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Catalyst for preparing 2, 2, 4, 4-tetramethyl-1, 3-cyclobutanediol with high cis-trans ratio, device and method thereof

A technology of cyclobutanediol and tetramethyl, applied in the field of catalyst preparation, can solve the problems of many by-products and low proportion

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

[0010] In order to solve 2,2,4,4-tetramethyl-1,3-cyclobutanedione hydrogenation process, there are many by-products, cis 2,2,4,4-tetramethyl-1,3-cyclobutane The technical problem of the low proportion of diols, the invention provides a catalyst, device and method for preparing 2,2,4,4-tetramethyl-1,3-cyclobutanediol with a high cis-trans ratio, The present invention can also obtain 2,2,4,4-tetramethyl-1 with high cis-trans ratio while ensuring high yield of 2,2,4,4-tetramethyl-1,3-cyclobutanediol , 3-cyclobutanediol product

Method used

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  • Catalyst for preparing 2, 2, 4, 4-tetramethyl-1, 3-cyclobutanediol with high cis-trans ratio, device and method thereof
  • Catalyst for preparing 2, 2, 4, 4-tetramethyl-1, 3-cyclobutanediol with high cis-trans ratio, device and method thereof
  • Catalyst for preparing 2, 2, 4, 4-tetramethyl-1, 3-cyclobutanediol with high cis-trans ratio, device and method thereof

Examples

Experimental program
Comparison scheme
Effect test

preparation example 1

[0110] First, weigh 0.207g RuCl 3 The powder was dissolved in a mixed solution of 400mL of ethanol and 50mL of water. Then weigh 2.131 g of PVP solid powder and add it to the above mixed solution, stir fully for 2 hours at a stirring rate of 500 rpm / min to completely dissolve the PVP; Quickly add 80mL NaBH 4 Solution (24mmol·L -1 ), fully stirred (500rpm / min) and continued to react for 3h to obtain metal nano-Ru particle sol.

[0111] Secondly, adjust the temperature of the water bath to 40°C, add 5g γ-Al 2 o 3 Add it into the nano-Ru sol, and stir continuously for 48h; when the carrier turns black and the solution is clear, filter the solution, repeatedly suction filter, and wash with ethanol and water several times; vacuum-dry at 110°C for 12h, and then Baking for 3 hours, the heating rate is 2°C / min.

[0112] Finally, the prepared powder-supported catalyst was loaded into the die of a tablet press, and a pressure of 15 tons was set to press the catalyst powder into ta...

preparation example 2

[0114] First, weigh 0.207g RuCl 3 with 0.1785g Zn(NO 3 ) 2 ·6H 2 O powder was dissolved in a mixed solution of 400 mL of ethanol and 50 mL of water. Then weigh 2.131g of PVP solid powder and add it to the above mixed solution, fully stir for 2 hours, and the stirring rate is 500rpm / min, so that the PVP is completely dissolved;

[0115] Then, use a water bath to heat the temperature to 80°C, adjust the pH to 9-11, and quickly add 80mL of NaBH to the beaker 4 Solution (24mmol·L -1 ), fully stirred (500rpm / min) and continued to react for 3h to obtain a metal nanoparticle sol.

[0116] Secondly, adjust the temperature of the water bath to 40°C, add 5g γ-Al 2 o 3 Add it into the nano-Ru-Zn sol, and stir continuously for 48h; when the carrier turns black and the solution is clear, filter the solution, repeatedly suction filter, wash with ethanol and water several times; vacuum dry at 110°C for 12h, and Roasting at ℃ for 3h, heating rate 2℃ / min.

[0117] Finally, the prepare...

preparation example 3

[0119] First, weigh 2.45g Ni(NO 3 ) 2 ·6H 2 O powder was dissolved in a mixed solution of 400 mL of ethanol and 50 mL of water. Then weigh 2.131g of PVP solid powder and add it to the above mixed solution, fully stir for 2 hours, and the stirring rate is 500rpm / min, so that the PVP is completely dissolved;

[0120] Then, use a water bath to heat the temperature to 80 ° C, adjust the pH to 9-11, and quickly add 80 mL of NaBH to the beaker 4 Solution (24mmol·L -1 ), fully stirred (500rpm / min) and continued to react for 3h to obtain a Ni nanoparticle sol.

[0121] Secondly, the temperature of the water bath was adjusted to 40°C, and 5g of γ-Al 2 o 3 Add it into the nano-Ni sol, and stir continuously for 48 hours; when the carrier turns black and the solution is clear, filter the solution, repeatedly suction filter, and wash with ethanol and water for several times; vacuum-dry at 110°C for 12h, and then Baking for 3 hours, the heating rate is 2°C / min.

[0122] Finally, the...

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Abstract

The invention relates to the field of catalyst preparation, and discloses a catalyst for preparing 2, 2, 4, 4-tetramethyl-1, 3-cyclobutanediol with a high cis-trans ratio, and discloses a device and amethod thereof , the catalyst comprises a hydrogenation catalytic component and an isomerization catalytic component; wherein the hydrogenation catalytic component comprises a metal component and a carrier, and the main active metal is one or more of Ru, Ni, Pd and Pt; the auxiliary metal comprises one or more of Cu, Fe, Co and Zn; wherein the isomerization catalytic component comprises a metal component and a carrier, the main active metal is Ru or Ni, and the auxiliary metal comprises one or more of Cu, Fe, Co and Zn. According to the catalyst, the device and the production method disclosedby the invention, a 2, 2, 4, 4-tetramethyl-1, 3-cyclobutanedione solution can be directly used as a raw material, and the 2, 2, 4, 4-tetramethyl-1, 3-cyclobutanediol with a high cis-trans ratio can be obtained while side reactions are inhibited in a continuous hydrogenation process.

Description

technical field [0001] The invention relates to the field of catalyst preparation, in particular to a catalyst, device and method for preparing 2,2,4,4-tetramethyl-1,3-cyclobutanediol with high cis-trans ratio. 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-performance copolyester products to replace traditional Polycarbonate (PC). The molecular formula of CBDO is C 8 h 16 o 2 , has a symmetrical structure, and also has two isomers, cis and trans, as shown in the following formula. Cis CBDO is C 4 The non-planar structure of the ring (the angle between the two sides is 17.5°), the trans-CBDO is C 4 The non-planar structure of the ring. The cis-to-trans ratio of CBDO (the mass ratio of cis-CBDO to trans-CBDO) has an important impact on the subsequent copolyester process and even product performance. Traditional polyester materials often have the disadv...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/46B01J23/60B01J23/755B01J23/89B01J31/22B01J35/00C07C29/145C07C29/56C07C35/04
CPCB01J23/462B01J23/60B01J23/755B01J23/8913B01J31/1691C07C29/145C07C29/56C07B2200/09C07C2601/04B01J2231/643B01J35/393C07C35/045
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