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Preparation method of hydrogenation catalyst with X/Ni/A1 hydrotalcite as precursor

A technology of hydrogenation catalyst and hydrotalcite, which is applied in the direction of metal/metal oxide/metal hydroxide catalyst, physical/chemical process catalyst, chemical instrument and method, etc., can solve the problems of expensive and difficult industrial production, and achieve The effect of cheap price, few steps, and simple and easy process

Inactive Publication Date: 2012-04-11
SOUTH CHINA UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Platinum, rhodium, and iridium complexes catalyze the reduction of LA to generate GVL. Although the yield can reach 87%–99%, the complexes of platinum, rhodium, and iridium, which are precious metals, are expensive and difficult to be widely used in industrial production.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Preparation of hydrogenation catalyst using copper-nickel-aluminum hydrotalcite as precursor (NiCuAl-LDHs): Add 34.812 g (0.12mol) Ni(NO) to a beaker 3 ) 2 ·6H 2 O, 9.664 g (0.04mol) Cu (NO 3 ) 2 ·3H 2 O and 15.004 g (0.04mol) Al(NO 3 ) 3 ·9H 2 O and add 200 ml of water to make solution A, add 20 g (0.5 mol) NaOH and 2.65 g (0.025 mol) Na to another beaker 2 CO 3 And add 250 ml of water to make solution B, pour solution A and solution B into acid burette and basic burette respectively and fix them on the iron stand, add a 500 ml beaker in the oil bath and place about 20 ml of distilled water, put in a magnet to stir, keep the temperature of the oil bath at 60 °C, control the dripping speed on both sides so that the pH in the beaker is always maintained at about 9.5, and ensure that all metal cations are completely precipitated. When the solution A is dripped, stop the lye dripping immediately, continue to stir the resulting mixture at 60 °C for 1 h, place the obtained prec...

Embodiment 2

[0024] Different M 2+ / M 3+ Preparation of nickel-copper-aluminum hydrotalcite (NiCuAl-LDHs): According to the method of Example 1, keep Ni(NO 3 ) 2 ·6H 2 O and Cu (NO 3 ) 2 ·6H 2 The molar ratio of O is 3:1 unchanged, changing Al(NO 3 ) 3 ·9H 2 The amount of O (always keep the total ion concentration of cations at 1 mol / L, and make M 2+ / M 3+ The molar ratio of is 1:1, 2:1, 3:1, 4:1 and 5:1), configure solution A and solution B according to the steps in implementation case 1, and add solution A and solution dropwise under stirring B. Obtain the corresponding mixed solution. Continue to stir the obtained mixed solution at 60 °C for 1 h. Place the obtained precipitate and mother liquor in a stainless steel crystallization kettle, seal and age at 100 °C for 12 hours. Filter and wash to neutrality, and finally dry and grind the precipitate at 100 °C to prepare 5 different M 2+ / M 3+ The nickel-copper-aluminum hydrotalcite (NiCuAl-LDHs) is calcined in a muffle furnace at 500°C for 5 ...

Embodiment 3

[0026] Preparation of nickel-copper-aluminum hydrotalcite (NiCuAl-LDHs) with different Ni / Mg molar ratios: According to the method of Example 1, keep M in NiCuAl-LDHs 2+ / M 3+ The molar ratio is 4:1 unchanged, keeping Al(NO 3 ) 3 ·9H 2 The amount of O is unchanged, and Ni(NO 3 ) 2 ·6H 2 O and Cu (NO 3 ) 2 ·6H 2 The amount of O added (always keep the total ion concentration of cations at 1mol / L, and make the molar ratio of Ni / Cu in NiCuAl-LDHs 1:1, 2:1, 3:1, 4:1 and 5:1) , Configure solution A and solution B according to the steps in implementation case 1, add solution A and solution B dropwise under stirring to obtain the corresponding mixed solution, and continue to stir the obtained mixed solution at 60 °C for 1 h, and the obtained The precipitate and mother liquor are placed in a stainless steel crystallization kettle, sealed and aged at 100 °C for 12 hours. The resulting precipitate is filtered and washed to neutrality. Finally, the precipitate is dried and ground at 100 °C t...

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PUM

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Abstract

The invention discloses a preparation method of hydrogenation catalyst with X / Ni / A1 hydrotalcite as precursor. The invention comprises adopting coprecipitation method to prepare X / Ni / A1 hydrotalcite with laminated structure, roasting at high temperature to produce X / Ni / A1 containing composite metal oxide, reducing by high temperature hydrogenation to obtain X / Ni / A1 containing hydrogenation catalyst with high dispersion and large specific surface area, in the presence of X / Ni / A1 containing composite metal oxide and under proper reaction conditions, making generation of gamma-valerolactone by levulinic acid hydrogenation with good effect. The catalyst of the invention has easily obtained and low cost raw materials, simple and feasible production techniques, large specific surface area and easily separated product.

Description

technical field [0001] The invention relates to a preparation method of a hydrogenation catalyst, in particular to a preparation method of a hydrogenation catalyst using X / Ni / Al hydrotalcite as a precursor. Background technique [0002] gamma – Valerolactone has vanillin and coconut aroma, and also contains fresh fruity, medicinal, and sweet aromas, and is soft and long-lasting, so it is widely used in food flavors and tobacco flavors. This product has already been commercialized in developed countries, and it is also produced in small batches in my country. However, the production process uses potassium borohydride as the reducing agent, which is expensive, difficult to transport, and in short supply, resulting in low product output and high cost. and poor efficiency, resulting in gamma – High price of valerolactone. Levulinic acid (LA) can be prepared in a variety of ways gamma – γ-valerolactone (GVL), Tang Tianshu et al. reported the synthesis of GVL from LA through mi...

Claims

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Application Information

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IPC IPC(8): B01J23/755C07D307/33
Inventor 庄军平林鹿蒋云飞庞春生
Owner SOUTH CHINA UNIV OF TECH
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