CN212222836U - Low-cost high-efficient industrialization diamine apparatus for producing - Google Patents
Low-cost high-efficient industrialization diamine apparatus for producing Download PDFInfo
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- CN212222836U CN212222836U CN202020807147.2U CN202020807147U CN212222836U CN 212222836 U CN212222836 U CN 212222836U CN 202020807147 U CN202020807147 U CN 202020807147U CN 212222836 U CN212222836 U CN 212222836U
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/584—Recycling of catalysts
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Abstract
The utility model belongs to the technical field of the diamine production, concretely relates to low-cost high-efficient industrialization diamine apparatus for producing, including high-pressure batch autoclave, be equipped with ammonia entry and dog-house on the high-pressure batch autoclave, the high-pressure batch autoclave discharge gate is connected with the washing cauldron, washing cauldron upper portion is equipped with the ammonia export, and the ammonia export is connected with ammonia recovery unit, and the washing cauldron bottom is connected with catalyst recovery unit, and the washing cauldron discharge gate is connected with hydrogenation cauldron A, hydrogenation cauldron B and rectifying column in proper order, and hydrogenation cauldron A and hydrogenation cauldron B series connection are equipped with microwave device in the hydrogenation cauldron B. The utility model discloses washing kettle adopts the hot water washing process to replace the distillation of dinitrile, simultaneously through hydrogenation cauldron A and hydrogenation cauldron B series connection, obtains the diamine product with thick dinitrile through the preparation of two-stage hydrogenation, and the hydrogenation process divides the two-stage to carry out can realize the process continuity, can reduce the energy consumption of this process, improves hydrogenation efficiency, further improves the dinitrile conversion rate, is convenient for carry out kiloton level scale production.
Description
Technical Field
The utility model belongs to the technical field of the diamine production, concretely relates to high-efficient industrialization diamine apparatus for producing of low-cost.
Background
1, 10-decamethylenediamine (decamethylenediamine), 1, 12-dodecanediamine, 1, 13-tridecanediamine and 1, 14-tetradecanediamine are important raw materials for the synthesis of polyamides and copolyamides. The synthesis and development of decamethylenediamine, dodecanediamine, tridecanediamine and tetradecanediamine are from the production needs of nylon 1010, 1212, 1313 and 1414 resins, and the nylon 1010, 1212, 1313 and 1414 resins can be widely used in the industries of garment materials, surfactants, various chemical resins and the like, so that the diamine is used as a fine chemical intermediate with wide application and is increased rapidly in the garment hot melt adhesive industry.
However, the problems of high production cost, low product yield and the like generally exist in the production of diamine at present, and the industrial scale production is not facilitated.
SUMMERY OF THE UTILITY MODEL
The to-be-solved technical problem of the utility model is: the method overcomes the defects of the prior art, provides a low-cost high-efficiency industrialized diamine production device, has scientific and reasonable process device, good quality of the prepared diamine product and high yield, and is convenient for kiloton-grade large-scale production.
The utility model discloses an adopt following technical scheme to realize:
the low-cost high-efficient industrialization diamine apparatus for producing, including high-pressure batch autoclave, high-pressure batch autoclave on be equipped with ammonia inlet and dog-house, the high-pressure batch autoclave discharge gate is connected with the washing cauldron, washing cauldron upper portion is equipped with the ammonia export, and the ammonia export is connected with ammonia recovery unit, and the washing cauldron bottom is connected with catalyst recovery unit, and the washing cauldron discharge gate is connected with hydrogenation cauldron A, hydrogenation cauldron B in proper order, hydrogenation cauldron A and hydrogenation cauldron B series connection, be equipped with the microwave device in the hydrogenation cauldron B, hydrogenation cauldron B discharge gate is connected with vapour and liquid separator through hydrogenation condenser, vapour and liquid separator liquid phase outlet is connected with the rectifying column.
The high-pressure batch autoclave in be equipped with the agitator, the agitator (mixing) shaft on from last to installing dispersion impeller and anchor frame formula stirring rake down in proper order.
The washing kettle is provided with a hot water inlet. The catalyst was recovered by washing with hot water.
The ammonia recovery device is connected with the ammonia inlet, and can recycle the recovered ammonia.
The hydrogenation kettle A is provided with a nickel catalyst inlet.
And a nickel-palladium-rhodium composite catalyst inlet is arranged on the hydrogenation kettle B.
The hydrogen inlet on the hydrogenation kettle A and the hydrogen inlet on the hydrogenation kettle B are both connected with a hydrogen pipeline, and the gas-liquid separator gas-phase outlet is connected with the hydrogen pipeline to recycle the hydrogen.
And a condenser is arranged at the top of the rectifying tower.
The working principle and the process are as follows:
adding aliphatic dibasic acid, ammonia water and a solid strong acid type resin catalyst into a high-pressure reaction kettle from a feeding port, introducing ammonia gas from an ammonia gas inlet, starting a stirrer to react, keeping the pressure at 0.5-3.0MPa, keeping the temperature at 100-130 ℃, keeping the temperature for 5-8 hours, and keeping the temperature at 230-280 ℃ for 2-4 hours to obtain crude binary nitrile; transferring the obtained crude binary nitrile into a washing kettle, adding hot water into a hot water inlet of the washing kettle, washing and recovering a catalyst by using hot water, controlling the temperature of the hot water to be 40-95 ℃, then deaminating and dehydrating under the vacuum degree of 20-40mmHg, recovering ammonia from an ammonia outlet to an ammonia recovery device for recycling, transferring the washed and recovered catalyst to a catalyst recovery device, then transferring the deaminated and dehydrated binary nitrile into a hydrogenation kettle A, adding a nickel catalyst and a cocatalyst into the hydrogenation kettle A from a nickel catalyst inlet, introducing hydrogen into the hydrogenation kettle A at 1.5-2.0MPa and 50-70 ℃, performing hydrogenation reaction for 60-90min, transferring a reaction liquid phase into a hydrogenation kettle B, performing secondary hydrogenation reaction, adding a nickel-palladium-rhodium composite catalyst into a nickel-palladium-rhodium composite catalyst inlet of the hydrogenation kettle B, introducing hydrogen into the hydrogenation kettle B at 4.0-6.0MPa and 100 ℃ for hydrogenation reaction at 120 ℃, when hydrogenation operation is carried out in the hydrogenation kettle B, according to the hydrogenation condition, intermittently starting a microwave device for microwave irradiation with the irradiation power of 50-200W, the irradiation time of 1-10min and the irradiation times of 1-5; after the hydrogenation reaction is finished, separating out the catalyst, condensing the reaction liquid through a hydrogenation condenser, then feeding the reaction liquid into a gas-liquid separator to separate hydrogen, feeding the liquid phase into a rectifying tower to carry out reduced pressure distillation, wherein the tower top temperature is 170-200 ℃ and the vacuum degree is 10-40mmHg, and condensing through the condenser to obtain a diamine product.
Compared with the prior art, the beneficial effects of the utility model are as follows:
1. the utility model discloses washing kettle adopts the hot water washing process to replace the distillation of dinitrile, can reduce the energy consumption of this process, can improve the dinitrile yield simultaneously.
2. The utility model discloses a hydrogenation cauldron A and hydrogenation cauldron B series connection obtain the diamine product with thick dinitrile through the preparation of two-stage hydrogenation, and the hydrogenation process divides the two-stage to carry out and can realize the process continuity, improves hydrogenation efficiency, improves the dinitrile conversion rate.
3. The utility model has the advantages of being scientific and reasonable, with low costs, production efficiency is high, and the diamine product of preparation simultaneously, the yield is high, of high quality, is convenient for carry out kiloton level scale production.
Drawings
Fig. 1 is a schematic structural view of the present invention;
in the figure: 1. a high-pressure reaction kettle; 2. a stirrer; 3. anchor frame type stirring paddle; 4. a dispersion tray; 5. an ammonia gas inlet; 6. a feeding port; 7. washing the kettle; 8. a hot water inlet; 9. an ammonia gas outlet; 10. an ammonia gas recovery device; 11. a catalyst recovery unit; 12. a hydrogenation kettle A; 13. a nickel catalyst inlet; 14. a hydrogen gas line; 15. a hydrogenation kettle B; 16. a microwave device; 17. a nickel-palladium-rhodium composite catalyst inlet; 18. a hydrogenation condenser; 19. a gas-liquid separator; 20. a rectifying tower; 21. a condenser.
Detailed Description
The present invention will be further described with reference to the accompanying drawings.
As shown in fig. 1, the low-cost high-efficiency industrialized diamine production device comprises a high-pressure reaction kettle 1, wherein an ammonia inlet 5 and a feed inlet 6 are arranged on the high-pressure reaction kettle 1, a discharge port of the high-pressure reaction kettle 1 is connected with a washing kettle 7, an ammonia outlet 9 is arranged on the upper part of the washing kettle 7, the ammonia outlet 9 is connected with an ammonia recovery device 10, a discharge port of the washing kettle 7 is sequentially connected with a hydrogenation kettle a 12 and a hydrogenation kettle B15, the hydrogenation kettle a 12 is connected with a hydrogenation kettle B15 in series, a microwave device 16 is arranged in the hydrogenation kettle B15, a discharge port of the hydrogenation kettle B15 is connected with a gas-liquid separator 19 through a hydrogenation condenser 18, and a liquid phase outlet of the gas-liquid separator 19 is connected with a.
High-pressure batch autoclave 1 in be equipped with agitator 2, agitator 2 (mixing) shaft on from last to installing dispersion impeller 4 and anchor frame formula stirring rake 3 down in proper order.
The washing kettle 7 is provided with a hot water inlet 8.
The ammonia gas recovery device 10 is connected with the ammonia gas inlet 5.
The hydrogenation kettle A12 is provided with a nickel catalyst inlet 13.
The hydrogenation kettle B15 is provided with a nickel-palladium-rhodium composite catalyst inlet 17.
The hydrogen inlet on the hydrogenation kettle A12 and the hydrogen inlet on the hydrogenation kettle B15 are both connected with a hydrogen pipeline 14, and the gas-phase outlet of the gas-liquid separator 19 is connected with the hydrogen pipeline 14.
The top of the rectifying tower 20 is provided with a condenser 21.
When the reactor works, adding aliphatic dibasic acid, ammonia water and a solid strong acid type resin catalyst into a high-pressure reaction kettle 1 from a feeding port 6, introducing ammonia gas from an ammonia gas inlet 5, starting a stirrer 2 to react, keeping the pressure at 2.0MPa, keeping the temperature at 120 ℃, keeping the temperature for 6 hours, heating to 230 ℃, keeping the temperature for 4 hours, and obtaining crude binary nitrile; transferring the obtained crude binary nitrile into a washing kettle 7, adding hot water into the washing kettle 7 from a hot water inlet 8, washing and recovering a catalyst by using hot water, carrying out deamination and dehydration at the temperature of 60 ℃, then carrying out ammonia recovery and recycling at the vacuum degree of 30mmHg from an ammonia outlet 9 to an ammonia recovery device 10, conveying the washed and recovered catalyst to a catalyst recovery device 11, then transferring the deaminated and dehydrated binary nitrile into a hydrogenation kettle A12, adding a nickel catalyst and a cocatalyst into a hydrogenation kettle A12 from a nickel catalyst inlet 13, introducing hydrogen at 1.5MPa and 60 ℃ for hydrogenation reaction, transferring a reaction liquid phase into a hydrogenation kettle B15 after reacting for 90min, carrying out secondary hydrogenation reaction, adding a nickel-palladium-rhodium composite catalyst into a nickel-palladium-rhodium composite catalyst inlet 17 of a hydrogenation kettle B15, introducing hydrogen, carrying out hydrogenation reaction at 5.0MPa and 120 ℃, and carrying out hydrogenation operation in a hydrogenation kettle B15, according to the hydrogenation condition, intermittently starting a microwave device 16 for microwave irradiation with the irradiation power of 200W, the irradiation time of 3min and the irradiation times of 3 times; after the hydrogenation reaction is finished, the catalyst is separated, the reaction liquid is condensed by a hydrogenation condenser 18 and then enters a gas-liquid separator 19 to separate hydrogen, the liquid phase is fed into a rectifying tower 18 to be subjected to reduced pressure distillation, the temperature at the top of the tower is 190 ℃, the vacuum degree is 30mmHg, and the diamine product is obtained after the condensation by the condenser 19.
Of course, the above description is only a preferred embodiment of the present invention, and should not be taken as limiting the scope of the embodiments of the present invention. The present invention is not limited to the above examples, and the technical field of the present invention is equivalent to the changes and improvements made in the actual range of the present invention, which should be attributed to the patent coverage of the present invention.
Claims (8)
1. The utility model provides a low-cost high-efficient industrialization diamine apparatus for producing, includes high-pressure batch autoclave (1), its characterized in that: high-pressure batch autoclave (1) on be equipped with ammonia entry (5) and dog-house (6), high-pressure batch autoclave (1) discharge gate is connected with washing cauldron (7), washing cauldron (7) upper portion is equipped with ammonia outlet (9), and ammonia outlet (9) are connected with ammonia recovery unit (10), and washing cauldron (7) bottom is connected with catalyst recovery unit (11), and washing cauldron (7) discharge gate is connected with hydrogenation cauldron A (12), hydrogenation cauldron B (15) in proper order, hydrogenation cauldron A (12) and hydrogenation cauldron B (15) series connection, be equipped with microwave device (16) in hydrogenation cauldron B (15), hydrogenation cauldron B (15) discharge gate is connected with vapour and liquid separator (19) through hydrogenation condenser (18), vapour and liquid separator (19) liquid phase export is connected with rectifying column (20).
2. The low-cost high-efficiency industrialized diamine production device according to claim 1, which is characterized in that: high-pressure batch autoclave (1) in be equipped with agitator (2), agitator (2) the (mixing) shaft on from last to installing dispersion impeller (4) and anchor frame formula stirring rake (3) down in proper order.
3. The low-cost high-efficiency industrialized diamine production device according to claim 1, which is characterized in that: the washing kettle (7) is provided with a hot water inlet (8).
4. The low-cost high-efficiency industrialized diamine production device according to claim 1, which is characterized in that: the ammonia gas recovery device (10) is connected with the ammonia gas inlet (5).
5. The low-cost high-efficiency industrialized diamine production device according to claim 1, which is characterized in that: the hydrogenation kettle A (12) is provided with a nickel catalyst inlet (13).
6. The low-cost high-efficiency industrialized diamine production device according to claim 1, which is characterized in that: and a nickel-palladium-rhodium composite catalyst inlet (17) is formed in the hydrogenation kettle B (15).
7. The low-cost high-efficiency industrialized diamine production device according to claim 1, which is characterized in that: the hydrogen inlet on the hydrogenation kettle A (12) and the hydrogen inlet on the hydrogenation kettle B (15) are both connected with a hydrogen pipeline (14), and the gas-phase outlet of the gas-liquid separator (19) is connected with the hydrogen pipeline (14).
8. The low-cost high-efficiency industrialized diamine production device according to claim 1, which is characterized in that: and a condenser (21) is arranged at the top of the rectifying tower (20).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202020807147.2U CN212222836U (en) | 2020-05-14 | 2020-05-14 | Low-cost high-efficient industrialization diamine apparatus for producing |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202020807147.2U CN212222836U (en) | 2020-05-14 | 2020-05-14 | Low-cost high-efficient industrialization diamine apparatus for producing |
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| CN212222836U true CN212222836U (en) | 2020-12-25 |
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| CN202020807147.2U Active CN212222836U (en) | 2020-05-14 | 2020-05-14 | Low-cost high-efficient industrialization diamine apparatus for producing |
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