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Separation method of p-chlorotoluene and o-chlorotoluene

A technology for p-chlorotoluene and o-chlorotoluene is applied in the field of separation of p-chlorotoluene and o-chlorotoluene, and can solve the problems of high energy consumption and complicated process, and achieve the effects of low energy consumption, simple operation and energy saving.

Active Publication Date: 2019-08-06
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] Aiming at the deficiencies in the art, and the large energy consumption and cumbersome process in the separation technology of p-chlorotoluene and o-chlorotoluene, the defects such as the need to use high-purity desorbent, the invention provides a kind of p-chlorotoluene and o-chlorotoluene The separation method of chlorotoluene, using bisdiethoxy column [n] aromatic hydrocarbon crystal material to adsorb and separate the mixture of p-chlorotoluene and o-chlorotoluene, has low energy consumption and simple process

Method used

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  • Separation method of p-chlorotoluene and o-chlorotoluene
  • Separation method of p-chlorotoluene and o-chlorotoluene
  • Separation method of p-chlorotoluene and o-chlorotoluene

Examples

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Effect test

Embodiment 1

[0028] Preparation of bisdiethoxy columnar[5]arene crystal material: Weigh 2g of bisdiethoxy column[5]arene into 20mL tetrahydrofuran, heat to boiling, add tetrahydrofuran solution dropwise until completely dissolved, place the solution in Store at 0°C overnight, collect the precipitated crystals by filtration, and vacuum-dry the obtained crystals at 50°C to obtain a white powder, which is designated as EtP5.

[0029] The product characterization data prepared in this embodiment are as follows:

[0030] EtP5, 1 H NMR (400MHz, CDCl 3 , 298K, ppm) δ6.72 (s, 10H), 3.83 (q, 20H), 3.76 (s, 10H), 1.55 (t, 30H).

[0031] PXRD test results such as figure 1 As shown in a, the obtained bisdiethoxypillar[5]arene crystalline material has good crystallinity.

Embodiment 2

[0033]Preparation of bisdiethoxy columnar[6]arene crystal material: Weigh 2g of bisdiethoxy column[6]arene into 20mL acetone, heat to boiling, add acetone dropwise until completely dissolved, place the solution at 0 Store at ℃ overnight, collect the precipitated crystals by filtration, dry the obtained crystals in vacuum at 50 ℃, and activate at 160 ℃ for 2 hours to obtain a white powder, which is marked as EtP6.

[0034] The product characterization data prepared in this embodiment are as follows:

[0035] EtP6, 1 H NMR (400MHz, CDCl 3 , 298K, ppm) δ6.70 (s, 12H), 3.83 (q, 36H), 1.28 (t, 36H).

[0036] PXRD test results such as figure 1 As shown in b, the obtained bisdiethoxypillar[6]arene crystal material has good crystallinity.

Embodiment 3

[0038] Adsorption of p-chlorotoluene or o-chlorotoluene alone by bisdiethoxy column[5]arene crystal material: Take two 20mL strain bottles, add 1mL p-chlorotoluene and 1mL o-chlorotoluene respectively, and name them as EtP5-PCT and EtP5-OCT, take 200mg of bisdiethoxy column [5] arene crystal material and place them in two 5mL strain bottles respectively, put two open 5mL strain bottles in two 20mL strain bottles, put 20mL The strain bottle was sealed well and placed in a water bath at 25°C for 30 hours.

[0039] The product characterization data prepared in this embodiment are as follows:

[0040] EtP5-PCT, 1 H NMR (400MHz, CDCl 3 ,298K,ppm)δ7.23(d,2H)7.11(d,2H)6.72(s,10H),3.83(q,20H),3.76(s,10H),2.32(s,3H),1.55(t ,30H).

[0041] EtP5-OCT, 1 H NMR (400MHz, CDCl 3 , 298K, ppm) δ6.72 (s, 10H), 3.83 (q, 20H), 3.76 (s, 10H), 1.55 (t, 30H).

[0042] 1 H NMR results showed that bisdiethoxypillar[5]arene crystalline materials adsorbed p-chlorotoluene in a stoichiometric ratio...

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Abstract

The invention discloses a separation method of p-chlorotoluene and o-chlorotoluene. A bis-diethoxy column [n] arene crystal material is utilized to adsorb and separate a p-chlorotoluene and o-chlorotoluene mixture, and the chemical structural formula of the bis-diethoxy column [n] arene crystal material is as shown in the specification, wherein n is 5 or 6. The separation method has simple separation process operation and low equipment requirement. No rectification operation is required in the separation process, the energy consumption is low, the energy is saved, and the production cost of the p-chlorotoluene is reduced. The crystal material used has high stability, and can be recycled, and the separation effect cannot be reduced.

Description

technical field [0001] The invention relates to the technical field of adsorption separation, in particular to a method for separating p-chlorotoluene and o-chlorotoluene. Background technique [0002] p-Chlorotoluene is an important chemical raw material, widely used in the synthesis of fine chemicals such as medicine, pesticides and dyes. Especially in the field of pesticide production, p-chlorotoluene is an intermediate in the production process of pesticides such as fenvalerate, paclobutrazol, uniconazole, trifluralin, mesocarb, and diuron. The demand for high-purity p-chlorotoluene in the chemical industry is increasing. p-Chlorotoluene is mainly prepared by the electrophilic substitution reaction of toluene and chlorine gas. Due to the electron-donating effect of the methyl group, in the process of producing p-chlorotoluene, o-chlorotoluene and m-chlorotoluene will also be produced simultaneously, and the content of m-chlorotoluene is very small, less than 0.3%. The...

Claims

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Application Information

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IPC IPC(8): C07C17/389C07C25/02
CPCC07C17/389C07C25/02
Inventor 黄飞鹤王孟宾周炯
Owner ZHEJIANG UNIV
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