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Hydrogenation method of hydroxyl terminated butyl nitrile (HTBN)

A liquid nitrile and hydroxyl-terminated technology, which is applied in the field of hydrogenation of new polymer-hydroxyl-terminated liquid nitrile, can solve problems such as poisoning and inability to realize hydrogenation of hydroxyl-terminated liquid nitrile rubber, and achieve simple process and hydrogenation high degree of effect

Inactive Publication Date: 2010-07-28
BEIJING UNIV OF CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, due to the existence of terminal hydroxyl groups, the noble metal catalyst will be poisoned during hydrogenation, so the hydrogenation of liquid nitrile rubber with terminal hydroxyl groups cannot be realized.

Method used

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  • Hydrogenation method of hydroxyl terminated butyl nitrile (HTBN)
  • Hydrogenation method of hydroxyl terminated butyl nitrile (HTBN)

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] According to the general procedure of above-mentioned hydrogenation, 7.5g (molecular weight is 7160, and acrylonitrile mass percent content is 20%) of end-capped hydroxyl liquid nitrile copolymer is dissolved in the xylene of 50ml, adds in the hydrogenation reactor of 100ml, in Add 0.06g of triphenylphosphine rhodium chloride and 0.48g of triphenylphosphine into the reaction kettle under a nitrogen atmosphere, control the temperature at 100°C, the pressure of hydrogen at 1MPa, and the reaction time of 8 hours. The hydrogenation results are shown in Table 1 .

Embodiment 2

[0028] Change the amount of the capped hydroxyl liquid butyronitrile into 2.5g, 5g, and 10g in Example 1, and others are the same as Example 1. The results are shown in Table 2.

[0029] Table 2

[0030] The mass of capped hydroxyl liquid butyronitrile (g)

Embodiment 3

[0032] Change the amount of triphenylphosphorus rhodium chloride into 0.045g, 0.09g, and 0.12g in Example 1, and others are the same as Example 1. The results are shown in Table 3.

[0033] table 3

[0034] The mass of triphenylphosphine rhodium chloride (g)

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Abstract

The invention relates to a hydrogenation method of hydroxyl terminated butyl nitrile (HTBN), in particular to a hydrogenation method of liquid nitrile containing terminated hydroxyl. The method is characterized by comprising the following steps: reacting terminated hydroxyl and silane of an unsaturated polymer before hydrogenation to obtain an unsaturated polymer capped with tetramethylsilane, dissolving hydroxyl terminated butyl nitrile in a benzene solvent according to the mass concentration of 5-30%, adding in a hydrogenated kettle, and performing hydrogenation reaction for 2-20h, wherein the temperature is 65-165 DEG C, the pressure is 0.4-5.0 MPa, the rotation speed is 200-400r / min, and the dosage of a catalyst is 0.1-5%. The invention has the advantages that the hydrogenated polymer is a novel polymer, and the hydrogenation degree can be more than 98%.

Description

technical field [0001] The invention relates to a novel polymer-hydrogenation method for hydroxyl-terminated liquid butyronitrile, in particular to a method for selectively hydrogenating unsaturated carbon-carbon double bonds on molecular chains containing terminal hydroxyl groups in a solution method. Background technique [0002] Unsaturated polymers and unsaturated polymers containing nitrile groups (such as butadiene-acrylonitrile copolymer), because the molecular chain contains carbon-carbon unsaturated double bonds, thus affecting the heat resistance and ozone resistance of unsaturated polymers and other performance. Through catalytic hydrogenation, a saturated single bond is generated, which can not only maintain the original properties of the polymer, but also improve its heat resistance and O resistance. 3 , SO 2 And other properties, so that the polymer after hydrogenation has excellent comprehensive properties. This material is widely used in harsh conditions, ...

Claims

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Application Information

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IPC IPC(8): C08C19/38C08C19/02
Inventor 岳冬梅张立群魏新鹏杨守法梁璐余婷
Owner BEIJING UNIV OF CHEM TECH
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