Magnetic core-shell hydrogenation catalyst and method for preparing 2,2,4,4-tetramethyl-1,3-cyclobutanediol

A hydrogenation catalyst, cyclobutanediol technology, applied in the direction of organic compound/hydride/coordination complex catalyst, metal/metal oxide/metal hydroxide catalyst, chemical instruments and methods, etc., can solve the loss of CBDO , high economic cost, complicated operation and other problems, to achieve the effect of fast magnetic separation, fast hydrogenation speed and high conversion rate

Active Publication Date: 2022-07-08
ZHEJIANG HENGYI PETROCHEMICAL RES INST CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the melting point of CBDO is 126-129°C, and CBDO is extremely easy to crystallize at room temperature, so hot filtration must be used, but this process is complicated to operate, high in economic costs, and inevitably leads to loss of CBDO and waste of catalysts
If larger particle catalysts or shaped catalysts are used, the hydrogenation activity of CBDK will be greatly reduced, and the selectivity of CBDO will decrease.

Method used

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  • Magnetic core-shell hydrogenation catalyst and method for preparing 2,2,4,4-tetramethyl-1,3-cyclobutanediol
  • Magnetic core-shell hydrogenation catalyst and method for preparing 2,2,4,4-tetramethyl-1,3-cyclobutanediol
  • Magnetic core-shell hydrogenation catalyst and method for preparing 2,2,4,4-tetramethyl-1,3-cyclobutanediol

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preparation example Construction

[0063] In a second aspect, the present invention provides a preparation method of the above-mentioned catalyst, the steps comprising:

[0064] a) Fe 3 O 4 Preparation of nanoparticles

[0065] Under nitrogen protection, the iron-containing precursor compound was dissolved in ethylene glycol to obtain a transparent iron-containing solution; sodium acetate, polyethylene glycol and sodium citrate were added and heated to 100-200 °C, and stirred for 1-3 h; Crystallize the uniformly mixed solution at 100-200°C for 8-16h; wash the crystallized black solution with ethanol, and vacuum dry at 60-80°C for 10-20h to obtain Fe 3 O 4 Nanoparticles;

[0066] b) Fe 3 O 4 Preparation of @S

[0067] will Fe 3 O 4 Nanoparticles were placed in dilute hydrochloric acid solution and ultrasonicated for 10-60min, surface acid treatment was performed, and Fe was magnetically separated. 3 O 4 nanoparticles and washed with ethanol; Fe 3 O 4 The nanoparticles are re-dispersed in the mixed s...

preparation example 1

[0104] First, 2.70 g of FeCl were weighed sequentially with an electronic balance. 3 ·6H 2 O, 7.67g of sodium acetate, 2.10g of polyethylene glycol and 0.80g of sodium citrate were dissolved in 150mL of ethylene glycol, and mixed well; the above mixed solution was heated to 170 ° C and mechanically stirred for 1 hour to obtain a uniform black color solution; put the above solution into a polytetrafluoroethylene liner with a volume of 200 mL, put it into a crystallization kettle and seal it, move it to a blast oven, and crystallize it at 200 ° C for 16 hours; wait for the crystallization kettle to cool to room temperature , the magnet separates Fe 3 O 4 Nanoparticles, washed several times with ethanol, moved to a vacuum drying oven, and dried at 60 °C for 12 hours;

[0105] Next, the Fe obtained above was 3 O 4 Nanoparticles (0.5g), dispersed in dilute hydrochloric acid (0.1mol / L) solution and ultrasonicated for 30min, washed with ethanol for 3 times and magnetically separ...

preparation example 2

[0109] First, 2.70 g of FeCl were weighed sequentially with an electronic balance. 3 ·6H 2 O, 7.67g of sodium acetate, 2.10g of polyethylene glycol and 0.80g of sodium citrate were dissolved in 150mL of ethylene glycol, and mixed well; the above mixed solution was heated to 170 ° C and mechanically stirred for 1 hour to obtain a uniform black color solution; put the above solution into a polytetrafluoroethylene liner with a volume of 200 mL, put it into a crystallization kettle and seal it, move it to a blast oven, and crystallize it at 200 ° C for 16 hours; wait for the crystallization kettle to cool to room temperature , the magnet separates Fe 3 O 4 The nanoparticles were washed several times with ethanol, moved to a vacuum drying oven, and dried at 60 °C for 12 hours; 3 O 4Nanoparticles (0.5g), dispersed in dilute hydrochloric acid (0.1mol / L) solution and ultrasonicated for 30min, washed with ethanol for 3 times, magnetically separated, and redispersed in a mixture con...

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Abstract

The invention relates to the field of catalyst preparation, and the invention discloses a magnetic core-shell type hydrogenation catalyst and a method for preparing 2,2,4,4-tetramethyl-1,3-cyclobutanediol, and the catalyst is expressed as Fe 3 O 4 @S / M; where Fe 3 O 4 is the core layer, S is the shell layer carrier, M is the main active metal and / or promoter metal supported on the shell layer carrier; the active metal is one or more of Ru, Ni, Ir, Pd and Pt, The loading amount is 1-50% by weight of the catalyst; the promoter is one or more of Cu, Fe, Co, Zn and Sn, and the molar ratio of the promoter to the main active metal is 0.1-10:1. The catalyst of the invention has the following advantages: (1) fast hydrogenation rate; (2) high conversion rate of raw materials and high selectivity to target products; (3) strong magnetism, which can realize rapid magnetic separation without filtering separation.

Description

technical field [0001] The invention relates to the field of catalyst preparation, in particular to a magnetic core-shell type hydrogenation catalyst and a method for preparing 2,2,4,4-tetramethyl-1,3-cyclobutanediol. Background technique [0002] 2,2,4,4-Tetramethyl-1,3-cyclobutanediol (CBDO) is an important aliphatic diol polyester monomer, mainly used in the production of high glass transition temperature, high transparency and anti- High-impact, high-performance copolyester products to replace traditional polycarbonate (PC). In order to improve the performance of polyester, PC materials need to add toxic bisphenol A, which obviously does not meet the requirements of future green products. The high-performance polyester copolymerized by CBDO, terephthalic acid and 1,4-cyclohexanedimethanol not only improves the temperature resistance, flexibility and transparency of the polyester material, but also does not need to add Toxic substances, green environmental protection ha...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J23/89B01J31/22B01J31/28B01J35/00C07C29/145C07C33/04
CPCB01J23/8906B01J31/1691B01J31/28B01J35/006B01J35/0033B01J35/008C07C29/145C07C2601/04B01J2231/643C07C35/045Y02P20/52
Inventor 杨磊成有为时强邱敏茜易磊张新平王韩
Owner ZHEJIANG HENGYI PETROCHEMICAL RES INST CO LTD
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