Preparation method of dibenzylamine

A technology of dibenzylamine and benzaldehyde, which is applied in the field of preparation of dibenzylamine, can solve the problem of low yield of dibenzylamine, and achieve the effects of reduced production cost, extended service life and improved conversion rate

Inactive Publication Date: 2012-06-20
ZHEJIANG XINHUA CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0012] The technical problem to be solved by the present invention is the problem that the yield of dibenzylamine from benzaldehyde is not high, and a new method fo

Method used

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  • Preparation method of dibenzylamine
  • Preparation method of dibenzylamine
  • Preparation method of dibenzylamine

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] In a 1000mL autoclave, add 200g of benzaldehyde, 45g of ammonia, 100g of pure water as a solvent, 5g of a catalyst, the content of the catalyst is 0.3% of Pd, 0.1% of Sn, and the rest is the carrier TiO 2 . The reaction temperature is 60° C., the hydrogen reaction pressure is 2.0 MPa by gauge pressure, the reaction time is 20 minutes, the conversion rate of benzaldehyde is 100%, and the yield of dibenzylamine is 97.2%.

[0020] The catalyst wherein is prepared as follows: soak the carrier in a 30% nitric acid solution, reflux at 100°C for 7 hours, wash to neutrality, add required amount of palladium chloride and sodium hydroxide solution in the aqueous solution of the carrier , and adding Sn as a cocatalyst for modification, and TiO 2 As a carrier, it is prepared after washing with water and drying.

Embodiment 2～5

[0022] According to each operation step and condition of embodiment 1, only change the composition of catalyst, its reaction result is listed in table 1.

[0023] Table 1

[0024]

Embodiment 6～10

[0026] According to each operation step and condition of embodiment 1, adopt the catalyst used among the embodiment 4, its consumption is 2.5% of benzaldehyde, solvent consumption is 50% of benzaldehyde, change reaction condition, its reaction result is listed in table 2.

[0027]

[0028] As can be seen from the data in Table 1 and Table 2, under the process conditions, benzaldehyde has a higher conversion rate and selectivity.

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Abstract

The invention relates to a chemical preparation method, and particularly relates to a preparation method of dibenzylamine. The invention prepares dibenzylamine by using benzaldehyde and ammonia as raw materials; the reaction temperature is 10-100 DEG C; the gauge pressure meter hydrogen reaction pressure is 1.0-5.0 Mpa; water, or lower aliphatic alcohol with 1-4 carbon atoms, or a mixture is used as a solvent; and the reaction is performed under the action of a catalyst for 0.1-5 hours; the catalyst comprises precious metal palladium used as a main catalyst; at least one of Ni, Ru, Os, Ir, Cu, Sn is selected and added as a cocatalyst; at least one of TiO2, SiO2, CeO2, SnO2 is used as a carrier; the advantages of the invention are that the preparation catalyst has a prolonged service life; the preparation cost is reduced; the conversion rate of benzaldehyde is high; and the dibenzylamine yield is increased.

Description

technical field [0001] The invention relates to a chemical preparation method, in particular to a preparation method of dibenzylamine. Background technique [0002] Dibenzylamine (Dibenzylamine), molecular formula C 14 h 15 N, molecular weight 197.28, relative density 1.026, melting point -26°C, boiling point 300°C, refractive index 1.574-1.576, flash point 143°C, water solubility 0.05G / L (20°C). Dibenzylamine is a colorless oily liquid with ammonia odor, soluble in ethanol and ether, insoluble in water. Strong irritant to skin and mucous membranes. [0003] Dibenzylamine is an important intermediate in organic synthesis, which can be used to synthesize penicillin and curing agent for rubber and plastic curing. It is mainly used to produce efficient and non-toxic vulcanization accelerators tetrabenzylthiuram disulfide (TBZTD) Zinc dithiocarbamate (ZBEC). It can also be used to determine cobalt, iron and cyanate, etc. [0004] The production methods of dibenzylamine mai...

Claims

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Application Information

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IPC IPC(8): C07C211/27C07C209/26
Inventor 谢海英王卫明谢自强陈宏邵永忠张绍志段小刚王晓明乔涛
Owner ZHEJIANG XINHUA CHEM
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