P-iodoaniline and preparation method thereof

A technology of p-iodoaniline and aniline, which is applied in the field of p-iodoaniline and its preparation, can solve the problems of increasing three wastes and high consumption of elemental iodine, and achieve the effect of less process pollution

Pending Publication Date: 2020-01-24
新岸诺亚(北京)催化科技有限公司 +1
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Problems solved by technology

[0003] In view of the above analysis, the embodiment of the present invention aims to provide a kind of p-iodoaniline and its preparation method, which is used to solve the problem of excessive consumption of elemental iodine in the existing preparation method of p-iodoaniline, and the increase of three wastes caused by the reaction of more sulfates. technical issues

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  • P-iodoaniline and preparation method thereof
  • P-iodoaniline and preparation method thereof

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[0025] This embodiment discloses a kind of preparation method of p-iodoaniline, and this preparation method comprises the following steps:

[0026] Step 1. Add aniline and water into the first reaction vessel in a certain proportion, then add iodine element in batches into the first reaction vessel and stir to prepare the first solution; cool the first solution to 0-20°C, drop Adding hydrogen peroxide with a mass concentration of 30%, sampling and analyzing until the mass percentage of aniline is less than 0.5%, to obtain a second solution;

[0027] The chemical reaction equation in step 1 is as follows:

[0028]

[0029] In above-mentioned step 1, the molar ratio of iodine element and aniline is 0.5~0.6:1, especially 0.55:1, because too little iodine element amount can cause aniline reaction to be incomplete, and the consumption of iodine element amount is too much then easy to generate excess iodide. In addition, the ratio of hydrogen peroxide to aniline is 0.5 to 1:1, ...

Embodiment 1

[0040] The invention provides a kind of preparation method of p-iodoaniline, the method comprises the following steps:

[0041] Step 1. Add 46.5g of aniline and 100g of water to the first reactor (for example, a 1L four-necked flask), and slowly add 64g of iodine simple substance under stirring, and stir for half an hour to prepare the first solution, and cool the first solution To 0-20°C, slowly add 42g of hydrogen peroxide with a mass concentration of 30% dropwise, take a sample and analyze, the mass percentage of aniline is 4%, and the content of p-iodoaniline is 96%, to obtain the second solution;

[0042] Step 2. Add 10 g of sodium bisulfite to the second solution prepared in step 1, and stir for 0.5 h to obtain the third solution. Use a suction filter to filter it to obtain a filter cake, and wash the filter cake with 100 g of water , and finally obtain brown crystals, the content of which is greater than 96%;

[0043] Step 3. Add the brown crystals obtained in step 2 i...

Embodiment 2

[0045] The invention provides a kind of preparation method of p-iodoaniline, the method comprises the following steps:

[0046] Step 1. Add 46.5 g of aniline and 100 g of water to the first reactor (such as a 1L four-neck flask), and slowly add 70.4 g of iodine elemental substance under stirring, and stir for half an hour to prepare the first solution. Cool to 0-20°C, slowly add 42g of hydrogen peroxide with a mass concentration of 30%, stir at room temperature for 1 hour, and take samples for analysis. 0.5%, to obtain the second solution;

[0047]Step 2. Add 10 g of sodium bisulfite to the second solution prepared in step 1, and stir for 0.5 h to obtain the third solution. Use a suction filter to filter it to obtain a filter cake, and wash the filter cake with 100 g of water , and finally obtain brown crystals, the content of which is greater than 98%;

[0048] Step 3. Add the brown crystals obtained in step 2 into a second reaction vessel (for example, a 1L flask), and add...

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Abstract

The invention provides p-iodoaniline and a preparation method thereof, and belongs to the technical field of organic synthesis. A purpose of the invention is to solve the problems of excessive elemental iodine consumption and increased three wastes caused by a large amount of sulfate generated by reaction in the existing p-iodoaniline preparation method. The method comprises: 1, adding aniline andwater into a first reaction container according to a certain ratio, adding elemental iodine into the first reaction container in a dropwise manner, stirring to prepare a first solution, cooling the first solution to 0-20 DEG C, adding hydrogen peroxide with a mass concentration of 30% in a dropwise manner, and carrying out sampling analyzing until the mass percentage content of aniline is less than 0.5% to obtain a second solution; 2, adding sodium sulfite into the second solution, stirring for 0.4-0.5 h to obtain a third solution, and carrying out suction filtration on the third solution toobtain a brown crystal; and 3, pouring the brown crystal into a second reaction container, and carrying out extraction purification treatment to obtain the p-iodoaniline finished product. According tothe invention, with the method, the consumption of elemental iodine is low, the crude product content is high, and the generation of sulfate is avoided.

Description

technical field [0001] The present invention relates to the technical field of organic synthesis, in particular to a kind of p-iodoaniline and preparation method thereof. Background technique [0002] The traditional p-iodoaniline preparation method needs excessive elemental iodine to be reacted in the presence of sodium bicarbonate, and this preparation process has the technical defect that the consumption of elemental iodine is too high; in addition, the preparation method of p-iodoaniline also uses The process of potassium iodide and hydrogen peroxide should also need to add sulfuric acid to react, which will produce more sulfate and increase the three wastes. Contents of the invention [0003] In view of the above analysis, the embodiment of the present invention aims to provide a kind of p-iodoaniline and its preparation method, which is used to solve the problem of excessive consumption of elemental iodine in the existing preparation method of p-iodoaniline, and the ...

Claims

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Application Information

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IPC IPC(8): C07C209/74C07C209/84C07C211/52
CPCC07C209/74C07C209/84C07C211/52
Inventor 胡海峰刘琳苗慧时金彪项业专
Owner 新岸诺亚(北京)催化科技有限公司
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