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Method for preparing bisphenol F by using 1-alkyl-3-methylimidazole acidic ionic liquid

A technology of acidic ionic liquids and methylimidazoles, applied in chemical instruments and methods, preparation of organic compounds, production of bulk chemicals, etc., can solve problems such as rapid decline in catalyst activity, impact on product scale application, and short catalyst life. To achieve the effect of avoiding difficult recycling and low utilization rate, maintaining good catalytic activity, and being easy to recycle and reuse

Inactive Publication Date: 2012-07-18
XIANGTAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] Patents JP08268943, JP08198790 and other patents report the catalytic synthesis of bisphenol F with organic acids such as oxalic acid and acetic acid, with an acid-aldehyde ratio of 5-50 and a temperature of 60-100°C. This method has a mild reaction and is less corrosive to equipment, but side reactions Many, the phenolic ratio is too high, and the yield is relatively low
[0007] Patent JP11269113 reports a method for synthesizing bisphenol F using zeolite molecular sieves as a catalyst, and patent CN101987812A discloses a method for synthesizing bisphenol F using mesoporous molecular sieves with a silicon-aluminum ratio of 60:1 to 150:1 as a catalyst. Product separation and catalyst recovery are relatively easy, but the phenol-formaldehyde ratio and reaction temperature are high, the reaction is difficult to control, and the consumption of raw materials is large
[0008] Patent JP 6340565 reported the method of synthesizing bisphenol F by co-catalyzing acid catalyst and urea-formaldehyde resin. This method is characterized in that it can improve the selectivity of 4,4'-isomers, and the urea-formaldehyde resin is easy to recycle after reaction, but the resin repeats Low utilization rate and rapid decline in activity
[0009] It has been reported that the methods of synthesizing bisphenol F always have the disadvantages of high phenol-formaldehyde ratio, low yield and selectivity, many side reactions, long reaction time, strong corrosion, fast decline in catalyst activity, and short catalyst life, which lead to the production of bisphenol F. High production cost affects the scale application of this product

Method used

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  • Method for preparing bisphenol F by using 1-alkyl-3-methylimidazole acidic ionic liquid

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Experimental program
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Effect test

Embodiment 1

[0022] Take 0.1mol 1-alkyl-3-methylimidazole acidic ionic liquid [Hmin][HSO 4 ] and 0.6mol phenol into the three-necked flask, the temperature was raised to 90°C, and 0.1mol formaldehyde was added dropwise. And samples were taken and analyzed at 0.5h, 1h, 2h, 3h, 4h, 5h, and 6h respectively. After the reaction was finished, it was cooled, washed with water and separated into layers. The aqueous phase was dehydrated by rotary evaporation under reduced pressure, and the remaining ionic liquid was recycled; the organic phase was distilled under reduced pressure to recover phenol to obtain a crude product, which was recrystallized from xylene to obtain bisphenol F product with a yield of 70.68%.

Embodiment 2

[0024] Take 0.1mol 1-alkyl-3-methylimidazole acidic ionic liquid [Emin][HSO 4 ] and 0.7 mol of phenol were added to the three-necked flask, the temperature was raised to 80°C, and 0.1 mol of formaldehyde was added dropwise. And samples were taken and analyzed at 0.5h, 1h, 2h, 3h, 4h, 5h, and 6h respectively. After the reaction was finished, it was cooled, washed with water and separated into layers. The aqueous phase was dehydrated by rotary evaporation under reduced pressure, and the remaining ionic liquid was recycled; the organic phase was distilled under reduced pressure to recover phenol to obtain a crude product, which was recrystallized from xylene to obtain bisphenol F product with a yield of 65.53%.

Embodiment 3

[0026] Take 0.1mol 1-alkyl-3-methylimidazole acidic ionic liquid [Bmin][HSO 4 ] and 0.8mol of phenol were added to the three-necked flask, the temperature was raised to 60°C, and 0.05mol of formaldehyde was added dropwise. And samples were taken and analyzed at 0.5h, 1h, 2h, 3h, 4h, 5h, and 6h respectively. After the reaction was finished, it was cooled, washed with water and separated into layers. The aqueous phase was dehydrated by rotary evaporation under reduced pressure, and the remaining ionic liquid was recycled; the organic phase was distilled under reduced pressure to recover phenol to obtain a crude product, which was recrystallized from xylene to obtain bisphenol F product with a yield of 69.58%.

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Abstract

The invention relates to a method for preparing bisphenol F by using a 1-alkyl-3-methylimidazole acidic ionic liquid. According to the invention, phenol and formaldehyde are used as raw materials, and the 1-alkyl-3-methylimidazole acidic ionic liquid is used as a solvent and a catalyst, and bisphenol F can be prepared by condensation reaction. As for the method, other organic solvents easy to volatilize are not used, the defects that the reaction time is long, recovery is difficult, the service life is short, the corrosivity is strong and the like when the bisphenol F is subjected to catalytic synthesis by common bronsted acid can be solved, and the method provided by the invention is a novel bisphenol F preparing method which is efficient and environment-friendly.

Description

technical field [0001] The invention relates to a method for preparing bisphenol F. Background technique [0002] The chemical name of bisphenol F (BPF) is dihydroxydiphenylmethane. It is an important chemical intermediate, due to its special chemical structure characteristics, when synthesizing epoxy resin, polyester resin and as phenolic resin modifier and flame retardant, the heat resistance and moisture resistance of the obtained product, insulation Performance and processing, injection molding, burning and casting are superior to similar products made of bisphenol A as raw material. Because of the many excellent properties of its finished products, it is widely used in the synthesis of high-solid coatings, electronic grade epoxy resins, special low-viscosity resins for injection molding and casting, high-performance polyester resins and polycarbon resins, and phenolic resins Modifiers and high-performance flame retardants. [0003] Catalyst is the key condition for t...

Claims

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Application Information

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IPC IPC(8): C07C39/16C07C37/20
CPCY02P20/542Y02P20/54
Inventor 刘跃进刘杰王庆陈桂李勇飞田娟
Owner XIANGTAN UNIV
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