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Method for producing tert-butylamine based on coupling reaction-separation

A technology of tert-butylamine and reaction, applied in the production field of organic compound tert-butylamine, can solve the problems of incapability of large-scale adoption, potential safety hazard and high reaction pressure, and achieve the effects of easy control of reaction conditions, convenient operation and good product yield

Inactive Publication Date: 2009-08-05
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0016] Among the seven methods for synthesizing TBA, from the perspective of atom economy, the element utilization rate of method (6) reaches 100%, but this method has high reaction pressure (up to 300 atmospheres), large equipment investment, and potential safety hazards. defects, so it has not been adopted on a large scale so far

Method used

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  • Method for producing tert-butylamine based on coupling reaction-separation
  • Method for producing tert-butylamine based on coupling reaction-separation
  • Method for producing tert-butylamine based on coupling reaction-separation

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] Embodiment 1, figure 1 A circulating pressurized reaction-rectification coupling device is given, including a raw material tank 1, a feed pump 2, a condenser 6, a reactive distillation column 7, a reboiler 9, and the like.

[0036] The raw material tank 1 communicates with the inlet of the collecting pipe 13 through the feed pipe 10, and the feed pipe 10 is provided with a stop valve 20, a feed pump 2 and a stop valve 21 in sequence according to the flow direction of the feed liquid; the purge gas pipe 11 It communicates with the inlet of the collecting pipe 13 , and a cut-off valve 22 is provided on the purge gas pipe 11 .

[0037] The reactive distillation tower 7 is a packed tower, the middle part of which is loaded with a loaded catalyst, and a material inlet is arranged in the middle part of the reactive distillation tower 7, and the material inlet is connected with the outlet of the collecting pipe 13. A preheater 3 is provided on the collecting pipe 13 . The ou...

Embodiment 2

[0041] Embodiment 2, the preparation of supported catalyst:

[0042] 1), the preparation of Co / HZSM5:

[0043] 50mL NH 4 ZSM5 was calcined in a muffle furnace at 200°C for 1h, heated to 350°C for 1h, and then heated to 540°C for 10h to obtain HZSM5; 20g Co(NO 3 ) 2 Prepare 60 mL of deionized aqueous solution, immerse the above-mentioned roasted HZSM5 in it for ion exchange, and immerse for 20 hours; roast the ion-exchanged HZSM5 at 550°C for 6 hours to obtain the finished supported catalyst.

[0044] In this supported catalyst (Co / HZSM5), Co accounts for 15% of the total weight of the supported catalyst.

[0045] 2), activation catalyst:

[0046] Put the above-mentioned 300ml Co / HZSM5 into the packing layer in the middle section of the reactive distillation column 7, and pass an appropriate amount of N through the purge gas pipe 11. 2 To remove the air in the reactive distillation tower 7, N 2 It passes through the pipe 16 and the condenser 6 in turn, and finally is disc...

Embodiment 3

[0049] Embodiment 3, a kind of method based on reaction-separation coupling production tert-butylamine, carries out following steps successively:

[0050] 1), Feed material:

[0051] Storage in raw material tank 1 is the raw material that molar ratio is 1:1 isobutene and ammonia composition, and the loaded catalyst after activation treatment is placed in the middle section of reactive distillation tower 7, and this loaded catalyst is the Co / HZSM5 of 300ml (as implemented obtained in Example 2).

[0052] Open the shut-off valve 22, pressurize the reactive distillation tower 7 through the purge gas pipe 11 and the collecting pipe 13 successively with nitrogen, so that the pressure at the top of the reactive distillation tower 7 reaches 1.5MPa, and this pressure value can be obtained from the pressure gauge 5 informed.

[0053] Then, the shutoff valve 20, the feed pump 2, the shutoff valve 21, the preheater 3, the shutoff valve 23, and the shutoff valve 24 are opened. Under th...

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Abstract

The invention discloses a method for preparing a tert-butylamine based on the reaction-separation coupling. The method comprises that: isobutylene and ammonia are used as raw materials, a reaction rectifying tower is used as a reactor, the inside of the middle segment of the reaction rectifying tower is filled with a support catalyst, the raw materials enter the middle segment of the reaction rectifying tower for reaction, the charging speed is between 50 and 200mL / h, the top pressure of the reaction rectifying tower is between 1.5 and 3.5MPa, and the reaction temperature is between 100 and 200 DEG C; and the incompletely reacted raw materials are discharged from the top part of the reaction rectifying tower, condensed by a condenser and returned to the reaction rectifying tower for circular reaction, and the products discharged from a reboiler on the bottom part of the reaction rectifying tower are coarse products of the tert-butylamine. The tert-butylamine prepared by the method has the characteristics of high yield and suitability for mass production.

Description

technical field [0001] The invention relates to a production method of an organic compound tert-butylamine (TBA). Background technique [0002] Tertiary butylamine (TBA) is an important intermediate in organic synthesis, widely used in synthetic rubber accelerators, drugs, insecticides, fungicides, herbicides, dyes and colorants, lubricating oil additives, etc. [0003] Due to the particularity of its molecular structure, TBA is difficult to synthesize. Although it was first produced in 1895, it was not until the 1940s that the synthesis of tert-butylurea from isobutylene (IBE) and urea, and the success of the synthesis of tert-butylsulfonamide from IBE and nitrile, laid the foundation for the industrial production of TBA. 50 In the early 1990s, TBA was industrialized by hydrolysis of tert-butylurea. [0004] At present, TBA has the following main production methods. [0005] (1), in H 2 SO 4 In the solution, tert-butyl urea can be prepared by condensation reaction of t...

Claims

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Application Information

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IPC IPC(8): C07C211/03C07C209/02C07C209/84B01J23/75B01J23/80B01J23/86
CPCY02P20/582
Inventor 陈新志周少东钱超
Owner ZHEJIANG UNIV
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