Process for synthesizing diisopropylamine from isopropylamine

A technology for diisopropylamine and isopropylamine, applied in the field of synthesizing diisopropylamine, can solve the problems of shortcoming in catalyst stability, short process flow, short service life, etc., and achieve the effects of reduced scale, fewer regeneration times, and reduced production cost

Active Publication Date: 2014-05-14
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

This method simplifies the original synthesis process, the process is short, and the product cost is reduced. However, because this method uses a high-temperature gas-phase synthesis method, the stability of the catalyst has disadvantages and the service life is short.

Method used

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  • Process for synthesizing diisopropylamine from isopropylamine

Examples

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Comparison scheme
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Embodiment 1

[0028] 70g of Hβ zeolite (SiO 2 / Al 2 o 3 The molecular ratio is 30) into 250mL 0.2M KCl solution, ion exchange is carried out at a temperature of 90~95°C, and the exchange time is 2.0h; after that, filter and wash until there is no Cl - ; Dry at 60°C for 4.0h, 110°C for 4.0h; then mix with 10g of aluminum hydroxide powder, add nitric acid and deionized water, knead and extrude on the extruder, and the amount of nitric acid added accounts for 0.5% of the dry material w%, the amount of deionized water added is subject to kneading and extruding. The strip-shaped catalyst was dried at 110°C for 4.0h, and then calcined in a muffle furnace at 550°C for 4.0h to obtain K / Hβ zeolite-Al 2 o 3 Catalyst, which contains 0.9w% potassium, 92.8w% Hβ zeolite, and the balance is γ-Al 2 o 3 , the catalyst number is AF-1.

Embodiment 2

[0030] Take 70g of Hβ zeolite (SiO 2 / Al 2 o 3 The molecular ratio is 42), according to the method described in Example 1, K / Hβ zeolite-Al 2 o 3 Catalyst, which contains potassium 1.6w%, contains Hβ zeolite 85.8w%, and the balance is γ-Al 2 o 3 , the catalyst number is AF-2.

Embodiment 3

[0032] Take 70g of Hβ zeolite (SiO 2 / Al 2 o 3 Molecular ratio is 66), according to the method described in embodiment 1, K / Hβ zeolite-Al is prepared 2 o 3 Catalyst, which contains potassium 1.6w%, contains Hβ zeolite 85.8w%, and the balance is γ-Al 2 o 3 , the catalyst number is AF-3.

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Abstract

The invention provides a process for synthesizing diisopropylamine from isopropylamine. Isopropylamine passes through a catalyst bed layer in the presence of hydrogen for a reaction so as to realize synthesis of diisopropylamine from isopropylamine. Reaction of isopropylamine in the presence of hydrogen is realized through the following two manners: 1, hydrogen is introduced into a reactor, and gas phase hydrogen is allowed to exist in the catalyst bed layer; 2, an isopropylamine raw material contacts with hydrogen before entering the reactor, hydrogen is dissolved in the isopropylamine raw material, then the isopropylamine raw material with dissolved hydrogen enters the reactor used for synthesis of diisopropylamine from isopropylamine, and gas phase hydrogen does not exist in the catalyst bed layer. Reaction conditions for synthesis of diisopropylamine from isopropylamine are as follows: reaction pressure is 1.0 to 8.0 MPa, reaction temperature is 150 to 350 DEG C, and liquid hour space velocity is 0.1 to 1.0 / h. The process greatly prolongs the service life of a catalyst and reduces reaction temperature while maintaining high selectivity and a high conversion rate.

Description

technical field [0001] The invention relates to a method for synthesizing diisopropylamine with isopropylamine as raw material. Background technique [0002] Diisopropylamine is an important intermediate in organic synthesis, widely used in the production of rubber accelerators, medicines, pesticides, surfactants, detergents, defoamers, etc. [0003] There are two traditional production methods of diisopropylamine (Edited by Liu Chong, Situ Yulian, etc., Petrochemical Handbook, Third Volume, Chemical Industry Press, 1987: 369; World Fine Chemical Products-Technical Economic Handbook. Ministry of Chemical Industry Published by Institute of Scientific and Technical Information, 1988: 247). The first is isopropanol hydrogenation, amination method to produce diisopropylamine, the reaction is divided into two steps. The reaction product contains isopropylamine 37w%, diisopropylamine 33w%, isopropanol 12w%, water 18w%, etc. The reaction product needs to be extracted, rectified ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C211/06C07C209/62
Inventor 艾抚宾乔凯祁文博徐彤袁毅金平程国香黎元生
Owner CHINA PETROLEUM & CHEM CORP
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