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Preparation method of fluorene-containing framework aromatic ether type compound

The technology of compound and fluorene skeleton is applied in the field of preparation of aryl ether compounds containing fluorene skeleton, and can solve the problems of unreusable catalyst, existence of waste water and waste residue and high production cost, and achieve the effects of simple operation, reducing pollution and improving production efficiency.

Pending Publication Date: 2018-11-23
HUANGHUA XINNUOLIXING FINE CHEM +2
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0007] In view of the technical defects in the prior art that the catalyst cannot be reused, there is waste water and waste residue, the environment is polluted, resources are wasted, and the production cost is high, the present invention provides a solid composite superacid catalyst for the preparation of aromatic ether compounds containing a fluorene skeleton. application in

Method used

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  • Preparation method of fluorene-containing framework aromatic ether type compound
  • Preparation method of fluorene-containing framework aromatic ether type compound
  • Preparation method of fluorene-containing framework aromatic ether type compound

Examples

Experimental program
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Embodiment 1

[0032] 3.6g 9-fluorenone, 11.3g phenoxyethanol, 3.5g loaded SO 4 2- / ZrO 2 -Fe 2 o 3 -SiO 2 Solid composite superacid catalyst, 0.3g 3-mercaptopropionic acid, and 30g chlorobenzene were successively added to a three-necked flask equipped with a stirrer, a thermometer, and a condenser; the stirring was started, heated to reflux (130° C.) and water separation, React for 6 hours, filter while hot after the reaction, and recover the solid composite superacid of the filter residue for the next reaction, distill the filtrate to get phenoxyethanol and chlorobenzene for recycling, add ethanol to cool down to 10°C, keep warm for 0.5 hours, and then filter with suction The gray crude product was obtained, and the obtained crude product was recrystallized with toluene-ethanol (volume ratio 3 to 1), dried after filtration, and obtained 7.9 g of white solid 9,9-bis[4-(2-hydroxyethoxy)phenyl] Fluorene, the yield is 90.2%, the measured melting point is 163-165°C, and the HPLC purity is ...

Embodiment 2

[0034] In a three-necked flask equipped with a stirrer, a thermometer and a condenser, add 3.6g 9-fluorenone, 6.3g phenoxyethanol, 0.3g 3-mercaptopropionic acid, the load SO recovered in Example 1 successively. 4 2- / ZrO 2 -Fe 2 o 3 -SiO 2 Solid composite superacid catalyst (used after 115°C activation for 2 hours) and reclaimed phenoxyethanol and chlorobenzene solution; the operation is the same as in Example 1 to obtain 8.1g of white solid 9,9-bis[4-(2-hydroxyethyl Oxygen)phenyl]fluorene, the yield is 92.5%, the measured melting point is 163.2-164.8°C, and the HPLC purity is 99.5%.

Embodiment 3

[0036] The operation is the same as in Example 2, adding 3.6g 9-fluorenone, 6.5g phenoxyethanol, 0.3g 3-mercaptopropionic acid, and recovering 4 times of loaded SO 4 2- / ZrO 2 -Fe 2 o 3 -SiO 2 Solid composite superacid catalyst (used after being activated for 2 hours at 115°C) and phenoxyethanol and chlorobenzene solutions recovered 4 times; 7.8 g of white solid 9,9-bis[4-(2-hydroxyethoxy)phenyl was obtained ] fluorene, the yield is 89.0%, the measured melting point is 163.4-165.2° C., and the HPLC purity is 99.3%.

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Abstract

The invention relates to a preparation method of a fluorene-containing framework aromatic ether type compound. The method is characterized in that a substituted 9-fluorenone type derivative and a substituted aromatic ether type or substituted aryloxy alcohol type compound are used as raw materials; through the catalytic reaction of SO4<2-> loaded solid composite super acidic catalysts, crude products in the fluorene-containing framework aromatic ether type compound are obtained; after the purification, the fluorene-containing framework aromatic ether type compound product is obtained. The solid composite super acidic catalysts are used for replacing catalysts used in the existing process, so that the method has the advantages that the catalysts and a reaction recovery solution can be repeatedly used; the production cost is reduced; the production efficiency is improved; the environment pollution is reduced; the reaction yield is high; the operation is simple and convenient; the productcan be easily purified; the method is more suitable for sustainable industrial production and development.

Description

technical field [0001] The invention relates to the field of chemistry and chemical industry, in particular to a method for preparing aromatic ether compounds containing a fluorene skeleton. Background technique [0002] The fluorene-skeleton-containing aryl ether acrylic resin synthesized by the present invention can improve the heat resistance of the polymer because of its unique structure, and has good optical properties and formability, and it also has excellent transparency and high refractive index and Soluble and other characteristics, so it has become a raw material or improver for the synthesis of new heat-resistant polycarbonate, epoxy resin and polyester, in military, aerospace, electronics, aircraft structural materials, missile warheads, engine nozzles and housings It is widely used in the field of automobile industry, and the resulting polymer can be used as heat-resistant materials, separation membrane materials and optical materials, etc., and has attracted g...

Claims

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Application Information

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IPC IPC(8): C07C43/23C07C41/30
CPCC07C41/30C07C43/23
Inventor 关金涛闻炎豪张智勇李小勇向陆军周小野
Owner HUANGHUA XINNUOLIXING FINE CHEM