Method for preparing bisphenol F by adopting polyoxymethylene dimethyl ethers as raw material

A technology of dimethyl ether and paraformaldehyde, applied in chemical instruments and methods, preparation of organic compounds, production of bulk chemicals, etc., can solve the impact of unseen yield and selectivity reports, heat transfer and mass transfer , limit further use and other issues, to achieve high yield, easy control, high selectivity effect

Active Publication Date: 2015-12-16
SHEYANG RES INST OF NANJING UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

In this patent, when the author mentions the source of formaldehyde, he introduces that in addition to 37% formaldehyde aqueous solution and paraformaldehyde, paraformaldehyde can also be used, but the inventor did not make further explanations on the process, nor did he see any specific results. Rate and Selective Reporting
[0006] Paraformaldehyde or paraformaldehyde is used as a raw material, and its disadvantage i

Method used

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  • Method for preparing bisphenol F by adopting polyoxymethylene dimethyl ethers as raw material
  • Method for preparing bisphenol F by adopting polyoxymethylene dimethyl ethers as raw material
  • Method for preparing bisphenol F by adopting polyoxymethylene dimethyl ethers as raw material

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Embodiment 1

[0032] Add phenol (the mol ratio of phenol and paraformaldehyde dimethyl ether is 15:1), phosphoric acid (the mol ratio of phosphoric acid and paraformaldehyde dimethyl ether is 6.4:1) and Water (the molar ratio of water and paraformaldehyde dimethyl ether is 14:1), the water bath is slowly heated to 80 ° C, and then slowly add 5 grams of paraformaldehyde dimethyl ether dropwise therein, and the temperature is controlled at 75 Between ℃-85℃. After dropping, keep the temperature at 80°C and continue the reaction for 4h. After the reaction of the raw materials is completed, the temperature is naturally lowered to 45°C, the reaction solution is poured into a separatory funnel, allowed to stand for stratification, and the phosphoric acid aqueous solution in the lower layer is recovered and used mechanically. The upper organic phase was neutralized by alkali, then concentrated under reduced pressure, and the excess phenol was recovered and used mechanically. The concentrated solu...

Embodiment 2

[0036] Add 90 grams of phenol (phenol and PODE 2 The molar ratio of 20.3:1), 6 grams of water (water and PODE 2 The mol ratio is 7.1:1) and 15 grams of solid acid catalyst (I, catalyst and PODE 2 The mass ratio of the water bath is 3:1), the water bath is slowly heated to 85 °C, and then 5 grams of PODE is slowly added dropwise to it 2 , Control the temperature at around 85°C during the dropwise addition. After dropping, keep the temperature at 85°C and continue the reaction for 16h. After the reaction of the raw materials is completed, the temperature is naturally lowered to 45° C., suction filtered, the solid acid catalyst in the upper layer is recovered and used mechanically, the filtrate in the lower layer is concentrated under reduced pressure, and excess phenol is recovered and used mechanically. The concentrated solution was diluted with ethyl acetate, washed with saturated ammonium chloride aqueous solution and water successively, dried over anhydrous sodium sulfate...

Embodiment 3

[0045] Add 26 grams of phenol (phenol and PODE 2 The molar ratio of 5.87:1), 6 grams of water (water and PODE 2 The molar ratio is 7.1:1) and 1.2 grams of solid acid catalyst (II, catalyst and PODE 2 The mass ratio is 0.24:1), the water bath is slowly heated to 80°C, and then 5 grams of PODE is slowly added dropwise to it 2 , Control the temperature at around 80°C during the dropwise addition. After dropping, keep the temperature at 80°C and continue the reaction for 4h. After the reaction of the raw materials is completed, the temperature is naturally lowered to 45° C., suction filtered, the solid acid catalyst in the upper layer is recovered and used mechanically, the filtrate in the lower layer is concentrated under reduced pressure, and excess phenol is recovered and used mechanically. The concentrated solution was diluted with anhydrous ether, washed with saturated ammonium chloride aqueous solution and water successively, dried over anhydrous sodium sulfate, filtered ...

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Abstract

The invention relates to a method for preparing bisphenol F by adopting polyoxymethylene dimethyl ethers (PODEn; n is larger than or equal to 2 and smaller than or equal to 8) as a raw material. The method comprises the main step of carrying out a hydroxyl alkylation reaction between phenyl hydroxide and PODEn under the condition of acid catalysis, so as to obtain a target product, wherein the hydroxyl alkylation reaction can be performed in the absence of water or in the presence of water. The method has the advantages that the solubility of PODEn in phenyl hydroxide and water is high, so that a bisphenol F synthesis system serves as a homogeneous-phase system, and is conducive to heat and mass transfer; besides, PODEn has an effect of quantitatively and slowly releasing formaldehyde, so that the hydroxyl alkylation reaction is mild and easy to control, side reactions are less, such by-products as triphenol and phenolic resin are unlikely to generate, and the advantages of high yield and selectivity are achieved.

Description

technical field [0001] The invention belongs to the field of chemical synthesis, in particular to the field of methods for preparing bisphenol F. Background technique [0002] Bisphenol F is an important chemical intermediate, which can be used in epoxy resin, polycarbonate and other fields. Its chemical name is dihydroxydiphenylmethane, which consists of 4,4-dihydroxydiphenylmethane (4,4-Isomer), 2,4-dihydroxydiphenylmethane (2,4-Isomer) and 2, 2-Dihydroxydiphenylmethane (2,2-Isomer) consists of three isomers. Bisphenol F is generally obtained by hydroxyalkylation reaction of phenol and formaldehyde monomer under acid catalysis. Among them, the source of formaldehyde monomer mainly includes the following four aspects: aqueous formaldehyde solution, paraformaldehyde, paraformaldehyde and methylal. Industrially, formaldehyde solution is used as the starting material to synthesize bisphenol F. There are many patents and professional papers on this route (USPatent2,792,429,...

Claims

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Application Information

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IPC IPC(8): C07C37/11C07C39/16
CPCY02P20/52C07C37/115
Inventor 王辉沈俭一赵宇培朱健汪洋
Owner SHEYANG RES INST OF NANJING UNIV
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