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Synthesis method of DPA

A synthesis method and autoclave technology, applied in the field of DPA synthesis, can solve the problems of complex operation, long reaction time, low yield, etc., and achieve the effect of mild reaction conditions, short reaction time and simple operation

Inactive Publication Date: 2020-01-03
胡婷
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, the production of DPA in China has not been industrialized, and some synthesis methods in the pilot test have disadvantages such as unavailable raw materials, long reaction time, complicated operation, high energy consumption, high temperature, high pressure, and low yield, which are not conducive to industrialization and lack of market. Competitiveness

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0010] (1) In a 200ml autoclave, add 4.7ml of o-nitrotoluene, 76.6ml of methanol, 2.7ml of distilled water, 0.02g of 3% Pt / C, seal the autoclave, replace the air with nitrogen for 3 times, and inject 0.1 Mpa of hydrogen, control the temperature at 50°C for 8 hours, stop the reaction, cool down to room temperature, take out the reaction solution and filter, distill off most of the methanol from the filtrate under reduced pressure, dilute the residual solution with water, neutralize the pH value with ammonia water to neutral , the upper organic phase was separated, the aqueous phase was extracted 3 times with ether, the organic phases were combined, and the organic phase was distilled under reduced pressure to remove fractions, the MMA purity was 98.9%;

[0011] (2) In a 200ml autoclave, add MMA26ml, phenol 106ml, cyclohexanone 4.2ml, 3% Pt / C0.28g, seal the autoclave, replace the air in the autoclave with nitrogen, and then adjust the nitrogen pressure to 1Mpa, control The tempe...

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PUM

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Abstract

The invention discloses a synthesis method of DPA. The method comprises the following steps: (1) adding methanol, o-nitrotoluene, a catalyst, concentrated sulfuric acid, distilled water into an autoclave, performing heating with stirring to 50 DEG C, evacuating air and then introducing hydrogen, controlling a pressure in the autoclave to 0.1 MPa, carrying out a reaction for 5 h, then performing suction filtration, distilling a filtrate to remove methanol, diluting a residual solution by adding water and then adjusting pH to be neutral with ammonia water, performing extracting with toluene, washing an organic phase with a dilute sodium hydroxide solution, and performing reduced pressure distillation on the organic phase to obtain 4-methoxy-2-methylaniline; and (2) adding 4-methoxy-2-methylaniline, phenol naphthalene, cyclohexanone, and the catalyst into an autoclave, replacing air with nitrogen, performing heating to 250 DEG C, controlling a pressure in the autoclave to 1 Mpa, performing cooling to room temperature after a reaction is completed, filtering a reaction solution, and performing reduced pressure distillation on a filtrate and collecting various fractions, wherein a latter fraction is DPA. The raw materials are cheap and easy to obtain, the operation is simple, the yield is high, the energy consumption is low, and the method has practical value and economic value, andis suitable for enterprise production.

Description

technical field [0001] The invention belongs to the technical field of compound synthesis, in particular to a synthesis method of DPA. Background technique [0002] With the continuous development of the dye industry, the use of dyes has developed from the dyeing of fibers and fabrics to high-tech information recording, energy conversion, medical diagnosis, microelectronics industry, and biological industry. Due to the rapid development of intelligence and information industry and the wide application of computers and fax machines, the demand for pressure-sensitive and heat-sensitive dyes is growing rapidly. In my country, fluorane pressure-sensitive and heat-sensitive dyes are being developed. With the rapid development of my country's economy, the demand for such products is increasing day by day, and the market potential is huge. The successful development of such dyes will bring economic benefits that cannot be underestimated. benefit. [0003] 2-Methyl-4-methoxydipheny...

Claims

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Application Information

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IPC IPC(8): C07C213/02C07C217/92
CPCC07C213/00C07C213/02C07C217/92C07C217/84
Inventor 王存亮许灵艳严学文黄焕军王小桥胡婷
Owner 胡婷
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