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Novel supercritical phase salicylic acid synthesis process

A supercritical phase, salicylic acid technology, applied in the preparation of carboxylate, the preparation of organic compounds, the production of bulk chemicals, etc., can solve the problems of poor mass transfer and heat transfer performance, small phase contact area, and complicated process control. , to achieve the effect of lowering operating temperature, good reaction selectivity and avoiding side reactions

Inactive Publication Date: 2006-02-15
QILU UNIV OF TECH
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

There are two kinds of medium pressure methods: direct method and solvent method: the pressure in the direct method is stable at 0.7-0.8MPa, and the carboxylation is carried out at 130°C-140°C for more than 6 hours, and the yield is more than 98%. This method uses gas-solid phase Direct carboxylation process, the reaction is carried out in a heterogeneous medium, the phase contact area between the reactants is small, and the mass and heat transfer performance of the process is poor
Carbon dioxide is introduced multiple times during the reaction, the process control is complicated, the reaction time is long, the conversion rate and yield of the reaction are low, and the material is easy to solidify in the reactor
Its disadvantages are: high reaction pressure, high equipment cost, high energy consumption and low yield

Method used

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  • Novel supercritical phase salicylic acid synthesis process
  • Novel supercritical phase salicylic acid synthesis process

Examples

Experimental program
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Effect test

Embodiment 1

[0024] Accurately weigh 60.40 g (1.51 mol) of sodium hydroxide, prepare a 50% solution with distilled water, and cool. Accurately weigh 141.165 g (1.5 mol) of phenol, heat the solid phenol to a liquid state, and add the phenol liquid into the sodium hydroxide solution under stirring. After stirring the mixture for 15 minutes, heat up and distill water under reduced pressure. When the solution becomes viscous, it is transferred to a vacuum oven for the first drying under reduced pressure. Control the vacuum degree to 0.085MPa-0.095MPa, and the temperature is at 160°C-170°C. When there is less water, cool down. Take out the solid sodium phenate, grind it into a fine powder in a mortar, and then perform a second drying at a temperature of 135°C-145°C and a vacuum degree of 0.090MPa-0.095MPa. Cool down until no water comes out. Take out the solid sodium phenate and transfer it to a volume of 500ml in an autoclave equipped with electromagnetic stirring and automatic temperature ...

Embodiment 2

[0026]Accurately weigh 410.00 g (10.25 mol) of sodium hydroxide, prepare a 50% solution with distilled water, and cool. Accurately weigh 941.10 g (10.0 mol) of phenol, heat the solid phenol to a liquid state, and add the phenol liquid into the sodium hydroxide solution under stirring. After stirring the mixture for 15 minutes, heat up and distill water under reduced pressure. When the solution becomes viscous, it is transferred to a vacuum oven for the first drying under reduced pressure. Control the vacuum degree to 0.085MPa-0.095MPa, and the temperature at 160°C-170°C. When less water comes out, cool down. Take out the solid sodium phenate, grind it into a fine powder in a mortar, and then dry it for the second time at a temperature of 130°C-145°C and a vacuum of 0.090MPa-0.095MPa, and cool down until no water comes out. Take out the solid sodium phenate and transfer it to a volume of 5000ml in an autoclave equipped with electromagnetic stirring and an automatic temperatur...

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Abstract

Disclosed is a novel supercritical phase salicylic acid synthesis process, which comprises making sodium phenolate through neutralizing phenol with NaOH aqueous solution, drying and grinding to obtain solid sodium phenolate, subjecting the sodium phenolate and carbon dioxide to supercritical homogeneous phase carboxylation reaction (Kolbe-Schmitt reaction) in heavy pressure reaction kettle, obtaining sodium salicylate, acidifying to prepare the salicylic acid.

Description

Technical areas: [0001] The present invention relates to a method for synthesizing salicylic acid, specifically to a new process for synthesizing salicylic acid under supercritical conditions. Background technique: [0002] Salicylic acid is an important raw material and intermediate in the pharmaceutical industry, food industry and fine chemical industry. In the pharmaceutical industry, salicylic acid is mainly used for analgesics, diuretics, acetylsalicylic acid (aspirin), sodium salicylate, salicylamide, hypoglycemic, niclosamide, phenyl salicylate, phenyl salicylate, Production of ethyl hydroxybenzoate, bismuth subsalicylate, sulfasalazine and other drugs; salicylic acid itself is also used as a disinfectant and antiseptic. Salicylic acid is also an important raw material for the production of high-value-added fine chemical products such as advanced dyes, rubber industry additives, spices, flame retardants, fabric protective agents, soil conditioners, etc. [0003] The...

Claims

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Application Information

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IPC IPC(8): C07C65/10C07C51/15
CPCY02P20/54
Inventor 邢存章吕海亮班青高菲
Owner QILU UNIV OF TECH
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