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Hydrogenation method for activation of hydroxy-terminated butyronitrile catalyst

A liquid nitrile and terminal hydroxyl technology, which is applied in chemical instruments and methods, physical/chemical process catalysts, organic compound/hydride/coordination complex catalysts, etc. Liquid nitrile application fields, adding process steps, etc.

Active Publication Date: 2013-02-06
BEIJING UNIV OF CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The advantage of this method is that the hydrogenation of the hydroxyl-terminated liquid butyronitrile is realized through the capping technology. The disadvantage is that the terminal hydroxyl group needs to be capped before hydrogenation, and the capped product needs to be unblocked by hydroxyl reduction after hydrogenation. terminal measures
This not only increases the very cumbersome process steps and high cost, and the end-capping agent is not easy to remove, which has a very significant negative impact on the catalytic activity of the catalyst, but also greatly limits the application field of hydroxyl-terminated liquid butyronitrile
At present, no reports have been found to point out that the hydrogenation method of the hydroxyl-terminated liquid butyronitrile without any end-capping protection treatment can be directly adopted

Method used

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  • Hydrogenation method for activation of hydroxy-terminated butyronitrile catalyst
  • Hydrogenation method for activation of hydroxy-terminated butyronitrile catalyst
  • Hydrogenation method for activation of hydroxy-terminated butyronitrile catalyst

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1-1

[0026] According to the above-mentioned general hydrogenation procedure, using hexamethyldiazide-capped liquid hydroxyl-terminated liquid butyronitrile (referred to as P-HTBN) as raw material, measure 150ML of hydroxyl-terminated liquid butyronitrile-butyronitrile xylene solution with a concentration of 16.7%, Put into a 0.5L reactor, catalyst rhodium chloride trihydrate 0.026g, cocatalyst methanol 10ml, control reaction temperature to 95°C, hydrogen pressure 3MPa, react for 6 hours, the results are shown in Table 1.

Embodiment 1-2

[0028] The raw material in Example 1-1 was changed to hydroxyl-terminated liquid butyronitrile (HTBN for short) without any capping and protection treatment, and other conditions were the same as in Example 1-1. The results are shown in Table 1.

[0029] Table 1 Comparison of hydrogenation degree between P-HTBN and HTBN (with co-catalyst)

[0030]

[0031] The above examples show that the hydrogenation activity of P-HTBN is not much different from that of HTBN when the co-catalyst is added, and the addition of the co-catalyst has a significant activation effect on the catalyst.

Embodiment 2

[0041] Change the methanol in Example 1-1 to ethanol, isopropanol and acetone, and other results are the same as in Example 1-1, and the results are shown in Table 3.

[0042] Table 3 Effect of cocatalyst type on degree of hydrogenation

[0043]

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Abstract

A hydrogenation method for activation of a hydroxy-terminated butyronitrile catalyst belongs to the field of hydrogenation catalysis. Raw hydrogenation materials adopted by the method comprise liquid hydroxy-terminated butyronitrile without any termination protection treatment and liquid hydroxy-terminated butyronitrile using hexamethyldisilazane for termination protection treatment. An activation method of the catalyst mainly comprises the steps of adding organic compounds such as alcohol and ketone as promotors and conducting selective hydrogenation on unsaturated double bonds of a polymer at 80-100 DEG C and 0-5 MPa for 2-12 h. According to the hydrogenation method, few organic compounds such as the alcohol and the ketone are used as the promotors, so that the reactivity of the catalyst is improved effectively, and the hydrogenation degree is increased greatly. In addition, the catalyst consumption required for reaching the same hydrogenation degree is reduced greatly, and the cost is saved significantly. According to the hydrogenation method, the high hydrogenation degree of the liquid hydroxy-terminated butyronitrile without any pretreatment is achieved for the first time, which cannot be achieved by other catalyst systems at present.

Description

technical field [0001] The invention relates to a hydrogenation method activated by a hydroxyl-terminated liquid butyronitrile catalyst, which is mainly used in the field of selective hydrogenation of carbon-carbon double bonds in molecular chains. Especially for hydroxyl-terminated liquid butyronitrile without any end-blocking protection treatment, the method involved in the present invention has very high hydrogenation activity, which is beyond the reach of other existing hydrogenation catalytic systems. Background technique [0002] Hydroxyl-terminated liquid butyronitrile is a telechelic polymer with butadiene and acrylonitrile as the main link, and hydroxyl groups at both ends of the molecular chain. It is a light yellow transparent liquid at room temperature, with a molecular weight between 2000-10000, referred to as HTBN . Hydroxyl-terminated liquid butyronitrile is a polymer with excellent performance, and its oil resistance and corrosion resistance are good. Due t...

Claims

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Application Information

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IPC IPC(8): C08C19/38C08C19/02B01J31/30
Inventor 岳冬梅严勇张立群李永鑫梁璐
Owner BEIJING UNIV OF CHEM TECH
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