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Preparation method of saturated hydrogenation Pd catalyst and method for catalyzing hydrogenation of polystyrene by virtue of saturated hydrogenation Pd catalyst

A technology for catalysts and copolymers, applied in catalyst activation/preparation, chemical instruments and methods, catalysts for physical/chemical processes, etc. Simple steps and the effect of improving the hydrogenation conversion rate

Inactive Publication Date: 2017-09-29
SHANDONG YUHUANG CHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] Now PS hydrogenation is still in the stage of laboratory research. The active components are mainly palladium and platinum. There have been a lot of reports on the research on the carrier, but there are still many problems to be solved: (1) The catalyst carrier includes non-porous materials, mesoporous materials and macroporous materials, non-porous and macroporous materials have very low specific surface area (10-20m 2 / g) make the unit mass catalyst have extremely low hydrogenation active site quantity, in order to ensure the hydrogenation activity, it is necessary to greatly increase the amount of catalyst, thus increasing the cost of hydrogenation
In addition, the particle size of the catalyst will be reduced, thereby increasing the difficulty of separating the catalyst and the polymer solution; (2) the use of a catalyst carrier with a high specific area will inevitably reduce the pore size of the catalyst, which may make the polymer molecules in the catalyst pores. Diffusion is limited, and hydrogenation occurs only on the outer surface of the catalyst, while the support-rich inner surface does not play a role

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Carrier preparation: Weigh 4.0g of P123 and place it in a 250mL beaker, add 75mL of 1.6mol / L HCl to it, stir magnetically in a water bath at 38°C for 12h to obtain a transparent solution, add 1.5g of TMB to the mixed solution, continue to stir for 4h, then drop into 8.6g TEOS, stop stirring after 5min, adjust the temperature to 40°C and let it stand for 20h, then transfer it into a 100mL autoclave, hydrothermally treat at 100°C for 24h, wash with absolute ethanol three times, dry at 80°C for 14h, and then bake at 550°C for 5h. The obtained carrier window, pore size and specific surface area are 10nm, 18nm, 712m 2 / g.

[0024] Catalyst preparation: first measure the amount of acetone adsorbed by 1.0g carrier, then weigh 1.0g carrier in a crucible, calculate according to the Pd loading capacity of 6.0wt%, and weigh the corresponding amount of palladium acetate, completely dissolve in acetone and gradually Add it dropwise to the carrier, ultrasonicate for 30 minutes, dry ...

Embodiment 2

[0028] Carrier preparation: Weigh 4.0g of P123 and place it in a 250mL beaker, add 75mL of 1.6mol / L HCl to it, stir magnetically in a water bath at 38°C for 12 hours to obtain a transparent solution, add 3g of TMB to the mixed solution, continue stirring for 4 hours, and then drop into 8.6g TEOS, stop stirring after 5min, adjust the temperature to 40°C and let stand for 20h, add 0.02g NH 4 F was stirred evenly and transferred to a 100mL autoclave, hydrothermally treated at 110°C for 24h, washed with absolute ethanol three times, dried at 90°C for 14h, and then calcined at 600°C for 5h. The obtained carrier window, pore size and specific surface area are 15nm, 37nm, 518m 2 / g.

[0029] Catalyst preparation: first measure the dilute hydrochloric acid whose adsorption concentration of 1.0g carrier is 2.0wt%, then weigh 1.0g carrier in the crucible, calculate according to the Pd load is 5.0wt% and take the corresponding amount of palladium chloride, completely dissolve in After ...

Embodiment 3

[0033] Carrier preparation: Weigh 4.0g P123 and place it in a 250mL beaker, add 75mL of 1.6mol / L HCl to it, stir magnetically in a water bath at 38°C for 12h to obtain a transparent solution, add 6g TMB to the mixed solution, continue stirring for 4h, then drop into 8.6g TEOS, stop stirring after 5min, adjust the temperature to 40°C and let stand for 20h, add 0.06g NH 4 F was stirred evenly and transferred into a 100mL autoclave, hydrothermally treated at 140°C for 24h, washed with absolute ethanol three times, dried at 80°C for 12h, and then calcined at 550°C for 5h. The obtained carrier window, pore size and specific surface area are 28nm, 60nm, 368m 2 / g.

[0034] Catalyst preparation: first measure the water absorption of 1.0g carrier, then weigh 1.0g carrier in the crucible, calculate according to the Pd loading of 4.0wt%, weigh the corresponding amount of palladium acetate, dissolve it in water, and gradually add it dropwise with a straw Put it into the carrier, ultrason...

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PUM

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Abstract

The invention relates to the technical field of catalytic hydrogenation and particularly discloses a preparation method of a saturated hydrogenation Pd catalyst and a method for catalyzing the hydrogenation of polystyrene by virtue of the saturated hydrogenation Pd catalyst. The preparation method is characterized by comprising the following steps: with P123 as a template, ethyl orthosilicate as a silicon source and 1,3,5-trimethylbenzene and ammonium fluoride as pore-enlarging agents, synthesizing by virtue of a hydrothermal method under an acidic condition, drying, and roasting, so as to obtain a powdery MCF material; calculating the mass of palladium metal salt according to a proportion that palladium is 1.0wt%-8.0wt% of the powdery MCF material, and dissolving the palladium metal salt, so as to prepare steeping liquid; and steeping the powdery MCF material into the steeping liquid, drying, roasting, and carrying out formation and sieving, so as to obtain a catalyst product. The preparation method has the beneficial effects that the steps are simple, and the catalyst is prepared from Pd as a main catalysis element as well as home-made MCF which has a relatively large specific surface, an adjustable super-large mesoporous and a three-dimensional penetrated pore system, so that the PS hydrogenation conversion rate is substantially increased.

Description

(1) Technical field [0001] The invention relates to the technical field of catalytic hydrogenation, in particular to a preparation of a saturated hydrogenation Pd catalyst and a method for catalyzing the hydrogenation of polystyrene. (2) Background technology [0002] Polystyrene (PS) is a resin polymerized from styrene and is one of the five general-purpose thermoplastic synthetic resins. Due to the shortcomings of PS, such as poor heat resistance, UV resistance, and brittleness, the current application of PS is limited to low-end products, such as food packaging, toys, hangers, foam plastics, and certain consumer electronics products. However, even in these fields, PS may gradually be replaced by cheaper raw material polypropylene. Polycyclohexylethylene or hydrogenated polystyrene (PCHE) with significantly improved physical properties (glass transition temperature, transparency, heat resistance, oxidation resistance and UV resistance, etc.) can be obtained after hydrogen...

Claims

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Application Information

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IPC IPC(8): B01J23/44C08F12/08C08F8/04
CPCC08F8/04B01J21/08B01J23/44B01J37/0009B01J37/0201B01J35/617B01J35/615B01J35/647C08F12/08
Inventor 崔春生景文肖博王玉强王建伟王胜伟
Owner SHANDONG YUHUANG CHEM CO LTD
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