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Method for preparing temperature-control hydrogenation catalyst and application in chemigum hydrogenation

A technology of nitrile rubber and catalyst, which is applied in the field of hydrogenation of nitrile rubber solution, can solve problems such as no use value, achieve high hydrogenation degree, improve hydrogenation activity, and simplify the removal process

Active Publication Date: 2010-06-16
BEIJING UNIV OF CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, such catalysts used in the field of catalytic hydrogenation of macromolecules, especially rubber macromolecules, are rarely seen in reports.
Yin Haichuan of Kunming University of Science and Technology developed a temperature-controlled phase separation catalyst tris-(p-phenoxypolyoxyethylene ether)-rhodium complex, and studied its catalytic hydrogenation effect on nitrile rubber, although the catalyst The highest removal rate can reach 96%, but the highest degree of hydrogenation of the product can only reach 65%, such hydrogenated nitrile rubber products are basically useless

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] Add the ligand of the type and amount shown in Table 1 No. 1 and an appropriate amount of ether in the reaction flask, and add the metal chloride in the amount shown in Table 1 No. 1 at the reflux temperature. After heating to reflux for 2 hours, remove Solvents are used to prepare Catalyst A used in the present invention.

[0027] Put 0.5g of nitrile rubber dry rubber, 50mL of xylene, 0.0025g of catalyst A and 0.005g of triphenylphosphine into the reaction kettle, replace the system with hydrogen and pressurize to 1MPa, heat to 140°C, keep the temperature for 4h, and the reaction is over Finally, the product was diluted to 250mL with xylene, 63mL of polyethylene glycol and 12.5mL of n-heptane were added and stirred for 30 minutes, and then stratified. The upper layer of nitrile rubber glue was taken out, and the hydrogenation degree was analyzed, and the lower layer was tested by ultraviolet spectroscopy.

[0028] Measured results: the hydrogenation degree is 66%; the ...

Embodiment 2

[0030] Add the ligand of the type and amount shown in Table 1 No. 1 and an appropriate amount of ether in the reaction flask, and add the metal chloride in the amount shown in Table 1 No. 1 at the reflux temperature. After heating to reflux for 2 hours, remove Solvents are used to prepare Catalyst A used in the present invention.

[0031] Put 5g of nitrile rubber dry rubber, 50mL of xylene, 0.4g of catalyst A and 0.004g of triphenylphosphine into the reaction kettle, replace the system with hydrogen and pressurize to 3MPa, heat to 175°C, keep the temperature for 4h, after the reaction Dilute the product to 250mL with xylene, add 100mL polyethylene glycol and 12.5mL n-heptane and stir for 30 minutes, then let it stand for stratification, take out the upper layer of nitrile rubber glue, and analyze the degree of hydrogenation, and the lower layer is tested by ultraviolet spectroscopy.

[0032] Measured results: the hydrogenation degree is 69%; the catalyst removal rate is 85%. ...

Embodiment 3

[0034] Add the ligand of the type and amount shown in No. 2 of Table 1 and an appropriate amount of absolute ethanol in the reaction flask, add the metal chloride in the amount shown in No. 2 of Table 1 at the reflux temperature, and heat to reflux for 2 hours. , Remove the solvent to obtain the catalyst B used in the present invention.

[0035] Put 2.5g of nitrile rubber dry rubber, 50mL of xylene, 0.075g of catalyst B and 0.15g of triphenylphosphine into the reaction kettle, replace the system with hydrogen and pressurize to 1.5MPa, heat to 155°C, keep the temperature for 8h, and react After the end, dilute the product with xylene to 250mL, add 75mL of polyethylene glycol and 12.5mL of n-heptane and stir for 30 minutes, then let it stand for stratification, take out the upper layer of nitrile rubber glue, and analyze the degree of hydrogenation, and the lower layer is tested by ultraviolet spectrum .

[0036] Measured results: the hydrogenation degree is 84%; the catalyst r...

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PUM

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Abstract

The invention provides a method for preparing temperature-control hydrogenation catalyst and an application in chemigum hydrogenation. The method of the invention uses a metal catalyst having a formula of MaXmLb to realize the hydrogenation of butyronitrile latex and recycle noble metal by the following technical scheme, wherein M is rhodium, X is Cl and L is phosphine compound. The technical scheme comprises the steps of: adding chemigum, solvent, catalyst and trivalence phosphine compound into a reaction device, using a hydrogen substitution system, pressurizing to 0.5 to 5 Mpa, heating to 100 to 175 DEG C, keeping temperature for 3 to 24 hours, adding polyethylene glycol and n-heptane into the resultant of reaction after finishing reaction, stirring 30 min, standing, layering, and then taking out the chemigum solution on upper layer, wherein the solution on lower layer contains the separated catalyst. The method of the invention ensures the chemigum hydrogenation catalyst having a fine temperature-control separating effect and improves the hydrogenation effect of the catalyst so the hydrogenation degree of the prepared chemigum is higher.

Description

technical field [0001] The invention belongs to the field of hydrogenation of nitrile rubber solution, and in particular relates to a method for hydrogenation of nitrile rubber by using a catalyst capable of controlling temperature changes and separating from glue. Background technique [0002] The hydrogenation of nitrile rubber is to selectively hydrogenate the butadiene chain segment, hydrogenate and saturate the double bonds on most of the butadiene chain segment, leaving only a small amount (1-5%) of 1,4 butadiene The double bond of the diene is used for cross-linking, and the CN group remains. [0003] Hydrogenated nitrile rubber not only inherits the oil resistance, solvent resistance and wear resistance of ordinary nitrile rubber, but also obtains the high temperature resistance, aging resistance, chemical medium corrosion resistance, high tensile strength and long-term compression permanent deformation bestowed by the high saturation structure. Small comprehensive ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J31/24C08F236/12C08F8/04
Inventor 岳冬梅张立群宁思敏杨守法魏新鹏
Owner BEIJING UNIV OF CHEM TECH
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