Method for catalyzed synthesis of bisphenol F by using modified hydroxyapatite

A hydroxyapatite modification technology, applied in chemical instruments and methods, preparation of organic compounds, catalyst activation/preparation, etc., can solve the problems of difficult catalyst separation, low yield and selectivity, and low reuse rate , to achieve product separation and follow-up processing convenience, to achieve industrial scale production, and to facilitate industrial scale production

Inactive Publication Date: 2014-05-07
XIANGTAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] The currently reported methods for synthesizing bisphenol F generally have problems such as high phenol-formaldehyde ratio, low yield and selectivity, many by-products, long reaction time, strong...

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] (1) Preparation of modified hydroxyapatite catalyst

[0020] Weigh 49.56g of calcium nitrate tetrahydrate and 14.26g of ammonium dihydrogen phosphate respectively, prepare calcium nitrate solution and ammonium dihydrogen phosphate solution with deionized water, and then adjust the ammonium dihydrogen phosphate solution to pH ≈ 10 with ammonia water, at 80°C Under the state of constant temperature stirring, slowly add the ammonium dihydrogen phosphate solution to the calcium nitrate solution dropwise, after the dropwise addition, adjust the pH of the system to about 10 with ammonia water, continue to stir at a constant temperature for 24 hours, then age for a period of time, and filter the precipitate Separate, wash with deionized water and ethanol for 3 to 4 times, dry, grind, and then roast at 600°C for about two hours to obtain hydroxyapatite.

[0021] A certain amount of hydroxyapatite was pretreated by drying at 120°C for 24h, then added to 6mmol / L pyrophosphate ace...

Embodiment 2

[0025] The operation steps are the same as in Example 1, except that the catalyst consumption is changed to 1g. Calculated by high performance liquid chromatography, the yield of bisphenol F is 33.4%, and the selectivity of bisphenol F is 92.8%.

Embodiment 3

[0027] The operation steps are the same as those in Example 1, except that the ratio of modifier aluminum trichloride to hydroxyapatite is 3 mmol / g, the reaction temperature is 80° C., and the reaction time is 3 hours. Calculated by high performance liquid chromatography, the yield of bisphenol F is 62.7%, and the selectivity of bisphenol F is 91.4%.

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Abstract

The invention discloses a method for the catalyzed synthesis of bisphenol F by using modified hydroxyapatite. The method is implemented by taking phenol and formaldehyde as raw materials and taking modified hydroxyapatite as a catalyst through a step of carrying out a condensation reaction on the raw materials and the catalyst so as to obtain bisphenol F. The adopted catalyst is prepared by carrying out load modification by taking hydroxyapatite subjected to preliminary pretreatment as a carrier and taking any one or more of aluminium chloride, zinc chloride, copper chloride, titanium tetrachloride or ferric chloride as modifiers. The adopted catalyst is cheap and easy to obtain, the catalyst is good in dispersibility, high in catalytic efficiency, easy to separate and reusable in the reaction, and overcomes the defects of too high by-products, strong corrosivity, and the like in the process of synthesizing bisphenol F by using other catalysts; and in the process of reaction, other organic solvents are not required to be added, therefore, the method conforms to the principle of green economy.

Description

technical field [0001] The invention relates to a preparation method of bisphenol F. Background technique [0002] Bisphenol F, whose chemical name is dihydroxydiphenylmethane, is suitable for the preparation of low-viscosity epoxy resin due to its chemical structure. All are better than bisphenol A epoxy resin, especially because it is easy to flow in injection molding and can add less or even no diluent. It is especially suitable for the processing and molding of epoxy resin for large wind turbine blades. processing environment. [0003] The reported prior art is to use phenol and formaldehyde as raw materials to catalyze the synthesis of bisphenol F. The difference lies in the difference of the catalysts used. Generally, there are inorganic acids, organic acids, molecular sieves, ion exchange resins, ionic liquids and heteropolyacids. catalytic method. [0004] Patent US4400554 reports a synthesis method using phosphoric acid as a catalyst, the phenol-formaldehyde rati...

Claims

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Application Information

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IPC IPC(8): C07C39/16C07C37/20B01J27/18B01J27/185
CPCY02P20/52C07C37/20B01J27/16B01J27/1808B01J27/1817B01J27/1853B01J37/24
Inventor 刘跃进董劲李勇飞吴志民谈瑛夏迪严家其
Owner XIANGTAN UNIV
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