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A kind of method that phosphotungstic acid modified metal-organic framework catalyzes the synthesis of bisphenol-F

A metal-organic framework, phosphotungstic acid technology, applied in the preparation of organic compounds, organic chemistry, chemical instruments and methods, etc., can solve the problems of small control range, complex process, difficult recycling of phosphoric acid catalysts, etc., to achieve no corrosion of equipment , Simple preparation process, easy separation and recovery and reusable effect

Inactive Publication Date: 2016-02-03
XIANGTAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Patent JP6340565 introduces the method of synthesizing bisphenol F by co-catalyzing acid catalyst and urea-formaldehyde resin. The feature of this method is that it can improve the selectivity of 4,4′-isomer. The urea-formaldehyde resin is easy to recycle after reaction, but the resin reuse rate Low, it is difficult to achieve recycling
Patents US5654382 and WO9702306 introduced that the ratio of the three bisphenol F isomers in the appropriate range can make the performance of the bisphenol F epoxy resin better, but did not mention the influence of the catalyst on the distribution and yield of the three isomers
Patent CN102070409A introduces a two-step method for synthesizing high-ortho bisphenol F with phosphoric acid: the first step is to mix molten phenol and phosphoric acid and adjust the pH value, add formaldehyde dropwise at a controlled temperature, and the second step is to add to the reaction solution under a controlled temperature. Catalyst phosphoric acid and formaldehyde were added to the bisphenol F product to obtain 2,2'-isomer mass percentages of 10.1% to 19.6%, 2,4'-position isomer mass percentages of 43.5% to 45.4%, and 4 , the mass percentage of the 4′-position isomer is in the range of 28.3% to 38.9%, but the process is complex, the distribution control range of the three isomers of bisphenol F is small, and the phosphoric acid catalyst is difficult to recycle

Method used

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  • A kind of method that phosphotungstic acid modified metal-organic framework catalyzes the synthesis of bisphenol-F
  • A kind of method that phosphotungstic acid modified metal-organic framework catalyzes the synthesis of bisphenol-F
  • A kind of method that phosphotungstic acid modified metal-organic framework catalyzes the synthesis of bisphenol-F

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Experimental program
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Effect test

Embodiment 1

[0027] (1) Preparation of catalyst

[0028] Add 25.02g (1.39mol) of deionized water, 2.02g (5.00mmol) of ferric nitrate nonahydrate, 0.69g (0.24mol) of phosphotungstic acid, 0.71g (3.35mmol) of trimesin to a 100mL polytetrafluoroethylene liner Formic acid, stirred for 30min, heated from room temperature to 160°C, kept at 160°C for 12 hours, cooled, filtered, refluxed with 60°C 95% ethanol for 3 hours, refluxed with 70°C deionized water for 3 hours, and finally Dry at 150°C for 24 hours to obtain catalyst A.

[0029] (2) Synthesis of bisphenol F

[0030] Add 14.1g (0.15mol) of phenol and 0.3g of catalyst to a three-necked round-bottomed flask equipped with a condensing reflux tube, a thermometer and a magnetic stirrer, keep the temperature at 80°C, stir for 15min, and add 0.41g of formaldehyde aqueous solution with a mass percentage of 37% at one time (5mmol), reacted at 80°C for 4 hours, and the yield of bisphenol F was 89.26%. 33.70%, 15.11%, 51.19%.

Embodiment 2

[0032] The operation steps are the same as in Example 1, the difference is that the amount of phenol added during the synthesis of bisphenol F is 4.70 g (0.05 mol), and the yield of bisphenol F is 33.44%, wherein 2,4'-, 4,4'-, 2 , The mass percentages of the three isomers at the 2'-position are 50.36%, 18.56%, and 31.08%, respectively.

Embodiment 3

[0034] The operation steps are the same as in Example 1, the difference is that the amount of catalyst A added during the synthesis of bisphenol F is 0.03 g, and the yield of bisphenol F is 49.14%, wherein 2,4'-, 4,4'-, 2,2' The mass percentages of the three isomers at the -position are 48.19%, 19.81%, and 32.00%, respectively.

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Abstract

The invention discloses a method for synthesizing bisphenol F from phenol and formaldehyde with a phosphotungstic acid modified metal organic frame catalyst. In the method, through selection of different metal source and modification amount of phosphotungstic acid, the phosphotungstic acid modified metal organic frame catalyst is prepared in a one-step manner. The catalyst is simple in preparation method, is convenient to separate and recycle and can be reused and is free of corrosion to devices. When being used for catalyzing the phenol and the formaldehyde to synthesizing the bisphenol F, the catalyst can regulating distributions of three isomers of a product of the bisphenol F. The invention provides a new method for catalytically synthesizing the bisphenol F.

Description

technical field [0001] A kind of method that phosphotungstic acid modified metal-organic framework catalyzes the synthesis of bisphenol F Background technique [0002] Bisphenol F, also known as dihydroxydiphenylmethane, has three isomers of 2,2'-, 2,4'- and 4,4'-dihydroxydiphenylmethane, which can be used to prepare low Viscosity modifier for epoxy and phenolic resins. Due to its chemical structure characteristics, the performance of the finished epoxy resin synthesized with bisphenol F is better than that of bisphenol A in many aspects, especially its characteristics of easy injection and casting flow, and can add less or even no diluent, which is especially suitable for The processing and molding of epoxy resin for large wind power blades also greatly reduces environmental pollution and improves the processing environment. [0003] Few of the reported methods for the synthesis of bisphenol F involve the distribution of bisphenol F isomers. Patent JP6340565 introduces t...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C39/16C07C37/20B01J31/22
CPCB01J31/1691B01J2231/347C07C37/20C07C39/16
Inventor 刘跃进严家其李勇飞吴志民谈瑛陈蒙潘浪胜
Owner XIANGTAN UNIV
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