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Nitration method of p-alkylphenol

A technology for p-alkyl phenol and nitric acid is applied in the field of nitration and synthesis of organic compound p-alkyl phenol, which can solve the problem of high synthesis cost and achieve the effects of high raw material utilization rate, good industrial application value and high yield.

Active Publication Date: 2021-12-03
福建振新化学有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Applied to nano-SiO 2 As a carrier, the use of acid is reduced, but the synthesis cost is higher

Method used

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  • Nitration method of p-alkylphenol
  • Nitration method of p-alkylphenol
  • Nitration method of p-alkylphenol

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0041] Embodiment 1, a kind of nitration method of p-cresol, carry out following steps successively:

[0042] (1), suspend 108g (1.0mol) p-cresol in 301mL of water, add 5g ferric nitrate, mix and stir, slowly add 77g fuming nitric acid (concentration 98%, 1.2mol) dropwise, control the reaction system during the dropwise addition The temperature does not exceed 25°C, and react at 20°C for 2 hours after the dropwise addition;

[0043] (2) The reaction solution obtained in step (1) was left to stand at 5° C. for 2 hours, and separated. The lower layer obtained by liquid separation is the product o-nitro-p-cresol; the upper layer obtained by liquid separation is dilute nitric acid aqueous solution (about 320ml). Remove the oil foam floating on the surface of the dilute nitric acid aqueous solution obtained by liquid separation, and then it can be used subsequently (the following cases are the same as this requirement).

[0044] Take 300mL of dilute nitric acid aqueous solution a...

Embodiment 2

[0053] Embodiment 2, a kind of nitration method of p-ethylphenol, carry out following steps successively:

[0054] (1), suspend 122g (1.0mol) of p-ethylphenol in 301mL of water, add 5g of copper nitrate, mix and stir, slowly add 77g of fuming nitric acid (concentration 98%, 1.2mol) dropwise, and control the reaction during the dropwise addition The temperature of the system does not exceed 25°C, and react at 20°C for 2 hours after the dropwise addition;

[0055] (2) The reaction solution obtained in step (1) was left to stand at 5° C. for 2 hours, and separated. Separate the product o-nitro-p-ethylphenol of the lower floor; get 300mL upper layer dilute nitric acid aqueous solution and mix and stir with 122g (1.0mol) p-ethylphenol, add dropwise 71g fuming nitric acid (concentration 98%, 1.1mol) circulation nitrification, dropwise During the addition process, control the temperature of the reaction system not to exceed 25°C, and react at 20°C for 2 hours after the dropwise addi...

Embodiment 3

[0058] Embodiment 3, a kind of nitration method of n-propyl phenol, carry out following steps successively:

[0059] (1), suspend 136g (1.0mol) of p-n-propylphenol in 301mL of water, add 10g of iron nitrate, mix and stir, slowly add 71g of fuming nitric acid (concentration 98%, 1.1mol) dropwise, control The temperature of the reaction system does not exceed 25°C, and react at 20°C for 2 hours after the dropwise addition;

[0060] (2) The reaction solution obtained in step (1) was left to stand at 5° C. for 2 hours, and separated. Separate the product o-nitro-p-n-propyl phenol in the lower layer; take 300mL upper dilute nitric acid aqueous solution and mix and stir with 136g (1.0mol) p-n-propyl phenol, add dropwise 71g fuming nitric acid (concentration 98%, 1.1mol) to circulate nitration , Control the temperature of the reaction system not to exceed 25°C during the dropwise addition, and react at 20°C for 2h after the dropwise addition is completed.

[0061] The yield is 87.6...

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Abstract

The invention discloses a nitration method for p-alkylphenols, which comprises the following steps in sequence: 1) adding p-alkylphenols as raw materials into a container, adding water and a catalyst, adding nitric acid dropwise under stirring conditions, adding dropwise During the process, the temperature of the material in the control container does not exceed 25°C; after the nitric acid is added dropwise, react at 10-20°C for 2-3 hours; For the product (o-nitro-p-alkylphenol). The supernatant solution obtained by stratification is recycled, that is, cyclic nitrification is carried out. By adopting the method of the present invention to synthesize o-nitro-p-alkylphenol, the utilization rate of raw materials is high, and waste acid and waste water are recycled, which not only reduces the discharge of three wastes, but also reduces the production cost, and at the same time, the product has high purity and high yield, and has good advantages. Industrial application value.

Description

technical field [0001] The present invention relates to the nitration synthesis method of organic compound p-alkylphenol. Background technique [0002] o-Nitro-p-alkylphenol, -R includes methyl, ethyl, n-propyl, isopropyl, n-butyl, sec-butyl, isobutyl, tert-butyl and the like. [0003] O-nitro-p-alkylphenol is an important class of fine chemical intermediates, mainly used in dye intermediates, pharmaceutical intermediates, and material intermediates. [0004] The reaction equation of o-nitro-p-alkylphenol is as follows: [0005] [0006] 1. Literature (Rasayan Journal of Chemistry, 2017, 10, 3, 790-798) uses sodium nitrite as a nitrating agent and acetonitrile as a solvent to nitrate p-cresol to generate o-nitro p- Cresol, the yield reaches 80%. This method uses nitrite and sulfate, which produces a large amount of inorganic salt wastewater, which does not meet the current requirements of green chemical industry. [0007] 2. Literature (International Journal of Chem...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C205/22C07C201/08
CPCC07C201/08C07C205/22
Inventor 毛崇智陈佳辉
Owner 福建振新化学有限公司