CN113845542A - Method and system for removing ethyl hydride in crude dimethyldichlorosilane - Google Patents

Method and system for removing ethyl hydride in crude dimethyldichlorosilane Download PDF

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Publication number
CN113845542A
CN113845542A CN202111270610.XA CN202111270610A CN113845542A CN 113845542 A CN113845542 A CN 113845542A CN 202111270610 A CN202111270610 A CN 202111270610A CN 113845542 A CN113845542 A CN 113845542A
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ethyl hydride
crude
conversion reactor
dimethyldichlorosilane
ethyl
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郭建伟
杨银银
杜鹃
张�杰
李军
张宏伟
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Xinjiang Jingshuo New Material Co ltd
Xinte Energy Co Ltd
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Xinjiang Jingshuo New Material Co ltd
Xinte Energy Co Ltd
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    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07FACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
    • C07F7/00Compounds containing elements of Groups 4 or 14 of the Periodic System
    • C07F7/02Silicon compounds
    • C07F7/08Compounds having one or more C—Si linkages
    • C07F7/20Purification, separation
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D3/00Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
    • B01D3/009Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping in combination with chemical reactions
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J23/00Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
    • B01J23/12Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of actinides
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J23/00Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
    • B01J23/38Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals
    • B01J23/40Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals of the platinum group metals
    • B01J23/44Palladium
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J8/00Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
    • B01J8/02Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with stationary particles, e.g. in fixed beds

Abstract

The invention provides a method and a system for removing ethyl hydride in a crude product of dimethyldichlorosilane, wherein the method comprises the following steps: adding crude dimethyldichlorosilane and hydrogen chloride in gaseous form into an ethyl hydride conversion reactor, carrying out catalytic conversion reaction in the reactor, chlorinating ethyl hydride in the crude dimethyldichlorosilane, and removing the chlorinated ethyl hydride by rectification. The catalyst used in the invention has excellent selectivity and thermal stability, has no corrosion to carbon steel, can effectively chlorinate the ethyl hydride in the dimethyldichlorosilane, and the boiling point of the chlorinated ethyl hydride is improved, so that the ethyl hydride in the dimethyldichlorosilane can be removed by a conventional rectification mode, and the stability of downstream products and the feasibility of a downstream production process are ensured. Meanwhile, the ethyl hydride conversion reactor used in the invention has the advantages of long device running period and short start-up time.

Description

Method and system for removing ethyl hydride in crude dimethyldichlorosilane
Technical Field
The invention relates to the technical field of organic silicon synthesis, in particular to a method and a system for removing ethyl hydride in a crude product of dimethyldichlorosilane.
Background
The development of the organic silicon industry is rapid, the market demand is increased every year, the total yield of organic silicon monomers in China leaps forward to the first in the world at present, and meanwhile, a large amount of high-quality organic silicon monomers are imported every year in China.
At the end of the operation of the monomer synthesis fluidized bed, as the yield of the dimethyldichlorosilane (dimethyl) is reduced, some impurities are also generated, wherein the impurities comprise ethyl hydride (ethylhydrosulfide), the content of the ethyl hydride is low and is in the level of ppm, but when the content of the ethyl hydride in the pure dimethyl exceeds 4ppm, the impurities can affect the post-system, the structure is easy to cause in the hydrolysis process, and the powder eating in the concrete processing process is difficult. Meanwhile, ethyl hydrogen chlorosilane in dimethyldichlorosilane also causes instability of downstream products and color differences such as yellowing and the like, so that ethyl hydride must be removed. However, because the boiling point of ethyl hydride (EtH) is very close to that of dimethyldichlorosilane (90 ℃), it is difficult to remove it from dimethyl by conventional rectification.
Disclosure of Invention
In view of the above, the invention provides a method and a system for removing ethyl hydride in a crude product of dimethyldichlorosilane. The method can effectively chlorinate the ethyl hydride in the dimethyldichlorosilane, and the boiling point of the chlorinated ethyl hydride is improved, so that the ethyl hydride in the dimethyldichlorosilane can be removed by a conventional rectification mode, and the stability of downstream products and the feasibility of a downstream production process are ensured.
In order to solve the technical problems, the invention adopts the following technical scheme:
in a first aspect, the present invention provides a method for removing ethyl hydride from a crude dimethyldichlorosilane product, the method comprising:
providing an ethyl hydride conversion reactor, wherein the inside of the reactor is filled with an alumina molecular sieve loaded with a catalyst, and the catalyst is a palladium catalyst and/or an actinium catalyst;
adding crude dimethyldichlorosilane and hydrogen chloride in gaseous form into the ethyl hydride conversion reactor, carrying out catalytic conversion reaction in the reactor, chlorinating ethyl hydride in the crude dimethyldichlorosilane, and removing the chlorinated ethyl hydride by rectification.
Further, the crude dimethyldichlorosilane is preheated to above 100 ℃ and then added into the ethyl hydride conversion reactor.
Further, the reaction temperature within the ethyl hydride conversion reactor is maintained above 90 ℃.
Further, the outside of the ethyl hydride conversion reactor is provided with a steam jacket.
Further, the flow rate of the crude dimethyldichlorosilane added into the ethyl hydride conversion reactor is 800-900 kg/h, and/or
The flow rate of the hydrogen chloride added into the ethyl hydride conversion reactor is 1.2-1.6 kg/h.
Further, the reaction pressure in the ethyl hydride conversion reactor is 0.6-1.0 barG.
Furthermore, the filling amount of the alumina molecular sieve loaded with the catalyst accounts for 1/2-3/4 of the internal volume of the ethyl hydride conversion reactor.
Further, a metal filter screen is arranged at the outlet of the lower part of the ethyl hydride conversion reactor.
Further, the ethyl hydride conversion reactor is provided with ceramic balls at the bottom and at the upper part thereof, respectively, and the catalyst-loaded alumina molecular sieve is positioned between the bottom ceramic ball and the upper ceramic ball.
In a second aspect, the present invention provides a system for removing ethyl hydride from a crude dimethyldichlorosilane product, the system comprising:
the system comprises a crude monomer tank, a first rectifying tower, a crude first-A tank, a high-boiling storage tank, an ethyl hydride conversion reactor, an anhydrous hydrogen chloride steel bottle, a second rectifying tower, a dimethyl storage tank and a waste storage tank;
the first rectifying tower is simultaneously connected with the crude monomer tank, the crude first methanol tank, the high-boiling storage tank and the ethyl hydride conversion reactor; the ethyl hydride conversion reactor is also connected with the anhydrous hydrogen chloride steel cylinder and the second rectifying tower; the second rectifying tower is also connected with the dimethyl storage tank and the waste storage tank.
The technical scheme of the invention has the following beneficial effects:
the invention provides a method for removing ethyl hydride in a crude product of dimethyldichlorosilane, which comprises the following steps: providing an ethyl hydride conversion reactor, wherein the inside of the reactor is filled with an alumina molecular sieve loaded with a catalyst, and the catalyst is a palladium catalyst and/or an actinium catalyst; adding crude dimethyldichlorosilane and hydrogen chloride in gaseous form into the ethyl hydride conversion reactor, carrying out catalytic conversion reaction in the reactor, chlorinating ethyl hydride in the crude dimethyldichlorosilane, and removing the chlorinated ethyl hydride by rectification. The catalyst used in the invention has excellent selectivity and thermal stability, has no corrosion to carbon steel, can effectively chlorinate the ethyl hydride in the dimethyldichlorosilane, and the boiling point of the chlorinated ethyl hydride is improved, so that the ethyl hydride in the dimethyldichlorosilane can be removed by a conventional rectification mode, and the stability of downstream products and the feasibility of a downstream production process are ensured. Meanwhile, the ethyl hydride conversion reactor used in the invention has the advantages of long device operation period and short start-up time, and the operation period of the ethyl hydride conversion reactor can reach 4 years.
Drawings
FIG. 1 is a schematic diagram of an ethyl hydride conversion reactor;
FIG. 2 is a process flow diagram for removing ethyl hydride from crude dimethyldichlorosilane;
FIG. 3 is a schematic diagram of a system for removing ethyl hydride from a crude dimethyldichlorosilane product.
Reference numerals:
the device comprises an ethyl hydride conversion reactor 1, an alumina molecular sieve 11 loaded with a catalyst, a steam jacket 12, a metal filter screen 13 and ceramic balls 14;
a crude product 21 of dimethyldichlorosilane, low-pressure steam 22, low-pressure condensate 23, an anhydrous hydrogen chloride steel cylinder 24 and a rectification system 25;
a crude monomer tank 31, a first rectifying tower 32, a crude first-stage tank 33, a high-boiling storage tank 34, a second rectifying tower 35, a dimethyl storage tank 36 and a waste storage tank 37.
Detailed Description
For a further understanding of the invention, reference will now be made to the preferred embodiments of the invention in conjunction with the following examples, but it will be understood that the description is intended to illustrate the features and advantages of the invention further, and not to limit the invention.
The following description will be further described with reference to fig. 1 to 3.
In a first aspect, the present invention provides a method for removing ethyl hydride from a crude dimethyldichlorosilane product, as shown in fig. 1 and fig. 2, the method comprises:
providing an ethyl hydride conversion reactor 1, wherein the inside of the reactor is filled with an alumina molecular sieve 11 loaded with a catalyst, and the catalyst is a palladium catalyst and/or an actinium catalyst;
crude dimethyldichlorosilane and hydrogen chloride are fed in gaseous form to the ethyl hydride conversion reactor 1, a catalytic conversion reaction is carried out in the reactor, ethyl hydride in the crude dimethyldichlorosilane is chlorinated, and the chlorinated ethyl hydride is removed by rectification.
According to some embodiments of the present invention, the crude dimethyldichlorosilane is preheated to a temperature above 100 ℃ and added to the ethyl hydride conversion reactor 1. In the present invention, the inventors have found through experiments that the crude dimethyldichlorosilane, once condensed in the ethyl hydride conversion reactor 1, greatly affects the extent of the catalytic reaction and the life of the catalyst in the reactor. In order to ensure the complete catalytic reaction and prolong the service life of the catalyst in the reactor, the crude dimethyldichlorosilane needs to be preheated to more than 100 ℃ and then added into the reactor. Preferably, the crude dimethyldichlorosilane is preheated to 120 ℃. As shown in FIG. 2, the preheating method of the crude dimethyldichlorosilane 21 comprises the following steps: heat is alternated with the low pressure steam 22 for superheating.
According to some embodiments of the invention, the reaction temperature within the ethyl hydride conversion reactor 1 is maintained above 90 ℃. As already mentioned above, the condensation of the crude dimethyldichlorosilane, once it has taken place in the ethyl hydride conversion reactor 1, greatly affects the extent of the catalytic reaction and the lifetime of the catalyst in the reactor. In order to ensure that no condensation occurs in the reactor during the reaction, the present invention ensures that the temperature inside the reactor is maintained above a certain temperature.
According to some embodiments of the present invention, as shown in fig. 1, the outside of the ethyl hydride conversion reactor 1 is provided with a steam jacket 12. According to the invention, the steam jacket 12 is arranged outside the reactor, and the reactor is continuously heated by steam, so that the phenomenon of condensation in the reactor is avoided.
According to some embodiments of the invention, the hydrogen chloride is sourced from a cylinder 24 of anhydrous hydrogen chloride.
According to some embodiments of the present invention, the flow rate of the crude dimethyldichlorosilane to the ethyl hydride conversion reactor 1 is 800 to 900kg/h, and/or the flow rate of the hydrogen chloride to the ethyl hydride conversion reactor 1 is 1.2 to 1.6 kg/h. The inventors have found through experiments that the flow rates of the crude dimethyldichlorosilane and the hydrogen chloride also affect the degree of the catalytic reaction, so that the raw materials need to be selected at proper flow rates. More preferably, the flow rate of the crude dimethyldichlorosilane to the ethyl hydride conversion reactor 1 is 830-850 kg/h, and the flow rate of the hydrogen chloride to the ethyl hydride conversion reactor 1 is 1.3-1.4 kg/h.
According to some embodiments of the invention, the reaction pressure within the ethyl hydride conversion reactor 1 is between 0.6 and 1.0 barG. The low pressure in the ethyl hydride conversion reactor 1 is set in the present invention, mainly to avoid the compaction of the catalyst-loaded alumina molecular sieve 11 in the reactor, and it is desirable to make the catalyst-loaded alumina molecular sieve 11 more fluffy.
According to some embodiments of the present invention, as shown in fig. 1, the loading of the catalyst-loaded alumina molecular sieve 11 is 1/2-3/4 of the internal volume of the ethyl hydride conversion reactor 1. More preferably, the loading of the catalyst-loaded alumina molecular sieves 11 is 2/3 of the internal volume of the reactor. In the present invention, the catalyst is not consumed as the reaction proceeds in principle and can be used for a long time without replacement. The filling amount of the catalyst-supported alumina molecular sieve 11 is 1/2-3/4 in the internal volume of the reactor, and is determined by comprehensively considering the contact area between the catalyst and the reactant, the addition amount of the reactant and other factors, and the filling amount of the catalyst-supported alumina molecular sieve 11 is preferably in the internal volume of the reactor.
According to some embodiments of the invention, the lower outlet of the ethyl hydride conversion reactor 1 is fitted with a metal screen 13. As shown in fig. 1, in the present invention, a metal screen 13 is installed at the lower outlet of the ethyl hydride conversion reactor 1 in order to prevent the catalyst from being carried away from the reactor when the generated product flows out from the lower outlet of the ethyl hydride conversion reactor 1, on the one hand, to contaminate the product and, on the other hand, to cause the loss of the catalyst in the reactor.
According to some embodiments of the present invention, as shown in fig. 1, the ethyl hydride conversion reactor 1 is provided with ceramic balls 14 at the bottom and at the upper part thereof, respectively, and the catalyst-loaded alumina molecular sieves 11 are positioned between the bottom ceramic balls 14 and the upper ceramic balls 14. In the present invention, the bottom and upper parts of the reactor are respectively provided with ceramic balls 14 to serve as a support and a distributor, and it is specifically understood that the alumina molecular sieve 11 loaded with the catalyst is prevented from being compacted, so that the bed pressure difference is increased, and the channeling is also prevented.
Specifically, the method for removing ethyl hydride in crude dimethyldichlorosilane 21 provided by the invention is explained by combining with fig. 2: firstly, the crude dimethyldichlorosilane 21 is superheated by low-pressure steam 22, and low-pressure condensate 23 is discharged after the superheating. The crude dimethyldichlorosilane 21 is preheated to a temperature above 100 ℃, and then enters the ethyl hydride conversion reactor 1 together with hydrogen chloride gas, wherein the hydrogen chloride gas comes from an anhydrous hydrogen chloride steel cylinder 24. The ethyl hydride conversion reactor 1 of the present invention is shown in fig. 1. As can be seen from fig. 1, the ethyl hydride conversion reactor 1 is filled with a catalyst-loaded alumina molecular sieve 11, while the outside of the ethyl hydride conversion reactor 1 is provided with a steam jacket 12. In the reaction of the present invention, under the action of a catalyst, the ethyl hydride in the crude dimethyldichlorosilane 21 reacts with the hydrogen chloride to generate chlorinated ethyl hydride. Chlorinated ethyl hydride, which has an increased boiling point compared to ethyl hydride, can be removed from the crude dimethyldichlorosilane 21 by a subsequent rectification system 25. It should be noted that during the catalytic chlorination reaction, the steam jacket 12 continuously heats the reactor to ensure that no condensation occurs in the reactor. Taking ethylhydrogenshlorosilane as an example, the ethylhydrogenshlorosilane and hydrogen chloride are reacted in the reactor as shown in formula 1:
Figure BDA0003328620410000061
the catalyst used in the invention has excellent selectivity and thermal stability, has no corrosion to carbon steel, can effectively chlorinate the ethyl hydride in the dimethyldichlorosilane, and the boiling point of the chlorinated ethyl hydride is improved, so that the ethyl hydride in the dimethyldichlorosilane can be removed by a conventional rectification mode, and the stability of downstream products and the feasibility of a downstream production process are ensured. The ethyl hydride conversion reactor 1 used in the present invention has the advantages of long device operation period and short start-up time, and the operation period of the ethyl hydride conversion reactor 1 can reach 4 years.
In a second aspect, the present invention provides a system for removing ethyl hydride from crude dimethyldichlorosilane, as shown in fig. 3, the system comprising:
a crude monomer tank 31, a first rectifying tower 32, a crude first methane tank 33, a high-boiling storage tank 34, an ethyl hydride conversion reactor 1, a anhydrous hydrogen chloride steel bottle 24, a second rectifying tower 35, a dimethyl storage tank 36 and a waste storage tank 37;
the first rectifying tower 32 is simultaneously connected with the crude monomer tank 31, the crude first methanol tank 33, the high-boiling storage tank 34 and the ethyl hydride conversion reactor 1, the ethyl hydride conversion reactor 1 is also connected with the anhydrous hydrogen chloride steel cylinder 24 and the second rectifying tower 35, and the second rectifying tower 35 is also connected with the second methanol storage tank 36 and the waste storage tank 37.
Specifically, the invention provides a system for removing ethyl hydride in a crude product of dimethyldichlorosilane, wherein a crude monomer synthesized by a fluidized bed system enters a crude monomer tank 31, then enters a first rectifying tower 32 from the crude monomer tank 31, and a first methyl in the crude monomer is rectified in the first rectifying tower 32 and enters a crude first methyl tank 33; discharging high-boiling chlorosilane in the crude monomer from the tower bottom of the first rectifying tower 32, and feeding the high-boiling chlorosilane into the high-boiling storage tank 34; the crude dimethyl (i.e., crude dimethyldichlorosilane) in the crude monomer is fed to the ethyl hydride conversion reactor 1. In the ethyl hydride conversion reactor 1, hydrogen chloride is simultaneously fed into the anhydrous hydrogen chloride cylinder 24 connected with the anhydrous hydrogen chloride cylinder, and ethyl hydride in the crude dimethyldichlorosilane is chlorinated under the action of a catalyst to generate chlorinated ethyl hydride. After the reaction, the product of the ethyl hydride conversion reactor 1 mixed with dimethyl and chlorinated ethyl hydride enters a second rectifying tower 35 at the rear end, the chlorinated ethyl hydride is removed by rectification in the second rectifying tower 35, the dimethyldichlorosilane enters the dimethyl storage tank 36 after rectification, and the chlorinated ethyl hydride and the high-boiling chlorosilane which is not separated in the first rectifying tower enter the waste storage tank 37.
According to some embodiments of the present invention, the system wherein the first rectification column 32 and the second rectification column 35 are operated simultaneously. In the present invention, since the ethyl hydride conversion reactor 1 is directly connected to the first rectifying tower 32 and the second rectifying tower 35, the ethyl hydride conversion reactor 1 and both rectifying towers must be on-line at the same time, if either one of the two rectifying towers is shut down, the ethyl hydride conversion reactor 1 should be purged to the second rectifying tower 35, if not purged, the gas phase dimethyl would be condensed in the ethyl hydride conversion reactor 1, and the liquid would deactivate the catalyst in the ethyl hydride conversion reactor 1.
It should be noted that during the operation of the system for removing ethyl hydride from the crude dimethyldichlorosilane, the product needs to be sampled and monitored, specifically, the method is as follows: the pure dimethyl material in the dimethyl tank 36 is sampled for testing and if the content of high boiling contaminants therein is above a target value, the ethyl hydride conversion reactor 1 needs to be calibrated. Namely, in the invention, pure dimethyl material is analyzed by sampling, and whether the ethyl hydride conversion reactor 1 normally operates is judged. Generally, the target level of high-boiling contaminants should be less than 2.5ppm, and the high-boiling contaminants are considered acceptable when the level is less than 3.5 ppm. The means for rectifying the ethyl hydride conversion reactor 1 comprises: (1) detecting the supply amount of the hydrogen chloride, and properly and slightly increasing the addition amount of the hydrogen chloride; (2) checking the reaction temperature of the ethyl hydride conversion reactor 1, if the temperature in the reactor is low, the conversion rate will be reduced; (3) the catalyst in the ethyl hydride conversion reactor 1 is replaced.
Unless defined otherwise, technical or scientific terms used herein shall have the ordinary meaning as understood by one of ordinary skill in the art to which this invention belongs. The use of "first," "second," and similar terms in the present application do not denote any order, quantity, or importance, but rather the terms are used to distinguish one element from another. The terms "connected" or "coupled" and the like are not restricted to physical or mechanical connections, but may include electrical connections, whether direct or indirect. "upper", "lower", "left", "right", and the like are used merely to indicate relative positional relationships, and when the absolute position of the object being described is changed, the relative positional relationships are changed accordingly.
While the foregoing is directed to the preferred embodiment of the present invention, it will be understood by those skilled in the art that various changes and modifications may be made without departing from the spirit and scope of the invention as defined in the appended claims.

Claims (10)

1. A method for removing ethyl hydride in a crude product of dimethyldichlorosilane is characterized by comprising the following steps:
providing an ethyl hydride conversion reactor, wherein the inside of the reactor is filled with an alumina molecular sieve loaded with a catalyst, and the catalyst is a palladium catalyst and/or an actinium catalyst;
adding crude dimethyldichlorosilane and hydrogen chloride in gaseous form into the ethyl hydride conversion reactor, carrying out catalytic conversion reaction in the reactor, chlorinating ethyl hydride in the crude dimethyldichlorosilane, and removing the chlorinated ethyl hydride by rectification.
2. The process of claim 1 wherein said crude dimethyldichlorosilane is preheated to a temperature above 100 ℃ prior to being fed to said ethyl hydride conversion reactor.
3. The method of claim 1, wherein the reaction temperature within the ethyl hydride conversion reactor is maintained above 90 ℃.
4. The process of claim 1 wherein the ethyl hydride conversion reactor is externally provided with a steam jacket.
5. The method as claimed in claim 1, wherein the flow rate of the crude dimethyldichlorosilane to the ethyl hydride conversion reactor is 800 to 900kg/h, and/or
The flow rate of the hydrogen chloride added into the ethyl hydride conversion reactor is 1.2-1.6 kg/h.
6. The process of claim 1, wherein the reaction pressure within the ethyl hydride conversion reactor is between 0.6 and 1.0 barG.
7. The method of claim 1, wherein the loading of the catalyst-loaded alumina molecular sieve is 1/2 to 3/4 of the internal volume of the ethyl hydride conversion reactor.
8. The process of claim 1 wherein the lower outlet of the ethyl hydride conversion reactor is fitted with a metal screen.
9. The method of claim 1, wherein the ethyl hydride conversion reactor is provided with ceramic balls at the bottom and top, respectively, and the catalyst-loaded alumina molecular sieves are positioned between the bottom ceramic balls and the top ceramic balls.
10. A system for removing ethyl hydride in a crude product of dimethyldichlorosilane is characterized by comprising:
the system comprises a crude monomer tank, a first rectifying tower, a crude first-A tank, a high-boiling storage tank, an ethyl hydride conversion reactor, an anhydrous hydrogen chloride steel bottle, a second rectifying tower, a dimethyl storage tank and a waste storage tank;
the first rectifying tower is simultaneously connected with the crude monomer tank, the crude first methanol tank, the high-boiling storage tank and the ethyl hydride conversion reactor; the ethyl hydride conversion reactor is also connected with the anhydrous hydrogen chloride steel cylinder and the second rectifying tower; the second rectifying tower is also connected with the dimethyl storage tank and the waste storage tank.
CN202111270610.XA 2021-10-29 2021-10-29 Method and system for removing ethyl hydride in crude dimethyldichlorosilane Pending CN113845542A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115010745A (en) * 2022-06-13 2022-09-06 聊城市鲁西化工工程设计有限责任公司 Method for effectively removing high-boiling-point impurities in dimethyldichlorosilane

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4985579A (en) * 1989-10-16 1991-01-15 Dow Corning Corporation Removal of hydrogen-containing silanes from organosilane mixtures
CN1090579A (en) * 1992-12-03 1994-08-10 瓦克化学有限公司 From methyl chlorosilane, remove the method for silane containing hydrogen
CN105906659A (en) * 2016-05-06 2016-08-31 合盛硅业股份有限公司 Dimethyldichlorosilance purification process and system
CN205653378U (en) * 2016-05-06 2016-10-19 合盛硅业股份有限公司 Dimethyl dichlorosilane's purification system
CN113444121A (en) * 2021-06-08 2021-09-28 天津大学 Method for removing ethyl dichlorosilane impurities in dimethyl dichlorosilane

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4985579A (en) * 1989-10-16 1991-01-15 Dow Corning Corporation Removal of hydrogen-containing silanes from organosilane mixtures
CN1090579A (en) * 1992-12-03 1994-08-10 瓦克化学有限公司 From methyl chlorosilane, remove the method for silane containing hydrogen
CN105906659A (en) * 2016-05-06 2016-08-31 合盛硅业股份有限公司 Dimethyldichlorosilance purification process and system
CN205653378U (en) * 2016-05-06 2016-10-19 合盛硅业股份有限公司 Dimethyl dichlorosilane's purification system
CN113444121A (en) * 2021-06-08 2021-09-28 天津大学 Method for removing ethyl dichlorosilane impurities in dimethyl dichlorosilane

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115010745A (en) * 2022-06-13 2022-09-06 聊城市鲁西化工工程设计有限责任公司 Method for effectively removing high-boiling-point impurities in dimethyldichlorosilane

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