阅读说明：本技术 一种染料分散蓝b56#的生产方法 (Production method of dye disperse blue B56# ) 是由 丁振中 张超 朱萌 王士刚 高小燕 方祥 陈娇 陆金森 张万宏 徐俊山 于 2020-06-01 设计创作，主要内容包括：本发明公开了一种染料分散蓝B56#的生产方法,属于化工染料技术领域。通过利用亚硫酸钠处理1-氨基蒽醌DMF残渣提纯生产混硝,然后再将混硝依次通过一硝化、一硝化精制、缩合、二硝化、水解、还原和溴化转型过程,最后得到产物分散蓝B56#；对水解回收母液进行再处理回收副产品2,4-二硝基苯酚。本发明分散蓝B56#滤饼水解反应过程中产生了2,4-二硝基苯酚钠盐,2,4-二硝基苯酚钠盐溶解在水解回收母液中,为有效利用其中的有效成分,减少三废排放量,通过酸化、过滤生产副产品2-4-二硝基苯酚,该副产品检测均符合标准,可用作生产涂料中间体的企业原料。(The invention discloses a production method of dye disperse blue B56#, belonging to the technical field of chemical dyes. Purifying and producing mixed nitrate by treating 1-aminoanthraquinone DMF residue with sodium sulfite, and then sequentially carrying out primary nitrification, primary nitrification refining, condensation, secondary nitrification, hydrolysis, reduction and bromination transformation on the mixed nitrate to finally obtain product disperse blue B56 #; the hydrolysis recovery mother liquor is reprocessed to recover the byproduct 2, 4-dinitrophenol. In the invention, 2, 4-dinitrophenol sodium salt is generated in the hydrolysis reaction process of the disperse blue B56# filter cake, and the 2, 4-dinitrophenol sodium salt is dissolved in the hydrolysis recovered mother liquor, so that the effective components in the mother liquor are effectively utilized, the discharge amount of three wastes is reduced, and the byproduct 2-4-dinitrophenol is produced by acidification and filtration, and the detection of the byproduct meets the standard, so that the product can be used as an enterprise raw material for producing a coating intermediate.)

1. A production method of dye disperse blue B56# is characterized in that sodium sulfite is used for treating 1-aminoanthraquinone DMF residue for purification to produce mixed nitrate, and then the mixed nitrate is subjected to primary nitrification, primary nitrification refining, condensation, secondary nitrification, hydrolysis, reduction and bromination transformation in sequence to obtain a product disperse blue B56 #; the hydrolysis recovery mother liquor is reprocessed to recover the byproduct 2, 4-dinitrophenol.

2. The method for producing dye disperse blue B56#, according to claim 1, wherein the recycling mother liquor of hydrolysis comprises the following steps:

(1) adding the hydrolysis recovery mother liquor into a refining kettle, and slowly adding sulfuric acid at room temperature;

(2) adding activated carbon into the solution obtained in the step (1), and stirring and decoloring for 0.5-1 h;

(3) pumping the material into an active carbon filter press for filtering, squeezing the filter cake to dry, collecting filtrate to an acid regulating kettle for regulating acid, pumping the feed liquid into the filter press for filtering, and squeezing the filter cake to dry to obtain a refined 2, 4-dinitrophenol filter cake.

3. The production method of the dye disperse blue B56#, according to claim 2, wherein if the product detection of the refined 2, 4-dinitrophenol filter cake is not qualified, the 2, 4-dinitrophenol filter cake is added into the refining kettle again, bottom water is added, the pH value is adjusted to 6-7, and then the steps (2) and (3) are repeated.

4. The method for producing dye disperse blue B56#, according to claim 2, wherein step (1) comprises adding sulfuric acid to adjust the pH value to 4-7.

5. The method for producing dye disperse blue B56#, according to claim 2, wherein the filtrate obtained in step (3) is added into an acid adjusting kettle to adjust the pH to 1.0 or less.

6. The method for producing the dye disperse blue B56#, according to claim 2, wherein the reaction temperature in step (1) is 60-70 ℃ and the reaction time is 0.5-1 h.

7. The production method of dye disperse blue B56#, according to claim 2, wherein the mass fraction of sulfuric acid is 90% -98%, and the amount of sulfuric acid is 40% -50% of the mass of hydrolysis recovery mother liquor.

8. The method for producing dye disperse blue B56#, according to claim 2, wherein the ratio of the amount of activated carbon used in step (2) to the mass of the hydrolysis recovery mother liquor is 1: 3-1: 5.

Technical Field

The invention belongs to the technical field of chemical dyes, and particularly relates to a production method of dye disperse blue B56 #.

Background

DMF distillation residue generated in the primary refining process in the existing 1-aminoanthraquinone production line is very large, the residue belongs to hazardous waste (HW12), and the existing disposal mode is to send to an incinerator in a factory for incineration treatment, so that a large amount of raw materials are wasted, and environmental pollution is also brought. Therefore, the solid residue is usually selected to be used in the production of dye disperse blue B56#, a large amount of washing water is used in the production process, a large amount of by-products exist in the washing water, the discharge of the washing water without treatment inevitably causes greater water pollution, and the waste of raw materials is great, so that a green, environment-friendly and economical production method and production process of dye disperse blue B56# are required to be found in order to save the production cost and protect the environment.

Disclosure of Invention

Aiming at the problems in the prior art, the invention aims to provide a production method of dye disperse blue B56#, which effectively utilizes the effective components in the hydrolyzed and recovered mother liquor, reduces the discharge amount of three wastes, and produces the byproduct 2-4-dinitrophenol through acidification and filtration.

In order to solve the problems, the technical scheme adopted by the invention is as follows:

a method for producing dye disperse blue B56# comprises purifying 1-aminoanthraquinone DMF residue with sodium sulfite to produce mixed nitrate, sequentially subjecting the mixed nitrate to primary nitrification, refining, condensation, dinitration, hydrolysis, reduction and bromination transformation to obtain product disperse blue B56 #; the hydrolysis recovery mother liquor is reprocessed to recover the byproduct 2, 4-dinitrophenol.

According to the production method of the dye disperse blue B56#, the retreatment of the hydrolyzed and recovered mother liquor specifically comprises the following steps:

(1) adding the hydrolysis recovery mother liquor into a refining kettle, and slowly adding sulfuric acid at room temperature;

(2) adding activated carbon into the solution obtained in the step (1), and stirring and decoloring for 0.5-1 h;

(3) pumping the material into an active carbon filter press for filtering, squeezing the filter cake to dry, collecting filtrate to an acid regulating kettle for regulating acid, pumping the feed liquid into the filter press for filtering, and squeezing the filter cake to dry to obtain a refined 2, 4-dinitrophenol filter cake. The reaction equation involved in the byproduct production process is mainly as follows:

according to the production method of the dye disperse blue B56#, if the product detection is unqualified for the refined 2, 4-dinitrophenol filter cake, the 2, 4-dinitrophenol filter cake is added into the refining kettle again, bottom water is added, the pH value is adjusted to be 6-7, and then the steps (2) and (3) are repeated.

According to the production method of the dye disperse blue B56#, sulfuric acid is added in the step (1) to adjust the pH value to be 4-7.

According to the production method of the dye disperse blue B56#, the filtrate obtained in the step (3) is added into an acid adjusting kettle to adjust the pH value to be less than or equal to 1.0.

According to the production method of the dye disperse blue B56#, the reaction temperature in the step (1) is 60-70 ℃, and the reaction time is 0.5-1 h.

According to the production method of the dye disperse blue B56#, the mass fraction of the sulfuric acid is 90% -98%, and the use amount of the sulfuric acid is 40% -50% of the mass of the hydrolyzed and recovered mother liquor.

According to the production method of the dye disperse blue B56#, the ratio of the using amount of the activated carbon in the step (2) to the mass of the hydrolyzed and recovered mother liquor is 1: 3-1: 5.

Has the advantages that: compared with the prior art, the invention has the advantages that:

in the invention, 2, 4-dinitrophenol sodium salt is generated in the hydrolysis reaction process of the disperse blue B56# filter cake, and the 2, 4-dinitrophenol sodium salt is dissolved in the hydrolysis recovered mother liquor, so that the effective components in the mother liquor are effectively utilized, the discharge amount of three wastes is reduced, and the byproduct 2-4-dinitrophenol is produced by acidification and filtration, and the detection of the byproduct meets the standard, so that the product can be used as an enterprise raw material for producing a coating intermediate.

Detailed Description

In order to make the aforementioned objects, features and advantages of the present invention comprehensible, embodiments accompanied with examples are described in detail below.