CN113019265A

CN113019265A - Reaction device and method for preparing final product by using same

Info

Publication number: CN113019265A
Application number: CN202110281394.2A
Authority: CN
Inventors: 刘见华; 赵雄; 万烨; 赵宇; 严大洲
Original assignee: China Silicon Corp ltd; China ENFI Engineering Corp
Current assignee: China Silicon Corp ltd; China ENFI Engineering Corp
Priority date: 2021-03-16
Filing date: 2021-03-16
Publication date: 2021-06-25
Anticipated expiration: 2041-03-16
Also published as: CN113019265B

Abstract

The invention belongs to the field of chemical industry, and particularly relates to a reaction device and a method for preparing a final product by using the reaction device. The reaction device comprises an intermediate product preparation device and a final product preparation device, wherein the intermediate product preparation device is provided with a first accommodating cavity, a raw material inlet and an intermediate product outlet, a first catalyst layer and a first rectification layer are arranged in the first accommodating cavity, the first rectification layer is positioned above the first catalyst layer, and the intermediate product outlet is positioned above the first rectification layer; the final product preparation device is provided with a second accommodating cavity, an intermediate product inlet and a first final product outlet, the intermediate product inlet is communicated with the intermediate product outlet, a second catalyst layer and a second rectifying layer are arranged in the second accommodating cavity, the second rectifying layer is positioned above the second catalyst layer, and the first final product outlet is positioned above the second rectifying layer. The reaction device provided by the embodiment of the invention has the advantages of loose reaction conditions, easiness in reaction control, less impurity generation, low reaction cost and the like.

Description

Reaction device and method for preparing final product by using same

Technical Field

The invention belongs to the field of chemical industry, and particularly relates to a reaction device and a method for preparing a final product by using the reaction device.

Background

Monochlorosilane is mainly used for deposition of nitride films in semiconductor manufacturing processes, has the advantages of low deposition temperature, high silicon content and low consumption in the deposition process compared with inorganic silicon such as trichlorosilane, dichlorosilane and the like, and is also a raw material for synthesizing trimethylsilyl. The demand for monochlorosilane is rapidly increasing due to rapid development of the semiconductor industry. The monochlorosilane is an intermediate product for preparing the silane by the disproportionation of the trichlorosilane, and the preparation of the silane by the disproportionation reaction of the trichlorosilane comprises the following three equilibrium reactions:

the first reaction is: performing disproportionation reaction on trichlorosilane to generate dichlorosilane and silicon tetrachloride, wherein the second reaction is as follows: performing disproportionation reaction on dichlorosilane to generate trichlorosilane and monochlorosilane, wherein the third reaction is as follows: and (3) carrying out a monochlorosilane disproportionation reaction to generate dichlorosilane and silane, wherein all three equilibrium reactions are reversible reactions.

The invention patent application with the application publication number of CN103354802A discloses a method and a device for preparing monochlorosilane, dichlorosilane and silane are used as raw materials and react under the action of a catalyst to generate the monochlorosilane, namely, the monochlorosilane is prepared by utilizing the reverse reaction of the third reaction. On one hand, the final product monochlorosilane has low conversion rate, low yield and large difficulty in large-scale preparation due to the limitation of reaction balance. On the other hand, the reaction product needs to be controlled by adjusting the ratio of the raw materials, and dichlorosilane is inevitably generated by other reactions in the reaction process, so that the ratio of the raw materials is difficult to control. In addition, dichlorosilane is expensive and has limited sources, which results in higher cost of monochlorosilane production.

Disclosure of Invention

The present invention is based on the discovery and recognition by the inventors of the following facts and problems:

the three reactions for preparing the silane by the trichlorosilane disproportionation reaction are all reversible reactions, and when a certain reaction reaches equilibrium, the reaction can be promoted to continue to the direction of generating the product by separating the product of the reaction.

The boiling point of trichlorosilane is 31.8 ℃, the boiling point of dichlorosilane is 8.3 ℃, the boiling point of silicon tetrachloride is 57.6 ℃, the boiling point of monochlorosilane is-30.4 ℃, the boiling point of silane is-111.9 ℃, and the difference of the boiling points of the five products is large.

The present invention is directed to solving, at least to some extent, one of the technical problems in the related art.

Therefore, the invention provides a reaction device in one aspect to improve the conversion rate of the final product and further realize the large-scale preparation of the final product.

In another aspect, the present invention provides a method for preparing a final product using a reaction apparatus.

According to the reaction device of the embodiment of the invention, the reaction device comprises:

the intermediate product preparation device is provided with a first accommodating cavity, and a raw material inlet and an intermediate product outlet which are communicated with the first accommodating cavity, wherein a first catalyst layer and a first rectification layer are arranged in the first accommodating cavity, the first rectification layer is positioned above the first catalyst layer, and the intermediate product outlet is positioned above the first rectification layer; and

the final product preparation ware, the final product preparation ware have the second hold the chamber and with the second holds the intermediate product import and the first final product export of chamber intercommunication, the intermediate product import with the intermediate product export intercommunication, wherein, the second holds the intracavity and is equipped with second catalyst layer and second rectification layer, the second rectification layer is located the top on second catalyst layer, first final product export is located the top on second rectification layer.

Therefore, the reaction device provided by the embodiment of the invention has the advantages of loose reaction conditions, easiness in reaction control, less impurity generation, low reaction cost and the like. Meanwhile, unreacted materials are separated through the reaction device provided by the embodiment of the invention and return to the corresponding catalyst layer again for reaction, so that the conversion rate of products and the utilization rate of raw materials are improved.

In some embodiments, the first containing cavity is further provided with a first stripping layer, the first stripping layer is positioned below the first catalyst layer, optionally, the first stripping layer comprises at least one of trays and packing, the first rectifying layer comprises at least one of trays and packing, optionally, the first rectifying layer and the first catalyst layer are arranged at intervals in the up-down direction, and the raw material inlet is positioned between the first rectifying layer and the first catalyst layer in the up-down direction.

Optionally, the reaction apparatus further comprises: the reboiler and first tee bend, the reboiler has reboiler import and reboiler export, first tee bend has first mouth, second mouth and third mouth, be equipped with first liquid export and gaseous phase import on the intermediate product preparation ware, first liquid export sets up in gaseous phase import below, gaseous phase import sets up in the below of first stripping layer, first liquid export with first mouth intercommunication, the second mouth with reboiler import intercommunication, the reboiler export with gaseous phase import intercommunication, each in second mouth and the third mouth all with first mouth intercommunication.

In some embodiments, the reaction apparatus further comprises: the first heat exchanger is provided with a first medium inlet, a first medium outlet, a first inlet, a first outlet and a second outlet, the first inlet is communicated with the intermediate product outlet, the first outlet is communicated with the intermediate product inlet, the intermediate product preparation device is further provided with a first liquid inlet, the first liquid inlet is positioned above the first rectification layer, and the second outlet is communicated with the first liquid inlet.

Optionally, a first liquid distributor is arranged in the first accommodating cavity, the first liquid distributor is provided with a first liquid distributor inlet and a first liquid distributor outlet, the first liquid distributor inlet is communicated with the first liquid inlet, and the first liquid distributor outlet is arranged above the first rectifying section.

In some embodiments, the second containing cavity is further provided with a second stripping layer, the second stripping layer is positioned below the second catalyst layer, optionally, the second stripping layer comprises at least one of trays and packing, and the second rectifying layer comprises at least one of trays and packing.

In some embodiments, the reaction apparatus further comprises: a final product separator having a third accommodating chamber and a final product inlet and a second final product outlet communicating with the third accommodating chamber, wherein a third rectifying layer is provided in the third accommodating chamber, the third rectifying layer including at least one of trays and packing, the third rectifying layer being located between the final product inlet and the second final product outlet in the up-down direction, the final product inlet communicating with the first final product outlet;

optionally, the reaction apparatus further comprises: condenser and second tee bend, the condenser have, condenser import, first condenser export and second condenser export, the second tee bend has fourth mouth, fifth mouth and sixth mouth, be equipped with liquid reflux mouth on the final product separator, liquid reflux mouth sets up the top on third rectification layer, the second final product with condenser import intercommunication, first condenser export with fourth mouth intercommunication, the fifth mouth with liquid reflux mouth intercommunication, the fourth mouth with each in the fifth mouth all with third mouth intercommunication.

In some embodiments, the reaction apparatus further comprises: a second heat exchanger having a second medium inlet, a second medium outlet, a second inlet, a third outlet, and a fourth outlet, the second inlet in communication with the first final product outlet, the third outlet in communication with the final product inlet, the final product separator further having a second liquid inlet, the second liquid inlet located above the second rectification layer, the fourth outlet in communication with the second liquid inlet;

optionally, a second liquid distributor is disposed in the second accommodating cavity, the second liquid distributor has a second liquid distributor inlet and a second liquid distributor outlet, the second liquid distributor inlet is communicated with the second liquid inlet, and the second liquid distributor outlet is disposed above the second rectifying section.

In some embodiments, the reaction apparatus further comprises: a first heat exchanger having a first medium inlet, a first medium outlet, a first inlet, a first outlet, and a second outlet, the first inlet in communication with the intermediate product outlet, the first outlet in communication with the intermediate product inlet, the intermediate product producer further having a first liquid inlet, the first liquid inlet being located above the first rectification layer, the second outlet in communication with the first liquid inlet;

the first heat exchanger is directly fixed at the upper end of the intermediate product preparation device, the final product preparation device is directly fixed at the upper end of the first heat exchanger, the second heat exchanger is directly fixed at the upper end of the final product preparation device, and the final product separator is directly fixed at the upper end of the second heat exchanger.

In some embodiments, the first outlet is disposed at an upper end of the first heat exchanger, the first outlet being disposed opposite the intermediate product inlet from above;

the third outlet is arranged at the upper end part of the second heat exchanger, and the third outlet and the final product inlet are arranged in an up-down opposite mode.

According to the preparation method of preparing a final product using a reaction apparatus of an embodiment of the present invention, the preparation method of preparing a final product using a reaction apparatus includes the steps of:

providing a feedstock to an intermediate product producer, the feedstock undergoing a first reaction within a first catalyst layer to produce an intermediate product;

separating the intermediate product from the raw material by using the first rectification layer;

introducing an intermediate product to a final product producer, the intermediate product undergoing a second reaction in a second catalyst layer to produce a final product; and

separating the final product and the intermediate product by using the second rectification layer;

optionally, the raw material is trichlorosilane, the intermediate product comprises dichlorosilane, the final product comprises monochlorosilane, the first reaction is a disproportionation reaction, the second reaction is a disproportionation reaction, and optionally, the intermediate product further comprises silicon tetrachloride.

Therefore, the preparation method for preparing the final product by using the reaction device has the advantages of loose reaction conditions, easy reaction control, less impurity generation, low reaction cost and the like.

In some embodiments, the final product is introduced to a final product separator for further separation of the final product and the intermediate product within the third rectification layer.

Drawings

FIG. 1 is a schematic structural view of a reaction apparatus according to an embodiment of the present invention.

Fig. 2 is a schematic diagram of the intermediate product producer, first heat exchanger, and reboiler of fig. 1.

Fig. 3 is a schematic diagram of the structure at the final product separator, the second heat exchanger and the condenser in fig. 1.

Reference numerals: a reaction apparatus 100; an intermediate product producer 101; a first receiving cavity 1011; first stripping layer 1012; a first catalyst layer 1013; first rectifying layer 1014; a raw material inlet 1015; an intermediate product outlet 1016; a first liquid inlet 1017; a first liquid outlet 1018; a gas phase inlet 1019; a final product producer 102; a second receiving chamber 1021; second stripping layer 1022; the second catalyst layer 1023; a second rectifying layer 1024; an intermediate product inlet 1025; a first final product outlet 1026; a second liquid inlet 1027; a final product separator 103; a third accommodating chamber 1031; third rectifying layer 1032; a final product inlet 1033; a second final product outlet 1034; liquid return 1035; a first heat exchanger 104; a first media inlet 1041; a first medium outlet 1042; a first inlet 1043; a first outlet 1044; a second outlet 1045; a second heat exchanger 105; a second media inlet 1051; a second media outlet 1052; a second inlet 1053; a third outlet 1054; a fourth outlet 1055; a condenser 106; condenser inlet 1061; a first condenser outlet 1062; a second condenser outlet 1063; a reboiler 107; a reboiler inlet 1071; a reboiler outlet 1072; a first liquid distributor 108; first liquid distributor inlet 1081; a first liquid distributor outlet 1082; a second liquid distributor 109; a second liquid distributor inlet 1091; a second liquid distributor outlet 1092; a first gas phase conduit 110; a second gas phase conduit 111; a first overflow pipe 112; a second overflow pipe 113.

Detailed Description

Reference will now be made in detail to embodiments of the present invention, examples of which are illustrated in the accompanying drawings. The embodiments described below with reference to the drawings are illustrative and intended to be illustrative of the invention and are not to be construed as limiting the invention.

As shown in fig. 1 to 3, a reaction apparatus 100 according to an embodiment of the present invention includes an intermediate product producer 101 and a final product producer 102.

The intermediate product preparation apparatus 101 has a first accommodation chamber 1011, and a first catalyst layer 1013 and a first rectification layer 1014 are provided in the first accommodation chamber 1011, and the first rectification layer 1014 is located above the first catalyst layer 1013. The intermediate product preparation vessel 101 also has a raw material inlet 1015 and an intermediate product outlet 1016 communicating with the first receiving chamber 1011, the intermediate product outlet 1016 being located above the first rectification layer 1014.

The final product preparation apparatus 102 has a second accommodation chamber 1021, a second catalyst layer 1023 and a second rectification layer 1024 are disposed in the second accommodation chamber 1021, and the second rectification layer 1024 is located above the second catalyst layer 1023. Final product preparation vessel 102 also has an intermediate product inlet 1025 and a first final product outlet 1026 communicating with second receiving chamber 1021, first final product outlet 1026 being located above second rectifying layer 1024.

Since the first catalyst layer 1013 and the first rectification layer 1014 are both disposed in the first accommodation chamber 1011 and the raw material inlet 1015 and the intermediate product outlet 1016 are communicated with the first accommodation chamber 1011, the first catalyst layer 1013, the first rectification layer 1014, the raw material inlet 1015 and the intermediate product outlet 1016 are all communicated. Similarly, since second catalyst layer 1023 and second rectifying layer 1024 are disposed in second accommodating chamber 1021 and intermediate product inlet 1025 and first final product outlet 1026 are communicated with second accommodating chamber 1021, second catalyst layer 1023, second rectifying layer 1024, intermediate product inlet 1025 and first final product outlet 1026 are communicated.

When a final product is produced by the reaction apparatus 100 according to the embodiment of the present invention, a raw material enters the first receiving chamber 1011 of the intermediate product producing apparatus 101 from the raw material inlet 1015, and the raw material undergoes a first reaction under the action of the catalyst of the first catalyst layer 1013 located in the first receiving chamber 1011 to produce an intermediate product. Since the first rectifying layer 1014 is located above the first catalyst layer 1013, the intermediate product outlet 1016 is disposed above the first rectifying layer 1014, so that the intermediate product and the unreacted raw material can be separated timely and continuously by the first rectifying layer 1014.

The concentration of the intermediate product in the intermediate product preparation vessel 101 is thus always low, so that the reaction equilibrium of the first reaction can be broken in time, and the first reaction is promoted to proceed toward the reaction direction in which the intermediate product is formed, so that the conversion of the raw material can be increased.

The separated intermediate product enters second receiving chamber 1021 of final product preparation vessel 102 through intermediate product outlet 1016 and intermediate product inlet 1025. In second receiving chamber 1021 of final product preparation vessel 102, the intermediate product undergoes a second reaction by the catalyst of second catalyst layer 1023 located in second receiving chamber 1021, so that a final product is produced. Since second rectifying layer 1024 is located above second catalyst layer 1023, first final product outlet 1026 is provided above second rectifying layer 1024, so that final products and unreacted intermediate products can be separated timely and continuously by second rectifying layer 1024. The separated final product exits final product producer 102 through first final product outlet 1026.

Therefore, the concentration of the final product in the final product preparation device 102 is always low, the reaction balance of the second reaction can be broken in time, the second reaction is promoted to be carried out towards the direction of generating the final product, the conversion rate of the intermediate product can be improved, the yield of the final product is further improved, and the large-scale preparation of the final product is facilitated.

In the prior art, the reaction balance limits cause low conversion rate of intermediate products, low yield of final products and large difficulty in large-scale preparation. In addition, the prior art uses intermediate products to produce final products, but the intermediate products are expensive, and the reaction products need to be adjusted by adjusting the raw material ratio and the reaction temperature, so that the reaction balance is not easy to control, and the impurity components are inevitably generated.

The reaction apparatus 100 according to the embodiment of the present invention includes the first rectifying layer 1014 disposed in the first receiving chamber 1011 and the second rectifying layer 1024 disposed in the second receiving chamber 1021, so that the intermediate product can timely and continuously flow out of the intermediate product preparation 101 and the final product can timely flow out of the final product preparation 102, and the reaction balance between the first reaction and the second reaction can timely be broken, the first reaction is promoted to proceed toward the direction of generating the intermediate product, and the second reaction is promoted to proceed toward the direction of generating the final product.

Therefore, by using the reaction apparatus 100 according to the embodiment of the present invention, the conversion rates of the raw materials and the intermediate products can be increased, and thus the yield of the final product can be increased, and the large-scale preparation of the final product can be realized.

Moreover, by using the reaction apparatus 100 according to the embodiment of the present invention, it is not necessary to use intermediate products to produce final products, so that it is possible to produce final products using inexpensive and easily available raw materials, and since intermediate products and final products can be respectively and timely and constantly discharged from the intermediate product producing device 101 and the final product producing device 102, it is not only possible to obtain final products without strictly controlling the raw material ratio and the reaction temperature, but also possible to reduce the production of impurities. Therefore, by using the reaction apparatus 100 according to the embodiment of the present invention, it is possible to reduce the reaction cost, relax the reaction conditions, reduce the difficulty of controlling the reaction, and reduce the generation of impurities.

For example, the starting material is trichlorosilane, the intermediate products include dichlorosilane (first intermediate product) and silicon tetrachloride (second intermediate product), and the final product includes monochlorosilane (target product) and trichlorosilane (by-product). The first reaction and the second reaction are both disproportionation reactions and are reversible reactions. And dichlorosilane (first intermediate) exits the intermediate product maker from intermediate product outlet 1016 and enters the final product maker 102 from intermediate product inlet 1025. Monochlorosilane (the target product) exits the end product preparation vessel 102 at a first end product outlet 1026.

Therefore, the reaction apparatus 100 according to the embodiment of the present invention has the advantages of loose reaction conditions, easy reaction control, less impurity generation, low reaction cost, etc.

Furthermore, a first intermediate product produced by a first reaction in intermediate product preparation 101 directly flows out of the intermediate product preparation from intermediate product outlet 1016 and a second reaction occurs in intermediate product preparation 102 from intermediate product inlet 1025 of end product preparation 102, whereby a continuous production of a reaction process having two reactions with an intermediate product produced by the first reaction as a raw material for the second reaction can be achieved with reaction apparatus 100 of an embodiment of the present invention.

As shown in fig. 2, in some embodiments, a first stripping layer 1012 is further disposed in the first receiving chamber 1011, and the first stripping layer 1012 is located below the first catalyst layer 1013. In this way, the first stripping layer 1012 can separate the second intermediate product, which is not related to the final product, from the raw material, thereby further promoting the first reaction to proceed toward the intermediate product, and further being beneficial to further improving the conversion rate of the raw material and the yield of the first intermediate product, for example, the silicon tetrachloride is the second intermediate product which is not related to the final product.

Optionally, first stripping layer 1012 includes at least one of trays and packing, and first rectifying layer 1014 includes at least one of trays and packing. Thereby facilitating the separation of the feed and first intermediate product by mass transfer. For example, separation of the feed and the second intermediate product is achieved with first stripping layer 1012, and separation of the feed and the first intermediate product is achieved with first rectifying layer 1014.

Alternatively, the first rectifying layer 1014 and the first catalyst layer 1013 are provided at a distance in the up-down direction, and the raw material inlet 1015 is located between the first rectifying layer 1014 and the first catalyst layer 1013 in the up-down direction. The first rectifying layer 1014 and the first catalyst layer 1013 are disposed at a distance in the up-down direction, so that the raw material can be introduced into the intermediate product preparation apparatus 101 and the first reaction can be performed in the first catalyst layer 1013.

As shown in fig. 1 and 2, optionally, the reaction apparatus 100 further comprises a reboiler 107 and a first tee, the reboiler 107 having a reboiler inlet 1071 and a reboiler outlet 1072, the first tee having a first port, a second port, and a third port. The intermediate product producer 101 is provided with a first liquid outlet 1018 and a gas phase inlet 1019, the first liquid outlet 1018 being disposed below the gas phase inlet 1019, and the gas phase inlet 1019 being disposed below the first stripping layer 1012. The first liquid outlet 1018 is in communication with the first port, the second port is in communication with the reboiler inlet 1071, the reboiler outlet 1072 is in communication with the vapor phase inlet 1019, and each of the second and third ports is in communication with the first port.

The second intermediate product (for example, silicon tetrachloride) separated in the first stripping layer 1012 sinks to the bottom of the intermediate product production apparatus 101, and the second intermediate product flows out of the intermediate product production apparatus 101 from the first liquid outlet 1018, and then a part of the second intermediate product is discharged to the outside through the first port and the third port in this order, and the remaining part of the second intermediate product enters the reboiler 107 through the first port, the second port, and the reboiler inlet 1071 in this order, and is heated to a gas by the reboiler 107, and then returns to the intermediate product production apparatus 101 through the reboiler outlet 1072 and the gas phase inlet 1019 in this order. Since the second intermediate product still contains a small amount of the raw material, the second intermediate product is returned to the intermediate product preparation apparatus 101 in a gaseous state by the reboiler 107, so that the raw material mixed in the second intermediate product more easily enters the first catalyst layer 1013 to perform the first reaction, thereby improving the utilization rate of the raw material.

As shown in fig. 1 and 2, in some embodiments, reaction apparatus 100 further comprises: the first heat exchanger 104, the first heat exchanger 104 has a first medium inlet 1041, a first medium outlet 1042, a first inlet 1043, a first outlet 1044 and a second outlet 1045. The first inlet 1043 is in communication with the intermediate product outlet 1016 and the first outlet 1044 is in communication with the intermediate product inlet 1025. The intermediate product producer 101 also has a first liquid inlet 1017, the first liquid inlet 1017 being located above the first rectification layer 1014, and a second outlet 1045 communicating with the first liquid inlet 1017.

Specifically, the first inlet 1043 and the intermediate product outlet 1016 communicate through the first gas phase conduit 110, and the second outlet 1045 and the first liquid inlet 1017 communicate through the first overflow conduit 112.

The first intermediate product flowing out of the intermediate product outlet 1016 contains a small amount of raw material, and the intermediate product is mostly in a gaseous state and is mostly in a liquid state, and the first intermediate product sequentially passes through the intermediate product outlet 1016 and the first inlet 1043 to enter the first heat exchanger 104 so as to exchange heat with the first medium flowing through the first heat exchanger 104 in the first heat exchanger 104, so as to obtain a first intermediate product mainly in a gaseous state and a raw material mainly in a liquid state, and then the first intermediate product mainly in a gaseous state enters the final product preparation device 102 through the first outlet 1044 and the intermediate product inlet 1025, and the raw material mainly in a liquid state returns to the intermediate product preparation device 101 through the second outlet 1045 and the first liquid inlet 1017 by its own weight.

The first heat exchanger 104 thus serves as both a condenser of the intermediate product preparation apparatus 101 and a reboiler of the final product preparation apparatus 102, and separates the first intermediate product and the raw material mixed therein by gas-liquid separation, so that the purity of the first intermediate product entering the final product preparation apparatus 102 is higher, thereby facilitating the production of the final product in the final product preparation apparatus 102. Compared with the prior art that the reboiler and the condenser are adopted to respectively realize heating and condensation, the quantity of the reboiler and the condenser is greatly reduced, equipment investment and the quantity of process control points are reduced, meanwhile, a cold source and a heat source are greatly saved, the operating cost is reduced, and the manufacturing economy is improved. In addition, the liquid-state-dominant raw materials can return to the intermediate product preparation device 101 by self weight, so that the use of a transmission device is reduced, and the operation reliability of the reaction device 100 is improved.

As shown in fig. 1 and 2, optionally, a first liquid distributor 108 is disposed in first receiving cavity 1011, first liquid distributor 108 has a first liquid distributor inlet 1081 and a first liquid distributor outlet 1082, first liquid distributor inlet 1081 is in communication with first liquid inlet 1017, and first liquid distributor outlet 1082 is disposed above first rectifying layer 1014. The liquid-based feedstock returned to intermediate product producer 101 can be uniformly distributed through first liquid distributor 108 to the top of first rectification layer 1014, increasing the mass transfer efficiency of first rectification layer 1014.

As shown in fig. 1, in some embodiments, a second stripping layer 1022 is further disposed in second receiving chamber 1021, and second stripping layer 1022 is located below second catalyst layer 1023. In this way, the second stripping layer 1022 can be utilized to separate the byproduct from the second intermediate product, and further promote the second reaction to proceed toward the direction of generating the final product, thereby being beneficial to further improving the conversion rate of the first intermediate product (for example, dichlorosilane) and the yield of the target product (for example, monochlorosilane).

As shown in fig. 1, optionally, second stripping layer 1022 includes at least one of trays and packing, and second rectifying layer 1024 includes at least one of trays and packing. Thereby facilitating the separation of intermediate and final products by mass transfer. For example, separation of the raw material and the first intermediate product is achieved by the second stripping layer 1022, and separation of the first intermediate product and the target product is achieved by the second rectifying layer 1024.

As shown in fig. 1 and 3, in some embodiments, reaction apparatus 100 further comprises: a final product separator 103, the final product separator 103 having a third accommodation chamber 1031 and a final product inlet 1033 and a second final product outlet 1034 communicating with the third accommodation chamber 1031. Wherein the third accommodating chamber 1031 is provided with a third rectification layer 1032 therein, the third rectification layer 1032 includes at least one of trays and packing, the third rectification layer 1032 is located between the final product inlet 1033 and the second final product outlet 1034 in the up-down direction, and the final product inlet 1033 is communicated with the first final product outlet 1026.

The final product enters the final product separator 103 through the first final product outlet 1026 and the final product inlet 1033, and the final product can be separated from a small amount of intermediate product (first intermediate product) by the mass transfer function of the third rectification layer 1032, and the final product with higher purity is discharged from the final product preparation device 102 through the second final product outlet 1034, so that the purity of the final product is improved.

As shown in fig. 1 and 3, optionally, the reaction apparatus 100 further comprises: the condenser 106 is provided with a condenser inlet 1061, a first condenser outlet 1062 and a second condenser outlet 1063, the second tee is provided with a fourth port, a fifth port and a sixth port, the final product separator 103 is provided with a liquid reflux port 1035, the liquid reflux port 1035 is arranged above the third rectifying layer 1032, the second final product is communicated with the condenser inlet 1061, the first condenser outlet 1062 is communicated with the fourth port, the fifth port is communicated with the liquid reflux port 1035, and each of the fourth port and the fifth port is communicated with the third port.

The final product discharged from the second final product outlet 1034 includes a target product, impurities (e.g., silane) and a small amount of the first intermediate product, the final product discharged from the second final product outlet 1034 enters the condenser 106 through the condenser inlet 1061 to be condensed, and the target product and the small amount of the first intermediate product are condensed into liquid by the condenser 106, and the impurities are discharged from the second condenser outlet 1063 in a gaseous form. Then, a part of the objective product (containing a small amount of the first intermediate product) is discharged to the outside through the first condenser outlet 1062, the third port, and the sixth port in this order, and the remaining part of the objective product is returned to the final product producing vessel 102 through the first condenser outlet 1062, the third port, the fifth port, and the first condenser outlet 1062 in this order. Since the final product discharged from second final product outlet 1034 includes the target product and impurities, the target product is condensed into a liquid by condenser 106, the impurities are still in a gaseous state, the gaseous impurities exit condenser 106 from second condenser outlet 1063, most of the higher purity, liquid target product is withdrawn from sixth port, and a small portion is returned to final product preparation vessel 102 from liquid reflux port 1035.

Thus, not only the target product and impurities are separated by the condenser 106 to improve the purity of the target product, but also the target product containing a small amount of the first intermediate product is returned to the final product producing vessel 102 in a liquid form, and it is easier to cause the first intermediate product mixed in the target product to flow toward the lower side of the final product separating vessel 103 by mass transfer and finally return to the final product producing vessel 102 to perform the second reaction, thereby contributing to further improvement in the utilization rate of the raw material.

As shown in fig. 1, preferably, the reaction apparatus 100 further includes: a second heat exchanger 105, the second heat exchanger 105 having a second medium inlet 1051, a second medium outlet 1052, a second inlet 1053, a third outlet 1054 and a fourth outlet 1055. Second inlet 1053 is in communication with first final product outlet 1026, third outlet 1054 is in communication with final product inlet 1033, and final product separator 103 further has a second liquid inlet 1027, second liquid inlet 1027 is positioned above second rectification layer 1024, and fourth outlet 1055 is in communication with second liquid inlet 1027. Specifically, the second inlet 1053 is communicated with the first final-product outlet 1026 via the second vapor-phase conduit 111, and the fourth outlet 1055 is communicated with the second liquid inlet 1027 via the second overflow conduit 113.

As with the first heat exchanger 104, through a second heat exchanger 105 to obtain a predominantly gaseous end product and a predominantly liquid first intermediate product. Therefore, the second heat exchanger 105 is used as a condenser of the final product preparation device 102 and a reboiler of the final product separator 103, and further realizes separation of the first intermediate product and the final product through gas-liquid separation, so that the purity of the final product entering the final product separator 103 is higher, and the purity of the target product is further improved. Compared with the prior art that the reboiler and the condenser are adopted to respectively realize heating and condensation, the quantity of the reboiler and the condenser is greatly reduced, equipment investment and the quantity of process control points are reduced, meanwhile, a cold source and a heat source are greatly saved, the operating cost is reduced, and the manufacturing economy is improved. In addition, the liquid-state-dominant first intermediate product can be returned to the intermediate product preparation apparatus 101 by its own weight, so that the use of a transmission device is reduced, and the improvement of the operational reliability of the reaction apparatus 100 is facilitated.

As shown in fig. 1, optionally, a second liquid distributor 109 is disposed in the second accommodating chamber 1021, the second liquid distributor 109 has a second liquid distributor inlet 1091 and a second liquid distributor outlet 1092, the second liquid distributor inlet 1091 is communicated with the second liquid inlet 1027, and the second liquid distributor outlet 1092 is disposed above the second rectifying section. The liquid-state-dominated first intermediate product returned to the final product preparation vessel 102 can be uniformly distributed over the top of the second rectification layer 1024 by the second liquid distributor 109, improving the mass transfer efficiency of the second rectification layer 1024.

As shown in fig. 1, the first heat exchanger 104 is directly fixed to an upper end portion of the intermediate product producer 101, the final product producer 102 is directly fixed to an upper end portion of the first heat exchanger 104, the second heat exchanger 105 is directly fixed to an upper end portion of the final product producer 102, and the final product separator 103 is directly fixed to an upper end portion of the second heat exchanger 105.

The intermediate product preparation device 101, the first heat exchanger 104, the final product preparation device 102, the second heat exchanger 105 and the final product separator 103 are sequentially and directly fixed to form a whole, and the lower part is used as a support seat of the upper part, so that the whole structure of the reaction device 100 is simplified. This increases the integration level of the reaction apparatus 100, and contributes to a reduction in the manufacturing cost of the reaction apparatus 100. In addition, the final product preparation device 102 may utilize a part of the heat source of the intermediate product preparation device 101, and the final product separator 103 may utilize a part of the heat source of the final product preparation device 102, so that the use of the heat sources of the final product preparation device 102 and the final product separator 103 can be reduced, which is advantageous to save energy.

As shown in fig. 1, preferably, a first outlet 1044 is disposed at an upper end of the first heat exchanger 104, the first outlet 1044 being disposed in an up-down opposite relationship to the intermediate product inlet 1025. A third outlet 1054 is provided at the upper end of the second heat exchanger 105, the third outlet 1054 being disposed opposite the final product inlet 1033. Thus, without the need for piping to connect first outlet 1044 to intermediate inlet 1025, the liquid feedstock can be returned to intermediate product producer 101; and without the need for piping to connect third outlet 1054 and final product outlet 1016, the first intermediate product in liquid form can be returned to final product preparation vessel 102, which facilitates simplifying the overall construction of reaction apparatus 100.

The preparation method for preparing the final product using the reaction apparatus 100 includes the steps of:

providing a feedstock to the intermediate product producer 101, the feedstock undergoing a first reaction within the first catalyst layer 1013 to produce a first intermediate product;

the first intermediate product and the raw material are separated by using a first rectification layer 1014;

introducing the first intermediate product into the final product producer 102, the intermediate product undergoing a second reaction in the second catalyst layer 1023 to produce a final product;

separating the final product from the first intermediate product by using a second rectifying layer 1024;

preferably, the final product is introduced into final product separator 103 for further separation of the final product and the first intermediate product within third rectification layer 1032.

The method for preparing the final product by using the reaction apparatus 100 shown in fig. 1 to 3 is described in detail by taking trichlorosilane as a raw material and monochlorosilane as a target product as an example:

trichlorosilane (raw material) enters the intermediate product preparation device 101 from the raw material inlet 1015, and a first reaction occurs in the first catalyst layer 1013 to generate dichlorosilane (first intermediate product) and silicon tetrachloride (second intermediate product). Then, trichlorosilane and silicon tetrachloride are separated by using the first stripping layer 1012, the separated silicon tetrachloride sinks into the bottom of the intermediate product preparation device 101, and the separated trichlorosilane flows to the first catalyst layer 1013 to continue to react. Dichlorosilane and trichlorosilane are separated by a first rectification layer 1014, the separated trichlorosilane enters a first catalyst layer 1013 to continue reacting, and the separated dichlorosilane flows out of the intermediate product preparation device 101 from an intermediate product outlet 1016.

Dichlorosilane flowing out of the intermediate product outlet 1016 enters the first heat exchanger 104 through the first gas phase pipeline 110 and the first inlet 1043, exchanges heat with a first medium in the first heat exchanger 104, and separates dichlorosilane and trichlorosilane (raw materials) through gas-liquid separation in the first heat exchanger 104.

Then, the separated trichlorosilane (raw material) returns to the upper part of the first liquid distributor 108 through the second outlet 1045, the first overflow pipe 112 and the first liquid inlet 1017, enters the first liquid distributor 108 from the first liquid distributor inlet 1081, flows out from the first liquid distributor outlet 1082, and finally enters the first catalyst layer 1013 for the first reaction. The separated dichlorosilane enters the final product producer 102 through a first outlet 1044 and an intermediate inlet 1025.

In the final product preparation device 102, dichlorosilane and a small amount of trichlorosilane (raw material) mixed therein are separated by the second stripping layer 1022, and the trichlorosilane separated by the second stripping layer 1022 is returned to the intermediate product preparation device 101 from the intermediate product inlet 1025, the first outlet 1044, the first heat exchanger 104 and the first overflow pipe 112 for the first reaction. Dichlorosilane separated by the second stripping layer 1022 enters the second catalyst layer 1023 to undergo a second reaction to generate monochlorosilane (a target product) and trichlorosilane (a byproduct). Then, monochlorosilane (target product) and dichlorosilane are separated by the second rectification layer 1024, dichlorosilane separated by the second rectification layer 1024 enters the second catalyst layer 1023 again to undergo a second reaction, and monochlorosilane separated by the second rectification layer 1024 flows out of the final product preparation device 102 from the first final product outlet 1026.

The monochlorosilane flowing out of the first final product outlet 1026 enters the second heat exchanger 105 through the second gas phase pipeline 111 and the second inlet 1053, exchanges heat with the second medium in the second heat exchanger 105, and is separated from dichlorosilane through gas-liquid separation in the second heat exchanger 105.

Thereafter, the separated dichlorosilane returns to the upper side of the second liquid distributor 109 through the fourth outlet 1055, the second overflow pipe 113 and the second liquid inlet 1027, and enters the second liquid distributor 109 from the second liquid distributor inlet 1091, and flows out from the second liquid distributor outlet 1092, and finally enters the second catalyst layer 1023 to undergo the second reaction. The separated monochlorosilane enters the final product separator 103 through a third outlet 1054 and a final product inlet 1033.

In the final product separator 103, monochlorosilane and dichlorosilane are separated by the third rectification layer 1032, and dichlorosilane separated by the third rectification layer 1032 returns to the final product preparation device 102 from the final product inlet 1033, the third outlet 1054, the second heat exchanger 105 and the second overflow pipe 113 to perform the second reaction. The monochlorosilane separated by third rectification layer 1032 exits end product separator 103 from second end product outlet 1034.

Monochlorosilane exiting second end product outlet 1034 enters condenser 106 through condenser inlet 1061. Impurities, such as silane, are produced during the preparation of monochlorosilane by the trichlorosilane reaction. In the condenser 106, the impurities (silane) are discharged in gaseous form from the second condenser outlet 1063, and most of the monochlorosilane (liquid) is returned to the final product preparation vessel 102 through the first condenser outlet 1062, the third port, the fifth port, and the liquid reflux port 1035 in this order; a small part of monochlorosilane (liquid) is discharged to the outside through the first condenser outlet 1062, the third port and the sixth port in this order, and is collected, and the collected target product is a target product.

A part of the silicon tetrachloride liquid at the bottom of the intermediate product preparation vessel 101 flows out from the first liquid outlet 1018, and then most of the silicon tetrachloride liquid is discharged through the first port and the third port in sequence, and a small part of the silicon tetrachloride liquid enters the reboiler 107 through the first port, the second port and the reboiler inlet 1071 in sequence, and is heated by the reboiler 107 to be in a gaseous state and then returns to the intermediate product preparation vessel 101 through the reboiler outlet 1072 and the gas phase inlet 1019.

By utilizing the reaction device 100 provided by the embodiment of the invention, the trichlorosilane which is easy to obtain can be used as a raw material, the intermediate product preparation device 101, the final product preparation device 102 and the final product separator 103 are coupled, the number of independent reactors and rectifying towers is reduced, and the process flow is simple. The intermediate product preparation apparatus 101, the final product preparation apparatus 102, and the final product separator 103 have independent chambers, respectively, and the intermediate product preparation apparatus 101, the final product preparation apparatus 102, and the final product separator 103 may be set to have a uniform diameter form as shown in fig. 1 or a form of being designed to be gradually reduced from bottom to top as needed, and the pressures in the chambers may be controlled as needed to make the pressures in the chambers uniform or different from each other, and the degree of freedom in adjustment and control of the reaction apparatus 100 is large.

The reaction device 100 of the embodiment of the present invention can realize the functions of three rectifying towers in the prior art, and thus the reaction device 100 of the embodiment of the present invention has the advantage of high integration level. In addition, compared with the prior art that each rectifying tower needs one reboiler and one condenser, the reaction device 100 of the embodiment of the present invention uses one first heat exchanger 104 to replace one reboiler and one condenser of one rectifying tower in the prior art, and uses one second heat exchanger 105 to replace one reboiler and one condenser of one rectifying tower in the prior art, thereby reducing the number of heat exchangers used in the reaction device 100, and enabling the reaction device 100 of the embodiment of the present invention to have the advantage of simple overall structure. The pressure of the intermediate product preparation device 101 is 10 to 1000KPa, preferably 50 to 400KPa, and the temperature of the first catalyst layer 1013 is 0 to 120 ℃, preferably 50 to 80 ℃. The pressure of the final product preparation device 102 is 10 to 1000KPa, preferably 50 to 400KPa, and the temperature of the second catalyst layer 1023 is 0 to 120 ℃, preferably 30 to 80 ℃. The pressure of the final product separator 103 is 10 to 1000KPa, preferably 50 to 400 KPa. The catalyst in the two catalyst layers is macroporous weak-base anion exchange resin with tertiary amine groups, and the catalyst is spherical particles with the particle size of 300-1200 mu m.

The temperature of the first medium of the first heat exchanger 104 is higher than the boiling point of dichlorosilane and lower than the boiling point of trichlorosilane under the operating pressure. The temperature of the second medium of the second heat exchanger 105 is higher than the boiling point of monochlorosilane and lower than the boiling point of dichlorosilane at the operating pressure. In other embodiments, the first medium and the second medium can be adjusted according to the material composition, and the cold sources with different temperatures and tastes can be utilized in a graded manner, which is beneficial to reducing the operation cost of the reaction device 100.

In the description of the present invention, it is to be understood that the terms "central," "longitudinal," "lateral," "length," "width," "thickness," "upper," "lower," "front," "rear," "left," "right," "vertical," "horizontal," "top," "bottom," "inner," "outer," "clockwise," "counterclockwise," "axial," "radial," "circumferential," and the like are used in the orientations and positional relationships indicated in the drawings for convenience in describing the invention and to simplify the description, and are not intended to indicate or imply that the referenced devices or elements must have a particular orientation, be constructed and operated in a particular orientation, and are therefore not to be considered limiting of the invention.

Furthermore, the terms "first", "second" and "first" are used for descriptive purposes only and are not to be construed as indicating or implying relative importance or implicitly indicating the number of technical features indicated. Thus, a feature defined as "first" or "second" may explicitly or implicitly include at least one such feature. In the description of the present invention, "a plurality" means at least two, e.g., two, three, etc., unless specifically limited otherwise.

In the present invention, unless otherwise expressly stated or limited, the terms "mounted," "connected," "secured," and the like are to be construed broadly and can, for example, be fixedly connected, detachably connected, or integrally formed; may be mechanically coupled, may be electrically coupled or may be in communication with each other; they may be directly connected or indirectly connected through intervening media, or they may be connected internally or in any other suitable relationship, unless expressly stated otherwise. The specific meanings of the above terms in the present invention can be understood by those skilled in the art according to specific situations.

In the present invention, unless otherwise expressly stated or limited, the first feature "on" or "under" the second feature may be directly contacting the first and second features or indirectly contacting the first and second features through an intermediate. Also, a first feature "on," "over," and "above" a second feature may be directly or diagonally above the second feature, or may simply indicate that the first feature is at a higher level than the second feature. A first feature being "under," "below," and "beneath" a second feature may be directly under or obliquely under the first feature, or may simply mean that the first feature is at a lesser elevation than the second feature.

In the present disclosure, the terms "one embodiment," "some embodiments," "an example," "a specific example," or "some examples" and the like mean that a specific feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the present disclosure. In this specification, the schematic representations of the terms used above are not necessarily intended to refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples. Furthermore, various embodiments or examples and features of different embodiments or examples described in this specification can be combined and combined by one skilled in the art without contradiction.

Although embodiments of the present invention have been shown and described above, it is understood that the above embodiments are exemplary and should not be construed as limiting the present invention, and that variations, modifications, substitutions and alterations can be made to the above embodiments by those of ordinary skill in the art within the scope of the present invention.

Claims

1. A reaction apparatus, comprising:

2. The reactor according to claim 1, wherein the first containing chamber is further provided with a first stripping layer, the first stripping layer is positioned below the first catalyst layer, optionally the first stripping layer comprises at least one of trays and packing, the first rectifying layer comprises at least one of trays and packing, optionally the first rectifying layer and the first catalyst layer are arranged at intervals along the up-down direction, and the raw material inlet is positioned between the first rectifying layer and the first catalyst layer along the up-down direction;

3. The reaction device of claim 1, further comprising: a first heat exchanger having a first medium inlet, a first medium outlet, a first inlet, a first outlet, and a second outlet, the first inlet in communication with the intermediate product outlet, the first outlet in communication with the intermediate product inlet, the intermediate product producer further having a first liquid inlet, the first liquid inlet being located above the first rectification layer, the second outlet in communication with the first liquid inlet;

4. The reactor apparatus of claim 1, wherein the second receiving chamber is further provided with a second stripping layer, the second stripping layer being located below the second catalyst layer, optionally the second stripping layer comprises at least one of trays and packing, and the second rectifying layer comprises at least one of trays and packing.

5. The reaction device of claim 1, further comprising: a final product separator having a third accommodating chamber and a final product inlet and a second final product outlet communicating with the third accommodating chamber, wherein a third rectifying layer is provided in the third accommodating chamber, the third rectifying layer including at least one of trays and packing, the third rectifying layer being located between the final product inlet and the second final product outlet in the up-down direction, the final product inlet communicating with the first final product outlet;

6. The reaction device of claim 5, further comprising: a second heat exchanger having a second medium inlet, a second medium outlet, a second inlet, a third outlet, and a fourth outlet, the second inlet in communication with the first final product outlet, the third outlet in communication with the final product inlet, the final product separator further having a second liquid inlet, the second liquid inlet located above the second rectification layer, the fourth outlet in communication with the second liquid inlet;

7. The reaction device of claim 6, further comprising: a first heat exchanger having a first medium inlet, a first medium outlet, a first inlet, a first outlet, and a second outlet, the first inlet in communication with the intermediate product outlet, the first outlet in communication with the intermediate product inlet, the intermediate product producer further having a first liquid inlet, the first liquid inlet being located above the first rectification layer, the second outlet in communication with the first liquid inlet;

8. The reaction device of claim 6, wherein the first outlet is arranged at the upper end of the first heat exchanger, and the first outlet is arranged opposite to the intermediate product inlet up and down;

9. A method for preparing a final product using a reaction apparatus, comprising the steps of:

10. The production method of a final product using a reaction device according to claim 9, wherein the final product is introduced into a final product separator to further perform separation of the final product and the intermediate product in the third rectifying layer.