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Crystallizing separating tech. of nitro methyl-phenoxide mixture

A technology of nitroanisole and p-nitroanisole, which is applied in the field of fine chemicals, can solve problems such as prolonging the crystallization time, and achieve the effects of increasing investment and operating costs, high reflux temperature, and high selectivity

Inactive Publication Date: 2007-09-19
CHANGZHOU JIASEN CHEM +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0012] Factors that affect the separation of nitroanisole mixtures by crystallization include: the ratio of raw materials to methanol, crystallization separation temperature, crystallization time, and whether the solution is cooled rapidly or slowly during the crystallization process, all of which have an impact on the purity of the crystals. The faster the upper crystallization, the lower the purity of the crystallization, but it can reduce the crystallization time and improve the production efficiency; if the crystallization is slow, the purity of the crystallization can be improved, but the crystallization time is prolonged

Method used

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  • Crystallizing separating tech. of nitro methyl-phenoxide mixture
  • Crystallizing separating tech. of nitro methyl-phenoxide mixture
  • Crystallizing separating tech. of nitro methyl-phenoxide mixture

Examples

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Effect test

Embodiment 1

[0035] As shown in the figure, a kind of nitroanisole mixture is raw material, the separation process of producing p-nitroanisole and o-nitroanisole.

[0036] In the stirring and dissolving kettle, add nitroanisole mixture (the content of o-nitroanisole, m-nitroanisole mixture is respectively 40% and 56%) and methyl alcohol, the content of nitroanisole mixture and methyl alcohol The ratio is: 400g: 500ml. Under stirring conditions, heat up to methanol reflux temperature to dissolve the material; add molecular sieve adsorbent to the dissolved material for decolorization and impurity removal operation, filter while it is hot, and the filtrate enters the first cooling crystallization kettle; In the first cooling crystallizer, the refined material is cooled to 13°C, p-nitroanisole is crystallized and separated, filtered, the filtrate enters the second cooling crystallization kettle, and the filter cake enters the p-nitroanisole recrystallizer; In the cooling crystallizer for the s...

Embodiment 2

[0038] Recrystallization Separation Experiment of o-Nitroanisole and p-Nitroanisole in Methanol Solution

[0039] Add 500ml of methanol into the flask, add 300g of nitroanisole mixture at room temperature, and heat slowly. During the heating process, observe the phenomenon: when the temperature rises to 40°C, the mixed ether is almost completely dissolved; continue to heat up to 60°C, the solution It is a brown homogeneous solution; reflux at 60°C for 30 minutes, slowly cool down, and stand at 40°C for more than 6 hours without solid precipitation; continue to cool down, and when the temperature drops to 18.5°C, needle-shaped crystals begin to precipitate , the temperature dropped to 13° C. and stood still at 13° C. for 10 hours, and the precipitated solid was suction-filtered and weighed to obtain 132 g of light yellow needle-like crystals. Then lower the temperature to 5°C, let it stand for 6 hours at 5°C, and heat-preserve and filter to obtain a crystallization amount of 58...

Embodiment 3

[0041] Recrystallization and separation of p-nitroanisole in methanol solution: heat the primary crystallization product obtained by filtration at 13°C to methanol in different ratios to 60°C, and reflux at 60°C for 30 minutes, and slowly cool down until the temperature drops to 60°C. to 13°C, stand at 13°C for a certain period of time, filter the precipitated solid with suction and weigh to obtain light yellow needle-like crystals. Then continue to lower the temperature to 5°C, let stand at 5°C for a certain period of time, filter, and weigh the obtained crystals. See Table 2 for the phenomena and results.

[0042]The primary crystallization product obtained by filtration at 5°C is heated up to 15°C to dissolve according to the ratio of raw material to methanol: 300g:500ml, then slowly lowered to 5°C and left to stand for 10 hours, then filtered to obtain the weight of the crystallized product. The phenomenon is similar to The results are shown in Table 2.

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Abstract

A crystallizing process for separation of nitro phenylmether mixture includes such steps as thermal dissolving of said mixture in methanol, decoloring, removing impurities, filtering to obtain refined liquid, cooling step by step for crystallizing, filtering to obtain p-nitro phenylmether and o-nitro phenylmether, respectively recrystallizing in methol, separation and refining to obtain refined two products.

Description

technical field [0001] The invention belongs to the technical field of fine chemicals, and in particular relates to a process for producing p-nitroanisole and o-nitroanisole by crystallization and separation in a methanol solvent using a nitroanisole mixture as a raw material. Background technique [0002] Properties and uses of p-nitroanisole and o-nitroanisole anisole [0003] p-Nitroanisole (P-Nitroanisole), C 7 h 7 NO 3 =153.14 [0004] [0005] p-Nitroanisole, light yellow prismatic crystal. The melting point is 54°C; the reflow temperature is 274°C; the relative density is 1.2012 (75 / 4°C). Soluble in alcohol, ether and boiling petroleum ether, slightly soluble in cold petroleum ether, insoluble in water. This product is an intermediate of dyes and other organic synthesis, used to make p-aminoanisole, blue salt VB, etc. [0006] o-Nitroanisole, C 7 h 7 NO 3 =153.14 [0007] [0008] o-Nitroanisole, colorless or light yellow liquid. The melting point ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C201/16C07C205/36
Inventor 许文林段玉辉刘学谦
Owner CHANGZHOU JIASEN CHEM
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