CN111635645A - Novel production process of acid red 405 - Google Patents
Novel production process of acid red 405 Download PDFInfo
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- CN111635645A CN111635645A CN202010503276.7A CN202010503276A CN111635645A CN 111635645 A CN111635645 A CN 111635645A CN 202010503276 A CN202010503276 A CN 202010503276A CN 111635645 A CN111635645 A CN 111635645A
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09B—ORGANIC DYES OR CLOSELY-RELATED COMPOUNDS FOR PRODUCING DYES, e.g. PIGMENTS; MORDANTS; LAKES
- C09B45/00—Complex metal compounds of azo dyes
- C09B45/02—Preparation from dyes containing in o-position a hydroxy group and in o'-position hydroxy, alkoxy, carboxyl, amino or keto groups
- C09B45/14—Monoazo compounds
- C09B45/16—Monoazo compounds containing chromium
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Abstract
The application discloses a novel production process of acid red 405, which is characterized by comprising the following steps: s1, preparing diazonium salt a; s2, dissolving to obtain a 1-phenyl-3-methyl-5 pyrazolone solution; s3, mixing diazonium salt and 1-phenyl-3-methyl-5 pyrazolone solution, and performing pressure filtration to obtain a coupling compound a filter cake; s4, adding 1500kg of water, 440kg of oxygen and 20kg of NNO dispersant into a 6300L reaction kettle, pulping for 30 minutes; s5, dissolving to obtain a 1-phenyl-3-methyl-5 pyrazolone solution; s6, slowly adding the dissolved 1-phenyl-3-methyl-5 pyrazolone solution into the 6300L reaction kettle in the step 4, cooling to 50 ℃ and pressing to obtain a coupling compound b; s7 preparation of complex b in 6300L autoclave; s8, adding 3500kg of water, the conjugate a and the complex b into a 5000L reaction kettle, and spray-drying after the reaction is finished to obtain the finished product 405 red. This application makes the reaction liquid mobility obtain improving, has reduced the content of salt in the waste water, reduces the workman and operates the degree of difficulty, raises the efficiency.
Description
Technical Field
The application relates to the field of acid red 405, in particular to a novel production process of acid red 405.
Background
Acid Red 405 is a chemical substance with the molecular formula of C36H22CRN9NA2O 9S. The current production process of acid red 405 is as follows: firstly, diazo a: 95.8kg of 2-amino-5-nitrophenol is put into a 5000L reaction kettle, 770kg of water is added, and 115.2kg of 30% liquid caustic soda is added. 190kg of 30% hydrochloric acid, 100kg of naphthalenesulfonic acid and 500kg of ice were slowly added while stirring. After stirring uniformly, sodium nitrite solution (prepared by dissolving 45kg of sodium nitrite in 130kg of water) is added and stirred for one hour. Dissolving 1-phenyl-3-methyl-5 pyrazolone: 450kg of water, 200kg of ice, 92.2kg of 30% liquid caustic soda and 115.2kg of 1-phenyl-3-methyl-5 pyrazolone are put into a reaction kettle and stirred for 15 minutes to be dissolved. Coupling a: 3kg of sulfamic acid and 61.5kg of ammonium bicarbonate were added after the diazo a reaction was completed for one hour. Pouring the dissolved 1-phenyl-3-methyl-5 pyrazolone solution into the diazo liquid a, and adjusting the pH value to 8-8.5 with hydrochloric acid to react for three hours. And adding 800kg of water, and then performing pressure filtration to obtain a coupling compound a filter cake. Fourthly, opening the ring of the ferrite: 420kg of water and 220kg of oxygen are put into a 6300L reaction kettle, 13kg of zinc chloride and about 29kg of ammonium bicarbonate are added to adjust the pH value to 1.4-1.6 for later use. Dissolving 1-phenyl-3-methyl-5 pyrazolone: 300kg of water, 120kg of 30% liquid caustic soda and 157kg of 1-phenyl-3-methyl-5-pyrazolone are put into a reaction kettle and stirred for 15 minutes to be dissolved. Coupling b: and slowly adding the dissolved 1-phenyl-3-methyl-5 pyrazolone solution into the oxygen for reaction within 20-30 minutes. And (3) controlling the pH value to be 7.5-8 after the addition, and reacting for two hours at the temperature of 15-20 ℃. Dissolving chromium solution: adding 250kg of water, 36.5kg of chromium powder and 10kg of sulfuric acid into a reaction kettle to dissolve the first part of chromium solution, adding 250kg of water, 33.9kg of chromium powder and 10kg of sulfuric acid into the reaction kettle to dissolve the second part of chromium solution, complexing the mixture of the first part of chromium solution and the second part of chromium solution (adding 250kg of water, 33.9: and b, adding 500kg of water, 25kg of salicylic acid and the first part of chromium solution after the coupling b is finished, and supplementing water to 4500L. Heating to 100-102 ℃ and preserving the temperature for three hours. Then the temperature is reduced to 95-98 ℃, and the pH is slowly adjusted to 5-5.5 by using liquid alkali for 30 minutes. 6300L of the mixture is transferred into a high-pressure autoclave, 35kg of salicylic acid and the second part of chromium solution are added, 150-200 kg of hydrochloric acid is used for adjusting the pH value to 0.85-0.9, and the temperature is increased to 120-125 ℃ for reaction for 10 hours. And after the reaction time is up, cooling to 70-75 ℃ and carrying out filter pressing. The filter cake was washed with 3000kg of water to give complex b. Ninthly, complexing c: 3000kg of water, a batch of conjugate a and a batch of complex b are added into a 5000L reaction kettle and beaten for 30 minutes. And raising the temperature to 85-90 ℃, simultaneously adding about 150kg of liquid alkali into the mixture in a trickle manner, maintaining the pH value between 7.0 and 7.5, and reacting for one hour under the condition of heat preservation. After the reaction, 700kg of industrial salt was added to precipitate the material. And (5) performing filter pressing and drying to obtain a finished product 405 red. When the method is used in practical application, the reaction liquid has poor liquidity, large amount of waste water, large environment-friendly investment, low productivity, difficult operation of workers and more waste salt and waste water. Therefore, a new process for producing acid red 405 is needed to solve the above problems
Disclosure of Invention
The application provides a novel production process of acid red 405, and solves the problem of wastewater produced in the production process of acid red 405 in the prior art.
The application provides a novel production process of acid red 405, which is characterized by comprising the following steps:
s1, adding 246.4kg of 2-amino-5-nitrophenol, 900kg of water and 80kg of 30% hydrochloric acid into a 5000L reaction kettle, heating to 60-65 ℃, and adding 230kg of naphthalenesulfonic acid; continuously heating to 95-98 ℃ for dissolution, and cooling circulating water to 35-40 ℃ after dissolution; adding 20kg of NNO dispersant, continuously cooling to 15 ℃, adding 500kg of ice, uniformly stirring, adding sodium nitrite solution, and stirring for one hour to obtain diazonium salt a;
s2, adding 600kg of water, 200kg of ice, 224kg of 30% caustic soda liquid and 281.2kg of 1-phenyl-3-methyl-5 pyrazolone into an empty reaction kettle, stirring for 15 minutes to dissolve the mixture to obtain a 1-phenyl-3-methyl-5 pyrazolone solution;
s3, adding 3kg of sulfamic acid, 400kg of ice and 500kg of water into the 5000L reaction kettle in the step 1, reacting the 1-phenyl-3-methyl-5 pyrazolone solution dissolved in the step 2 for three hours in an environment with the pH value of 8-8.5, adding 50kg of hydrochloric acid to adjust the pH value to 3-3.5, and performing pressure filtration to obtain a coupling compound a filter cake;
s4, adding 1500kg of water, 440kg of oxygen and 20kg of NNO dispersant into a 6300L reaction kettle, pulping for 30 minutes;
s5, adding 1000kg of water, 240kg of 30% caustic soda liquid and 314kg of 1-phenyl-3-methyl-5 pyrazolone into an empty reaction kettle to dissolve to obtain a 1-phenyl-3-methyl-5 pyrazolone solution;
s6, slowly adding the 1-phenyl-3-methyl-5 pyrazolone solution dissolved in the step 5 into the 6300L reaction kettle in the step 4 for 40-60 minutes, controlling the pH value to be 7.8-8.2 after the addition, reacting for two hours at the temperature of 35-40 ℃, adjusting the pH value to be 1-1.5 by using 160kg of hydrochloric acid, cooling to 50 ℃ and pressing to obtain a coupling compound b;
s7, adding 3000kg of water into a 6300L high-pressure autoclave, adding coupling compound b, 40kg of salicylic acid, 240kg of 50% sulfuric acid and 520kg of chromium powder industrial product, adjusting the volume to 5500L, heating to 130-135 ℃ for reacting for 8 hours, cooling to 60-70 ℃ for pressing, and recycling the filtrate to obtain a complex b;
s8, adding 3500kg of water, the conjugate a and the complex b into a 5000L reaction kettle, pulping for 30 minutes, heating to 80-5 ℃, simultaneously adding 450kg of liquid alkali in trickle flow, keeping the pH value at 8.0-8.5, keeping the temperature and reacting for one hour, and spraying to dry after the reaction is finished to obtain the finished product 405 red.
Further, the novel production process of the acid red 405 is characterized in that the sodium nitrite solution is 115kg of sodium nitrite dissolved in 200kg of water.
According to the technical scheme, the novel production process of the acid red 405 is provided, the dispersing agent NNO is added, the fluidity of the reaction liquid is improved, the 2-amino-5-nitrophenol alkali dissolution step is removed, the consumption of liquid alkali hydrochloric acid is reduced, the content of salt in the waste water is reduced, the operation difficulty of workers is reduced, the efficiency is improved, the waste water is mechanically used, the output of the waste water is reduced, the waste water is finally sprayed, the salting-out is not needed, and the waste salt is reduced while no waste water is output.
Detailed Description
In order to make those skilled in the art better understand the technical solutions in the present application, the technical solutions in the embodiments of the present application are clearly and completely described below.
According to the technical scheme, the novel production process of the acid red 405 comprises the following steps:
s1, adding 246.4kg of 2-amino-5-nitrophenol, 900kg of water and 80kg of 30% hydrochloric acid into a 5000L reaction kettle, heating to 60-65 ℃, and adding 230kg of naphthalenesulfonic acid; continuously heating to 95-98 ℃ for dissolution, and cooling circulating water to 35-40 ℃ after dissolution; adding 20kg of NNO dispersant, continuously cooling to 15 ℃, adding 500kg of ice, uniformly stirring, adding sodium nitrite solution, and stirring for one hour to obtain diazonium salt a;
s2, adding 600kg of water, 200kg of ice, 224kg of 30% caustic soda liquid and 281.2kg of 1-phenyl-3-methyl-5 pyrazolone into an empty reaction kettle, stirring for 15 minutes to dissolve the mixture to obtain a 1-phenyl-3-methyl-5 pyrazolone solution;
s3, adding 3kg of sulfamic acid, 400kg of ice and 500kg of water into the 5000L reaction kettle in the step 1, reacting the 1-phenyl-3-methyl-5 pyrazolone solution dissolved in the step 2 for three hours in an environment with the pH value of 8-8.5, adding 50kg of hydrochloric acid to adjust the pH value to 3-3.5, and performing pressure filtration to obtain a coupling compound a filter cake;
s4, adding 1500kg of water, 440kg of oxygen and 20kg of NNO dispersant into a 6300L reaction kettle, pulping for 30 minutes;
s5, adding 1000kg of water, 240kg of 30% caustic soda liquid and 314kg of 1-phenyl-3-methyl-5 pyrazolone into an empty reaction kettle to dissolve to obtain a 1-phenyl-3-methyl-5 pyrazolone solution;
s6, slowly adding the 1-phenyl-3-methyl-5 pyrazolone solution dissolved in the step 5 into the 6300L reaction kettle in the step 4 for 40-60 minutes, controlling the pH value to be 7.8-8.2 after the addition, reacting for two hours at the temperature of 35-40 ℃, adjusting the pH value to be 1-1.5 by using 160kg of hydrochloric acid, cooling to 50 ℃ and pressing to obtain a coupling compound b;
s7, adding 3000kg of water into a 6300L high-pressure autoclave, adding coupling compound b, 40kg of salicylic acid, 240kg of 50% sulfuric acid and 520kg of chromium powder industrial product, adjusting the volume to 5500L, heating to 130-135 ℃ for reacting for 8 hours, cooling to 60-70 ℃ for pressing, and recycling the filtrate to obtain a complex b;
s8, adding 3500kg of water, the conjugate a and the complex b into a 5000L reaction kettle, pulping for 30 minutes, heating to 80-5 ℃, simultaneously adding 450kg of liquid alkali in trickle flow, keeping the pH value at 8.0-8.5, keeping the temperature and reacting for one hour, and spraying to dry after the reaction is finished to obtain the finished product 405 red.
Preferably, the sodium nitrite solution is 115kg of sodium nitrite dissolved in 200kg of water.
1. During the preparation of the "diazonium salt a" in reaction step 1, dispersant NNO is added to improve the fluidity of the reaction solution.
2. The feeding amount of the coupling compound a is increased to 2 times of that of the original process in the production process, and the equipment productivity is greatly improved. Compared with the prior art, the method has the advantages of reducing the amount of waste water and correspondingly reducing the treatment cost and the environmental protection investment.
3. In the preparation process of the diazonium salt a in the step 1, the step of alkali dissolution of 2-amino-5-nitrophenol is removed, the consumption of hydrochloric acid is reduced, and the content of salt in the wastewater is reduced.
4. And a dispersant NNO is added into the oxygen ring opening and coupling compound b, so that the fluidity of the reaction liquid is improved.
Direct high pressure synthesis during preparation of "complex b" 1: 1, without first reacting to 1: 2, the operation difficulty of workers is reduced, and the efficiency is improved.
Reduction of wastewater production during the preparation of "complex b".
8. the reaction solution in the complex c is sprayed and dried without salting out, thereby reducing waste salt and simultaneously generating no waste water.
The following table is a comparison table of new and old processes
Other embodiments of the present application will be apparent to those skilled in the art from consideration of the specification and practice of the application disclosed herein. This application is intended to cover any variations, uses, or adaptations of the invention following, in general, the principles of the application and including such departures from the present disclosure as come within known or customary practice within the art to which the invention pertains. It is intended that the specification and examples be considered as exemplary only, with a true scope of the disclosure being indicated by the following claims.
It is to be understood that the present application is not limited to what has been described above, and that various modifications and changes may be made without departing from the scope thereof. The above-described embodiments of the present application do not limit the scope of the present application.
Claims (2)
1. A novel production process of acid red 405 is characterized by comprising the following steps:
s1, adding 246.4kg of 2-amino-5-nitrophenol, 900kg of water and 80kg of 30% hydrochloric acid into a 5000L reaction kettle, heating to 60-65 ℃, and adding 230kg of naphthalenesulfonic acid; continuously heating to 95-98 ℃ for dissolution, and cooling circulating water to 35-40 ℃ after dissolution; adding 20kg of NNO dispersant, continuously cooling to 15 ℃, adding 500kg of ice, uniformly stirring, adding sodium nitrite solution, and stirring for one hour to obtain diazonium salt a;
s2, adding 600kg of water, 200kg of ice, 224kg of 30% caustic soda liquid and 281.2kg of 1-phenyl-3-methyl-5 pyrazolone into an empty reaction kettle, stirring for 15 minutes to dissolve the mixture to obtain a 1-phenyl-3-methyl-5 pyrazolone solution;
s3, adding 3kg of sulfamic acid, 400kg of ice and 500kg of water into the 5000L reaction kettle in the step 1, reacting the 1-phenyl-3-methyl-5 pyrazolone solution dissolved in the step 2 for three hours in an environment with the pH value of 8-8.5, adding 50kg of hydrochloric acid to adjust the pH value to 3-3.5, and performing pressure filtration to obtain a coupling compound a filter cake;
s4, adding 1500kg of water, 440kg of oxygen and 20kg of NNO dispersant into a 6300L reaction kettle, pulping for 30 minutes;
s5, adding 1000kg of water, 240kg of 30% caustic soda liquid and 314kg of 1-phenyl-3-methyl-5 pyrazolone into an empty reaction kettle to dissolve to obtain a 1-phenyl-3-methyl-5 pyrazolone solution;
s6, slowly adding the 1-phenyl-3-methyl-5 pyrazolone solution dissolved in the step 5 into the 6300L reaction kettle in the step 4 for 40-60 minutes, controlling the pH value to be 7.8-8.2 after the addition, reacting for two hours at the temperature of 35-40 ℃, adjusting the pH value to be 1-1.5 by using 160kg of hydrochloric acid, cooling to 50 ℃ and pressing to obtain a coupling compound b;
s7, adding 3000kg of water into a 6300L high-pressure autoclave, adding coupling compound b, 40kg of salicylic acid, 240kg of 50% sulfuric acid and 520kg of chromium powder industrial product, adjusting the volume to 5500L, heating to 130-135 ℃ for reacting for 8 hours, cooling to 60-70 ℃ for pressing, and recycling the filtrate to obtain a complex b;
s8, adding 3500kg of water, the conjugate a and the complex b into a 5000L reaction kettle, pulping for 30 minutes, heating to 80-5 ℃, simultaneously adding 450kg of liquid alkali in trickle flow, keeping the pH value at 8.0-8.5, keeping the temperature and reacting for one hour, and spraying to dry after the reaction is finished to obtain the finished product 405 red.
2. The novel process for producing acid red 405 as claimed in claim 1, wherein the sodium nitrite solution is 115kg sodium nitrite dissolved in 200kg water.
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| CN202010503276.7A CN111635645A (en) | 2020-06-05 | 2020-06-05 | Novel production process of acid red 405 |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4933437A (en) * | 1984-03-08 | 1990-06-12 | Ciba-Geigy Corporation | Preparation of 1:2 chromium complex azo dyes asymmetrically substituted with solubilizing groups |
| PL153839B1 (en) * | 1988-09-29 | 1991-06-28 | Os Bad Rozwojowy Przem Barwni | HOW TO OBTAIN A NEW AZO DYE CHROMO COMPLEX 1: 2 |
| CN105985663A (en) * | 2015-02-11 | 2016-10-05 | 上海雅运纺织化工股份有限公司 | Black acid dye composition and dyeing application thereof |
| CN109593382A (en) * | 2018-11-20 | 2019-04-09 | 恒升化工有限公司 | A kind of preparation method of red complexing type dye |
-
2020
- 2020-06-05 CN CN202010503276.7A patent/CN111635645A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4933437A (en) * | 1984-03-08 | 1990-06-12 | Ciba-Geigy Corporation | Preparation of 1:2 chromium complex azo dyes asymmetrically substituted with solubilizing groups |
| PL153839B1 (en) * | 1988-09-29 | 1991-06-28 | Os Bad Rozwojowy Przem Barwni | HOW TO OBTAIN A NEW AZO DYE CHROMO COMPLEX 1: 2 |
| CN105985663A (en) * | 2015-02-11 | 2016-10-05 | 上海雅运纺织化工股份有限公司 | Black acid dye composition and dyeing application thereof |
| CN109593382A (en) * | 2018-11-20 | 2019-04-09 | 恒升化工有限公司 | A kind of preparation method of red complexing type dye |
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Application publication date: 20200908 |