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A kind of preparation method of o-hydroxybiphenyl

A technology of o-hydroxybiphenyl and sodium hydride, applied in the preparation of organic compounds, chemical instruments and methods, organic chemistry, etc., can solve the problems of high pressure required for the reaction, expensive metal lithium, harsh reaction conditions, etc., and achieve production Low cost, convenient operation, less side effects

Active Publication Date: 2020-06-02
中国中化股份有限公司 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The disadvantages of this method are: the dehydrogenation is carried out at a high temperature of 350°C, the reaction conditions are harsh, the equipment investment is high, and the energy consumption is large.
The disadvantages of this method are: the flash point of petroleum ether, easy to catch fire; the pressure required for the reaction is high, the requirements for equipment are high, and the investment in equipment is large
The disadvantage of this method is: the price of metal lithium is expensive, the production cost is high, and industrialization is meaningless

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Under the protection of nitrogen, add 300g of oxyfluorene to a 500ml four-necked flask, raise the temperature to 180-182°C, add 22g of sodium hydride (purity is 60%) in 10 batches under stirring, add 2.2g each time, and control the addition of sodium hydride The time is 2 hours (i.e. the condensation time). After the addition of sodium hydride is completed, the temperature is kept at 180-182°C for 6 hours. After the heat-retention reaction is completed, the temperature is lowered to 85-90°C. sodium hydride until no bubbles are produced. After the destruction of sodium hydride is completed, 200ml of water is added to extract the sodium salt in the reaction solution, and the temperature is raised to 85-90° C., and kept at this temperature for 30 minutes. After the heat preservation is finished, lower to normal temperature, remove the unreacted oxyfluorene by filtration, and wash the filter cake with 100ml of water, and obtain 166g after dehydration of the oxyfluorene filt...

Embodiment 2

[0023] Under the protection of nitrogen, add 400g of oxyfluorene to a 1000ml four-necked flask, raise the temperature to 190-192°C, add 18g of sodium hydride (purity is 60%) in 10 batches under stirring, add 1.8g each time, and control the addition of sodium hydride The time is 2 hours (i.e. the condensation time). After the addition of sodium hydride is completed, the heat preservation reaction is carried out at 190-192°C for 5 hours. After the heat preservation reaction is completed, the temperature is lowered to 85-90°C. sodium hydride until no bubbles are produced. After the destruction of sodium hydride is completed, 200ml of water is added to extract the sodium salt in the reaction solution, and the temperature is raised to 85-90° C., and kept at this temperature for 30 minutes. After the heat preservation is completed, lower to normal temperature, filter to remove unreacted oxyfluorene, and wash the filter cake with 100ml of water, and obtain 260g of oxyfluorene filter ...

Embodiment 3

[0026] Under the protection of nitrogen, add 500g of dioxyfluorene to a 1000ml four-neck flask, heat up to 160-162°C, add 24g of sodium hydride (purity is 60%) in 10 batches under stirring, add 2.4g each time, control the addition of sodium hydride The time is 2 hours (i.e. the condensation time). After the addition of sodium hydride is completed, the heat preservation reaction is carried out at 160-162°C for 7 hours. After the heat preservation reaction is completed, the temperature is lowered to 90-95°C. Unreacted sodium hydride until no bubbles are generated. After the destruction of sodium hydride is completed, 200ml of water is added to extract the sodium salt in the reaction solution, the temperature is raised to 90-95°C, and the temperature is kept at this temperature for 30 minutes. After the heat preservation is completed, lower to normal temperature, filter to remove unreacted oxyfluorene, and wash the filter cake with 100ml of water, and obtain 327g of oxyfluorene f...

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Abstract

The invention relates to a preparation method of o-hydroxydiphenyl and in particular relates to a method for preparing the o-hydroxydiphenyl by opening the ring of dibenzofuran. The preparation method comprises the following steps: performing a condensation reaction on the dibenzofuran and sodium hydride at 140-250 DEG C for 1-3 hours, and preserving heat at 140-250 DEG C for 5-7 hours; after heat preservation, destroying the non-reacting sodium hydride by use of a solvent at 85-100 DEG C, and then adding water and preserving heat at 85-100 DEG C for 1-3 hours; after the heat preservation treatment, cooling to the room temperature and filtering, standing and layering the filtrate by use of an extraction filtrate, removing the organic layer, acidifying the water layer by use of an acid and standing and layering at 50-95 DEG C, dehydrating the organic layer and performing reduced pressure distillation on the organic layer to obtain the o-hydroxydiphenyl.

Description

technical field [0001] The invention relates to a preparation method of o-hydroxybiphenyl, in particular to a method for preparing o-hydroxybiphenyl by opening the ring of oxyfluorene (disconnecting the carbon-oxygen bond). Background technique [0002] O-hydroxybiphenyl (abbreviation: OPP) is an important new fine chemical product and organic intermediate, and foreign countries began to research and produce o-hydroxybiphenyl since the 1970s. At present, the global market demand reaches 30,000 tons / year. O-hydroxybiphenyl is widely used in the synthesis of new phosphorus-containing flame retardant materials, bactericidal preservatives, printing and dyeing auxiliaries and surfactants and other fields. [0003] At present, the cyclohexanone method is mainly used to prepare o-hydroxybiphenyl at home and abroad, that is, cyclohexanone is used as raw material, and the dimer is obtained by condensation and dehydration under acid catalysis, and the dimer is dehydrogenated under th...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C39/15C07C37/00
CPCC07C37/055C07C37/72C07C37/74C07C39/15
Inventor 尹永波孙朝辉郭林宋丽凤唐勇
Owner 中国中化股份有限公司
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