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Application of ferro-nickel hydrotalcite catalyst in preparation of benzyl alcohol

A technology of benzyl alcohol and catalyst, which is applied in the application field of nickel-iron hydrotalcite catalyst in the preparation of benzyl alcohol, can solve the problems of high production equipment requirements, complicated process, high cost, etc., and achieve reduction of production cost, broaden application range, and facilitate recycling Effect

Active Publication Date: 2019-04-26
JIANGNAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] (1) Using the Carnichalo reaction, benzaldehyde is disproportionated under strong alkali conditions to generate corresponding alcohols and acids. This process has high requirements for production equipment, and it needs to be resistant to strong acids and strong alkalis. After the reaction, a large amount of solvents are required for the reaction solution. Extraction, in addition, the corresponding by-products need to be reduced with potassium borohydride catalyst, the process is complicated and the cost is high
[0005] (2) Utilize the improved potassium borohydride catalyst to catalyze the reduction of benzaldehyde, which has certain advantages compared with potassium borohydride reduction, but the catalyst has disadvantages such as high preparation cost, low reaction yield, low selectivity, and acid corrosion, Not conducive to mass production
[0006] (3) take benzaldehyde as reaction substrate, use hydrogen as hydrogen donor, adopt noble metal nano-catalyst (such as platinum, palladium and ruthenium etc.) to carry out catalytic transfer hydrogenation to prepare benzyl alcohol, this method requires very high to production equipment and hydrogen There are great unsafe factors in the storage and transportation of
[0007] The above-mentioned method for preparing benzyl alcohol inevitably uses expensive equipment resistant to strong acid and strong alkali corrosion, or uses explosive hydrogen as the harsh reaction conditions of the hydrogen donor. Therefore, it is necessary to find a simpler preparation Benzyl Alcohol Method

Method used

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  • Application of ferro-nickel hydrotalcite catalyst in preparation of benzyl alcohol
  • Application of ferro-nickel hydrotalcite catalyst in preparation of benzyl alcohol
  • Application of ferro-nickel hydrotalcite catalyst in preparation of benzyl alcohol

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preparation example Construction

[0041] The preparation method of the heterogeneous nickel-iron hydrotalcite catalyst used in the present invention, the steps are as follows:

[0042] ①Weigh Ni(NO 3 ) 2 ·6H 2 O and Fe(NO 3 ) 3 9H 2 O and a certain amount of urea are added to the polytetrafluoroethylene-lined hydrothermal reactor, where the molar weight of urea is 3.3 times the sum of the metal molar weight; ② add deionized water to dissolve and magnetically stir at room temperature One hour; ③ After the solid matter is completely dissolved, seal the stainless steel high-pressure reactor, then raise the temperature to 140 ° C, stop heating after 20 hours of hydrothermal reaction, and naturally cool to room temperature; ④ Suction filter the cooled material, and use it separately Wash with ionized water and ethanol for 2 to 5 times, dry in vacuum at 60°C, and grind to obtain a light yellow powder, which is a heterogeneous nickel-iron hydrotalcite catalyst (abbreviated as: Ni-Fe(3 / 1) LDH).

[0043] In addit...

Embodiment 1

[0045] A method for preparing benzyl alcohol using a nickel-iron hydrotalcite catalyst, comprising the following steps:

[0046] Add 0.2g of Ni-Fe(3 / 1) LDH to the lining of a clean autoclave, then add 1mmol of benzaldehyde, 5mL of isopropanol and a magnet of appropriate size. After packaging the stainless steel autoclave, Under the action of magnetic stirring, react at 150° C. for 10 h, and after the reaction is completed and cooled, the supernatant is detected and analyzed by a gas chromatograph (such as figure 1 ), it can be seen that benzyl alcohol has been prepared.

Embodiment 2-3

[0048] The present embodiment 2-3 compared the influence of different catalysts on the preparation of benzyl alcohol.

[0049] Add 0.2 g of hydrotalcites (Ni-Fe(2 / 1) LDH and Ni-Fe(4 / 1) LDH) with different nickel-iron molar ratios to the lining of a clean autoclave, and then add 1 mmol of benzaldehyde, 5mL of isopropanol and magnets of appropriate size were packaged in a stainless steel autoclave, and reacted at 150°C for 10 hours under the action of magnetic stirring. After the reaction was completed and cooled, the supernatant was taken for detection and analysis.

[0050]The specific experimental results are shown in Table 1. From the contents of Table 1, it can be seen that when using Ni-Fe(3 / 1) LDH as a catalyst, under the same conditions, the yield and selectivity of benzyl alcohol are the best.

[0051] Catalytic reaction results under different catalysts in table 1

[0052] Example

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Abstract

The invention discloses application of a ferro-nickel hydrotalcite catalyst in preparation of benzyl alcohol, and belongs to the technical field of synthesis of benzyl alcohol. In the application, thebenzyl alcohol is prepared by catalyzing benzaldehyde via a catalytic transfer hydrogenation reaction under the own pressure condition in a hydrothermal reaction kettle by taking alcohol compounds asa solvent and a hydrogen donor and taking Ni-Fe(2 / 1)LDH, Ni-Fe(3 / 1)LDH or Ni-Fe(4 / 1)LDH as a catalyst, the reaction temperature is 110-160 DEG C, and the reaction time is 6-11 hours. A method for preparing the benzyl alcohol is simple in process and convenient in operation and is safe and environmentally friendly. The ferro-nickel hydrotalcite catalyst is prepared from common non-noble metals, islow in cost and is easy to obtain; the ferro-nickel hydrotalcite catalyst can be also used for reducing other compounds containing C=O bonds and is beneficial for commercial application.

Description

technical field [0001] The invention relates to the technical field of benzyl alcohol synthesis, in particular to the application of a nickel-iron hydrotalcite catalyst in the preparation of benzyl alcohol. Background technique [0002] Benzyl alcohol is an important organic intermediate, which can be used as a fixative and an indispensable fragrance in the preparation of fragrances. It can be used to make soaps and daily fragrances; it can also be used as a paint solvent, a photographic developer, and a polyvinyl chloride stabilizer. agent etc. In addition, benzyl alcohol can also be used as local anesthetic, drug tranquilizer and drug synthesis in the field of medicine. With the development of relevant industries and the opening of the international market, the demand for benzyl alcohol at home and abroad will increase day by day. [0003] The preparation of benzyl alcohol from benzaldehyde mainly contains the following three methods at present: [0004] (1) Using the C...

Claims

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Application Information

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IPC IPC(8): C07C29/14C07C33/22
CPCC07C29/14C07C33/22
Inventor 王海军汪涛胡爱云刘晨徐广志夏咏梅刘湘
Owner JIANGNAN UNIV
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