A production method of disperse blue 56

Abstract

The application discloses a production method of disperse blue 56, which comprises the following steps: mixing phenoxy, sulfuric acid and nitric acid to carry out a dinitration reaction, and obtaining filter cake A through pressure filtration; beating the filter cake A to obtain dinitration slurry; mixing the dinitration slurry with liquid alkali to carry out a hydrolysis reaction, and obtaining filter cake B and washing wastewater C through pressure filtration and water washing; beating the filter cake B to obtain hydrolysis slurry; mixing the hydrolysis slurry with a sodium sulfide solution to carry out a reduction reaction, and obtaining filter cake D and washing wastewater E through pressure filtration and water washing; drying the filter cake D to obtain a reduction product; and carrying out a bromination reaction on the reduction product to obtain the disperse blue 56; the washing wastewater E obtained in the application is used for beating the filter cake B, preparing the sodium sulfide solution and constant volume of the reduction reaction of the hydrolysis slurry, so that the washing wastewater can be recycled and reused, the reduction product in the washing wastewater can be recovered, the yield of the reduction product is improved, the consumption of the reduction raw material is reduced, and the production cost is reduced.

Description

TECHNICAL FIELD

[0001] The present application belongs to the technical field of dye production, and in particular relates to a production method of disperse blue 56. BACKGROUND

[0002] Disperse blue 56, also known as disperse blue 2BLN, is a mixture of 1,5-dihydroxy-4,8-diaminoanthraquinone bromide and 1,8-dihydroxy-4,5-diaminoanthraquinone bromide, and its CAS number is 12217-79-7. It is an important disperse blue dye, which has high sunlight fastness and medium sublimation fastness, and has good dyeing depth, level dyeing, covering ability, and the bath pH and temperature have little effect on the color light. It is mainly used for dyeing of polyacetic fiber, cotton yarn, polyester and blended fabrics, etc. It constitutes the three primary colors with disperse red 3B and disperse yellow S-RGFL.

[0003] The production method of disperse blue 56 dinitration mainly has mercury method and non-mercury method, wherein the mercury method has serious environmental pollution due to residual mercury in waste liquid, and has been eliminated. At present, mixed acid nitration process is generally used to prepare dinitroanthraquinone, that is, anthraquinone is subjected to one nitration reaction with mixed acid to generate 1,5-dinitroanthraquinone, then subjected to methyl oxidation reaction to obtain 1,5-diphenoxyanthraquinone, and then subjected to secondary nitration reaction, hydrolysis reaction, reduction reaction and bromination reaction in turn to obtain fuel filter cake. Compared with the mercury method process, the number of processes is reduced, and mercury pollution is avoided, but the non-mercury production method produces a large amount of water washing wastewater in the production process, which is very difficult to treat subsequently, and increases the treatment cost of wastewater.

[0004] In view of this, the present application is proposed. SUMMARY

[0005] The technical problem to be solved by the present application is to overcome the shortcomings of the prior art, and the present application provides a production method of disperse blue 56 which can improve the yield of reduced material and reduce the consumption of reduced raw material.

[0006] To solve the above technical problems, the basic idea of the technical solution of the present application is:

[0007] The present application provides a production method of disperse blue 56, comprising the following steps:

[0008] S1: mixing phenoxy material, sulfuric acid and nitric acid, and then performing dinitration reaction, and obtaining filter cake A by pressure filtration, and then beating the filter cake A to obtain dinitration slurry;

[0009] S2: mixing the dinitration slurry with liquid alkali, and then performing hydrolysis reaction, and then obtaining filter cake B and water washing wastewater C by pressure filtration and water washing, and then beating the filter cake B to obtain hydrolysis slurry;

[0010] S3: the hydrolysis slurry is mixed with sodium sulfide solution to carry out a reduction reaction, and then filtered, washed to obtain filter cake D and washing wastewater E; the filter cake D is dried to obtain a reduction product, and the reduction product is subjected to a bromination reaction to obtain Disperse Blue 56;

[0011] The washing wastewater E obtained in the step S3 is used for the beating of the filter cake B and / or the preparation of the sodium sulfide solution and / or the volume setting of the hydrolysis slurry reduction reaction.

[0012] In the above scheme, the washing wastewater E contains unreacted sodium sulfide and a large amount of reduction product 1,5-dihydroxy-4,8-diaminoanthraquinone. Directly discharging the washing wastewater E not only causes waste of the reduction product, but also pollutes the environment. The present application uses a part of the washing wastewater E for the beating of the filter cake B and / or the preparation of the sodium sulfide solution and / or the volume setting of the hydrolysis slurry reduction reaction, which not only recycles the reduction product, but also reduces the consumption of raw materials for the reduction reaction.

[0013] In addition, the washing wastewater E can also flush the residual substances in the material conveying pipeline, avoiding the additional treatment of wastewater caused by flushing the material conveying pipeline with a large amount of tap water. After flushing the material conveying pipeline, the washing wastewater E flows into the reduction reaction kettle, which indirectly sets the volume of the reduction reaction kettle, reducing the amount of manual operation for setting the volume of the reduction reaction kettle.

[0014] Further, the volume of the washing wastewater E used for the beating of the filter cake B accounts for 25-30% of the total volume of the washing wastewater E, and the volume of the washing wastewater E used for the preparation of the sodium sulfide solution accounts for 15-18% of the total volume of the washing wastewater E.

[0015] In the process of beating the filter cake, the reduction product in the wastewater can be more fully dispersed in the slurry, and then the reduction product can be uniformly dispersed in the filter cake through filtration, avoiding the concentration of a large amount of reduction product on the surface of the filter cake, which causes a large amount of reduction product to be lost after further washing. Therefore, the present application uses more washing wastewater E for the beating of the filter cake B than for the preparation of the sodium sulfide solution, which not only improves the yield of the reduction product, but also greatly reduces the production cost.

[0016] Further, the volume of the washing wastewater E used for the volume setting of the hydrolysis slurry reduction reaction accounts for 18-20% of the total volume of the washing wastewater E.

[0017] The present application directly recycles and reuses the washing wastewater E, and the volume of the recycled and reused washing wastewater E accounts for more than 60% of the total volume of the washing wastewater E. Only less than 40% of the washing wastewater is discharged to the sewage treatment plant for treatment, which greatly reduces the treatment cost of the wastewater.

[0018] Further, the step S3 at least includes a first washing process and a second washing process carried out in sequence.

[0019] The washing wastewater produced by the first washing process is used for the beating of the filter cake B and / or the preparation of the sodium sulfide solution, and the washing wastewater produced by the second washing process is used for the constant volume of the hydrolysis pulp reduction reaction.

[0020] Further, when the hydrolysis pulp in the step S3 is subjected to the reduction reaction for the first time, the sodium sulfide solution is added and then the constant volume is performed by using clean water.

[0021] Further, the filter cake B in the step S2 is beaten by using clean water for the first time.

[0022] Further, the washing wastewater C obtained in the step S2 is used for the beating of the filter cake A and / or the constant volume of the hydrolysis reaction of the di-nitrated pulp.

[0023] In the above scheme, since the washing wastewater C contains a large amount of hydrolyzate, directly discharging the washing wastewater C will cause the waste of the hydrolyzate and the pollution to the environment. By using the washing wastewater C for the beating of the filter cake A, the hydrolyzate can be recycled. In addition, since the washing wastewater C after the hydrolysis reaction also contains unreacted liquid alkali, using the washing wastewater C for the constant volume of the hydrolysis reaction of the di-nitrated pulp can reduce the consumption of the liquid alkali.

[0024] Further, the step S2 comprises at least a first washing process and a second washing process performed in sequence.

[0025] The washing wastewater produced by the first washing process is used for the beating of the filter cake A, and the washing wastewater produced by the second washing process is used for the constant volume of the hydrolysis reaction of the di-nitrated pulp.

[0026] Further, the filter cake A in the step S1 is beaten by using clean water for the first time, and the liquid alkali is added to adjust the pH to 8-10.

[0027] Further, when the di-nitrated pulp in the step S2 is subjected to the hydrolysis reaction for the first time, the liquid alkali is added and then the constant volume is performed by using clean water.

[0028] Further, in the step S3, the hydrolysis pulp is subjected to the reduction reaction with the sodium sulfide solution, and after the pressure filtration, the filter cake is washed by using clean water at 60-80℃.

[0029] In the above scheme, after the washing by using hot water, the washing effect of the filter cake is better, and the salt impurities in the washing water do not reach the saturation state, so that the purity of the filter cake meets the production requirements.

[0030] After the above technical scheme is adopted, the present application has the following beneficial effects compared with the prior art:

[0031] The application provides a production method of disperse blue 56, which uses part of the washing wastewater E to beat the filter cake B and / or prepare a sodium sulfide solution and / or fix the volume of a hydrolysis reduction reaction of the pulp, so that the reduction material can be recycled and used, the yield of the reduction material is improved, and the consumption of the raw material of the reduction reaction is reduced.

[0032] The application provides a production method of disperse blue 56, which uses the obtained washing wastewater C to beat the filter cake A and / or fix the volume of a hydrolysis reaction of the dinitration pulp, so that the washing wastewater can be recycled and reused, the treatment amount of the hydrolysis wastewater is reduced, the hydrolysis material in the washing wastewater is recovered, and the yield of the hydrolysis material is improved.

[0033] The application provides a production method of disperse blue 56, which uses the washing wastewater E for beating the filter cake B in an amount greater than that of the washing wastewater E for preparing the sodium sulfide solution, so that the yield of the reduction material is improved, and the production cost is reduced to a greater extent.

[0034] The specific embodiments of the application are described in detail below with reference to the accompanying drawings. BRIEF DESCRIPTION OF DRAWINGS

[0035] The accompanying drawings are part of the present application and serve to provide a further understanding of the present application, the schematic embodiments of the present application and the descriptions thereof serve to explain the present application, but do not constitute an improper limitation on the present application. Obviously, the accompanying drawings in the following description are only some embodiments, and other drawings can be obtained by those skilled in the art without creative labor. In the drawings:

[0036] Figure 1 It is a process flow chart for producing disperse blue 56 in the prior art.

[0037] Figure 2 It is a process flow chart for producing disperse blue 56 in the present application.

[0038] It should be noted that the drawings and the written description are not intended to limit the scope of the concept of the present application in any way, but to illustrate the concept of the present application to those skilled in the art by referring to specific embodiments. DETAILED DESCRIPTION

[0039] In order to make the purpose, technical scheme and advantages of the embodiments of the present application more clear, the technical scheme in the embodiments is described clearly and completely below, and the following embodiments are used to illustrate the present application, but not to limit the scope of the present application.

[0040] Embodiment 1

[0041] In this embodiment, the process flow for producing disperse blue 56 is as shown in Figure 2 The specific steps are as follows:

[0042] S1: In the reaction kettle, 10.870m 3 of sulfuric acid and 2.033m 3 of nitric acid were added, and then 2400 kg of phenoxy compound was added, and a dinitration reaction was carried out at a temperature of 43-48℃, and after 8h of reaction, filter cake A was obtained by pressure filtration, and the filter cake A was slurried, wherein the filter cake A was first added 8m 3 of clean water for slurry, and then liquid alkali was added to adjust the pH to 8-10, to obtain dinitration slurry;

[0043] S2: The dinitration slurry was mixed with 3.00m 3 of liquid alkali and constant volume, and then a hydrolysis reaction was carried out, and filter cake B and water washing wastewater C were obtained by pressure filtration and water washing, and the filter cake B was slurried to obtain hydrolysis slurry, wherein the filter cake B was first added 9m 3 of clean water for slurry;

[0044] 8m 3 of water washing wastewater C obtained in step S2 was added to the subsequent filter cake A for slurry, and 12m 3 of water washing wastewater C was used for constant volume of the subsequent dinitration slurry hydrolysis reaction;

[0045] S3: The hydrolysis slurry was mixed with water, and a sodium sulfide solution was added for reduction reaction, and filter cake D and water washing wastewater E were obtained by pressure filtration and water washing with 80℃ clean water, and the filter cake D was dried to obtain 1.33t of reduction product;

[0046] A part of 10.8m 3 of water washing wastewater E obtained was used for slurry of the subsequent filter cake B, and 3.00t of sodium sulfide was added to a part of 5.4m 3 of water washing wastewater E to prepare the above-mentioned sodium sulfide solution for reduction reaction of the hydrolysis slurry;

[0047] S4: The reduction product was added to 452kg of bromine, and a bromination reaction was carried out at a temperature of 82-86℃, and after pressure filtration and washing, dispersion blue 56 was obtained.

[0048] Example 2

[0049] In this embodiment, the process flow for producing dispersion blue 56 is as shown in Figure 2 , and the specific steps are as follows:

[0050] S1: In the reaction kettle, 10.855m 3 of sulfuric acid and 2.014m 3 of nitric acid were added, and then 2398 kg of phenoxy compound was added, and a dinitration reaction was carried out at a temperature of 43-48℃, and after 8h of reaction, filter cake A was obtained by pressure filtration, and the filter cake A was slurried, wherein the filter cake A was first added 8m3 The water is used for beating, and then liquid alkali is added to adjust PH = 8-10 to obtain the dinitration slurry;

[0051] S2: The dinitration slurry is mixed with 3.00m 3 After mixing with liquid alkali and constant volume, the hydrolysis reaction is carried out, and the filter cake B and the water washing wastewater C are obtained through pressure filtration and water washing, and the filter cake B is beaten to obtain the hydrolysis slurry, wherein 9m 3 The water is used for beating;

[0052] The 8m 3 The water washing wastewater C is added to step S1 to beat the subsequent filter cake A, 12m 3 The water washing wastewater C is used for constant volume of the subsequent dinitration slurry hydrolysis reaction;

[0053] S3: After mixing the hydrolysis slurry with water, the reduction reaction is carried out by adding sodium sulfide solution, and the filter cake D and the water washing wastewater E are obtained through pressure filtration and water washing at 80℃, and the filter cake D is dried to obtain 1.35t of reduction product;

[0054] A part of the 9m 3 The water washing wastewater E is used for beating the subsequent filter cake B, and 6m 3 The water washing wastewater E is added with 2.98t of sodium sulfide to prepare the above-mentioned sodium sulfide solution, which is used for the reduction reaction of the hydrolysis slurry, and another part of the 7m 3 The water washing wastewater E is used for constant volume of the subsequent hydrolysis slurry reduction reaction;

[0055] S4: The reduction product is added to 459kg of bromine, and the bromination reaction is carried out at a temperature of 82-86℃, and then the dispersion blue 56 is obtained through pressure filtration and washing.

[0056] Example 3

[0057] In this embodiment, the process flow for producing dispersion blue 56 is as shown in Figure 2 The specific steps are as follows:

[0058] S1: 10.850m 3 of sulfuric acid and 2.011m 3 of nitric acid are added to a reaction kettle, and then 2399kg of phenoxy material is added, and the dinitration reaction is carried out at a temperature of 43-48℃, and after 8h of reaction, the filter cake A is obtained through pressure filtration, and the filter cake A is beaten, wherein 8m 3 The water is used for beating, and then liquid alkali is added to adjust PH = 8-10 to obtain the dinitration slurry;

[0059] S2: The dinitration slurry is mixed with 2.99m 3The hydrolysis reaction is carried out after mixing and constant volume of the liquid alkali, and filter cake B and water washing wastewater C are obtained through pressure filtration and water washing. The filter cake B is beaten to obtain the hydrolysis slurry, wherein 9 m 3 The clear water is beaten;

[0060] 8 m 3 The water washing wastewater C is added to step S1 to beat the subsequent filter cake A, 12 m 3 The water washing wastewater C is used for constant volume of the subsequent dinitration slurry hydrolysis reaction;

[0061] S3: After mixing the hydrolysis slurry and water, the reduction reaction is carried out by adding sodium sulfide solution, and filter cake D and water washing wastewater E are obtained through pressure filtration and water washing with 80 DEG C clear water. The filter cake D is dried to obtain 1.30 t reduction;

[0062] 3.15 t sodium sulfide is added to the obtained 6.5 m 3 The water washing wastewater E is dissolved to prepare the above-mentioned sodium sulfide solution, which is used for the reduction reaction of the hydrolysis slurry;

[0063] S4: The reduction is added to 442 kg bromine, and the bromination reaction is carried out at a temperature of 82-86 DEG C. Disperse blue 56 is obtained through pressure filtration and washing.

[0064] Example 4

[0065] In this embodiment, the process flow for producing disperse blue 56 is as shown in Figure 2 The specific steps are as follows:

[0066] S1: 10.867 m 3 Sulfuric acid and 2.029 m 3 Nitric acid are added to the reaction kettle, and then 2398 kg phenoxy substance is added. The dinitration reaction is carried out at a temperature of 43-48 DEG C. After 8 h of reaction, filter cake A is obtained through pressure filtration. The filter cake A is beaten, wherein 8 m

[0067] S2: The dinitration slurry is mixed with 2.99 m 3 Liquid alkali and constant volume are carried out after the hydrolysis reaction, and filter cake B and water washing wastewater C are obtained through pressure filtration and water washing. The filter cake B is beaten to obtain the hydrolysis slurry, wherein 9 m 3 The clear water is beaten;

[0068] 8 m 3 The water washing wastewater C is added to step S1 to beat the subsequent filter cake A, 12 m 3 The water washing wastewater C is used for constant volume of the subsequent dinitration slurry hydrolysis reaction;

[0069] S3: After mixing the hydrolysis slurry and water, 3.12t of sodium sulfide was added for reduction reaction, and filter cake D and water washing wastewater E were obtained by pressure filtration and water washing with 80℃ clean water. After drying the filter cake D, 1.31t of reduction product was obtained;

[0070] The obtained 9m 3 The water washing wastewater E was used for the subsequent beating of filter cake B.

[0071] S4: The reduction product was added to 446kg of bromine, and bromination reaction was carried out at a temperature of 82-86℃. After pressure filtration and washing, dispersion blue 56 was obtained.

[0072] Comparative Example 1

[0073] In this comparative example, the process flow for producing dispersion blue 56 is shown as follows: Figure 1 The specific steps are as follows:

[0074] S1: 10.873m 3 of sulfuric acid and 2.037m 3 of nitric acid were added to a reaction kettle, and then 2400kg of phenoxy product was added. The dinitration reaction was carried out at a temperature of 43-48℃. After 8h of reaction, filter cake A was obtained by pressure filtration. 8m 3 of clean water was added for beating, and liquid alkali was added to adjust the pH to 8-10, obtaining dinitration slurry.

[0075] S2: The dinitration slurry was mixed with 4.00m 3 of liquid alkali and water was added to constant volume, and then hydrolysis reaction was carried out. After pressure filtration and water washing, filter cake B and water washing wastewater C were obtained. The water washing wastewater C was discharged, and the filter cake B was beaten to obtain hydrolysis slurry. 9m 3 of clean water was added to the filter cake B for beating.

[0076] S3: 3.30t of sodium sulfide was dissolved in clean water to form a sodium sulfide solution, which was mixed with the hydrolysis slurry and constant volume with clean water, and then reduction reaction was carried out. After pressure filtration and water washing with 80℃ clean water, filter cake D and water washing wastewater E were obtained. The water washing wastewater E was discharged, and the filter cake D was dried to obtain 1.1t of reduction product.

[0077] S4: The reduction product was added to 395kg of bromine, and bromination reaction was carried out at a temperature of 82-86℃. After pressure filtration and washing, dispersion blue 56 was obtained.

[0078] In each batch of dispersion blue 56 production process, clean water was used for beating, water washing and constant volume.

[0079] The reduction product reaction yield results of Examples 1-4 and Comparative Example 1 are shown in Table 1:

[0080] Table 1

[0081]

[0082] From the data of examples 1-4 and comparative example 1, it can be seen that the production method of disperse blue 56 provided by the present application effectively recycles the reducing substance in the washing wastewater, increases the yield of the reducing substance from 66.67% to 81.77%, and further improves the production capacity of disperse blue; the production method of disperse blue 56 provided by the present application can reduce the consumption of sodium sulfide and liquid alkali, reduce the production cost, and also reduce the discharge amount of washing wastewater and environmental pollution.

[0083] The above merely describes preferred embodiments of the present application and is not intended to limit the present application in any form. Although the present application has been disclosed with the above preferred embodiments, it is not intended to limit the present application. Any person skilled in the art can make some minor changes or modifications to the above-mentioned technical content without departing from the technical solution range of the present application, and any simple modification, equivalent change and modification of the above embodiments according to the technical essence of the present application are still within the scope of the present application.

Claims

1. A method for producing Disperse Blue 56, characterized by, It comprises the following steps: S1: mixing phenoxy, sulfuric acid and nitric acid to carry out dinitration reaction, and obtaining filter cake A by pressure filtration, and then beating the filter cake A to obtain dinitration slurry; S2: mixing the dinitration slurry with liquid alkali to carry out hydrolysis reaction, and obtaining filter cake B and washing wastewater C by pressure filtration and water washing, and then beating the filter cake B to obtain hydrolysis slurry; S3: mixing the hydrolysis slurry with sodium sulfide solution to carry out reduction reaction, and obtaining filter cake D and washing wastewater E by water washing at 60-80℃ after pressure filtration, and then drying the filter cake D to obtain reduction product, and then carrying out bromination reaction on the reduction product to obtain disperse blue 56; the washing wastewater E obtained in the step S3 is used for beating the filter cake B and / or preparation of sodium sulfide solution and / or constant volume of hydrolysis slurry reduction reaction, wherein the volume of the washing wastewater E used for beating the filter cake B accounts for 25-30% of the total volume of the washing wastewater E, the volume of the washing wastewater E used for preparation of sodium sulfide solution accounts for 15-18% of the total volume of the washing wastewater E, and the volume of the washing wastewater E used for constant volume of hydrolysis slurry reduction reaction accounts for 18-20% of the total volume of the washing wastewater E.

2. The production method of disperse blue 56 according to claim 1, characterized in that: the step S3 at least comprises first water washing process and second water washing process carried out in sequence; the washing wastewater produced in the first water washing process is used for beating the filter cake B and / or preparation of sodium sulfide solution, and the washing wastewater produced in the second water washing process is used for constant volume of hydrolysis slurry reduction reaction.

3. The production method of disperse blue 56 according to claim 1, characterized in that: the hydrolysis slurry in the step S3 is first subjected to reduction reaction, and then constant volume is carried out by using clean water after adding sodium sulfide solution.

4. The production method of disperse blue 56 according to claim 1, characterized in that: the filter cake B in the step S2 is first beaten by using clean water.

5. The production method of disperse blue 56 according to any one of claims 1-4, characterized in that: the washing wastewater C obtained in the step S2 is used for beating the filter cake A and / or constant volume of dinitration slurry hydrolysis reaction.

6. The production method of disperse blue 56 according to claim 5, characterized in that: the step S2 at least comprises first water washing process and second water washing process carried out in sequence; the washing wastewater produced in the first water washing process is used for beating the filter cake A, and the washing wastewater produced in the second water washing process is used for constant volume of dinitration slurry hydrolysis reaction.

7. The production method of disperse blue 56 according to claim 1, characterized in that: the filter cake A in the step S1 is first beaten by using clean water, and liquid alkali is added to adjust the PH value to 8-10.

8. The production method of disperse blue 56 according to claim 1, characterized in that: the dinitration slurry in the step S2 is first subjected to hydrolysis reaction, and then constant volume is carried out by using clean water after adding liquid alkali.

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