An apparatus for the synthesis of triethylsilane

Abstract

This utility model relates to the field of triethylsilane synthesis technology and discloses an apparatus for triethylsilane synthesis, comprising: a raw material storage component for storing synthesis raw materials; a mixing device for mixing the raw materials output from the raw material storage component; and a fixed-bed reactor filled with a catalyst. By providing the temperature required for the reaction, the mixed raw materials react with each other on the catalyst surface under certain pressure and temperature to generate the desired substance. This utility model provides a production apparatus for triethylsilane, which is a fully continuous process device including reaction and separation processes. This apparatus supports the production of triethylsilane from tetrahydrosilane and ethylene via fixed-bed catalytic reaction. The apparatus has a simple process, high atom utilization, simplified flow, no solvent use, low waste, and can achieve continuous and automated operation.

Description

Technical Field

[0001] This utility model relates to the field of triethylsilane synthesis technology, and in particular to an apparatus for the synthesis of triethylsilane. Background Technology

[0002] Triethylsilane is a widely used fine chemical. In the pharmaceutical field, it is a highly selective reducing agent. It is used as a reducing agent in all diabetes drugs such as dapagliflozin, empagliflozin, quercetin, and iodaggliflozin. It is also used in the synthesis of the antiviral drug oseltamivir phosphate. This product is also used in the chip manufacturing process.

[0003] Currently, the main industrial method for producing triethylsilane is the Grignard process, which uses chloroethane and trichlorosilane as starting materials.

[0004]

[0005]

[0006] First, in an ether solvent, chloroethane and magnesium shavings or powder undergo a Grignard reaction to generate ethyl magnesium chloride Grignard reagent. Then, trichlorosilane is added to generate triethylsilane and magnesium chloride. After quenching, washing, concentration, and distillation, triethylsilane is obtained.

[0007] Although the raw materials used in this method are relatively inexpensive, it has the following drawbacks:

[0008] The Grignard reaction between chloroethane and metallic magnesium is a dangerous reaction. During the initiation process, it can easily cause hazards such as material spillage and explosion. Moreover, the use of diethyl ether as a solvent, which has a low boiling point, further exacerbates the danger.

[0009] The second step of the reaction releases a large amount of heat, and each molecule of product generates three molecules of salt. The reaction process has a high solid content, making stirring difficult, which is not conducive to heat exchange and makes the reaction difficult to control.

[0010] The production process is cumbersome, has low atom utilization, is lengthy, and consumes a lot of energy.

[0011] It produces a large amount of magnesium chloride that has no value for use, and its environmental treatment is difficult. Utility Model Content

[0012] The purpose of this invention is to solve the problems existing in the prior art by proposing an apparatus for the synthesis of triethylsilane.

[0013] To achieve the above objectives, the present invention adopts the following technical solution:

[0014] An apparatus for the synthesis of triethylsilane, comprising:

[0015] Raw material storage components are used to store synthetic raw materials;

[0016] A mixing device for mixing the raw materials output from the raw material storage component;

[0017] A fixed-bed reactor, filled with catalyst, provides the temperature required for the reaction, allowing the mixed raw materials to react in contact with the catalyst surface under certain pressure and temperature to generate the desired substances;

[0018] Forward distillation columns are used to separate unwanted components from the products of fixed-bed reactors.

[0019] The finished product distillation column is used to purify the product output from the fore-distillation column.

[0020] Preferably, the raw material storage component includes a silicon tetrahydrogenate cylinder and an ethylene cylinder, and the output ends of the silicon tetrahydrogenate cylinder and the ethylene cylinder are connected to the input end of the mixing device in sequence through a pressure reducer, a gas mass flow meter and a one-way valve.

[0021] Preferably, the output of the mixing device enters the fixed-bed reactor sequentially through a pressure gauge at the column front.

[0022] Preferably, the fixed-bed reactor is provided with a jacket on the outside, and the temperature required for the reaction is provided by injecting a heat source into the jacket.

[0023] Preferably, the output end of the fixed-bed reactor is connected to the input end of the foredistillation column via a back pressure valve, and the back pressure valve maintains the reaction pressure inside the fixed-bed reactor.

[0024] Preferably, the top of the foredistillation column is connected in sequence to a top condenser and a foredistillation receiving tank via pipelines. When the material enters the foredistillation column, the reaction mixture diethylsilane and triethylsilane are separated between the trays. The gaseous diethylsilane is cooled into liquid in the top condenser and collected in the foredistillation receiving tank, ensuring that the diethylsilane in the high-boiling-point components in the column is completely distilled off.

[0025] Preferably, the foredistillation column is connected to the product distillation column via a delivery pump.

[0026] Preferably, the top of the product distillation column is connected in sequence to a product condenser and a product receiving tank via pipelines. A high-boiling mixture containing diethylsilane enters the product distillation column via a transfer pump. Triethylsilane and tetraethylsilane are separated on the trays. Triethylsilane has a lower boiling point than tetraethylsilane. The gaseous triethylsilane is condensed into a liquid state in the product condenser and collected in the product receiving tank.

[0027] Compared with the prior art, the beneficial effects of this utility model are:

[0028] This invention provides a production apparatus for producing triethylsilane, which is a fully continuous process device including a reaction process device and a separation process device. The device supports the production of triethylsilane from tetrahydrosilane and ethylene via fixed-bed catalytic reaction. The device has a simple process, high atom utilization, simplified process, does not use solvents, produces less waste, and can achieve continuous and automated operation. Attached Figure Description

[0029] Figure 1 This is a schematic diagram of the apparatus for the synthesis of triethylsilane proposed in this utility model.

[0030] In the diagram: 1. Silicon tetrahydrogenate cylinder; 2. Ethylene cylinder; 3. Pressure regulator; 4. Gas mass flow meter; 5. Check valve; 6. Mixer; 7. Column pressure gauge; 8. Fixed bed reactor; 9. Back pressure valve; 10. Fore-distillation column; 11. Top condenser; 12. Fore-distillation receiving tank; 13. Transfer pump; 14. Finished product distillation column; 15. Finished product condenser; 16. Finished product receiving tank. Detailed Implementation

[0031] To make the technical means and objectives and effects of this utility model easier to understand, the embodiments of this utility model will be described in detail below with reference to specific figures.

[0032] It should be noted that all directional and positional terms used in this utility model, such as "up," "down," "left," "right," "front," "back," "vertical," "horizontal," "inner," "outer," "top," "lower," "lateral," "longitudinal," and "center," are only used to explain the relative positional relationships and connection arrangements between components in a specific state (as shown in the accompanying drawings). They are merely for the convenience of describing this utility model and do not require that this utility model be constructed and operated in a specific orientation; therefore, they should not be construed as limitations on this utility model. Furthermore, descriptions involving "first," "second," etc., in this utility model are for descriptive purposes only and should not be construed as indicating or implying their relative importance or implicitly specifying the number of technical features indicated.

[0033] In the description of this utility model, unless otherwise explicitly specified and limited, the terms "installation," "connection," and "joining" should be interpreted broadly. For example, they can refer to a fixed connection, a detachable connection, or an integral connection; they can refer to a mechanical connection; they can refer to a direct connection or an indirect connection through an intermediate medium; and they can refer to the internal connection of two components. Those skilled in the art can understand the specific meaning of the above terms in this utility model based on the specific circumstances.

[0034] In the description of this specification, the references to terms such as "one embodiment," "some embodiments," "illustrative embodiment," "example," "specific example," or "some examples," etc., indicate that a specific feature, structure, material, or characteristic described in connection with that embodiment or example is included in at least one embodiment or example of the present invention. In this specification, the illustrative expressions of the above terms do not necessarily refer to the same embodiment or example. Furthermore, the specific features, structures, materials, or characteristics described may be combined in any suitable manner in one or more embodiments or examples.

[0035] Reference Figure 1 An apparatus for the synthesis of triethylsilane, comprising:

[0036] Raw material storage components are used to store synthetic raw materials;

[0037] The mixing device is used to mix the raw materials output from the raw material storage component. The mixing device adopts a gas mixer 6, which is used to mix the two gases evenly before they enter the catalyst, which is the key to improving the reaction selectivity.

[0038] Fixed-bed reactor 8 is the key reaction site and is filled with catalyst. By providing the temperature required for the reaction, the mixed raw materials react with the catalyst surface under certain pressure and temperature. The products leave the catalyst under the impetus of gravity, diffusion and gas flow, thus achieving the purpose of the reaction.

[0039] Forward distillation column 10 is used to separate unwanted components from the products generated by fixed-bed reactor 8;

[0040] The finished product distillation column 14 is used to purify the product output from the fore-distillation column 10.

[0041] Compared with the prior art, this application provides a production apparatus for producing triethylsilane, which is a fully continuous process apparatus including a reaction process apparatus and a separation process apparatus. The apparatus supports the production of triethylsilane from tetrahydrosilane and ethylene via fixed-bed catalytic reaction. The apparatus has a simple process, high atom utilization, simplified process, does not use solvents, produces less waste, and can achieve continuous and automated operation, making it suitable for widespread promotion and application.

[0042] In this embodiment, the raw material storage component includes a silicon tetrahydrogenate cylinder 1 and an ethylene cylinder 2. The output ends of both the silicon tetrahydrogenate cylinder 1 and the ethylene cylinder 2 are connected to the input end of the mixing device in sequence through a pressure reducer 3, a gas mass flow meter 4, and a one-way valve 5. The gas mass flow meter 4 is a thermal mass flow meter with control function, used for accurate gas measurement. It has a control function and can automatically adjust according to the set value of the control system to stabilize the gas flow rate at the set value. This is the key to ensuring that the silicon tetrahydrogenate and ethylene gases react in proportion. The one-way valve 5 is installed to prevent materials from flowing back into the flow meter or even the cylinder when the pipeline pressure is unbalanced.

[0043] In this embodiment, the output of the mixing device enters the fixed bed reactor 8 sequentially through the column pressure gauge 7.

[0044] In this embodiment, a jacket is provided on the outside of the fixed bed reactor 8, and the temperature required for the reaction is provided by injecting a heat source into the jacket.

[0045] In this embodiment, the output end of the fixed bed reactor 8 is connected to the input end of the fore-distillation column 10 through the back pressure valve 9. The back pressure valve 9 is a key device for maintaining a certain pressure inside the fixed bed reactor 8. When the pressure is greater than the set pressure, the reactants break through the elastic device of the back pressure valve 9 and leave the reactor.

[0046] In this embodiment, the top of the foredistillation column 10 is connected in sequence to the top condenser 11 and the foredistillation receiving tank 12 via pipelines. Although the catalytic reaction ensures high selectivity, it inevitably generates byproducts such as diethylsilane and tetraethylsilane, which need to be purified by distillation. The function of the foredistillation column 10 is to separate the diethylsilane and triethylsilane reaction mixture between the trays when the material enters the foredistillation column 10. The gaseous diethylsilane is cooled into liquid in the top condenser 11 and collected in the foredistillation receiving tank 12, ensuring that the diethylsilane in the high-boiling-point components in the column is completely distilled off.

[0047] In this embodiment, the fore-distillation column 10 is connected to the product distillation column 14 via a transfer pump 13. The top of the product distillation column 14 is connected in sequence to the product condenser 15 and the product receiving tank 16 via pipelines. A high-boiling mixture containing diethylsilane enters the product distillation column 14 via the transfer pump 13. Triethylsilane and tetraethylsilane are separated on the trays. Triethylsilane has a lower boiling point than tetraethylsilane. The gaseous triethylsilane is condensed into a liquid state in the product condenser 15 and collected in the product receiving tank 16.

[0048] Working principle:

[0049] Silicon tetrahydrode cylinder 1 and ethylene cylinder 2 store silicon tetrahydrode gas and ethylene gas respectively. Pressure regulators 3 are installed to control the output pressure. Pressure regulator 3 is connected to a gas mass flow meter 4 via a pipeline. This gas mass flow meter 4 has the function of controlling the flow rate according to set requirements, aiming to control the reaction equivalence of the two gaseous raw materials. Accurate equivalence control is beneficial to increasing the proportion of the main product. A one-way valve 5 is connected to the outlet of gas mass flow meter 4 to prevent gas or liquid backflow from damaging the gas mass flow meter 4 under pressure fluctuations. The silicon tetrahydrode gas and ethylene gas pipelines converge at a T-junction and enter a mixer 6. Under gas flow conditions, the two gases are mixed uniformly. The pressure of the mixed gas is measured by a column pressure gauge 7. It is then connected to a fixed-bed reactor 8 via a pipeline. The fixed-bed reactor 8 is equipped with a jacket, and the required temperature for the reaction can be provided by a heat source such as an oil bath or steam. The fixed-bed reactor 8 is filled with a granular catalyst. The gas reacts on the catalyst surface under a certain pressure and temperature to generate the desired substances. The reaction formula is as follows:

[0050]

[0051] A back pressure valve 9 is connected to the outlet of the fixed-bed reactor 8 to maintain a specific reaction pressure within the reactor. The back pressure valve 9 is connected to a foredistillation column 10. Since the reaction process involves the production of diethylsilane, which has a boiling point of 56°C (lower than the product boiling point of 109°C), it is split at the top of the foredistillation column 10. Triethylsilane and the byproduct tetraethylsilane remain in the bottom of the column. The foredistillation column 10 has 30 trays and 15 feed trays. A foredistillation condenser 11 is connected to the top of the foredistillation column 10 to condense the vapor phase components. The condensate flows through a pipeline into the foredistillation receiving tank 12. The bottom material is pumped by a transfer pump 13 into the finished product distillation column 14, which has 30 trays and a feed height of 25 trays to ensure the purity of the triethylsilane. The vapor phase is cooled by the finished product condenser 15 and collected in the finished product receiving tank 16.

[0052] The above description is only a preferred embodiment of the present utility model, but the protection scope of the present utility model is not limited thereto. Any equivalent substitutions or changes made by those skilled in the art within the technical scope disclosed in the present utility model, based on the technical solution and the inventive concept of the present utility model, should be included within the protection scope of the present utility model.

Claims

1. An apparatus for the synthesis of triethylsilane, characterized in that: include: Raw material storage components are used to store synthetic raw materials; A mixing device for mixing the raw materials output from the raw material storage component; A fixed-bed reactor (8) is filled with a catalyst. By providing the temperature required for the reaction, the mixed raw materials react on the surface of the catalyst under a certain pressure and a certain temperature to generate the desired substances. A foredistillation column (10) is used to separate unwanted components from the products generated by the fixed-bed reactor (8); The finished product distillation column (14) is used to purify the product output from the foredistillation column (10).

2. The apparatus for the synthesis of triethylsilane according to claim 1, characterized in that: The raw material storage assembly includes a silicon tetrahydrogen cylinder (1) and an ethylene cylinder (2). The output ends of the silicon tetrahydrogen cylinder (1) and the ethylene cylinder (2) are connected to the input end of the mixing device in sequence through a pressure reducer (3), a gas mass flow meter (4), and a one-way valve (5).

3. The apparatus for the synthesis of triethylsilane according to claim 2, characterized in that: The output of the mixing device enters the fixed bed reactor (8) sequentially through the column pressure gauge (7).

4. The apparatus for the synthesis of triethylsilane according to claim 3, characterized in that: The fixed-bed reactor (8) is provided with a jacket on the outside, and the temperature required for the reaction is provided by injecting a heat source into the jacket.

5. The apparatus for the synthesis of triethylsilane according to claim 4, characterized in that: The output end of the fixed bed reactor (8) is connected to the input end of the foredistillation column (10) through a back pressure valve (9), and the back pressure valve (9) maintains the reaction pressure inside the fixed bed reactor (8).

6. The apparatus for the synthesis of triethylsilane according to claim 5, characterized in that: The top of the pre-distillation column (10) is connected in sequence to the top condenser (11) and the pre-distillation receiving tank (12) via pipelines. When the material enters the pre-distillation column, the reaction mixture diethylsilane and triethylsilane are separated between the trays. The gaseous diethylsilane is cooled into liquid in the top condenser (11) and collected in the pre-distillation receiving tank (12), ensuring that the diethylsilane in the high-boiling-point components in the column is completely distilled off.

7. The apparatus for the synthesis of triethylsilane according to claim 6, characterized in that: The fore-distillation column (10) is connected to the finished product distillation column (14) via a transfer pump (13).

8. The apparatus for the synthesis of triethylsilane according to claim 7, characterized in that: The top of the product distillation column (14) is connected to the product condenser (15) and the product receiving tank (16) in sequence through pipelines. The high-boiling mixture containing diethylsilane enters the product distillation column (14) through the transfer pump (13). Triethylsilane and tetraethylsilane are separated on the tray. The boiling point of triethylsilane is lower than that of tetraethylsilane. The gaseous triethylsilane is condensed into liquid in the product condenser (15) and collected in the product receiving tank (16).

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