Method for synthesizing bisphenol-F with catalysis of phosphotungstic acid modified short channel HPW-Zr/SBA-15 catalyst

A catalyst and short-channel technology, which is applied in the field of catalytic synthesis of bisphenol F, can solve problems such as unfavorable mass transfer and reaction, difficulty in separation and recovery, and poor thermal stability, so as to improve mass transfer and reaction efficiency, high catalytic activity, and corrosion resistance. small effect

Inactive Publication Date: 2016-05-11
XIANGTAN UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Since pure phosphotungstic acid (HPW) has problems such as low specific surface area, poor thermal stability, easy solubility in polar solvents to contaminate products, and difficulty in separation and recovery, immobilization of phosphotungstic acid can effectively increase its dispersion degree and improve catalytic efficiency, while the traditional SBA-15 molecular sieve has long pores, which is not conducive to mass transfer and reaction, so the modification makes its pores shorter to improve mass transfer and reaction efficiency

Method used

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  • Method for synthesizing bisphenol-F with catalysis of phosphotungstic acid modified short channel HPW-Zr/SBA-15 catalyst
  • Method for synthesizing bisphenol-F with catalysis of phosphotungstic acid modified short channel HPW-Zr/SBA-15 catalyst
  • Method for synthesizing bisphenol-F with catalysis of phosphotungstic acid modified short channel HPW-Zr/SBA-15 catalyst

Examples

Experimental program
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Embodiment 1

[0027] (1) Preparation of short-channel HPW-Zr / SBA-15 catalyst modified by phosphotungstic acid

[0028] Using phosphotungstic acid as the active component and zirconium oxychloride as the modifier, a short-channel HPW-Zr / SBA-15 catalyst was synthesized by one-step method: 2g polyethylene oxide-polypropylene oxide-polyethylene oxide three Add the block copolymer (P123) into a 250mL reactor, add 15g of deionized water and 60ml of 2mol / L dilute hydrochloric acid, control the reaction temperature at 40°C, stir evenly at 300rpm, slowly add 3.2g of zirconium oxychloride, stir and dissolve , then add 4.7g ethyl orthosilicate and 10mL aqueous solution dissolved with 0.7g phosphotungstic acid, keep stirring for 24h, then transfer the mixed solution into a polytetrafluoroethylene hydrothermal kettle to crystallize at 100°C for 24h, filter and wash , dried at 80°C for 8h, moved to a muffle furnace, and was calcined at 2°C / min to 550°C for 6h to prepare the short-channel HPW-Zr / SBA-15 ca...

Embodiment 2

[0037] The operation steps are the same as in Example 1, the difference is that the amount of formaldehyde is 3.24g, so that the molar ratio of phenol to formaldehyde is 25:1, the reaction time is 30min, and the yield of bisphenol F is 97.2%.

Embodiment 3

[0039] The operation steps are the same as in Example 1, the difference is that the reaction temperature is 70° C., the reaction time is 5 minutes, and the yield of bisphenol F is 41.66%.

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Abstract

The invention discloses a method for synthesizing bisphenol-F with the catalysis of phosphotungstic acid modified short channel HPW-Zr/SBA-15 catalyst. According to the method, the bisphenol-F is catalytically synthesized by taking the phosphotungstic acid modified short channel HPW-Zr/SBA-15 as a catalyst and taking phenol and formaldehyde as raw materials. The adopted catalyst is synthesized through a one step method by taking polyethylene oxide-polypropylene oxide-polyethylene oxide triblock copolymer (P123) as a template, taking tetraethylortho silicate as a silicon source, taking phosphotungstic acid as a catalyst active component, and taking zirconium oxychloride as a modifying agent, and is simple in preparation process, short in channel, favourable to improve the mass transfer and reaction efficiency, high in reaction activity, short in reaction time, high in catalytic efficiency, easy to separate, reusable, green and environment-friendly; any organic solvent is not required to be added in the reaction process.

Description

technical field [0001] The invention relates to a method for catalytically synthesizing bisphenol F, belonging to the field of organic catalytic synthesis of fine chemicals. Background technique [0002] Bisphenol F is an important chemical intermediate, which is suitable for the preparation of low-viscosity epoxy resins. Compared with bisphenol A-based epoxy resins, it has the characteristics of low viscosity and excellent workability. Bisphenol F can also be used as a modification and stabilizer of phenolic resin. The modified phenolic resin produced by bisphenol F can significantly improve the processing and mechanical properties of phenolic resin, especially beneficial to the processing of epoxy resin for large wind turbine blades Forming reduces environmental pollution and improves the processing environment. [0003] Patents JP58177928US4400554 and CN200810072071 report methods for catalytically synthesizing bisphenol F with sulfuric acid, hydrochloric acid, and phosp...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C37/20C07C39/16B01J29/03B01J35/10
CPCY02P20/52C07C37/20B01J29/0341B01J35/1061C07C39/16
Inventor 刘跃进周健李勇飞谈瑛吴志民王艳聂真何晓建李蒙骆战涛
Owner XIANGTAN UNIV
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