CN215250516U - Secondary hydrogenation device for byproducts in cyclohexylamine production process - Google Patents
Secondary hydrogenation device for byproducts in cyclohexylamine production process Download PDFInfo
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- CN215250516U CN215250516U CN202121202301.4U CN202121202301U CN215250516U CN 215250516 U CN215250516 U CN 215250516U CN 202121202301 U CN202121202301 U CN 202121202301U CN 215250516 U CN215250516 U CN 215250516U
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Abstract
The utility model discloses a by-product hydrogenation device once more in cyclohexylamine production process, the device is including crude jar, pre-heater, reactor, hydrogen circulation system, the hydrogen heater that connects gradually, and the hydrogen heater is connected with the reactor, the reactor receives the groove with the product and is connected, the reactor is connected with gas-water separator. The byproduct generated in the production process of the cyclohexylamine can be reduced into the dicyclohexylamine by the secondary hydrogenation device, so that the conversion rate of the aniline is improved.
Description
Technical Field
The utility model relates to a cyclohexylamine synthetic method technical field especially relates to a by-product hydrogenation device once more in cyclohexylamine production process.
Background
Cyclohexylamine is an important chemical raw material and a fine chemical intermediate, can be used as a raw material of a surfactant to produce alkyl benzene sulfonic acid cyclohexylamine, and is used for an emulsifier and a foaming agent; used for perfume raw materials to produce cyclohexyl allyl propionate; the method is used for dye raw materials to produce acid blue 62, disperse fluorescein H5GL, weak acid blue BRN, disperse blue 6 and dye auxiliary agents; used as raw material of food additive sweetener. The synthesis method of the medicine comprises the following steps: aniline is subjected to catalytic (nickel or cobalt) reduction at high temperature and high pressure to prepare a cyclohexylamine finished product; or prepared by taking cyclohexanol and cyclohexanone obtained by catalytic reduction of phenol as raw materials and performing amination on the cyclohexanol and cyclohexanone and ammonia. The aniline is catalyzed at high temperature and high pressure, so that the method has the advantages of simple process, easy operation, high safety, easily obtained raw materials, stable quality and the like, and is the most common cyclohexylamine synthesis method in China at present. However, in the production process, byproducts such as cyclohexylaniline and cyclohexene aniline are generated, and the utilization of the byproducts is only rarely reported at present.
SUMMERY OF THE UTILITY MODEL
In order to overcome the defects, the utility model aims to provide a hydrogenation technology and device once more for byproducts in the production process of cyclohexylamine, the byproducts can be reduced into the dicyclohexylamine through the hydrogenation technology once more, and the dicyclohexylamine is an important chemical raw material and a fine chemical intermediate and is mainly used in the fields of synthetic rubber accelerators, metal corrosion inhibitors, surfactants, oilfield chemicals, medicines, pesticides and the like. With the technological progress, new applications are continuously developed, and fine chemicals synthesized by the new applications are mostly new products with development prospects.
In order to achieve the above purpose, the utility model adopts the following technical scheme:
the utility model relates to a by-product hydrogenation technology once more in cyclohexylamine production process, its characterized in that: the method comprises the following steps:
s1, boosting the pressure of the fresh hydrogen and the recycle hydrogen to a set pressure through a hydrogen compressor and a recycle hydrogen compressor respectively; and pressurizing the system to keep the pressure at 0.5-0.8 MPa, preferably 0.5-0.65 MPa, stopping the hydrogen compressor when the system pressure reaches 0.65MPa, keeping the system pressure at 0.5-0.65 MPa and keeping the system pressure below 0.5MPa, and then starting the hydrogen compressor.
S2, heating the reactor (3) filled with the catalyst in advance; the catalyst is chemical catalyst nickel. The reactor is of a shell pass structure, is connected with the gas-water separator, and is heated by steam in the gas-water separator; the temperature of the reactor is controlled to be 170-190 ℃ in the reaction process, and because the reaction heat of the hydrogenation reaction is not enough to ensure the reaction temperature, 1.2Mpa steam is required to be introduced to maintain the temperature, and the steam pressure of the gas-water separator is used for adjusting and controlling.
S3, circulating the hydrogen in the reactor to stabilize the temperature of the inlet and outlet of the reactor (3) and the temperature of the inside of the pipe; the inlet temperature of the hydrogen compressor is controlled to be less than 50 ℃, and the outlet temperature is controlled to be less than 80 ℃.
S4, starting steam of the hydrogen heater (5) to heat the hydrogen; the temperature control range is 160-180 ℃, and preferably, the temperature is 165 ℃.
S5, pumping the crude dicyclic product in the crude product tank (1) to the reactor (3), controlling the temperature of the crude product in the feeding process to be 160-175 ℃, and controlling the feeding initial flow to be 0.5m3The feed temperature of the crude product is adjusted by adjusting the steam content of the preheater.
S6, sampling and analyzing the liquid in the lower part of the reactor (3), and discharging the liquid into the product receiving tank (12). When the reaction is normal and the product at the outlet of the reactor is qualified by detection, the reaction feeding amount is gradually increased to 1.0m3H, maximum feeding flow 2.5m3/h。
The utility model provides a pair of accessory substance hydrogenation technology and device once more in cyclohexylamine production process, including crude jar, pre-heater, reactor, hydrogen circulation system, the hydrogen heater that connects gradually, the hydrogen heater is connected with the reactor, the reactor receives the groove with the product and is connected, the product receives the groove and dicyclo storage tank is connected, the reactor is connected with deareator, deareator and soft water multistage pump are connected. The hydrogen circulating system comprises a hydrogen heat exchanger, a hydrogen cooler, a circulating hydrogen buffer tank, a circulating hydrogen compressor and a high-pressure hydrogen buffer which are sequentially connected, wherein the hydrogen heat exchanger is respectively connected with the reactor and the hydrogen heater. The high-pressure buffer is sequentially connected with the hydrogen compressor and the new hydrogen buffer tank. The lower cylinder of the reactor is provided with a liquid level warning lamp. When the red light is on, the liquid level is indicated to be ultrahigh, the discharge is increased in time, otherwise, the hydrogen flows to form a liquid seal, and the circulation is not smooth.
The beneficial effects of the utility model are that, the utility model aims to provide a by-product hydrogenation technology and device once more in the cyclohexylamine production process, the by-product can be reduced into dicyclohexylamine with the by-product that produces in the technology production process through hydrogenation technology and device once more, has improved the conversion of aniline, and this technology easy operation, equipment are few, efficient, the three wastes are few.
Drawings
FIG. 1 is a diagram of a secondary hydrogenation apparatus for byproducts produced in the production of cyclohexylamine according to a preferred embodiment of the present invention;
in the figure: 1. a crude product tank; 2. a preheater; 3. a reactor; 4. a hydrogen gas heat exchanger; 5. a hydrogen heater; 6. a fresh hydrogen buffer tank; 7. a hydrogen compressor; 8. a high pressure hydrogen buffer; 9. a recycle hydrogen compressor; 10. a recycle hydrogen buffer tank; 11. a hydrogen gas cooler; 12. the product is subjected to a groove; 13. a two-ring storage tank; 14. a gas-water separator; 15. soft water multistage pump.
Detailed Description
The following detailed description of the preferred embodiments of the present invention will be provided in conjunction with the accompanying drawings, so as to enable those skilled in the art to more easily understand the advantages and features of the present invention, and thereby define the scope of the invention more clearly and clearly.
Referring to the attached FIG. 1, the secondary hydrogenation process of the cyclohexylamine production process in this example is operated as follows:
1) and opening the new hydrogen buffer tank 6, setting the pressure to be 0.65MPa, starting automatic adjustment hydrogen supply to the high-pressure hydrogen buffer tank, setting the system pressure to be 0.65MPa, starting the hydrogen compressor 7 to pressurize the system, and stopping the hydrogen compressor 7 when the system pressure reaches 0.65 MPa. And keeping the system pressure within the range of 0.5-0.65 MPa and lower than 0.5MPa, and then starting the hydrogen compressor 7 to boost the pressure.
2) And opening a vent valve of the gas-water separator 14, starting the soft water multistage pump 15, feeding water into the gas-water separation tank, enabling the water to flow into the shell side of the reactor 3 from the gas-water separation tank, stopping feeding the water when the liquid level of the gas-water separator reaches 30%, and stopping the soft water multistage pump 15.
3) And opening a low-pressure steam valve of the gas-water separator 14 to heat the reactor 3, and closing an emptying valve when steam is emitted from an emptying port of the gas-water separator 14.
4. Starting a hydrogen cooler 11 to cool water, starting a circulating hydrogen compressor 9 to enable hydrogen to circulate in a hydrogen heat exchanger 4, the hydrogen cooler 11, a circulating hydrogen buffer tank 10, the circulating hydrogen compressor 9 and a high-pressure hydrogen buffer 8, simultaneously circulating the hydrogen among a reactor 3, a hydrogen heat exchanger and a hydrogen heater 5, circulating the hydrogen in the reactor 3 until the temperature of an inlet and an outlet of the reactor 3 and the temperature in a pipe are stable, controlling the inlet temperature of the hydrogen compressor 7 to be less than 50 ℃ and the outlet temperature to be less than 80 ℃; the inlet pressure is 0.3 MPa; the outlet pressure is less than 0.6 MPa.
5. Starting a hydrogen heater 5 for steam, heating the hydrogen inlet gas to 165 ℃, and controlling the temperature within the range of 160-180 ℃.
6. When the temperature of the bed layer of the reactor 3 rises to 165 ℃, starting the steam of the tube pass of the preheater 2, starting a raw material pump, pumping the crude bicyclic product in the crude product tank 1, and controlling the initial flow of the feeding material to be 0.5m3And about/h. Adjusting the steam quantity of the preheater 2, raising the feeding temperature to 165 ℃ and controlling the temperature within the range of 160-175 ℃.
7. Maintaining the circulation of hydrogen and the continuous feeding of raw materials, sampling and analyzing after liquid exists at the lower part of the reactor 3, and discharging the product into a product receiving tank 12 after the product sampling inspection is qualified. The qualified product standards include that the mass fraction of dicyclohexylamine is more than or equal to 99%, the mass fraction of cyclohexane is less than or equal to 0.1%, the mass fraction of cyclohexylamine is less than or equal to 0.1%, and the mass fraction of cyclohexanol is less than or equal to 0.1%. In this case, the reaction feed amount may be gradually increased to 1.0m3H, maximum feeding flow 2.5m3H is used as the reference value. The liquid level of the product receiving tank 12 is set to be 0.5-1.5 m, when the liquid level of the product receiving tank 12 exceeds 15m,
the product is automatically discharged to the hydrogenation bicyclic storage tank 13.
The utility model provides a pair of accessory substance hydrogenation technology and device once more in cyclohexylamine production process, including crude jar 1, pre-heater 2, reactor 3, hydrogen circulation system, hydrogen heater 5 that connect gradually, hydrogen heater is connected with reactor 3, reactor 3 receives groove 12 with the product to be connected, the product receives groove 12 and dicyclo storage tank 13 to be connected, reactor 3 is connected with deareator 14, deareator 14 and soft water multistage pump 15 are connected. The hydrogen circulation system comprises a hydrogen heat exchanger 4, a hydrogen cooler 11, a recycle hydrogen buffer tank 10, a recycle hydrogen compressor 9 and a high-pressure hydrogen buffer 8 which are connected in sequence, wherein the hydrogen heat exchanger 4 is respectively connected with the reactor 3 and the hydrogen heater 5. The high-pressure buffer is connected with a hydrogen compressor 7 and a new hydrogen buffer tank 6 in sequence. A liquid level warning lamp is arranged on the lower barrel of the reactor 3. When the red light is on, the liquid level is indicated to be ultrahigh, the discharge is increased in time, otherwise, the hydrogen flows to form a liquid seal, and the circulation is not smooth.
The above embodiments are only for illustrating the technical concept and features of the present invention, and the purpose thereof is to enable those skilled in the art to understand the contents of the present invention and implement the present invention, so as not to limit the protection scope of the present invention, and all equivalent changes or modifications made according to the spirit of the present invention should be covered in the protection scope of the present invention.
Claims (4)
1. The technical device for secondary hydrogenation of byproducts in the production process of cyclohexylamine is characterized by comprising a crude product tank (1), a preheater (2), a reactor (3), a hydrogen circulation system and a hydrogen heater (5) which are sequentially connected, wherein the hydrogen heater (5) is connected with the reactor (3).
2. The apparatus for re-hydrogenation of byproducts in the production process of cyclohexylamine according to claim 1, wherein the hydrogen circulation system comprises a hydrogen heat exchanger (4), a hydrogen cooler (11), a recycle hydrogen buffer tank (10), a recycle hydrogen compressor (9) and a high pressure hydrogen buffer (8) which are connected in sequence, wherein the hydrogen heat exchanger (4) is connected with the reactor (3) and the hydrogen heater (5) respectively.
3. The apparatus for re-hydrogenation of byproducts in the production process of cyclohexylamine according to claim 2, wherein the high pressure hydrogen buffer is connected with the hydrogen compressor (7) and the fresh hydrogen buffer tank (6) in sequence.
4. The apparatus for re-hydrogenation of byproducts produced in the production of cyclohexylamine according to claim 3, further comprising a product receiving tank (12) and a dicyclic storage tank (13), wherein said reactor (3) is connected to said product receiving tank (12), and said product receiving tank (12) is connected to said dicyclic storage tank (13); still include deareator (14) and soft water multistage pump (15), reactor (3) with deareator (14) are connected, deareator (14) with soft water multistage pump (15) are connected, reactor (3) lower part barrel is equipped with the liquid level warning light.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202121202301.4U CN215250516U (en) | 2021-05-31 | 2021-05-31 | Secondary hydrogenation device for byproducts in cyclohexylamine production process |
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| CN202121202301.4U CN215250516U (en) | 2021-05-31 | 2021-05-31 | Secondary hydrogenation device for byproducts in cyclohexylamine production process |
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| CN215250516U true CN215250516U (en) | 2021-12-21 |
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| CN202121202301.4U Active CN215250516U (en) | 2021-05-31 | 2021-05-31 | Secondary hydrogenation device for byproducts in cyclohexylamine production process |
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