Preparation method and applications of supported ionic liquid catalyst

An ionic liquid and supported technology, which is used in the preparation and application of supported ionic liquid catalysts, can solve the problems of ruthenium sublimation and loss, and achieve the effects of not easy to lose, easy to operate, excellent catalytic activity and stability

Inactive Publication Date: 2018-03-02
ZHEJIANG UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The purpose of the present invention is to fundamentally solve the difficult problem of ruthenium sublimation and loss of active components in the reaction of ruthenium catalyst for the synthesis of vinyl chloride by acetylene hydrochlorination, and provide a ruthenium acetylene hydrochloride-based catalyst with good stability and high reactivity

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0043] Select columnar activated carbon as the carrier, its particle size is 30 mesh, the ash content is 2.5wt%, and the specific surface area is 800m 2 / g, pore volume 0.6ml / g, and treated with 200ml of 10wt% hydrochloric acid at 25°C for 3.5h. Dry at 110°C for 10 hours and set aside. 25ml of RuCl 3 After mixing the solution (in which the Ru content is 0.004g / ml) and 5g of 1-butyl-3-methylimidazolium chloride salt, add an appropriate amount of deionized water to make the volume to 60ml, and dissolve the mixed solution under the action of ultrasonic waves at 30°C Add it dropwise onto 100g of activated carbon carrier, and soak for 5 hours under the action of ultrasonic waves. Then, the above mixture was pre-frozen at -40°C for 10 hours; the frozen mixture was moved into a freeze dryer with a vacuum of 0.09MPa, and the temperature was raised to -15°C at a heating rate of 4°C / min , the frozen mixture was maintained at this temperature for 15 hours; continue to maintain the vac...

Embodiment 2

[0046] Columnar carbon nanotubes are selected as the carrier, the particle size is 40 mesh, the ash content is 3.5wt%, and the specific surface area is 200m 2 / g, the pore volume is 0.66ml / g. After mixing 50ml of ammonium hexachlororuthenate solution (in which the Ru content is 0.02g / ml) and 20g of tributylethylphosphine bromide, add an appropriate amount of deionized water to make the volume reach 66ml. The mixed solution was added dropwise to 100 g of carbon nanotube carrier, and the soaking time was 4 hours under the action of ultrasonic waves. Then, the above mixture was pre-frozen at -35°C for 14 hours; the frozen mixture was moved into a freeze dryer with a vacuum of 0.08 MPa, and the temperature was raised to -20°C at a heating rate of 3°C / min , the frozen mixture was maintained at this temperature for 12 hours; continue to maintain the vacuum degree of the freeze dryer at 0.08MPa, and then raise the temperature of the frozen mixture to 35°C at a heating rate of 3°C / mi...

Embodiment 3

[0049] Choose columnar graphene as carrier, its particle size is 70 mesh, ash content 1.5wt%, specific surface area 2630m 2 / g, the pore volume is 1.5ml / g. After mixing 10ml of potassium pentachlororuthenate (III) solution (wherein the Ru content is 0.05g / ml) and 15g of tetrabutylphosphine chloride, add an appropriate amount of deionized water to make the volume to 150ml. The mixed solution is added dropwise on the 100g graphene carrier under the action of ultrasonic waves, and the immersion time is 4 hours under the action of ultrasonic waves. Then the above mixture was pre-frozen at -50°C for 12 hours; the frozen mixture was moved into a freeze dryer with a vacuum of 0.1 MPa, and the temperature was raised to -25°C at a heating rate of 3°C / min. The frozen mixture was maintained at this temperature for 19 hours; the vacuum degree of the freeze dryer was maintained at 0.1 MPa, and then the temperature of the frozen mixture was raised to 45°C at a heating rate of 3°C / min, and ...

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Abstract

The invention discloses a ruthenium-based catalyst used for producing vinyl chloride through acetylene hydrochlorination, wherein the ruthenium-based catalyst is prepared by using a freeze drying method, such that the influence on the stability of the catalyst due to the migration of the active component in the pore channel of the catalyst onto the carrier surface along with the volatilization ofthe water during the preparing in the catalyst in the common vacuum drying method is avoided. According to the present invention, with the application of the ruthenium-based catalys in the vinyl chloride production through acetylene hydrochlorination, the ruthenium-based catalyst has high stability, the ruthenium loss is not detected within the detection limit of the detector after the long-time operation for 8000 h, the acetylene conversion rate can be up to 99.8%, and the vinyl chloride selectivity can be up to 100%.

Description

Background technique [0001] Polyvinyl chloride (PVC) is the third largest general-purpose plastic, and is generally obtained by polymerization of its monomer vinyl chloride. Due to the energy occurrence characteristics of rich coal, poor oil and little gas in my country, the preparation of vinyl chloride by coal-based calcium carbide acetylene method is the mainstream process of polyvinyl chloride production in my country. In industry, the catalyst currently used for synthesizing vinyl chloride is mercury chloride, which limits the application of polyvinyl chloride because it causes serious pollution to the environment, and the synthesized polyvinyl chloride contains a small amount of mercury. Therefore, mercury chloride catalysts will be gradually eliminated, and the synthesis of vinyl chloride under the action of mercury-free catalysts is the main direction for the future sustainable development of calcium carbide method PVC. Mercury-free catalysts mainly use metal chloride...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J31/30B01J31/22B01J31/24B01J31/28C07C17/08C07C21/06
CPCB01J31/2295B01J31/2404B01J31/28B01J31/30B01J2231/32B01J2531/821C07C17/08C07C21/06
Inventor 李小年赵佳张群峰丰枫狄淑霞翟媛媛卢春山许孝良马磊
Owner ZHEJIANG UNIV OF TECH
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