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Preparation method of catalyst for alpha-pinene hydrogenation

A catalyst and pinene technology, applied in the direction of catalysts, hydrogenation hydrocarbons, molecular sieve catalysts, etc., can solve the problems of poor reproducibility, poor thermal and mechanical stability, and weak anti-oxidation ability of skeleton nickel catalysts, and shorten the crystallization time , It is not easy to fall off, and the effect of reducing the cost of raw materials

Inactive Publication Date: 2017-04-26
KUNMING UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Nickel-based catalysts mainly include nano-nickel, skeletal nickel and supported nickel-based catalysts. Nano-nickel catalysts have high synthesis costs, complex operations, poor thermal and mechanical stability, and skeletal nickel catalysts have poor reproducibility and weak oxidation resistance.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] (1) Mix aluminum hydroxide, orthophosphoric acid, and diisopropylamine in a molar ratio of 1:1:2, H 2 O and Al 2 o 3 The molar ratio was 20:1 for feeding, and after stirring for 1 h, the initial gel was transferred to a stainless steel reactor.

[0022] (2) Put the reaction kettle into an oven, adjust the temperature to 180°C for 120 hours of crystallization, after the crystallization is completed, quench, filter, wash with water, dry in an oven at 110°C for 5 hours, and raise the temperature to Insulate at 200°C for 0.5h, then raise the temperature to 350°C at a rate of 2°C / min for 2 hours, then raise the temperature to 550°C at a rate of 10°C / min for 4 hours to obtain APO-11 molecular sieves, The specific surface area is 178.55m 2 / g.

[0023] (3) Use the above-mentioned APO-11 as a catalyst carrier, press NiCl 2 ·6H 2 O, APO-11 mass ratio 1:1 for feeding, dropwise add 10mol / L NaOH, adjust pH=7, then add NaH according to molar ratio Ni / P=1:6 2 PO 2 ·H 2 O was...

Embodiment 2

[0026] (1) Mix aluminum hydroxide, orthophosphoric acid, and diisopropylamine in a molar ratio of 1:1:3, H 2 O and Al 2 o 3 The molar ratio was 20:1 for feeding, and after stirring for 1 h, the initial gel was transferred to a stainless steel reactor.

[0027] (2) Put the reactor into an oven and adjust the temperature to 210°C for 18 hours of crystallization. After crystallization, quench, filter, wash with water, dry in an oven at 110°C for 5 hours, raise the temperature to 200°C for 2 hours at a rate of 10°C / min, and then raise the temperature to 380°C at a rate of 5°C / min ℃ for 0.5h, and then according to the heating rate of 5℃ / min, the temperature was raised to 550℃ and roasted for 10h to obtain APO-11 molecular sieve with a specific surface area of ​​155.44m 2 / g.

[0028] (3) Use the above-mentioned APO-11 as a catalyst carrier, press NiCl 2 ·6H 2 O. Feed APO-11 with a mass ratio of 1:3, add 10mol / L NaOH dropwise, adjust pH=8, and then add NaH at a molar ratio of ...

Embodiment 3

[0031] (1) Mix aluminum hydroxide, orthophosphoric acid, and diisopropylamine in a molar ratio of 1:1:1, H 2 O and Al 2 o 3 The molar ratio was 20:1 for feeding, and after stirring for 1 h, the initial gel was transferred to a stainless steel reactor.

[0032] (2) Put the reaction kettle into an oven and adjust the temperature to 200°C for 48 hours of crystallization. After crystallization, quench, filter, wash with water, dry in an oven at 110°C for 5 hours, raise the temperature to 200°C for 0.5h at a rate of 1°C / min, and then raise the temperature to Insulate at 400°C for 3h, then heat up to 550°C for 1h at a heating rate of 1°C / min to obtain APO-11 molecular sieve with a specific surface area of ​​188.93 m 2 / g.

[0033] (3) Use the above-mentioned APO-11 as a catalyst carrier, press NiCl 2 ·6H 2 O, APO-11 mass ratio 1:1 for feeding, dropwise add 10mol / L NaOH, adjust pH=8, then add NaH according to molar ratio Ni / P=1:2 2 PO 2 ·H2 O was reduced and reacted for 4h to...

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Abstract

The invention relates to a preparation method of a catalyst for alpha-pinene hydrogenation, and belongs to the field of chemical engineering. The method comprises the processing steps that aluminum hydroxide, orthophosphoric acid, diisopropylamine, H2O and Al2O3 are mixed and stirred and then put in a stainless steel reaction kettle, crystallization is conducted in a drying oven with the temperature of 180-210 DEG C for 18-120 hours, filtration, washing and drying are conducted, and a well-crystallized molecular sieve APO-11 is obtained after calcinations is conducted for 1-10 hours at the temperature of 550 DEG C, wherein the molar ratio of aluminum hydroxide to orthophosphoric acid to diisopropylamine is 1:1:(1-3), and the molar ratio of H2O to Al2O3 is 20:1; the prepared APO-11 is mixed with NiCl2.6H2O according to the mass ratio of 1:(1-3), pH is regulated to 7-9, then NaH2PO2-H2O is added for reduction, and Ni-P / APO-11 is prepared after the reaction is conducted for 1-12 hours, wherein the molar ratio of Ni to P is 1:(2-6); the prepared Ni-P / APO-11 is added to a high-pressure reaction kettle, the high-pressure reaction kettle is sealed, N2 replacement and H2 replacement are conducted respectively, then hydrogen pressure is raised to 2-5 Mpa, pressure maintaining and leakage detecting are conducted, the reaction is conducted for 45-180 minutes at the temperature of 120-140 DEG C, and high-selectivity pinane is obtained, wherein the mass of the Ni-P / APO-11 accounts for 3-7% of the mass of turpentine oil. According to the method, the cost of the raw materials is low, the crystallization conditions are mild, energy consumption is low, and when the prepared material is used in an alpha-pinene hydrogenation reaction, high-selectivity cis-pinane can be obtained.

Description

technical field [0001] The invention relates to a preparation method of a catalyst used for α-pinene hydrogenation reaction, belonging to the field of chemical industry. Background technique [0002] my country has abundant reserves of turpentine, and its export volume of raw materials ranks second in the world. Its main components, α-pinene and β-pinene, can be used to produce important synthetic intermediate pinane through hydrogenation reaction. Pinane is also an important raw material for spices and other pinene deep processing industries. Because pinane contains cis and There are two isomers in the trans-type, and there is a large steric hindrance in the structure of the trans-pinane, which makes its activity far lower than that of cis-pinane, so the preparation of highly selective cis-pinane becomes pinene plus The key to the hydrogen reaction. [0003] At present, α-pinene hydrogenation catalysts can be divided into noble metal catalysts and non-noble metal catalyst...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J29/83C07C5/03C07C13/40
CPCC07C5/03B01J29/83C07C2529/83C07C13/40
Inventor 蒋丽红潘登王亚明贾庆明陕绍云杨晨王鹤林焦星星刘磊钟申洁郑文龙
Owner KUNMING UNIV OF SCI & TECH
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