride, mother liquor is returned to the crystallization kettle for recycling, and is mixed with reaction liquid for continuous crystallization to prepare crystalline aluminum trichloride.
The preparation method has simple steps, does not need to add new substances in a reaction system to neutralize hydrogen chloride, can effectively utilize the by-products obtained after preparation, and has high utilization value.
A preparation device of diphenyldimethoxysilane comprises the following components:
a methanol storage tank 1: is used for storing the methanol raw material,
monomer storage tank 2: is used for storing the diphenyl dichlorosilane monomer,
esterification tower 3: is used for carrying out the counter-current esterification reaction,
and (4) a rectifying tower: used for rectifying and separating the crude diphenyldimethoxysilane product generated after the esterification reaction;
the methanol storage tank 1 is communicated with the bottom of the esterification tower 3 through a methanol feeding pump and a first rotor flowmeter, the monomer storage tank 2 is communicated with the top of the esterification tower 3 through a monomer feeding pump and a second rotor flowmeter, and the esterification tower 3 is communicated with the rectifying tower 4 through an intermediate pump.
The top of the esterification tower 3 is also connected with a falling film absorber 5 for recovering hydrochloric acid.
The heating pipe 36 is used for heating the interior of the esterification tower 3 to control the temperature of the interior of the esterification tower to be 70-85 ℃, the temperature of the bottom of the esterification tower is also controlled to be 70-85 ℃, so that methanol is gasified, the countercurrent esterification reaction of methanol gas and diphenyl dichlorosilane liquid is realized, the cooling spacer sleeve 37 is used for being connected with cooling water, the top of the tower is cooled by the cooling water to control the temperature of the top of the tower to be 40-55 ℃, and the methanol can be liquefied again and flows back into the tower body when entering the top of the esterification tower 3.
The upper air outlet 32 is sequentially connected with a condenser 6 and a reflux tank 7, the top of the reflux tank 7 is communicated with the falling film absorber 5, and the bottom of the reflux tank 7 is communicated with the second reaction zone 320 of the esterification tower 3.
The hydrogen chloride generated by the reaction is discharged from the upper gas outlet 32, is cooled by the condenser 6 and flows to the reflux tank 7, and other gases such as methanol are possibly contained in the hydrogen chloride discharging process, so that other substances can be liquefied again after condensation, are collected by the reflux tank 7 and then flow back to the esterification tower 3 for re-reaction, and the purity of the hydrogen chloride gas can be ensured, and the use amount of the raw materials can be conveniently controlled.
The flow guide channel is provided with a shaping support 312, the shaping support 312 comprises a plurality of separation nets 313 horizontally arranged with the first sieve plate 311, the separation nets 313 are provided with non-woven fabrics 314, and flow guide gaps 315 are arranged between the separation nets 313 and the non-woven fabrics 314.
The first reaction zone 310 is also provided with a mounting plate frame for fixing the first sieve plate 311, the shaping support further comprises a support fixed on the mounting plate frame, the separation net 313 is connected with the support, the separation net 313 can be made of flexible material, the surface of the separation net 313 can be provided with a positioning protrusion 316 and a clamping pin 317, the non-woven fabric 314 is fixed on the clamping pin 317, the non-woven fabric 314 abuts against the positioning protrusion 316, so that a flow guide gap 315 is formed between the separation net 313 and the non-woven fabric 314, the shaping support 312 is only used for fixing the non-woven fabric 314, the non-woven fabric 314 is made of fiber filaments and has good air permeability, the flow of the diphenyldichlorosilane liquid on the non-woven fabric 314 is slow, the methanol gas can flow transversely or vertically with the corresponding non-woven fabric 314, the sufficient contact between the diphenyldichlorosilane liquid and the methanol gas is facilitated, the reaction probability is improved, the product yield is improved, the distance between, ensures that the reaction rate and the air permeability can be improved.
The second sieve plate 321 is of a double-layer structure and comprises an upper plate body 322 and a lower plate body 323, sieve holes are formed in the upper plate body 322 and the lower plate body 323, the sieve holes of the upper plate body 322 and the sieve holes of the lower plate body 323 are arranged in a staggered mode, and the distance between the upper plate body 322 and the lower plate body 323 is 0.8-1.2 mm.
Because the distance between the upper plate body 322 and the lower plate body 323 is smaller, a liquid film layer is easily formed between the upper plate body 322 and the lower plate body 323 by liquid, when the amount of the gasified methanol at the bottom of the esterification tower 3 is increased, the gasified methanol can break through the liquid film layer and enter the first reaction zone 310, and because the sieve holes of the upper plate body 322 and the sieve holes of the lower plate body 323 are arranged in a staggered way, namely are not directly communicated, the flow mode of the gasified methanol in the second sieve plate 321 is horizontal flow, the gas-liquid contact area is greatly improved, the reaction probability is enhanced, and the product yield is improved; the distance between the two groups of second sieve plates 321 can be larger, so that the gas floating upwards is accelerated; through multiple experiments, when the distance between the upper plate body 322 and the lower plate body 323 is smaller than 0.8, and the liquid or gas fluidity between the upper plate body 322 and the lower plate body 323 is gradually reduced along with the reduction of the distance, the reaction rate is too slow, the hydrogen chloride gas generated by the reaction is not easy to float, when the distance between the upper plate body 322 and the lower plate body 323 is larger than 1.2mm, and along with the increase of the distance, the contact between the gas and the liquid is reduced, and the reaction probability is reduced, so that the distance between the upper plate body 322 and the lower plate body 323 is controlled to be 0.8-1.2mm, and the optimal value is 1 mm.
The filler 331 in the third reaction zone 330 may be a plurality of spherical ceramic beads, and after stacking, gaps between the spherical ceramic beads are used for liquid to flow downwards and gas to float upwards, so that the gas and the liquid can further realize counter-flow to generate esterification reaction.
The first reaction zone 310 has the advantages that: due to the arrangement of the non-woven fabric 314, the liquid can seep downwards along the non-woven fabric 314, the flow rate is slow, but the liquid can fully react with the floating methanol gas, and the generated hydrogen sulfide gas can quickly pass through the flow guide gap 315 and be discharged; the advantages of the second reaction zone 320 are: gas and liquid can be fully contacted, the reaction probability is greatly improved, and the esterification reaction effect is optimal; the third reaction zone 330 has the advantages that: because the filler 331 is spherical, the air permeability between the filler 331 is good, the seepage velocity of the liquid is fast, and the liquid can flow along the spherical surface, the flow surface area is large, and the gas-liquid countercurrent esterification reaction between the methanol gas can be realized more easily.
The first reaction zone 310 realizes pre-reaction, hydrogen chloride gas is discharged quickly, the second reaction zone 320 realizes full reaction, the third reaction zone 330 realizes further reaction on the residual small amount of the unreacted diphenyldichlorosilane liquid, the esterification reaction is full through the combination of the first reaction zone 310, the second reaction zone 320 and the third reaction zone 330, and hydrogen chloride can be discharged quickly along with methanol gas in a floating way, so that the possibility of side reaction is reduced, in addition, the structure of the esterification tower 3 is simplified, the height of the esterification tower 3 can be reduced, the manufacturing cost is low, the maintenance is easy, and the yield of the rectified diphenyldimethoxysilane reaches more than 97%.
The relevant indexes of the diphenyldimethoxysilane prepared by the preparation method and the preparation device are as follows:
appearance: a colorless transparent liquid;
the content is as follows: more than or equal to 97 percent;
density at 20 ℃ temperature: 1.06-1.1g/cm3；
Refractive index of 1.535-1.545 ηD 20。
The above embodiments are only preferred embodiments of the present invention, and the protection scope of the present invention is not limited thereby, so: all equivalent changes made according to the structure, shape and principle of the invention are covered by the protection scope of the invention.
Claims (7)
1. A preparation method of diphenyldimethoxysilane is characterized by comprising the following steps: the preparation device adopted comprises:
methanol reservoir (1): is used for storing the methanol raw material,
monomer storage tank (2): is used for storing the diphenyl dichlorosilane monomer,
esterification column (3): is used for carrying out the counter-current esterification reaction,
rectifying column (4): used for rectifying and separating the crude diphenyldimethoxysilane product generated after the esterification reaction;
the methanol storage tank (1) is communicated with the bottom of the esterification tower (3) through a methanol feeding pump and a first rotor flowmeter, the monomer storage tank (2) is communicated with the top of the esterification tower (3) through a monomer feeding pump and a second rotor flowmeter, and the esterification tower (3) is communicated with the rectifying tower (4) through an intermediate pump;
the esterification tower (3) comprises a tower top, a tower body and a tower bottom which are sequentially connected, wherein an upper feeding port (31), an upper gas outlet (32) and a temperature measuring port (33) are arranged on the tower top, a first reaction zone (310), a second reaction zone (320) and a third reaction zone (330) which are sequentially arranged from top to bottom are arranged in the tower body, a plurality of vertically-installed first sieve plates (311) which are arranged in pairs are arranged on the first reaction zone (310), a flow guide channel is formed between every two adjacent first sieve plates (311), a plurality of horizontally-arranged second sieve plates (321) are arranged in the second reaction zone (320), a plurality of fillers (331) are arranged in the third reaction zone (330), a lower feeding port (34) and a lower discharging port (35) are arranged on the tower bottom, a heating pipe (36) is arranged in the tower body, and a cooling spacer;
a shaping support (312) is arranged on the flow guide channel, the shaping support (312) comprises a plurality of separation nets (313) horizontally arranged with the first sieve plate (311), non-woven fabrics (314) are arranged on the separation nets (313), and flow guide gaps (315) are formed between the separation nets (313) and the non-woven fabrics (314);
the preparation method comprises the following steps:
the methanol is metered by a methanol feed pump through a first rotor flow meter and then is conveyed to the bottom of the esterification tower (3), and the diphenyl dichlorosilane monomer is metered by a monomer feed pump through a second rotor flow meter and then is conveyed to the top of the esterification tower (3); carrying out counter-current esterification reaction on methanol and a diphenyl dichlorosilane monomer in an esterification tower; and (3) discharging hydrogen chloride gas produced after the esterification reaction from the top of the esterification tower (3), keeping the generated diphenyl dimethoxysilane crude product at the bottom of the esterification tower (3), pumping the crude product to a rectifying tower (4) for rectification separation through an intermediate pump, obtaining a qualified diphenyl dimethoxysilane product at the top of the rectifying tower (4) after rectification, and obtaining a high-boiling-point substance at the bottom of the rectifying tower (4).
2. The method for preparing diphenyldimethoxysilane as claimed in claim 1, wherein the method comprises the following steps: the temperature in the tower body of the esterification tower (3) is controlled to be 70-85 ℃, and the temperature at the top of the esterification tower is controlled to be 40-55 ℃.
3. The method for preparing diphenyldimethoxysilane as claimed in claim 1, wherein the method comprises the following steps: and the high-boiling residues at the bottom of the rectification tower (4) after rectification and separation are decolorized and filtered.
4. The method for preparing diphenyldimethoxysilane as claimed in claim 1, wherein the method comprises the following steps: the hydrogen chloride tail gas discharged from the top of the esterification tower (3) in the esterification reaction is absorbed by a falling film to prepare hydrochloric acid with the concentration of 31 percent.
5. The method for preparing diphenyldimethoxysilane according to claim 1, wherein the method comprises the following steps: the top of the esterification tower (3) is also connected with a falling film absorber (5).
6. The method for preparing diphenyldimethoxysilane as claimed in claim 5, wherein the method comprises the following steps: the upper air outlet (32) is sequentially connected with a condenser (6) and a reflux tank (7), the top of the reflux tank (7) is communicated with the falling film absorber (5), and the bottom of the reflux tank (7) is communicated with a second reaction zone (320) of the esterification tower (3).
7. The method for preparing diphenyldimethoxysilane according to claim 1, wherein the method comprises the following steps: the second sieve plate (321) is of a double-layer structure and comprises an upper plate body (322) and a lower plate body (323), sieve holes are formed in the upper plate body (322) and the lower plate body (323), the sieve holes of the upper plate body (322) and the sieve holes of the lower plate body (323) are arranged in a staggered mode, and the distance between the upper plate body (322) and the lower plate body (323) is 0.8-1.2 mm.
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| CN113387978B (en) * | 2021-06-11 | 2022-05-10 | 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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| 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 |
| CN102924504A (en) * | 2012-11-20 | 2013-02-13 | 江西晨光新材料有限公司 | Preparation method of propyl trimethoxy silane |
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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 |
| CN102924504A (en) * | 2012-11-20 | 2013-02-13 | 江西晨光新材料有限公司 | Preparation method of propyl trimethoxy silane |
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