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Hydrogenation catalyst composition and hydrogenation method thereof

A composition and compound technology, applied in organic compound/hydride/coordination complex catalysts, chemical instruments and methods, hydrogenation to hydrocarbons, etc., can solve the problems of poor hydrogenation rate, difficult to control hydrogenation rate, difficult to store, etc. , to achieve the effect of improving hydrogenation efficiency, good stability and reproducibility, and easy storage

Active Publication Date: 2010-09-15
TSRC CORP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, because the compound has hydrogen atoms, it is easy to cause hydrolysis, and it is easy to react with oxygen atoms or strong polar functional groups, so it is not easy to store at room temperature.
In addition, from the examples of this patent, it can be seen that the maximum temperature of the hydrogenation reaction is about 60°C, and the hydrogenation reaction cannot be continuously carried out in a high temperature environment, and this catalyst combination is easily deactivated during the high temperature hydrogenation reaction, so it

Method used

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  • Hydrogenation catalyst composition and hydrogenation method thereof
  • Hydrogenation catalyst composition and hydrogenation method thereof
  • Hydrogenation catalyst composition and hydrogenation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Example Embodiment

[Example 1-Preparation of SBS copolymer]

A 10L sleeve heater with a stirrer was filled with 5400 g of cyclohexane, 7.4 mmol of n-butyl lithium and 252 mmol of tetrahydrofuran, and 96 g of styrene was added to it. The polymerization reaction is carried out at ℃. After the polymerization reaction in the reaction system, 400 grams of 1,3-butadiene was added for the reaction. After the reaction, 96 grams of styrene were added to continue the polymerization, placed in a tank sealed with nitrogen, and then repeated the same polymerization steps described above. Also placed in the same nitrogen-sealed tank, after mixing, a solid content of 9.7%, a weight average molecular weight of 230,000 SBS (styrene-butadiene-styrene) triblock copolymer solution can be obtained .

Example Embodiment

[Example 2]

Take 1000g of the polymer solution of the SBS triblock copolymer prepared in Example 1, move it to a pressure-resistant hydrogenation tank, keep it in a nitrogen environment, and prepare 0.11 mmol of bis(trimethoxysilyl)hexane at room temperature [bis(trimethoxysilyl)hexane] In 10ml of cyclohexane, pre-mix 0.11mmol of bis(trimethoxysilyl)hexane in cyclohexane solution and 0.16mmol of n-butyllithium, and 0.055mmol in a glove box The bis (cyclopentadienyl) titanium dichloride and 0.66 mmol of triisobutyl aluminum in 20 ml of cyclohexane were added to the SBS polymer prepared above, and hydrogen was blown into it to make the pressure reach 25Kg / cm 2 , Carry out hydrogenation at 100°C.

Figure 1 shows the infrared spectra of SBS polymers before and after hydrogenation. This spectrum shows that the SBS triblock copolymer is at a wavelength of 968cm before being hydrogenated. -1 And 995cm -1 The functional group of the trans double bond is found everywhere, at a wavelen...

Example Embodiment

[Example 3]

In the same way as in Example 3, 0.11mmol of bis(diethoxymethylsilyl)ethane [bis(diethoxymethylsilyl)ethane] was mixed in 10ml of cyclohexane at room temperature, and 0.055 was pre-mixed in the glove box. mmol bis(cyclopentadienyl)diphenyl titanium in 10 ml of cyclohexane, and 0.66 mmol of diisobutylaluminum hydride in 10 ml of cyclohexane, respectively add to the SBS polymer solution prepared above , Blow hydrogen into it to make the pressure reach 25Kg / cm 2 , Carry out hydrogenation at 100°C. After 1 hour, the measured hydrogenation rate reached 94.3%, and after 2 hours, the hydrogenation rate reached 98.5%. The data of the hydrogenation reaction are summarized in Table 1.

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Abstract

The invention provides a special catalyst composition of a hydrogenation conjugated diene polymer and a method for selectively hydrogenating the conjugated diene polymer by using the special catalyst composition. The method comprises the step of reacting conjugated diene polymer dissolved in an inert organic solvent with hydrogen in the presence of a hydrogenation catalyst composition to selectively hydrogenate unsaturated double bonds of conjugated diene units in the conjugated diene polymer. The hydrogenation catalyst composition comprises (a) a titanium compound, (b) a compound shown in a formula (II) and (c) an alkyl aluminum compound, wherein in the formula (II), R5 is alkyl, vinyl, amino, ether, ketone group or ester group of C1 to C12; R3 and R6 are alkyl or vinyl of C1 to C12; R4 and R7 are alkyl, vinyl, amino, ether, ketone group or ester group of C1 to C12; and n is more than or equal to 1 and less than or equal to 3, and m is more than or equal to 1 and less than or equal to 3.

Description

technical field The invention relates to a hydrogenation catalyst composition and a hydrogenation reaction method thereof, in particular to a special catalyst composition for hydrogenating conjugated diene polymers and a method for selectively hydrogenating conjugated diene polymers using the special catalyst composition. Background technique In industry, the single polymerization or copolymerization of conjugated diene monomer is usually carried out to obtain the polymer containing unsaturated ethylenic group in the polymer molecular chain. This polymer is quite favorable for vulcanization, but because of the presence of a large number of unsaturated double bonds, it will cause poor weather resistance, heat resistance, oxidation resistance and other properties. In particular, the thermoplastic rubber used for polymerization of conjugated diene and vinyl aromatic hydrocarbon (vinyl aromatic hydrocarbon) as a monomer is a polymer with physical crosslinking, and its situation ...

Claims

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Application Information

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IPC IPC(8): B01J31/14C08F136/04C08F236/10C08F8/04C07C5/03
Inventor 谢其诚蔡智光李彦贤
Owner TSRC CORP
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