Preparation of novel hydrogenation catalyst

A hydrogenation catalyst, a new type of technology, used in the preparation and application of catalytic materials, can solve the problems of harsh reaction conditions, failure to meet market demand, and limit industrial applications, and achieve excellent performance, excellent hydrogenation effect, and simple and effective preparation methods Effect

Inactive Publication Date: 2014-12-24
BEIJING UNIV OF CHEM TECH
View PDF3 Cites 4 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In 2011, my country's SEBS consumption was 261,000 tons, while only Baling Petrochemical in China has a SEBS pilot plant with an annual output of 20,000 tons, which is far from meeting market demand
In 2009, Finke's research group prepared a new homogeneous hydrogenation catalyst [(1,5-COD)Ir(μ-O 2 C 8 h 15 )] 2 , Co (neoclecanoate) 2 and Ni(2-ethylhexanoate) 2 +AlEt 3 For copolymer hydrogenation, the best process conditions: room temperature, N 2 Protection, Al / Ir=1, Al / Ni=2, Al / Co=2-4, for Co system, the water in the solvent will reduce the hydrogenation activity
Due to the low hydrogenation performance and harsh reaction conditions of Ziegler-Natta catalysts, their industrial applications are also limited.

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • Preparation of novel hydrogenation catalyst
  • Preparation of novel hydrogenation catalyst
  • Preparation of novel hydrogenation catalyst

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] Step 1, the preparation of titanocene dichloride:

[0033] N 2 Under protection, the method of two-stage distillation is adopted, and 25g of dicyclopentadiene is added to the three-necked flask, and the temperature is slowly raised to 190°C at a rate of 5°C / min. In the flask, the temperature of the second stage was raised to 50°C, and the distilled components were collected under ice bath to obtain 17.7g of cyclopentadiene; 5ml of TiCl 4 The solution was added to a three-necked flask in an ice bath, and 70ml of THF was added dropwise to the TiCl with a dropping funnel. 4 During the process, a yellow precipitate was formed, and the precipitate was slowly dissolved by continuing dropwise addition. Add 20ml of anhydrous diethylamine after the dropwise addition and stir for a certain period of time, the solution turns gray-green, then freshly distill 20ml of cyclopentadiene solution, the solution color turns brownish red. The temperature was raised to 60°C, refluxed for ...

Embodiment 2

[0043] Step 1, the preparation of titanocene dichloride:

[0044] N 2 Adopt the method of two-stage distillation under protection, add 30g of dicyclopentadiene into the three-necked flask, slowly raise the temperature to 200°C, the heating rate is 10°C / min, and collect the distillate in the second-stage distillation under normal pressure In the flask, the temperature of the second stage was raised to 70°C, and the distilled components were collected under ice bath to obtain 20 g of cyclopentadiene; 15 ml of TiCl 4 The solution was added to a three-necked flask in an ice bath, and 100ml of THF was added dropwise to TiCl with a dropping funnel. 4 During the process, a yellow precipitate was formed, and the precipitate was slowly dissolved by continuing dropwise addition. Add 50ml of anhydrous diethylamine after the dropwise addition and stir for a certain period of time, the solution turns gray-green, then add 50ml of the cyclopentadiene solution of step (1), and the solution ...

Embodiment 3

[0054] Step 1, the preparation of titanocene dichloride:

[0055] N 2 Adopt the method of two-stage distillation under protection, add 50g of dicyclopentadiene into the three-necked flask, slowly raise the temperature to 220°C, the heating rate is 15°C / min, and collect the distillate in the second-stage distillation under normal pressure In the flask, the temperature of the second stage was raised to 60°C, and the distilled components were collected under ice bath to obtain 35.8g of cyclopentadiene; 20ml of TiCl 4 The solution was added to a three-necked flask in an ice bath, and 80ml of THF was added dropwise to the TiCl with a dropping funnel. 4 During the process, a yellow precipitate was formed, and the precipitate was slowly dissolved by continuing dropwise addition. Add 70ml of anhydrous diethylamine after the dropwise addition and stir for a certain period of time, the solution turns gray-green, then add 70ml of the cyclopentadiene solution of step (1), and the soluti...

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to view more

PUM

No PUM Login to view more

Abstract

The invention relates to preparation of a novel hydrogenation catalyst. The invention is characterized in that a two-stage distillation method is employed to prepare titanocene Cp2TiCl2, then a simple method is taken to prepare the lithium salt complex LiN(2, 6-Me2C6H3)(Me), the two prepared compounds are utilized to prepare the target product Cp2TiCl[N(2, 6-Me2C6H3)(CH3)] in an ether solution. The catalyst shows excellent hydrogenation performance in SBS hydrogenation, does not need to be removed after reaction, and has no influence to the chemical properties of the product SEBS. The novel hydrogenation catalyst has wide application prospects in the field of polymer hydrogenation.

Description

technical field [0001] The invention relates to the preparation of a novel hydrogenation catalyst, which belongs to the field of preparation and application of catalytic materials. Background technique [0002] SEBS copolymer does not contain unsaturated bonds, has stable physical and chemical properties, has the advantages of high temperature resistance, corrosion resistance, oxidation resistance, etc., and is widely used in industry and life: auto parts, wire and cable sheathing, medical treatment, copolymer additives Wait. In 2011, my country's SEBS consumption was 261,000 tons, while only Baling Petrochemical in China has a SEBS pilot plant with an annual output of 20,000 tons, which is far from meeting market demand. [0003] The key to preparing SEBS by hydrogenation of SBS is the catalyst. The earliest hydrogenation catalysts used were heterogeneous catalysts, and Chang’s group used Pd(CH 3 COO) 2 load to Al 2 o 3 The hydrogenation catalyst is prepared on the ca...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to view more

Application Information

Patent Timeline
no application Login to view more
Patent Type & Authority Applications(China)
IPC IPC(8): B01J31/22C08F8/04C08F297/00
Inventor 刘洪涛刘松松徐春艳刘媛
Owner BEIJING UNIV OF CHEM TECH
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Try Eureka
PatSnap group products