CN111825237A - Environment-friendly production process of 1-aminoanthraquinone - Google Patents
Environment-friendly production process of 1-aminoanthraquinone Download PDFInfo
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Abstract
The invention discloses a green and environment-friendly production process of 1-aminoanthraquinone, belonging to the technical field of chemical product production. Anthraquinone is used as a reaction raw material, 1-aminoanthraquinone is produced by adopting a nitration reduction method, and the produced wastewater is subjected to resource treatment in the production process. Adding the wastewater into an adsorption reaction kettle, and adding high molecular resin into the adsorption reaction kettle to obtain a treatment solution 1; adding acid into the treatment solution 1, adjusting the pH value of the wastewater to acidity, absorbing harmful acidic gas generated in the acid adding process by using ammonia water, and then filtering to obtain a treatment solution 2; adding an alkaline solution into the treatment solution 2 to adjust the treatment solution to be alkaline, and adding an oxidant to oxidize the treatment solution to obtain a treatment solution 3; adding acid into the treatment solution 3 to adjust the solution to acidity, adding activated carbon, adsorbing and decoloring, adjusting to neutrality, and concentrating and crystallizing. The method solves the problems of large amount of wastewater generated in the production process of the 1-aminoanthraquinone and difficult treatment, and recovers sodium salt products while effectively treating the wastewater.
Description
Technical Field
The invention belongs to the technical field of chemical product production, and particularly relates to a green and environment-friendly production process of 1-aminoanthraquinone.
Background
1-aminoanthraquinone is an intermediate for synthesizing vat dyes, disperse dyes, reactive dyes, acid dyes and the like, the prior method for synthesizing 1-aminoanthraquinone is to sulfonate anthraquinone into anthraquinone-1-sulfonic acid under the catalysis of mercury, and then to obtain 1-aminoanthraquinone through ammonolysis, and due to the pollution to the environment, the mercury-containing sewage must be treated, or mercury is recovered from the waste water, so the production cost is increased. The method for producing 1-aminoanthraquinone by using anthraquinone direct nitration reduction method does not use high-pressure kettle, is easy to solve equipment, convenient to popularize and capable of eliminating mercury hazard, and has the defects that a large amount of waste water is produced in the production process and is not easy to treat, but no other feasible method is used for replacing the nitration reduction method so far. The nitrification reduction wastewater generated in the production process of the 1-amino green onion has complex composition, large difficulty of organic matters, high chroma, more difficultly degraded substances and large change of water quality and water quantity, and 15 tons of sulfuration reduction wastewater is generated every 1 ton of the 1-amino green onion. If the waste water is discharged into the environment without being treated, the water body or the soil can be acidified, the ecological environment is harmed, and a large amount of resources are wasted. The traditional wastewater treatment methods, such as neutralization-coagulation precipitation, air flotation, sand filtration, chemical precipitation, biochemical methods (anaerobic treatment method and aerobic treatment method) and the like, are used for treating the wastewater, the wastewater cannot reach the discharge standard, and the adverse effect on the environment is caused, so that the traditional wastewater treatment method becomes a bottleneck for restricting the development of the industry. The problem of waste water treatment in the production process is inevitably solved if a green and environment-friendly production process of the 1-aminoanthraquinone is obtained.
Disclosure of Invention
Aiming at the problems in the prior art, the invention aims to provide an environment-friendly production process of 1-aminoanthraquinone, solve the problems of large amount of wastewater and difficult treatment in the production process of 1-aminoanthraquinone, and recover and obtain sodium salt products while effectively treating the wastewater.
In order to solve the problems, the technical scheme adopted by the invention is as follows:
an environment-friendly production process of 1-aminoanthraquinone, which takes anthraquinone as a reaction raw material, adopts a nitration reduction method to produce 1-aminoanthraquinone, and carries out resource treatment on the produced wastewater in the production process.
The green and environment-friendly production process of the 1-aminoanthraquinone comprises the following steps of:
(1) adding the 1-aminoanthraquinone nitration reduction wastewater into an adsorption reaction kettle, and adding high molecular resin into the adsorption reaction kettle to obtain a treatment solution 1; adsorbing part of organic pollutants in the wastewater; then adding the resin saturated by adsorption into a desorption regeneration reaction kettle for desorption and regeneration under an alkaline condition;
(2) adding acid into the treatment solution 1, adjusting the pH value of the wastewater to acidity, absorbing harmful acidic gas generated in the acid adding process by using ammonia water, and then filtering to obtain a treatment solution 2;
(3) adding an alkaline solution into the treatment solution 2, adjusting to be alkaline, and adding an oxidant for oxidation treatment to obtain a treatment solution 3:
(4) adding acid into the treatment solution 3 to adjust the solution to acidity, adding activated carbon, adsorbing and decoloring, adjusting to neutrality, and concentrating and crystallizing.
The green and environment-friendly production process of the 1-aminoanthraquinone is characterized in that the adsorbent is polystyrene resin or polyacrylate resin.
The environment-friendly production process of the 1-aminoanthraquinone is characterized in that the dosage of the high polymer resin is 0.5-0.6 kg/L.
The green and environment-friendly production process of the 1-aminoanthraquinone comprises the step (2) of adding acid into the treatment solution 1 to adjust the pH value to 3-6.
In the environment-friendly production process of the 1-aminoanthraquinone, harmful acid gases are absorbed in a spraying absorption mode in the step (2); the concentration of the ammonia water is 8-10%. The concentration of the ammonia water is selected, so that the production process is more stable and safer, and harmful acid gases generated in the acid adding process can be well removed;
according to the environment-friendly production process of the 1-aminoanthraquinone, the alkaline solution in the step (3) is a sodium hydroxide solution.
In the environment-friendly production process of the 1-aminoanthraquinone, the oxidant in the step (3) is at least one of ozone, hydrogen peroxide, chlorine dioxide liquid, chlorine dioxide solid or sodium hypochlorite.
Has the advantages that: compared with the prior art, the invention has the advantages that:
in the nitration reduction production process of the 1-aminoanthraquinone, the produced wastewater is subjected to resource treatment, the influence of the wastewater on the environment is reduced, the sodium salt product can be effectively recovered, the development requirement of environmental protection is met, the production cost is saved, and greater economic benefit is brought.
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.
Example 1
The COD of 1-aminoanthraquinone nitration reduction wastewater of a certain batch of the enterprise is 28330mg/L, NH3The sewage with 580mg/L of N, 11.9 percent of salt content, 13 of pH and poor biodegradability is treated as follows:
(1) adding the 1-aminoanthraquinone nitration reduction wastewater into an adsorption reaction kettle, and adding polystyrene resin into the adsorption reaction kettle to obtain a treatment solution 1; the dosage of the polystyrene resin is 0.52kg/L, and part of organic pollutants in the wastewater are adsorbed; then adding the resin saturated by adsorption into a desorption regeneration reaction kettle for desorption and regeneration under an alkaline condition;
(2) adding sulfuric acid into the treatment solution 1, adjusting the pH value of the wastewater to be about 3-3.5, absorbing harmful acidic gas generated in the process of adding the sulfuric acid by using ammonia water with the concentration of 8%, and filtering to obtain a treatment solution 2;
(3) adding a sodium hydroxide solution into the treatment solution 2, adjusting to be alkaline, and introducing ozone for oxidation treatment to obtain a treatment solution 3;
(4) adding sulfuric acid into the treatment solution 3 to adjust the solution to acidity, adding activated carbon, adsorbing and decoloring, adjusting to neutrality, concentrating and crystallizing to obtain sodium sulfate solid, filtering, and evaporating concentrated acid again from the filtered mother solution to obtain sodium thiosulfate solid. The purity of the sodium sulfate solid reaches about 96 percent; the purity of the sodium thiosulfate product reaches about 96 percent.
Example 2
The COD of 1-aminoanthraquinone nitration reduction wastewater of a certain batch of the enterprise is 29039mg/L, NH3-N is 557mg/L, salt content 11%, pH 13, biodegradability, the sewage is treated as follows:
(1) adding the 1-aminoanthraquinone nitration reduction wastewater into an adsorption reaction kettle, and adding polystyrene resin into the adsorption reaction kettle to obtain a treatment solution 1; the dosage of the polystyrene resin is 0.55kg/L, and part of organic pollutants in the wastewater are adsorbed; then adding the resin saturated by adsorption into a desorption regeneration reaction kettle for desorption and regeneration under an alkaline condition;
(2) adding sulfuric acid into the treatment solution 1, adjusting the pH value of the wastewater to be about 4-4.5, absorbing harmful acidic gas generated in the sulfuric acid adding process by using ammonia water with the concentration of 8%, and filtering to obtain a treatment solution 2;
(3) adding a sodium hydroxide solution into the treatment liquid 2, adjusting to be alkaline, and adding hydrogen peroxide for oxidation treatment to obtain a treatment liquid 3;
(4) adding sulfuric acid into the treatment solution 3 to adjust the solution to acidity, adding activated carbon, adsorbing and decoloring, adjusting to neutrality, concentrating and crystallizing to obtain sodium sulfate solid, filtering, and evaporating concentrated acid again from the filtered mother solution to obtain sodium thiosulfate solid. The purity of the sodium sulfate solid reaches about 90 percent; the purity of the sodium thiosulfate product reaches about 93 percent.
Example 3
The COD of 1-aminoanthraquinone nitration reduction wastewater of a certain batch of the enterprise is 31050mg/L, NH3-N is 615mg/L, salt content is 15%, pH 11, biodegradability is very poor, the sewage is treated as follows:
(1) adding the 1-aminoanthraquinone nitration reduction wastewater into an adsorption reaction kettle, and adding polyacrylate resin into the adsorption reaction kettle to obtain a treatment solution 1; the dosage of the polystyrene resin is 0.55kg/L, and part of organic pollutants in the wastewater are adsorbed; then adding the resin saturated by adsorption into a desorption regeneration reaction kettle for desorption and regeneration under an alkaline condition;
(2) adding sulfuric acid into the treatment solution 1, adjusting the pH value of the wastewater to be about 5-5.5, absorbing harmful acidic gas generated in the acid adding process by using ammonia water with the concentration of 9%, and filtering to obtain a treatment solution 2;
(3) adding a sodium hydroxide solution into the treatment solution 2, adjusting to be alkaline, and adding sodium hypochlorite for oxidation treatment to obtain a treatment solution 3;
(4) adding sulfuric acid into the treatment solution 3 to adjust the solution to be acidic, adding activated carbon, adsorbing and decoloring, adjusting to be neutral, concentrating and crystallizing sodium sulfate solid, filtering, and evaporating concentrated acid again from the filtered mother solution to obtain sodium thiosulfate solid. The purity of the sodium sulfate solid reaches about 97 percent; the purity of the sodium thiosulfate product reaches about 93 percent.
Example 4
The COD of 1-aminoanthraquinone nitration reduction wastewater of a certain batch of the enterprise is 27850mg/L, NH3N510 mg/L, salt content 10%, pH 11, biodegradability, the following treatments were carried out on the wastewater:
(1) adding the 1-aminoanthraquinone nitration reduction wastewater into an adsorption reaction kettle, and adding polystyrene resin into the adsorption reaction kettle to obtain a treatment solution 1; the dosage of the polystyrene resin is 0.52kg/L, and part of organic pollutants in the wastewater are adsorbed; then adding the resin saturated by adsorption into a desorption regeneration reaction kettle for desorption and regeneration under an alkaline condition;
(2) adding acid into the treatment solution 1, adjusting the pH value of the wastewater to be about 3-3.5, absorbing harmful acidic gas generated in the acid adding process by using ammonia water with the concentration of 8%, and filtering to obtain a treatment solution 2;
(3) adding a sodium hydroxide solution into the treatment solution 2, adjusting to be alkaline, and adding ozone for oxidation treatment to obtain a treatment solution 3:
(4) and adding acid into the treatment solution 3 to adjust the solution to be acidic, adding activated carbon, adsorbing and decoloring, adjusting to be neutral, concentrating and crystallizing to obtain a sodium sulfate solid, filtering, and evaporating concentrated acid from the filtered mother solution again to obtain a sodium thiosulfate solid. The purity of the sodium sulfate solid reaches about 98 percent; the purity of the sodium thiosulfate product reaches about 97 percent.
Example 5
The COD of 1-aminoanthraquinone nitration reduction wastewater of a certain batch of the enterprise is 34650mg/L, NH3-N650 mg/L, salt content 15%, pH 14, biodegradability, the following treatments were carried out on the wastewater:
(1) adding the 1-aminoanthraquinone nitration reduction wastewater into an adsorption reaction kettle, and adding polystyrene resin into the adsorption reaction kettle to obtain a treatment solution 1; the dosage of the polystyrene resin is 0.55kg/L, and part of organic pollutants in the wastewater are adsorbed; then adding the resin saturated by adsorption into a desorption regeneration reaction kettle for desorption and regeneration under an alkaline condition;
(2) adding sulfuric acid into the treatment solution 1, adjusting the pH value of the wastewater to be about 4-4.5, absorbing harmful acidic gas generated in the sulfuric acid adding process by using ammonia water with the concentration of 8%, and filtering to obtain a treatment solution 2;
(3) adding a sodium hydroxide solution into the treatment solution 2, adjusting to be alkaline, adding hydrogen peroxide for oxidation treatment to obtain a treatment solution 3:
(4) adding sulfuric acid into the treatment solution 3 to adjust the solution to acidity, adding activated carbon, adsorbing and decoloring, adjusting to neutrality, concentrating and crystallizing to obtain sodium sulfate solid, filtering, and evaporating concentrated acid again from the filtered mother solution to obtain sodium thiosulfate solid. The purity of the sodium sulfate solid reaches about 90 percent; the purity of the sodium thiosulfate product reaches about 93 percent.
Claims (8)
1. An environment-friendly production process of 1-aminoanthraquinone is characterized in that anthraquinone is used as a reaction raw material, 1-aminoanthraquinone is produced by adopting a nitration reduction method, and the produced wastewater is subjected to resource treatment in the production process.
2. The environment-friendly production process of 1-aminoanthraquinone according to claim 1, characterized in that the resource treatment of waste water comprises the following steps:
(1) adding the 1-aminoanthraquinone nitration reduction wastewater into an adsorption reaction kettle, and adding high molecular resin into the adsorption reaction kettle to obtain a treatment solution 1; adsorbing part of organic pollutants in the wastewater; then adding the resin saturated by adsorption into a desorption regeneration reaction kettle for desorption and regeneration under an alkaline condition;
(2) adding acid into the treatment solution 1, adjusting the pH value of the wastewater to acidity, absorbing harmful acidic gas generated in the acid adding process by using ammonia water, and then filtering to obtain a treatment solution 2;
(3) adding an alkaline solution into the treatment solution 2, adjusting to be alkaline, and adding an oxidant for oxidation treatment to obtain a treatment solution 3;
(4) adding acid into the treatment solution 3 to adjust the solution to acidity, adding activated carbon, adsorbing and decoloring, adjusting to neutrality, and concentrating and crystallizing.
3. An environmentally friendly process for the production of 1-aminoanthraquinone according to claim 2, wherein said adsorbent is a polystyrene resin or a polyacrylate resin.
4. The environment-friendly production process of 1-aminoanthraquinone according to claim 2, wherein the dosage of said polymeric resin is 0.5-0.6 kg/L.
5. The environment-friendly production process of 1-aminoanthraquinone according to claim 2, wherein in the step (2), the pH value of the treatment solution 1 is adjusted to 3-6 by adding acid.
6. The environment-friendly production process of 1-aminoanthraquinone according to claim 2, characterized in that in the step (2), harmful acid gases are absorbed by adopting a spraying absorption mode; the concentration of the ammonia water is 8-10%.
7. An environmentally friendly process for the production of 1-aminoanthraquinone according to claim 2, wherein said alkaline solution in step (3) is sodium hydroxide solution.
8. The environment-friendly production process of 1-aminoanthraquinone according to claim 2, characterized in that the oxidant in step (3) is at least one of ozone, hydrogen peroxide, chlorine dioxide liquid, chlorine dioxide solid or sodium hypochlorite.
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| CN105502779A (en) * | 2014-12-31 | 2016-04-20 | 浙江奇彩环境科技股份有限公司 | Treatment method of waste water generated in condensation reaction during disperse blue 56 production process |
| CN110759545A (en) * | 2019-12-02 | 2020-02-07 | 江苏永葆环保科技有限公司 | Treatment method of anthraquinone dye waste acid |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105502779A (en) * | 2014-12-31 | 2016-04-20 | 浙江奇彩环境科技股份有限公司 | Treatment method of waste water generated in condensation reaction during disperse blue 56 production process |
| CN105060552A (en) * | 2015-04-10 | 2015-11-18 | 浙江奇彩环境科技有限公司 | Method for treating disperse blue 56 reduction mother liquor wastewater |
| CN105174582A (en) * | 2015-09-15 | 2015-12-23 | 山东农业大学 | Resource treatment process of 1-amino anthraquinone sulfurization reduction wastewater |
| CN110759545A (en) * | 2019-12-02 | 2020-02-07 | 江苏永葆环保科技有限公司 | Treatment method of anthraquinone dye waste acid |
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