A new green process for preparing high-purity m-cresol

A technology of cresol and o-chlorotoluene, which is applied in the field of organic synthesis, can solve problems such as harsh reaction conditions, poor product quality, and small meta-position ratio, and achieve the effect of reducing post-processing links

Active Publication Date: 2019-01-25
菏泽智慧新材料科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

But the reaction conditions are harsh, high temperature, high pressure, many impurities, small proportion of meta site, difficult to separate meta site and para site, poor product quality

Method used

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  • A new green process for preparing high-purity m-cresol
  • A new green process for preparing high-purity m-cresol

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] Add 1mol of o-chlorotoluene, 2.3mol of sodium hydroxide (22%), 400ml of water, 5g of catalyst, and 3g of 18-crown-6 into the reactor, heat it to 270°C, keep it warm for 6h, stop the reaction, and drop to normal temperature and pressure. Then add hydrochloric acid until the pH value reaches about 5. After layering, add benzene to the water layer for extraction, rectify under reduced pressure, collect the fraction at 80°C, and collect the fraction at 84°C.

Embodiment 2～5

[0019] The reaction conditions of Examples 2-5 are basically the same as those of Example 1, except that the reaction temperature is changed, which is 250, 220, 200, and 180° C., respectively. The results obtained are as follows

[0020]

Embodiment 6～8

[0022] The reaction conditions of Examples 6-8 are basically the same as those of Example 1, except that the reaction time is changed to 4, 2, and 1 h, respectively. The results obtained are as follows

[0023]

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Abstract

The invention discloses a new green process for preparing high-purity m-cresol. Particularly, the preparation method of m-cresol comprises the following steps: by using ortho-chlorotoluene as a raw material, adding sodium hydroxide (the mole ratio of the sodium hydroxide to the ortho-chlorotoluene is (2-3):1), a catalyst and 18-crown ether-6, carrying out reaction at 250-270 DEG C under the pressure of 1-1.6 MPa for 1-6 hours, stopping reaction, dropping to normal temperature and pressure, adding hydrochloric acid until the pH value is 5 or so, stratifying, adding an extractant into the water layer, carrying out extraction, and carrying out rectification under vacuum to obtain the m-cresol.

Description

technical field [0001] The invention belongs to the technical field of organic synthesis, and in particular relates to a new green process for preparing high-purity m-cresol. Background technique [0002] There are three isomers of cresol, ortho, meta, and p-cresol, which are very important fine chemical raw materials. Various products such as antioxidants, pesticides, resins, dyes, medicines, and spices can be derived from cresol as a raw material, and their applications involve various fields of the national economy. m-cresol is mainly used as a pesticide intermediate to produce insecticides such as fenitrothion, thionon, methiocarb, and permethrin. It is also an intermediate for color film, resin, vitamin E, and spices. In addition, it can also be used to synthesize thymol, and can further synthesize menthol. [0003] The preparation methods of cresol mainly include natural extraction method, isopropyl toluene method, xylene oxidation method, phenol methanol catalytic h...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C39/07C07C37/00C07C37/02B01J29/00
CPCB01J29/00B01J2229/18C07C37/00C07C37/02C07C39/07
Inventor 钟华陆敏山陈秀珍朱旭辉殷恒波
Owner 菏泽智慧新材料科技有限公司
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