Catalyst, preparation method thereof, and apparatus and method for preparing 2,2,4,4-tetramethyl-1,3-cyclobutanediol

A catalyst, tetramethyl technology, applied in the field of equipment for preparing 2,2,4,4-tetramethyl-1,3-cyclobutanediol, which can solve the problem of less catalyst consumption, low production cost, easy catalyst Avoid problems such as wear and tear, and achieve the effects of reducing production costs, high conversion rate, high yield and high cis-trans isomerization molar ratio

Inactive Publication Date: 2019-08-16
ZHEJIANG HENGYI PETROCHEMICAL RES INST CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] The purpose of the present invention is to overcome the existing problems in the prior art that the catalyst used in the preparation of CBDO is easy to wear, the catalyst utilization rate is low, the conversion rate of TMCB is low, etc., to provide a catalyst and a preparation method thereof and to prepare 2,2,4,

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  • Catalyst, preparation method thereof, and apparatus and method for preparing 2,2,4,4-tetramethyl-1,3-cyclobutanediol

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preparation example Construction

[0045] The preparation method of the catalyst is not particularly limited in the present invention, as long as the catalyst of the above composition is obtained. In the present invention, the preparation method of the catalyst can be a quenching method, a chemical reduction method, a chemical deposition method, and the like. The second aspect of the present invention provides a method for preparing the above-mentioned catalyst, comprising: impregnating the carrier with a solution containing a main active metal element compound and an optional auxiliary active metal element compound, and then adding an alkali solution containing a reducing agent to adjust the pH The value is adjusted and dried; wherein, the reducing agent is a compound containing the metalloid element.

[0046] The present invention has a wide selection range for the type of the main active metal element compound, which can be any substance converted into the main active metal element in the subsequent process, ...

preparation example 1

[0109] 0.201g of NiCl 2 .6H 2 O with 0.0129g of RuCl 3 .3H 2 O and 70g of water were added into a three-necked flask and mixed, and the magnetic stirring was started at a stirring speed of 60r / min. Then, 0.425g of γ-alumina was added to the flask, and immersed at 25°C for 8h.

[0110] Add 45mL of 0.015mol / L NaOH aqueous solution into a 100mL beaker, and then add NaBH with a concentration of 1mol / L 4 Aqueous solution, stirred and mixed to obtain lye containing reducing agent, set aside for clarification.

[0111]Gradually add the lye containing the reducing agent into the three-necked flask, and at the same time place the three-necked flask in an ice bath at 0°C, and control the pH of the solution in the three-necked flask to 7.5. When no obvious bubbles are formed in the solution, wash with ultrapure water in turn The black solid was processed 5 times, and finally it was dried in a vacuum oven at 90° C. for 4 hours to obtain a catalyst, which was designated as C1.

[0112...

preparation example 2

[0115] 1.239g of Ni(NO 3 ) 2 .6H 2 O with 0.0873g of IrCl 3 .3H 2 O and 115g of water were added into a three-necked flask and mixed, and the magnetic stirring was started at a stirring speed of 90r / min. Then, 0.205g of γ-alumina was added to the flask, and immersed at 40°C for 16h.

[0116] Add 80mL of 0.017mol / L NaOH aqueous solution into a 100mL beaker, and then add NaH with a concentration of 1.2mol / L 2 PO 2 The aqueous solution is stirred and mixed to obtain a lye solution containing a reducing agent, which is left to stand for clarification.

[0117] Add the lye containing the reducing agent dropwise into the three-necked flask, and at the same time place the three-necked flask in an ice bath at 0°C, control the pH of the solution in the three-necked flask to 8, and wash it with ultrapure water in turn when no obvious bubbles are formed in the solution The black solid was obtained three times, and finally it was dried in a vacuum oven at 130° C. for 12 hours to obt...

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Abstract

The invention relates to the field of production of 2,2,4,4-tetramethyl-1,3-cyclobutanediol, and concretely relates to a catalyst, a preparation method thereof, and an apparatus and a method for preparing 2,2,4,4-tetramethyl-1,3-clobutanediol. The catalyst comprises a main active metal element, a metalloid element, a carrier and an optional coactive metal element, the main active metal element isone or more of Fe, Co and Ni, the metalloid element is B and/or P, and the coactive active metal element is one or more of Co, Ru, Pd, Rh, Ir, and Pt; and the content of the main active metal elementin the catalyst is 1-70 wt%. The catalyst, the apparatus and the preparation methods of the invention are used to realize high-efficiency conversion of ketones, improve the cis-trans isomer molar ratio of the 2,2,4,4-tetramethyl-1,3-cyclobutanediol product and reduce the wearing and consumption of the catalyst.

Description

technical field [0001] The invention relates to the production field of 2,2,4,4-tetramethyl-1,3-cyclobutanediol, in particular to a catalyst and a preparation method thereof and the preparation of 2,2,4,4-tetramethyl-1,3 - Apparatus and method for cyclobutanediol. Background technique [0002] 2,2,4,4-Tetramethyl-1,3-cyclobutanediol (CBDO) is mainly used to synthesize high-performance polyester that can replace polycarbonate (PC), and its special molecular structure makes it rigid Strong and good thermal stability advantages. Adding CBDO for copolymerization can significantly improve the glass transition temperature, weather resistance and transparency of polyester. More importantly, the synthesized copolyester does not release toxic substances such as bisphenol A. Copolyester with CBDO as raw material is an ideal substitute for PC, with better market application prospects and value. [0003] CBDO is mainly prepared by hydrogenation of 2,2,4,4-tetramethyl-1,3-cyclobutane...

Claims

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Application Information

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IPC IPC(8): B01J23/755B01J23/89B01J27/185B01J35/02B01J35/10C07C29/145C07C35/04B01J8/18B01J8/22
CPCB01J8/1809B01J8/1836B01J8/1872B01J8/228B01J23/755B01J23/892B01J27/1856B01J35/023B01J35/1019B01J35/1038B01J35/1042B01J2208/00433B01J2208/00769B01J2208/00938C07C29/145C07C2601/04C07C35/045
Inventor 时强王韩徐锦龙成有为李希
Owner ZHEJIANG HENGYI PETROCHEMICAL RES INST CO LTD
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