Pd-ZnO/Al2O3 catalyst and preparation method and application thereof

A catalyst and co-catalyst technology, used in metal/metal oxide/metal hydroxide catalysts, physical/chemical process catalysts, chemical instruments and methods, etc. The problem of harsh reaction conditions, etc., achieves the effects of high catalytic activity, simple preparation process and low cost.

Pending Publication Date: 2020-04-10
SHANXI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, judging from the few literature reports so far, polydivinyl acetylene hydrogenation modified catalysts still have disadvantages such as harsh reaction conditions, low degree of hydrogenation, and high loading of noble metals in the catalyst.

Method used

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  • Pd-ZnO/Al2O3 catalyst and preparation method and application thereof
  • Pd-ZnO/Al2O3 catalyst and preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] Weigh 0.1 g PdCl 2 , 1.76 g Zn(NO 3 ) 2 ·6H 2 O, 35.88 g Al(OH) 3 Mix it with 10 g of dicyandiamide and grind it thoroughly. Place the ground mixed sample in a tube furnace and introduce H with a flow rate of 50 mL / min. 2 / N 2 Mixed gas (H 2 / N 2 The volume ratio is 1:5), the temperature is increased to 80 ℃ at a rate of 1 ℃ / min for 8 h, and then the temperature is increased to 400 ℃ at a rate of 8 ℃ / min for 4 h. After the treatment, the heating is stopped and the H 2 / N 2 The mixed gas is switched to helium with a flow rate of 50 mL / min, and it is naturally cooled to room temperature to obtain Pd-ZnO / Al 2 O 3 catalyst. The mass percentage of Pd is 0.25 wt%, the mass percentage of ZnO is 2.0 wt%, and the mass percentage of Al 2 O 3 The mass percentage of is 97.75 wt%.

[0035] Mix 30 g PDVA toluene solution (PDVA concentration 20%) and 0.2 g Pd-ZnO / Al 2 O 3 The catalyst was added to the autoclave, and nitrogen was introduced for three times, and then hydrogen was introduced....

Embodiment 2

[0037] Weigh 0.15 g Pd(NO 3 ) 2 ·2H 2 O, 1.76 g Zn(NO 3 ) 2 ·6H 2 O, 35.88 g Al(OH) 3 And 10 g of dicyandiamide, using the preparation method of Example 1 to prepare Pd-ZnO / Al 2 O 3 catalyst. The mass percentage of Pd is 0.25wt%, the mass percentage of ZnO is 2.0wt%, Al 2 O 3 The mass percentage is 97.75wt%.

[0038] Using the reaction conditions and measurement method of Example 1, the degree of hydrogenation of polydivinyl acetylene was calculated to be 25.4%.

Embodiment 3

[0040] Weigh out 0.05 g PdCl 2 , 0.88 g Zn(NO 3 ) 2 ·6H 2 O, 35.88 g Al(OH) 3 And 10 g of dicyandiamide, using the preparation method of Example 1 to prepare Pd-ZnO / Al 2 O 3 catalyst. The mass percentage of Pd is 0.13 wt%, the mass percentage of ZnO is 1.02 wt%, and the mass percentage of Al 2 O 3 The mass percentage of is 98.85 wt%.

[0041] Using the reaction conditions and measurement methods of Example 1, the degree of hydrogenation of polydivinyl acetylene was calculated to be 18.7%.

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Abstract

The invention discloses a Pd-ZnO/Al2O3 catalyst and a preparation method and application thereof. The catalyst uses Pd as an active component, ZnO as a cocatalyst and Al2O3 as a carrier, and comprisesthe following components in percentage by mass: 0.1%-0.25% of Pd, 0.5%-2.0% of ZnO and 97.75%-99.4% of Al2O3. The preparation method comprises the following steps: uniformly mixing a Pd source, a Znsource, an Al source and dicyandiamide, carrying out full grinding, putting the ground mixture into a tubular furnace, introducing H2/N2 mixed gas, conducting heating treatment, and carrying out cooling to room temperature in an N2 or inert atmosphere after the treatment is finished, thereby obtaining the catalyst. The prepared catalyst is used for a hydrogenation reaction of polydivinylacetylene,and the hydrogenation degree of polydivinylacetylene can reach 25.8% under relatively mild reaction conditions.

Description

Technical field [0001] The invention relates to a Pd-ZnO / Al 2 O 3 The catalyst and its preparation method and application belong to the technical field of catalyst preparation. Background technique [0002] Synthetic rubber is generally divided into general synthetic rubber and semi-universal synthetic rubber, of which neoprene is a semi-universal type. Chloroprene rubber not only has the general properties of most general synthetic rubbers, but also has its outstanding properties, such as solvent resistance, chemical stability, heat resistance, aging resistance and air tightness, etc., so it has a wide range of applications. There are two main methods for producing chloroprene rubber, the acetylene method and the butadiene method. my country mainly uses the acetylene method to produce neoprene. However, in the process of producing neoprene by the acetylene method, divinyl acetylene (DVA) is produced as a by-product. [0003] The equation for producing neoprene by acetylene meth...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/60C08F8/04C08F38/04
CPCB01J23/60C08F8/04C08F38/04
Inventor 王永钊田雨润武瑞芳幸忠王晶晶王淑娟
Owner SHANXI UNIV
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