Recovery apparatus and recovery method for amine-silane by-products

Abstract

The application provides a recovery device and recovery method of amine-based silane by-product. The recovery device comprises a liquid ammonia reactor, a flash tank and a filter. The liquid ammonia reactor has an inlet and an outlet, the inlet is connected with a liquid ammonia source and an amine-based hydrochloride source respectively, the liquid ammonia reactor is used for neutralization reaction of raw materials including liquid ammonia and amine-based hydrochloride to obtain a product system; the flash tank has an inlet, a flash ammonia gas outlet and a flash liquid outlet, the inlet is connected with the outlet of the liquid ammonia reactor, the flash tank is used for flash treatment of the product system to obtain flash ammonia gas and flash liquid; and the filter has an inlet and an outlet, the inlet is connected with the flash liquid outlet, the filter is used for solid-liquid separation of the flash liquid to obtain an ammonium chloride solid filter cake and an amine product. Compared with the prior art, the technical scheme of the application reduces environmental pollution from the source, simplifies the equipment, reduces the equipment investment and energy consumption, and is suitable for large-scale production.

Description

Technical Field

[0001] This invention relates to the field of aminosilane by-product recovery technology, and more specifically, to an apparatus and method for recovering aminosilane by-products. Background Technology

[0002] Aminosilane precursors are used in various deposition processes, primarily as novel precursors for the preparation of silicon oxide and silicon nitride using low-temperature atomic layer vapor deposition (ALD) technology. They are also used as novel materials for the preparation of silicon-based high-k thin films and for advanced integrated circuit manufacturing processes (28nm and below).

[0003] In recent years, with rapid economic development, the raw material and production costs of aminosilanes have been increasing, and environmental protection and energy consumption requirements have become increasingly stringent. The treatment of amino hydrochloride, a byproduct of aminosilane production, has become urgent. The recycling of amino hydrochloride not only recovers the raw materials needed for production, reducing production costs and energy consumption, but more importantly, it reduces environmental pollution, resulting in significant economic and environmental benefits.

[0004] In their research on the direct ammoniation of isobutylene to produce tert-butylamine, Yang Liping et al. mentioned that the post-treatment method for converting tert-butylamine to hydrochloride yielded a one-time yield of approximately 4%. 67 g (1.2 mol) of isobutylene and 45 g (2.65 mol) of ammonia were introduced into a high-pressure reactor containing a HY catalyst, and the reaction was carried out at 256 °C and 50 kg pressure for 8 h. The tert-butylamine product was absorbed with hydrochloric acid, the absorbent was concentrated, filtered, and the filtrate was adjusted to alkalinity with sodium hydroxide and extracted with dichloromethane. 1:1 hydrochloric acid was added to the extract to make it strongly acidic, and the mixture was separated. The aqueous phase was evaporated to obtain tert-butylamine hydrochloride (mp 278–280 °C, decomposes at 291 °C). The hydrochloride, 6g sodium hydroxide, and 1mol water were then mixed and fractionally distilled. The fraction collected at 40-50℃ yielded 3.5g tert-butylamine, with a yield of approximately 4% (first-time conversion). Gas chromatography analysis showed a content of 95%. The above process introduced an alkaline aqueous solution. If the water content is too high, the aminosilane product will hydrolyze, polymerize, and deteriorate, making it unusable as a raw material for production.

[0005] Hu Jianghua et al. disclosed a process for preparing diaminosilane and processing its byproducts in Chinese patent application CN 102898460 A. The process involves controlling a certain temperature and pressure to prepare diaminosilane, with ethylenediamine hydrochloride as the lower byproduct. Calcium oxide with an effective content of 99% is added to the lower ethylenediamine hydrochloride, and ethylenediamine is obtained by distillation under a vacuum of -0.08 MPa with stirring at 100 rpm. The ethylenediamine content after reaction recovery and salt recovery is above 98%, with a water content of approximately 0.002%. This process requires a solid-solid reaction, and a small amount of water is generated during the reaction. Subsequent vacuum purification is used to treat the diethylamine. The process involves multiple processing devices and a complex process route. Summary of the Invention

[0006] The main objective of this invention is to provide a device and method for recovering aminosilane byproducts, in order to solve the problems of complex equipment, complex process routes, and easy partial deterioration of products in the prior art for processing aminosilane byproducts.

[0007] To achieve the above objectives, according to one aspect of the present invention, an apparatus for recovering aminosilane byproducts is provided. The apparatus includes a liquid ammonia reactor, a flash tank, and a filter. The liquid ammonia reactor has an inlet and an outlet, the inlet of which is connected to a liquid ammonia source and an amino hydrochloride source, respectively. The liquid ammonia reactor is used to neutralize raw materials including liquid ammonia and amino hydrochloride to obtain a product system. The flash tank has an inlet, a flash ammonia gas outlet, and a flash liquid outlet, the inlet of which is connected to the outlet of the liquid ammonia reactor. The flash tank is used to flash-treat the product system to obtain flash ammonia gas and flash liquid. The filter has an inlet and an outlet, the inlet of which is connected to the flash liquid outlet. The filter is used to perform solid-liquid separation on the flash liquid to obtain ammonium chloride solid filter cake and amine products.

[0008] Furthermore, the aforementioned recovery device also includes a condenser having an inlet and an outlet, the inlet of which is connected to the flash ammonia outlet for condensing the flash ammonia.

[0009] Furthermore, the outlet of the aforementioned condenser is connected to the inlet of the liquid ammonia reactor.

[0010] In another typical embodiment of this application, a method for recovering aminosilane byproducts is provided. The recovery method includes step S1, neutralizing a raw material including liquid ammonia and amino hydrochloride to obtain a product system; step S2, flash evaporating the product system to obtain flash ammonia gas and flash liquid; and step S3, performing solid-liquid separation on the flash liquid to obtain ammonium chloride solid filter cake and amine product.

[0011] Furthermore, the above recovery method also includes step S4, which involves condensing the flash ammonia gas to obtain condensed flash ammonia gas; preferably, the condensed flash ammonia gas is returned to step S1; preferably, the condensation temperature is -60 to -30°C.

[0012] Furthermore, the above-mentioned recovery method also includes returning the amine product to step S1, preferably with a purity of 93-99%, more preferably 97-99%, and preferably the amine product is selected from any one or more of primary amines, secondary amines, and tertiary amines.

[0013] Further, in step S1 above, the molar ratio of liquid ammonia to amino hydrochloride is 1 to 35:1; preferably, the pressure of the neutralization reaction is 0.01 to 0.6 MPa, the temperature of the neutralization reaction is -60 to 10°C, and the time of the neutralization reaction is 1 to 3 hours; preferably, the amino hydrochloride is selected from any one or more of primary amine hydrochloride, secondary amine hydrochloride, and tertiary amine hydrochloride.

[0014] Furthermore, the liquid ammonia is added to the neutralization reaction system while stirring, preferably at a stirring speed of 5 to 300 r / min, and preferably at a temperature of -60 to -30°C.

[0015] In step S2 above, the pressure of the flash evaporation treatment is 10 kPa to 0.3 MPa, and the preferred temperature of the flash evaporation treatment is 25 to 28°C.

[0016] In step S3 above, solid-liquid separation is achieved through filtration.

[0017] By applying the technical solution of this application, the above-mentioned recovery device neutralizes the aminosilane byproduct aminohydrochloride with liquid ammonia to obtain a product system. This product system is then flash-evaporated in a flash tank to obtain flash ammonia gas and flash liquid. The flash liquid undergoes solid-liquid separation in a filter to obtain ammonium chloride solid filter cake and amine products, thereby reducing environmental pollution at the source. The ammonium chloride solid filter cake is discharged from the system and used in industrial batteries, electroplating, dyeing and textiles, casting, pharmaceuticals, and chemical intermediates. This recovery device can completely treat the aminosilane byproduct aminohydrochloride, and the recovered amine products can be reused as raw materials, improving raw material utilization and reducing environmental pollution. Compared with existing technologies, the technical solution of this application simplifies equipment, reduces equipment investment and energy consumption, and is suitable for large-scale production. Attached Figure Description

[0018] The accompanying drawings, which form part of this application, are used to provide a further understanding of the invention. The illustrative embodiments of the invention and their descriptions are used to explain the invention and do not constitute an undue limitation of the invention. In the drawings:

[0019] Figure 1 A schematic diagram of an apparatus for recovering aminosilane byproducts according to Embodiment 1 of the present invention is shown;

[0020] Figure 2 A schematic diagram of a recovery process for an aminosilane byproduct provided in Embodiment 1 of the present invention is shown.

[0021] The above figures include the following reference numerals:

[0022] 1. Liquid ammonia reactor; 2. Flash tank; 3. Filter; 4. Condenser. Detailed Implementation

[0023] It should be noted that, unless otherwise specified, the embodiments and features described in this application can be combined with each other. The present invention will now be described in detail with reference to the accompanying drawings and embodiments.

[0024] As analyzed in the background section of this application, the existing technology has problems such as complex equipment and process routes for processing aminosilane by-products, and the products are prone to partial deterioration. In order to solve this problem, this application provides an apparatus and method for recovering aminosilane by-products.

[0025] In a typical embodiment of this application, a device for recovering aminosilane byproducts is provided, such as... Figure 1 As shown, the recovery device includes a liquid ammonia reactor 1, a flash tank 2, and a filter 3. The liquid ammonia reactor 1 has an inlet and an outlet, with its inlet connected to a liquid ammonia source and an amino hydrochloride source, respectively. The liquid ammonia reactor 1 is used to neutralize the raw materials, including liquid ammonia and amino hydrochloride, to obtain a product system. The flash tank 2 has an inlet, a flash ammonia gas outlet, and a flash liquid outlet. Its inlet is connected to the outlet of the liquid ammonia reactor 1. The flash tank 2 is used to flash-treat the product system to obtain flash ammonia gas and flash liquid. The filter 3 has an inlet and an outlet, with its inlet connected to the flash liquid outlet. The filter 3 is used to perform solid-liquid separation on the flash liquid to obtain ammonium chloride solid filter cake and amine products.

[0026] This application utilizes the above-mentioned recovery device to neutralize the aminosilane byproduct aminohydrochloride with liquid ammonia to obtain a product system. This product system is then flash-evaporated in flash tank 2 to obtain flash ammonia gas and flash liquid. The flash liquid undergoes solid-liquid separation in filter 3 to obtain ammonium chloride solid filter cake and amine products, thereby reducing environmental pollution at the source. The ammonium chloride solid filter cake, after being discharged from the system, is used in industrial batteries, electroplating, dyeing and textiles, casting, pharmaceuticals, and chemical intermediates. This recovery device can completely treat the aminosilane byproduct aminohydrochloride, and the recovered amine products can be reused as raw materials, improving raw material utilization and reducing environmental pollution. Compared with existing technologies, the technical solution of this application simplifies equipment, reduces equipment investment and energy consumption, and is suitable for large-scale production.

[0027] In one embodiment of this application, the above-mentioned recovery device further includes a condenser 4, which has an inlet and an outlet, the inlet of which is connected to the flash ammonia outlet for condensing the flash ammonia.

[0028] Condenser 4 helps to regulate the temperature and pressure of flash ammonia gas, thereby condensing it into liquid ammonia.

[0029] In some embodiments of this application, the outlet of the condenser 4 is preferably connected to the inlet of the liquid ammonia reactor 1, thereby returning the condensed liquid ammonia to the liquid ammonia reactor 1, thus achieving the reuse of liquid ammonia and reducing raw material costs. Preferably, the components of the above-mentioned recovery device are made of 304 stainless steel or 316 stainless steel, which helps to improve the corrosion resistance of the recovery device to reagents such as liquid ammonia. Preferably, the above-mentioned recovery device is equipped with a stirrer and a jacketed or coiled heat exchanger.

[0030] In another typical embodiment of this application, a method for recovering aminosilane byproducts is provided, such as... Figure 2 As shown, the recovery method includes: step S1, neutralizing the raw materials including liquid ammonia and amino hydrochloride to obtain a product system; step S2, flash evaporating the product system to obtain flash ammonia gas and flash liquid; and step S3, performing solid-liquid separation on the flash liquid to obtain ammonium chloride solid filter cake and amine product.

[0031] The recovery method described in this application involves neutralizing the aminosilane byproduct aminohydrochloride with liquid ammonia to obtain a product system comprising an amine product and ammonium chloride, with the ammonium chloride dissolved in the liquid ammonia. The product system is then subjected to flash evaporation to obtain flash ammonia gas and flash liquid. The flash liquid undergoes solid-liquid separation to obtain an ammonium chloride solid filter cake and the amine product. The ammonium chloride solid filter cake is discharged from the system and supplied for use in industrial batteries, electroplating, dyeing and textiles, casting, pharmaceuticals, and chemical intermediates. This recovery method can completely treat the aminosilane byproduct aminohydrochloride, and the recovered amine product can be reused as a raw material. Compared with existing technologies, the technical solution of this application eliminates the alkaline water treatment process and avoids the introduction of water content, reducing environmental pollution at the source, improving raw material utilization, and reducing energy consumption and costs.

[0032] In one embodiment of this application, the above-mentioned recovery method further includes: step S4, condensing the flash ammonia gas to obtain condensed flash ammonia gas; preferably, returning the condensed flash ammonia gas to step S1; preferably, the condensation temperature is -60 to -30°C.

[0033] The condensation temperature (e.g., -60℃, -50℃, -40℃ or -30℃) facilitates the rapid condensation of flash ammonia. It is preferable to return the condensed flash ammonia to step S1, which is beneficial for the reuse of liquid ammonia and thus reduces raw material costs.

[0034] In one embodiment of this application, the above-mentioned recovery method further includes: returning the amine product to step S1, wherein the purity of the amine product is preferably 93-99%, more preferably 97-99%, and preferably the amine product is selected from any one or more of primary amines, secondary amines, and tertiary amines.

[0035] The separated amine product has high purity and can be directly returned to the raw material reaction tank as a production raw material to continue participating in the reaction, thereby reducing costs.

[0036] In one embodiment of this application, in step S1 above, the molar ratio of liquid ammonia to amino hydrochloride is 1 to 35:1; preferably, the pressure of the neutralization reaction is 0.01 to 0.6 MPa, preferably, the temperature of the neutralization reaction is -60 to 10°C, and preferably, the time of the neutralization reaction is 1 to 3 hours; preferably, the amino hydrochloride is selected from any one or more of primary amine hydrochloride, secondary amine hydrochloride, and tertiary amine hydrochloride.

[0037] Preferred molar ratios of liquid ammonia to amino hydrochloride (e.g., 1:1, 3:1, 5:1, 7:1, 10:1, 15:1, 20:1, 25:1, 30:1, or 35:1), neutralization reaction pressures (e.g., 0.01 MPa, 0.05 MPa, 0.1 MPa, 0.15 MPa, 0.2 MPa, 0.25 MPa, 0.3 MPa, 0.35 MPa, 0.4 MPa, 0.45 MPa, 0.5 MPa, 0.55 MPa, or 0.6 MPa), temperatures (e.g., -60°C, -50°C, -40°C, -30°C, -20°C, -10°C, 0°C, or 10°C), and time contribute to improving the efficiency and effectiveness of the neutralization reaction. The type of amino hydrochloride corresponds to the type of amine product generated in the neutralization reaction.

[0038] In one embodiment of this application, liquid ammonia is added to the neutralization reaction system while it is being stirred. Preferably, the stirring speed is 5 to 300 r / min (e.g., 5 r / min, 20 r / min, 50 r / min, 100 r / min, 150 r / min, 200 r / min, 250 r / min or 300 r / min), and preferably, the liquid ammonia is added to the neutralization reaction system at a temperature of -60 to -30°C (e.g., -60°C, -50°C, -40°C or -30°C).

[0039] Controlling the above conditions helps to improve the control of the exothermic reaction, thereby maintaining the reaction system in a relatively stable state and improving the safety of the entire reaction system.

[0040] Preferably, in step S2 above, the pressure of the flash evaporation treatment is 10 kPa to 0.3 MPa (e.g., 80 kPa, 100 kPa, 150 kPa, 200 kPa, 250 kPa or 300 kPa), and the temperature of the flash evaporation treatment is preferably 25 to 28°C (e.g., 27 to 28°C, 26 to 27°C or 20 to 22°C), which helps to improve the efficiency and effect of flash evaporation.

[0041] In one embodiment of this application, in step S3 above, solid-liquid separation is filtration.

[0042] To improve the ease of solid-liquid separation, filtration is preferred as the solid-liquid separation method. The ammonium chloride solid filter cake obtained after filtration is used in industrial batteries, electroplating, dyeing and weaving, casting, pharmaceuticals, chemical intermediates, and other fields.

[0043] The beneficial effects of this application will be further illustrated below with reference to embodiments and comparative examples.

[0044] Example 1

[0045] according to Figure 1 The apparatus shown is for the recovery of aminosilane byproducts. Figure 2 The schematic diagram shown illustrates the recovery process of aminosilane byproducts, specifically the recovery of tert-butylamine hydrochloride.

[0046] 5 L of liquid ammonia (stirring speed 300 r / min, -60℃) was added to liquid ammonia reactor 1. 3 kg of tert-butylamine hydrochloride was weighed and added to the reactor (molar ratio of liquid ammonia to tert-butylamine hydrochloride was 7:1). Stirring was started at 15–30 r / min to allow the tert-butylamine hydrochloride to neutralize with the liquid ammonia. The neutralization reaction pressure was 0.1 MPa, and the temperature was -30℃. After 3 hours of reaction, a product system containing tert-butylamine and ammonium chloride was generated, in which the ammonium chloride dissolved in the liquid ammonia. The reactor discharge valve was opened, and the product system entered flash tank 2 for flash evaporation. The flash tank pressure was controlled at 80 kPa, and the temperature at 25–28℃, yielding flash ammonia gas and flash liquid. The flash ammonia gas was condensed in cooler 4 (-60℃), and the resulting liquid ammonia was returned to liquid ammonia reactor 1 for reuse. After being filtered through filter 3, the flash liquid yielded approximately 1.30 kg of ammonium chloride solid filter cake and approximately 1.30 kg of tert-butylamine. GC testing showed that the purity of the tert-butylamine product was 98.3%, and it could be directly returned to the raw material tank for reuse as a production raw material.

[0047] Example 2

[0048] Add 5L of liquid ammonia (stirring speed 300r / min, -50℃) to liquid ammonia reactor 1. Weigh 3kg of tert-butylamine hydrochloride and add it to the reactor (molar ratio of liquid ammonia to tert-butylamine hydrochloride is 7:1). Start stirring at 15-30r / min to allow the tert-butylamine hydrochloride to neutralize with the liquid ammonia. The neutralization reaction pressure is 0.2MPa, and the neutralization reaction temperature is -40℃. After 1 hour of reaction, a product system containing tert-butylamine and ammonium chloride is generated, in which ammonium chloride is dissolved in liquid ammonia. Open the reactor outlet valve, and the product system enters flash tank 2 for flash evaporation. Control the flash tank pressure at 80KPa and the temperature at 25-28℃ to obtain flash ammonia gas and flash liquid. After the flash ammonia gas is condensed in cooler 4 (-40℃), the resulting liquid ammonia is returned to liquid ammonia reactor 1 for reuse. After being filtered through filter 3, the flash liquid yielded approximately 0.90 kg of ammonium chloride solid filter cake and approximately 1.10 kg of tert-butylamine. GC testing showed that the purity of the tert-butylamine product was 97.5%, and it could be directly returned to the raw material tank for reuse as a production raw material.

[0049] Example 3

[0050] The difference from Example 1 is that,

[0051] 5 L of liquid ammonia (stirring speed 300 r / min, -60℃) was added to liquid ammonia reactor 1. 3 kg of diethylamine hydrochloride was weighed and added to the reactor (molar ratio of liquid ammonia to tert-butylamine hydrochloride was 7:1). Stirring was started at 15–30 r / min to allow the diethylamine hydrochloride to neutralize with the liquid ammonia. The neutralization reaction pressure was 0.1 MPa, and the temperature was -30℃. After 3 hours of reaction, a product system containing diethylamine and ammonium chloride was generated, in which the ammonium chloride dissolved in the liquid ammonia. The reactor outlet valve was opened, and the product system entered flash tank 2 for flash evaporation. The flash tank pressure was controlled at 80 kPa, and the temperature at 25–28℃, yielding flash ammonia gas and flash liquid. The flash ammonia gas was condensed in cooler 4 (-30℃), and the resulting liquid ammonia was returned to liquid ammonia reactor 1 for reuse. After being filtered through filter 3, the flash liquid yielded approximately 1.30 kg of ammonium chloride solid filter cake and approximately 1.25 kg of diethylamine. GC testing showed that the purity of the diethylamine product was 98.9%, and it could be directly returned to the raw material tank for reuse as a production raw material.

[0052] Example 4

[0053] The difference from Example 1 is that the pressure of the flash tank is controlled at 300 kPa and the temperature is 27-28°C to obtain flash ammonia and flash liquid, and finally ammonium chloride solid filter cake and tert-butylamine.

[0054] Example 5

[0055] The difference from Example 1 is that the pressure of the flash tank is controlled at 150 kPa and the temperature is 26-27°C to obtain flash ammonia and flash liquid, and finally ammonium chloride solid filter cake and tert-butylamine.

[0056] Example 6

[0057] The difference from Example 1 is that the pressure of the flash tank is controlled at 8 kPa and the temperature at 20-22°C to obtain flash ammonia and flash liquid, and finally ammonium chloride solid filter cake and tert-butylamine.

[0058] Example 7

[0059] The difference from Example 1 is that the molar ratio of liquid ammonia to tert-butylamine hydrochloride is 15:1, and the final product is ammonium chloride solid filter cake and tert-butylamine.

[0060] Example 8

[0061] The difference from Example 1 is that the molar ratio of liquid ammonia to tert-butylamine hydrochloride is 45:1, and the final product is ammonium chloride solid filter cake and tert-butylamine.

[0062] Example 9

[0063] The difference from Example 1 is that the neutralization reaction pressure was 0.01 MPa, the neutralization reaction temperature was -60°C, and the neutralization reaction time was 6 hours, ultimately yielding ammonium chloride solid filter cake and tert-butylamine.

[0064] Example 10

[0065] The difference from Example 1 is that the neutralization reaction pressure was 0.6 MPa, the neutralization reaction temperature was 10°C, and the neutralization reaction time was 2 h, ultimately yielding ammonium chloride solid filter cake and tert-butylamine.

[0066] Example 11

[0067] The difference from Example 1 is that the neutralization reaction pressure was 0.7 MPa, the neutralization reaction temperature was 20°C, and the neutralization reaction time was 2 hours, ultimately yielding ammonium chloride solid filter cake and tert-butylamine.

[0068] Example 12

[0069] The difference from Example 1 is that the stirring speed was 20 r / min, liquid ammonia was added at -30°C, and ammonium chloride solid filter cake and tert-butylamine were finally obtained.

[0070] The mass of the ammonium chloride solid filter cake and amine product obtained in Examples 1 to 12 above were measured respectively. The purity of the amine product was detected by GC. The results are shown in Table 1 below.

[0071] Table 1

[0072]

[0073] In Example 8, the excessively high molar ratio of liquid ammonia to tert-butylamino hydrochloride leads to an excessive amount of liquid ammonia. Consequently, during the flash evaporation process of the product system, some ammonium chloride and amine products enter the flash ammonia gas and flash liquid along with the ammonia gas, resulting in a smaller amount of ammonium chloride solid filter cake and amine products collected in the end.

[0074] As can be seen from the above description, the embodiments of the present invention achieve the following technical effects:

[0075] This application utilizes the aforementioned recovery device to neutralize the aminosilane byproduct aminohydrochloride with liquid ammonia, yielding a product system. This product system is then flash-evaporated in a flash tank to obtain flash ammonia gas and flash liquid. The flash liquid undergoes solid-liquid separation in a filter to obtain ammonium chloride solid filter cake and amine products, thereby reducing environmental pollution at its source. The ammonium chloride solid filter cake, after being discharged from the system, is supplied to industrial batteries, electroplating, dyeing and textiles, casting, pharmaceuticals, and chemical intermediates. This recovery device can completely treat the aminosilane byproduct aminohydrochloride, and the recovered amine products can be reused as raw materials, improving raw material utilization and reducing environmental pollution. Compared with existing technologies, the technical solution of this application simplifies equipment, reduces equipment investment and energy consumption, and is suitable for large-scale production.

[0076] The above description is merely a preferred embodiment of the present invention and is not intended to limit the invention. Various modifications and variations can be made to the present invention by those skilled in the art. Any modifications, equivalent substitutions, improvements, etc., made within the spirit and principles of the present invention should be included within the scope of protection of the present invention.

Claims

1. A device for recovering aminosilane byproducts, characterized in that, The recycling device includes: The liquid ammonia reactor (1) has an inlet and an outlet. Its inlet is connected to a liquid ammonia source and an amino hydrochloride source, respectively. The liquid ammonia reactor (1) is used to neutralize raw materials including liquid ammonia and amino hydrochloride to obtain a product system. A flash tank (2) has an inlet, a flash ammonia gas outlet, and a flash liquid outlet. Its inlet is connected to the outlet of the liquid ammonia reactor (1). The flash tank (2) is used to flash-treat the product system to obtain flash ammonia gas and flash liquid. The filter (3) has an inlet and an outlet, the inlet of which is connected to the outlet of the flash liquid. The filter (3) is used to perform solid-liquid separation on the flash liquid to obtain ammonium chloride solid filter cake and amine product.

2. The recycling device according to claim 1, characterized in that, The recycling device also includes: The condenser (4) has an inlet and an outlet, the inlet of which is connected to the flash ammonia outlet for condensing the flash ammonia.

3. The recycling device according to claim 2, characterized in that, The outlet of the condenser (4) is connected to the inlet of the liquid ammonia reactor (1).

4. A method for recovering aminosilane byproducts, characterized in that, The recycling method includes: Step S1 involves neutralizing the raw materials, including liquid ammonia and amino hydrochloride, to obtain the product system. Step S2 involves flash evaporation of the product system to obtain flash ammonia gas and flash liquid; and Step S3: Perform solid-liquid separation on the flash liquid to obtain ammonium chloride solid filter cake and amine product.

5. The recycling method according to claim 4, characterized in that, The recycling method further includes: Step S4: The flash ammonia gas is condensed to obtain condensed flash ammonia gas.

6. The recycling method according to claim 5, characterized in that, The condensed flash-evaporated ammonia gas is returned to step S1.

7. The recycling method according to claim 5, characterized in that, The condensation treatment temperature is -60~-30℃.

8. The recycling method according to any one of claims 4 to 7, characterized in that, The recycling method further includes: The amine product is returned to step S1.

9. The recycling method according to any one of claims 4 to 7, characterized in that, The purity of the amine product is 93-99%.

10. The recycling method according to claim 9, characterized in that, The purity of the amine product is 97-99%.

11. The recycling method according to any one of claims 4 to 7, characterized in that, The amine product is selected from any one or more of primary amines, secondary amines, and tertiary amines.

12. The recycling method according to any one of claims 4 to 7, characterized in that, In step S1, the molar ratio of liquid ammonia to amino hydrochloride is 1~35:

1.

13. The recycling method according to any one of claims 4 to 7, characterized in that, The pressure of the neutralization reaction is 0.01~0.6 MPa.

14. The recycling method according to any one of claims 4 to 7, characterized in that, The neutralization reaction occurs at a temperature of -60 to 10°C.

15. The recycling method according to any one of claims 4 to 7, characterized in that, The neutralization reaction takes 1 to 3 hours.

16. The recycling method according to any one of claims 4 to 7, characterized in that, The amino hydrochloride is selected from any one or more of primary amine hydrochloride, secondary amine hydrochloride, and tertiary amine hydrochloride.

17. The recycling method according to any one of claims 4 to 7, characterized in that, The liquid ammonia is added to the neutralization reaction system while being stirred.

18. The recycling method according to any one of claims 17, characterized in that, The stirring speed is 5~300 r / min.

19. The recycling method according to claim 17, characterized in that, The liquid ammonia is added to the neutralization reaction system at a temperature of -60 to -30°C.

20. The recycling method according to any one of claims 4 to 7, characterized in that, In step S2, the pressure of the flash evaporation treatment is 10 kPa to 0.3 MPa.

21. The recycling method according to any one of claims 4 to 7, characterized in that, In step S2, the temperature of the flash evaporation treatment is 25~28℃.

22. The recycling method according to any one of claims 4 to 7, characterized in that, In step S3, the solid-liquid separation is filtration.

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