阅读说明：本技术 4.4-二氨基二苯砜制备方法 (Preparation method of 4, 4-diamino diphenyl sulfone ) 是由 郑会金 于 2019-09-13 设计创作，主要内容包括：本发明公开了一种4.4-二氨基二苯砜制备方法,具体步骤为：将氯苯砜加入高压釜内,再加入氨水和氯化亚铜,升温、升压、保温,蒸氨出料,得氨苯砜粗品。将氨苯砜粗品加入反应釜中,再加入乙醇、氢氧化钠,升温、回流、降温、离心、烘干。反应釜中加入调好的乙醇、中性活性炭,再加入氨苯砜,升温、回流,压滤器脱色、脱渣,冷却、离心、烘干；得到产品4.4二氨基二苯砜。本发明的制备方法原料成本低,金属离子不超标,产品质量好,明显提高产品的纯度和收率,无污水排放量,无环境污染,同时经济效益也大幅提高。(The invention discloses a preparation method of 4, 4-diamino diphenyl sulfone, which comprises the following steps: adding the chlorobenzene sulfone into a high-pressure kettle, adding ammonia water and cuprous chloride, heating, boosting pressure, preserving heat, distilling ammonia and discharging to obtain the crude product of the dapsone. Adding the crude product of dapsone into a reaction kettle, adding ethanol and sodium hydroxide, heating, refluxing, cooling, centrifuging and drying. Adding the adjusted ethanol and neutral activated carbon into a reaction kettle, adding dapsone, heating, refluxing, decoloring by a filter press, removing residues, cooling, centrifuging and drying; the product 4.4 diamino diphenyl sulfone is obtained. The preparation method has the advantages of low raw material cost, no standard exceeding of metal ions, good product quality, obvious improvement of product purity and yield, no sewage discharge, no environmental pollution and great improvement of economic benefit.)

1. A preparation method of 4, 4-diamino diphenyl sulfone is characterized by comprising the following steps:

the method comprises the following steps: weighing the dried chlorobenzene sulfone, adding the weighed chlorobenzene sulfone into an autoclave, adding a proper amount of ammonia water and cuprous chloride, heating to 200-240 ℃, boosting the temperature to 4.5-5.0 MPa, preserving the temperature for 11 hours, transferring into another reaction kettle, and performing ammonia evaporation and discharging to obtain a crude product of dapsone.

Step two: adding the dried crude dapsone into a reaction kettle, adding ethanol and sodium hydroxide into the reaction kettle, heating to 70-80 ℃, refluxing for 1 hour, cooling to below 15 ℃, centrifuging and drying.

Step three: adding the adjusted ethanol and neutral activated carbon into a 5000L reaction kettle, adding dapsone, heating to 70-80 ℃, refluxing for 1 hour, decoloring and deslagging through a filter press, cooling to 25 ℃, centrifuging and drying; the product 4.4 diamino diphenyl sulfone is obtained.

2. The preparation method according to claim 1, wherein the mass ratio of the materials fed in the first step is as follows: the mass ratio of the chlorobenzene sulfone to the ammonia water with the concentration of 28% to the cuprous chloride is 15-18: 38-42: 1.

3. The preparation method according to claim 1, wherein the mass ratio of the materials fed in the step two is as follows: the mass ratio of the dapsone, the 35% ethanol and the sodium hydroxide is 55-65: 145-150: 1.

4. The preparation method according to claim 1, wherein the material feeding mass ratio in step three is as follows: the mass ratio of the dapsone, the 75% ethanol and the neutral activated carbon is 25-35: 70-75: 1.

Technical Field

The invention belongs to the technical field of organic chemical synthesis, and relates to a preparation method of 4, 4-diamino diphenyl sulfone.

Background

4, 4-diamino diphenyl sulfone is an important aromatic sulfone compound refined by ammonification reaction at high temperature and high pressure, and is mainly applied to synthesis of polysulfone amide resin and other high polymer synthetic materials, and synthesis of various acidic azo dyes and disperse dyes. Can be used as epoxy resin curing agent, insulating material in electrical appliance industry, textile equipment, catalyst, and medicine industry for treating leprosy, dermatitis herpetiformis, AIDS, etc.

There have been some reports on the production method of 4.4-diaminodiphenyl sulfone. For example, in chinese patent CN103641753, p-nitrobenzenesulfonyl chloride is used as a raw material, methanol is used as a solvent, under the action of copper acetate, p-dinitrophenylsulfone is obtained through a self-desulfurization coupling reaction, and then sodium disulfite is added in a reaction system, so as to obtain 4, 4-diaminodiphenylsulfone. The preparation method has the main defects of slow reaction progress, difficult reagent obtaining, high price and difficult product separation. In the chinese patent CN106518735, chlorobenzene is used as an initial raw material, and dehydration reaction and ammoniation reaction are performed under an acidic condition to obtain a target product. Although the preparation method has high yield, the sewage discharge amount is large, and the environment is polluted.

Disclosure of Invention

In order to solve the defects of the prior art, the invention aims to: provides a preparation method of 4, 4-diamino diphenyl sulfone. The method has the advantages of low cost of raw materials, high product yield, good quality, no sewage discharge and no environmental pollution.

The purpose of the invention is realized by the following technical scheme:

a preparation method of 4, 4-diamino diphenyl sulfone comprises the following steps:

weighing the dried chlorobenzene sulfone, adding the weighed chlorobenzene sulfone into an autoclave, adding a proper amount of ammonia water and cuprous chloride, heating to 200-240 ℃, boosting the temperature to 4.5-5.0 MPa, preserving the temperature for 11 hours, transferring into another reaction kettle, and performing ammonia evaporation and discharging to obtain a crude product of dapsone.

In the scheme, the material feeding mass ratio is as follows: the mass ratio of the chlorobenzene sulfone to the ammonia water with the concentration of 28% to the cuprous chloride is 15-18: 38-42: 1.

First refining treatment: adding the dried crude dapsone into a reaction kettle, adding ethanol and sodium hydroxide into the reaction kettle, heating to 70-80 ℃, refluxing for 1 hour, cooling to below 15 ℃, centrifuging and drying.

In the scheme, the material feeding mass ratio is as follows: the mass ratio of the dapsone, the 35% ethanol and the sodium hydroxide is 55-65: 145-150: 1.

And (3) second refining treatment: adding the adjusted ethanol and neutral activated carbon into a 5000L reaction kettle, adding dapsone, heating to 70-80 ℃, refluxing for 1 hour, decoloring and deslagging through a filter press, cooling to 25 ℃, centrifuging and drying; the product 4.4 diamino diphenyl sulfone is obtained.

In the scheme, the material feeding mass ratio is as follows: the mass ratio of the dapsone, the 75% ethanol and the neutral activated carbon is 25-35: 70-75: 1.

Compared with the prior art, the invention has the beneficial effects that: the preparation method has the advantages of low raw material cost, no standard exceeding of metal ions, good product quality, obvious improvement of product purity and yield, no sewage discharge and no environmental pollution.

Detailed Description

The technical solutions and effects of the present invention will be illustrated below in the form of examples, but the present invention is not limited to the following examples.