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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 , complex operation, high economic cost and other problems, to achieve the effect of high conversion rate, high selectivity and fast hydrogenation speed

Active Publication Date: 2020-12-04
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

Examples

Experimental program
Comparison scheme
Effect test

preparation example Construction

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

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

[0065] Under the protection of nitrogen, dissolve the iron-containing precursor compound in ethylene glycol to obtain a transparent iron-containing solution; add sodium acetate, polyethylene glycol and sodium citrate, heat to 100-200°C, and stir for 1-3 hours; Crystallize the uniformly mixed solution at 100-200°C for 8-16 hours; wash the crystallized black solution with ethanol, and dry it in vacuum at 60-80°C for 10-20 hours to obtain Fe 3 o 4 Nanoparticles;

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

[0067] Will Fe 3 o 4 Nanoparticles are placed in dilute hydrochloric acid solution and ultrasonicated for 10-60 minutes to carry out surface acid treatment and magnetic separation of Fe 3 o 4 nanoparticles and washed with ethanol; the Fe 3 o 4 Nanoparticles are redispersed in the mixed s...

preparation example 1

[0104] First, weigh 2.70 g of FeCl in sequence 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 uniformly; 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 200mL, put it into a crystallization kettle and seal it, move it to a blast oven, and crystallize 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] Secondly, the above obtained Fe 3 o 4 Nanoparticles (0.5g) were dispersed in dilute hydrochloric acid (0.1mol / L) solution and ultrasonicated for 30min, washed with ethanol for 3 times and magnetically separated, redi...

preparation example 2

[0109] First, weigh 2.70 g of FeCl in sequence 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 uniformly; 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 200mL, put it into a crystallization kettle and seal it, move it to a blast oven, and crystallize at 200°C for 16 hours; wait for the crystallization kettle to cool to room temperature , the magnet separates Fe 3 o 4 Nanoparticles were washed several times with ethanol, moved to a vacuum oven, and dried at 60°C for 12 hours; secondly, the Fe obtained above 3 o 4Nanoparticles (0.5g), dispersed in dilute hydrochloric acid (0.1mol / L) solution and sonicated for 30min, washed with ethanol for 3 times and magnetically separated, redispersed into a mixture ...

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Abstract

The invention relates to the field of catalyst preparation, and discloses a magnetic core-shell hydrogenation catalyst and a method for preparing 2, 2, 4, 4-tetramethyl-1,3-cyclobutanediol, the catalyst is represented as Fe3O4 (at) S / M; wherein Fe3O4 is a core layer, S is a shell layer carrier, and M is a main active metal and / or an auxiliary metal loaded on the shell layer carrier; the active metal is one or more of Ru, Ni, Ir, Pd and Pt, and the loading capacity is 1-50 wt% of the catalyst; wherein the auxiliary metal is one or more of Cu, Fe, Co, Zn and Sn, and the molar ratio of the auxiliary metal to the main active metal is 0.1-10: 1. The catalyst has the following advantages: 1, the hydrogenation speed is high; (2) the catalyst has high conversion rate on raw materials and high selectivity on target products; (3) strong magnetism is achieved, rapid magnetic separation can be achieved, and filtering separation is not needed;.

Description

technical field [0001] The invention relates to the field of catalyst preparation, in particular to a magnetic core-shell 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 the 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 polyester materials, but also does not need to add Toxic substances, green and environmental protection hav...

Claims

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Application Information

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IPC IPC(8): B01J23/89B01J31/22B01J31/28B01J35/00C07C29/145C07C33/04
CPCB01J23/8906B01J31/1691B01J31/28C07C29/145C07C2601/04B01J2231/643B01J35/397B01J35/393B01J35/33C07C35/045Y02P20/52
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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