CN111995523B - Resource utilization method of waste acid liquid of nitrobenzoic acid derivatives - Google Patents
Resource utilization method of waste acid liquid of nitrobenzoic acid derivatives Download PDFInfo
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- C01B17/69—Sulfur trioxide; Sulfuric acid
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Abstract
The invention relates to a recycling method of nitrobenzoic acid derivative waste acid liquid, wherein after the waste acid liquid is subjected to unit operation treatment such as pre-concentration, nitration, primary separation, nitric acid concentration, secondary separation, sulfuric acid recovery and the like, nitrobenzoic acid derivative and nitric acid in the waste acid liquid can be effectively recovered, the recovery rate of the nitrobenzoic acid derivative is more than or equal to 95%, and the recovery rate of the nitric acid is more than or equal to 95%; according to the treatment method disclosed by the invention, various effective resources in the waste liquid are effectively recovered, the recycling utilization of the waste acid liquid of the nitrobenzoic acid derivatives is completed, the zero emission is realized in the whole process, and the method has good environmental protection significance and economic benefits.
Description
Technical Field
The invention belongs to the technical field of chemical industry, and particularly relates to a resource utilization method of waste acid liquid of nitrobenzoic acid derivatives.
Background
The nitrobenzoic acid derivative chemical products are important intermediates for producing pesticides, medicines, fine chemical products and explosives, the products mostly adopt the production process of nitric acid nitration, and water is added to dilute the products after the nitration reaction is finished to crystallize and separate out required organic matters, so that a large amount of waste nitric acid containing the nitrobenzoic acid derivative is produced.
Because the waste acid has high organic matter content and low nitric acid content, and is difficult to directly use, the waste acid is usually treated by a dilution neutralization salt recovery method, sodium hydroxide or ammonia water is added into the waste acid liquid, the pH value is regulated to about 7, and the waste acid is filtered and evaporated to obtain salt. The method has the advantages that the dosage of the neutralizing treatment agent is large, the neutralized waste liquid needs secondary treatment, the operation cost is high, and the development of enterprises is limited while the resources are seriously wasted.
Patent CN 109052775A discloses a method for treating p-nitrobenzoic acid production wastewater, which comprises the following steps: (1) resin adsorption: introducing the wastewater into a container filled with adsorption resin for resin adsorption to obtain adsorption liquid; (2) and (3) low-temperature concentration: introducing the adsorption liquid into concentrating equipment, and concentrating at the temperature of 70-95 ℃ to obtain nitric acid recovery liquid and condensate; (3) resin regeneration: introducing a regenerant into the container containing the adsorbed resin in the step (1) for regeneration to obtain a regenerated liquid, and rectifying the regenerated liquid to obtain a rectifying component and a bottom liquid; the invention mainly aims at the treatment of wastewater containing nitric acid, methanol is needed to be used as a resin regenerant, and organic matters such as benzoic acid, nitrobenzoic acid and the like are directly burnt for treatment, so that resources are wasted; and the resin has requirements on the content of nitric acid in the wastewater, and the application range is limited.
Patent CN108218710a discloses a comprehensive utilization method of m-methylbenzoic acid nitration reaction solid waste, which comprises the following steps: (1) Dissolving the solid waste of the m-methylbenzoic acid nitration reaction with alkaline water, and controlling the PH value of the solution to be 7.5-13 to obtain a clear solution; (2) Regulating the pH value of the clarified solution to 4.0-5.5 by using acid to obtain slurry, filtering to obtain a first filtrate and a first filter cake, pulping and filtering the first filter cake by using water to obtain a 3-methyl-4-nitrobenzoic acid product; (3) Adjusting the pH value of the first filtrate to 2.5-4.0 by using acid, filtering to obtain a second filtrate and a second filter cake, pulping and filtering the second filter cake by using water to obtain a 2-nitro-3-methylbenzoic acid product; (4) And (3) regulating the pH value of the second filtrate to 0-2.5 by using acid, filtering to obtain a third filtrate and a third filter cake, pulping and filtering the third filter cake by using water to obtain a 2-nitro-5-methylbenzoic acid product. The invention mainly recovers nitrobenzoic acid organic matters in solid waste, needs to respectively adjust the pH value by alkali and acid, increases consumption and forms secondary pollution.
Patent CN108128826a discloses a nitric acid-containing wastewater treatment device and a treatment method, which are used for treating pure nitric acid nitrified wastewater, and realizing zero emission in the whole process. The treatment device comprises a nitrifying kettle, a first closed filter, a beating pot, a filter press, a diluting kettle, a second closed filter, a distilling kettle, a condenser, a nitrifying mother liquor collecting tank, a diluting mother liquor storage tank and a nitric acid recovery storage tank, wherein the outlet of the nitrifying kettle is connected with the inlet of the first closed filter, the first outlet of the first closed filter is connected with the inlet of the nitrifying mother liquor collecting tank, the second outlet of the first closed filter is connected with the first inlet of the beating pot, the outlet of the beating pot is connected with the first inlet of the filter press, the first outlet of the filter press is connected with the first inlet of the diluting kettle, the outlet of the diluting kettle is connected with the inlet of the second closed filter, and the outlet of the second closed filter is connected with the inlet of the diluting mother liquor storage tank, the distilling kettle, the condenser and the nitric acid recovery storage tank in sequence. The invention mainly adopts a gradient washing mode to treat the nitrified substances after the nitration reaction of m-nitrobenzoic acid.
Along with the increasing strictness of environmental protection policy, it is urgent to find a method for treating waste liquid of nitrobenzoic acid derivatives, which is environment-friendly and saves resources, and has good environmental protection significance and economic benefit.
Disclosure of Invention
The invention aims to provide a resource utilization method of waste acid liquid of nitrobenzoic acid derivatives, which effectively recovers various resources in the waste acid liquid, recovers and converts the waste acid liquid into nitric acid meeting production requirements, and recycles the nitric acid into a production device; and simultaneously, organic matters are recycled and turned into wealth, and zero emission is realized in the whole process.
In order to achieve the above purpose, the invention adopts the following technical scheme:
a method for recycling waste acid liquid of nitrobenzoic acid derivatives comprises the following steps:
(1) Pre-concentration: treating the waste acid liquid by a pre-concentration tower, removing part of water from the tower top, and obtaining pre-concentrated nitric acid liquid from the tower bottom;
(2) Nitrifying: pre-concentrated nitric acid solution and a certain amount of N 2 O 5 The gas is subjected to nitration reaction in a nitration reactor, and benzoic acid derivatives remained in the waste acid liquid are converted into nitrobenzoic acid derivatives, so that nitration reaction liquid is obtained;
(3) Primary separation: the nitration reaction liquid obtained by the nitration reaction is subjected to cooling treatment and solid-liquid separation to obtain primary separation filtrate, and part of nitrobenzoic acid derivatives are recovered;
(4) Concentrating nitric acid: feeding the primary separation filtrate into a nitric acid concentration tower, concentrating nitric acid in the presence of a dehydrating agent, and obtaining finished nitric acid at the tower top;
(5) Secondary separation: cooling the bottom liquid of the nitric acid concentration tower, completely separating out the solid of the residual nitrobenzoic acid derivatives, and carrying out solid-liquid separation again to obtain the residual nitrobenzoic acid derivatives, so that the organic matters in the waste acid liquid can be completely recovered;
(6) Sulfuric acid recovery: concentrating the secondary separation filtrate under reduced pressure to obtain recovered sulfuric acid, and circularly sleeving the recovered sulfuric acid in the step (4).
Preferably, the nitrifying liquid obtained in the step (2) contains nitrobenzoic acid derivatives, and the nitrobenzoic acid derivatives have a structure shown in a chemical formula 1:
1 (1)
Wherein R is a straight or branched hydrocarbon group of 1 to 8 carbon atoms; n is an integer of 0 to 4; m is an integer of 1 to 4, and the sum of n and m is not more than 5.
Preferably, the pre-concentration treatment in step (1) is performed under normal pressure or reduced pressure.
Preferably, the pre-concentration treatment in step (1) is carried out at a pressure of 20-101KPa.
Preferably, the mass concentration of the pre-concentrated nitric acid solution in the step (1) is 50% -68%.
Preferably, in step (2), N 2 O 5 The molar ratio of the benzoic acid derivative to the benzoic acid derivative in the waste acid liquid in the step (1) is 1-2:1.
Preferably, the dehydrating agent in the nitric acid concentration in the step (4) is non-volatile sulfuric acid, and the mass fraction of the sulfuric acid is 80-98%.
Preferably, the mass ratio of the dehydrating agent to the primary separation filtrate in the step (4) is 1.2-2.5:1.
Preferably, in the step (4), the mass concentration of the obtained finished nitric acid is 95-98%.
Preferably, in the step (6), the mass concentration of the recovered sulfuric acid is 80% -96%.
Preferably, in step (6), the reaction pressure is 2-15Kpa and the reaction temperature is 180-190 ℃.
By adopting the technology, compared with the prior art, the invention has the following beneficial effects:
1) The process is simple, the operation is convenient, no alkali is needed for neutralization in the treatment process, and secondary pollution is avoided;
2) The sulfuric acid is used as a dehydrating agent for nitric acid concentration, so that nitric acid and organic matters can be effectively separated, good dehydrating capability can be maintained, the recovered sulfuric acid can be recycled, and no new three wastes are generated;
3) The environmental protection benefit is obvious, the three wastes discharge is effectively reduced, the whole process realizes zero discharge, and the environmental protection is realized;
4) The finished nitric acid can be directly used for the nitration reaction of benzoic acid derivatives, and the recovered nitrobenzoic acid derivatives can be used in the fields of medicines and pesticides after being refined, so that the production cost is reduced, waste is turned into wealth, resources are saved, and good economic benefits are achieved.
Drawings
FIG. 1 is a process flow diagram of the resource utilization of waste acid liquid of nitrobenzoic acid derivatives;
in the figure: 1. the device comprises a pre-concentration tower, a nitration reactor, 3 # solid-liquid separators, 1# solid-liquid separators, 4 # nitric acid concentration towers, 5 # solid-liquid separators, 2# solid-liquid separators, 6 # sulfuric acid concentration towers.
Detailed Description
The invention is further elucidated below in connection with the drawings and the detailed description.
The specific components of the acid pickle used in the following examples are as follows:
the waste acid liquid of nitrobenzoic acid derivatives of certain Shandong enterprise has the mass concentration of nitric acid of about 30%, the mass concentration of benzoic acid derivatives of about 1%, the mass concentration of nitrobenzoic acid derivatives of about 2% and the balance of water.
COD was found to be about 20000mg/l as determined by the protocol in HJ 828-2017.
Example 1
The waste acid liquid continuously enters the pre-concentration tower 1 at the flow rate of 1000 kg/h. Heating and concentrating the distilled water by controlling the pressure in the tower to be 101KPa, continuously extracting, condensing and collecting distilled water from the top of the pre-concentrating tower 1, controlling the extraction temperature of the tower kettle to be 115 ℃, and continuously extracting to obtain nitric acid liquid with the nitric acid mass concentration of 50%; then with N 2 O 5 Continuously pumping gas into a continuous nitration reactor 2 to carry out nitration reaction, and controlling N 2 O 5 The gas flow rate is 3.0 m 3 And (h) cooling the obtained nitration reaction liquid to room temperature, and then, entering a No. 1 solid-liquid separator 3, and carrying out solid-liquid separation to obtain nitrobenzoic acid derivatives and primary filtrate; continuously feeding the filtrate into a nitric acid concentration tower 4 at a flow rate of 580kg/h, continuously adding 98% sulfuric acid as a dehydrating agent at a flow rate of 750kg/h, heating and distilling to obtain nitric acid steam from the tower top, condensing, bleaching, and removing NO x Obtaining finished nitric acid; cooling tower bottom liquid to room temperature, and then entering a No. 2 solid-liquid separator 5, and carrying out solid-liquid separation to obtain nitrobenzoic acid derivatives and secondary filtrate again; the secondary filtrate enters a sulfuric acid concentration tower 6, is continuously distilled at the temperature of 2KPa and 180 ℃, water is extracted from the top of the tower and is condensed and collected, and the recovered sulfuric acid extracted from the tower bottom is recycled after being collected.
Detection and analysis: the mass concentration of the finished nitric acid is 96.3%, and the recovery rate of nitric acid is 97.1%; the COD of the finished nitric acid is 520mg/l; the total recovery rate of the organic matters (nitrobenzoic acid derivatives) is 95.6 percent; the mass concentration of sulfuric acid in the recovered sulfuric acid is 95.6%, and the COD of the recovered sulfuric acid is 120mg/l.
Example 2
The waste acid liquid continuously enters the pre-concentration tower 1 at the flow rate of 1000 kg/h. Heating and concentrating the distilled water at 50KPa, continuously extracting, condensing and collecting the distilled water from the top of the pre-concentrating tower 1, controlling the extraction temperature of the tower kettle to be 117 ℃, and continuously extracting to obtain nitric acid liquid with the mass concentration of 57%; then with N 2 O 5 Continuously pumping gas into a continuous nitration reactor 2 to carry out nitration reaction, and controlling N 2 O 5 The gas flow rate is 2.5 m 3 And (h) cooling the obtained nitration reaction liquid to room temperature, and then, entering a No. 1 solid-liquid separator 3, and carrying out solid-liquid separation to obtain nitrobenzoic acid derivatives and primary filtrate; the filtrate continuously enters a nitric acid concentration tower 4 at the flow rate of 510kg/h, simultaneously, 95 percent of recovered sulfuric acid is continuously added at the flow rate of 800kg/h to be used as a dehydrating agent, nitric acid steam obtained from the tower top is heated and distilled, and NO is removed after condensation and bleaching treatment x Obtaining finished nitric acid; cooling tower bottom liquid to room temperature, and then entering a No. 2 solid-liquid separator 5, and carrying out solid-liquid separation to obtain nitrobenzoic acid derivatives and secondary filtrate again; the secondary filtrate enters a sulfuric acid concentration tower 6, is continuously distilled at the temperature of 3KPa and 185 ℃, water is extracted from the top of the tower and is condensed and collected, and the recovered sulfuric acid extracted from the tower bottom is recycled after being collected.
Detection and analysis: the mass concentration of the finished nitric acid is 96.8%, and the recovery rate of the nitric acid is 96.3%; the COD of the finished nitric acid is 440mg/l; the total recovery rate of the organic matters (nitrobenzoic acid derivatives) is 95.4 percent; the mass concentration of sulfuric acid in the recovered sulfuric acid is 95.2%, and the COD of the recovered sulfuric acid is 142mg/l.
Example 3
The waste acid liquid continuously enters the pre-concentration tower 1 at the flow rate of 1000 kg/h. Heating and concentrating the distilled water at 50KPa pressure, continuously extracting, condensing and collecting distilled water from the top of the pre-concentrating tower 1, controlling the extraction temperature of the tower kettle to be 119 ℃, and continuously extracting to obtain nitric acid liquid with the nitric acid mass concentration of 65%; then with N 2 O 5 Continuously pumping gas into a continuous nitration reactor 2 to carry out nitration reaction, and controlling N 2 O 5 The gas flow rate is 2.0. 2.0 m 3 And (h) cooling the obtained nitration reaction liquid to room temperature, and then, entering a No. 1 solid-liquid separator 3, and carrying out solid-liquid separation to obtain nitrobenzoic acid derivatives and primary filtrate; the filtrate continuously enters a nitric acid concentration tower 4 at a flow rate of 445kg/h, 92 percent of recovered sulfuric acid is continuously added at a flow rate of 900kg/h to be used as a dehydrating agent, nitric acid steam obtained from the tower top is heated and distilled, and NO is removed after condensation and bleaching treatment x Obtaining finished nitric acid; cooling tower bottom liquid to room temperature, and then entering a No. 2 solid-liquid separator 5, and carrying out solid-liquid separation to obtain nitrobenzoic acid derivatives and secondary filtrate again; the secondary filtrate enters a sulfuric acid concentration tower 6, is continuously distilled under the conditions of 7KPa and 190 ℃, water is extracted from the top of the tower and is condensed and collected, and the recovered sulfuric acid extracted from the tower bottom is recycled after being collected.
Detection and analysis: the mass concentration of the finished nitric acid is 97.9%, and the recovery rate of nitric acid is 95.4%; the COD of the finished nitric acid is 470mg/l; the total recovery rate of the organic matters (nitrobenzoic acid derivatives) is 95.8 percent; the mass concentration of sulfuric acid in the recovered sulfuric acid is 92.4%, and the COD of the recovered sulfuric acid is 133mg/l.
Example 4
The waste acid liquid continuously enters the pre-concentration tower 1 at the flow rate of 1000 kg/h. Heating and concentrating the distilled water at the pressure of 30KPa, continuously extracting, condensing and collecting distilled water from the top of the pre-concentrating tower 1, controlling the extraction temperature of the tower kettle to be 120 ℃, and continuously extracting to obtain nitric acid liquid with the nitric acid mass concentration of 68%; then with N 2 O 5 Continuously pumping gas into a continuous nitration reactor 2 to carry out nitration reaction, and controlling N 2 O 5 The gas flow rate is 2.0. 2.0 m 3 And (h) cooling the obtained nitration reaction liquid to room temperature, and then, entering a No. 1 solid-liquid separator 3, and carrying out solid-liquid separation to obtain nitrobenzoic acid derivatives and primary filtrate; the filtrate continuously enters a nitric acid concentration tower 4 at a flow rate of 425kg/h, simultaneously, 90 percent of recovered sulfuric acid is continuously added at a flow rate of 1000kg/h to be used as a dehydrating agent, nitric acid steam obtained from the tower top is heated and distilled, and NO is removed after condensation and bleaching treatment x Obtaining finished nitric acid; cooling tower bottom liquid to room temperature and then enteringA No. 2 solid-liquid separator 5 for solid-liquid separation to obtain nitrobenzoic acid derivatives and secondary filtrate again; the secondary filtrate enters a sulfuric acid concentration tower 6, is continuously distilled at the temperature of 10KPa and 185 ℃, water is extracted from the top of the tower and is condensed and collected, and the recovered sulfuric acid extracted from the tower bottom is recycled after being collected.
Detection and analysis: the mass concentration of the finished nitric acid is 98.0%, and the recovery rate of nitric acid is 95.0%; the COD of the finished nitric acid is 411mg/l; the total recovery rate of the organic matters (nitrobenzoic acid derivatives) is 95.2 percent; the mass concentration of sulfuric acid in the recovered sulfuric acid is 90.2%, and the COD of the recovered sulfuric acid is 162mg/l.
Example 5
The waste acid liquid continuously enters the pre-concentration tower 1 at the flow rate of 1000 kg/h. Heating and concentrating the distilled water at the pressure of 20KPa, continuously extracting, condensing and collecting distilled water from the top of the pre-concentrating tower 1, controlling the extraction temperature of the tower kettle to be 115 ℃, and continuously extracting to obtain nitric acid liquid with the nitric acid mass concentration of 50%; then with N 2 O 5 Continuously pumping gas into a continuous nitration reactor 2 to carry out nitration reaction, and controlling N 2 O 5 The gas flow rate is 3.2 m 3 And (h) cooling the obtained nitration reaction liquid to room temperature, and then, entering a No. 1 solid-liquid separator 3, and carrying out solid-liquid separation to obtain nitrobenzoic acid derivatives and primary filtrate; continuously feeding the filtrate into a nitric acid concentration tower 4 at a flow rate of 580kg/h, continuously adding 88% recovered sulfuric acid as a dehydrating agent at a flow rate of 1200kg/h, heating and distilling to obtain nitric acid steam from the tower top, condensing, bleaching, and removing NO x Obtaining finished nitric acid; cooling tower bottom liquid to room temperature, and then entering a No. 2 solid-liquid separator 5, and carrying out solid-liquid separation to obtain nitrobenzoic acid derivatives and secondary filtrate again; the secondary filtrate enters a sulfuric acid concentration tower 6, is continuously distilled at 15KPa and 180 ℃, water is extracted from the top of the tower and is condensed and collected, and the recovered sulfuric acid extracted from the tower bottom is recycled after being collected.
Detection and analysis: the mass concentration of the finished nitric acid is 97.2%, and the recovery rate of nitric acid is 95.7%; the COD of the finished nitric acid is 454mg/l; the total recovery rate of the organic matters (nitrobenzoic acid derivatives) is 95.9 percent; the mass concentration of sulfuric acid in the recovered sulfuric acid is 88.7%, and the COD of the recovered sulfuric acid is 188mg.
The above embodiments are only preferred embodiments of the present invention, and should not be construed as limiting the present invention, and the protection scope of the present invention should be defined by the claims, including the technical equivalents of the technical features in the claims, as the protection scope, that is, the equivalent replacement and improvement within the protection scope of the present invention.
Claims (4)
1. A method for recycling waste acid liquid of nitrobenzoic acid derivatives is characterized by comprising the following steps: after pre-concentrating, nitrifying, primary separating, concentrating nitric acid, secondary separating and recycling sulfuric acid, recycling organic matters and nitric acid in the waste acid liquid;
the method comprises the following steps:
(1) Pre-concentration: treating the waste acid liquid by a pre-concentration tower to obtain pre-concentrated nitric acid liquid;
(2) Nitrifying: pre-concentrated nitric acid solution and a certain amount of N 2 O 5 The gas is subjected to nitration reaction in a nitration reactor, and benzoic acid derivatives remained in the waste acid liquid are converted into nitrobenzoic acid derivatives, so that nitration reaction liquid is obtained;
(3) Primary separation: the nitration reaction liquid is cooled and subjected to solid-liquid separation to obtain primary separation filtrate, and organic matters are recovered;
(4) Concentrating nitric acid: sending the primary separation filtrate into a nitric acid concentration tower, and concentrating nitric acid in the presence of a dehydrating agent to obtain finished nitric acid;
(5) Secondary separation: cooling and solid-liquid separating the bottom liquid of the nitric acid concentration tower to obtain secondary separation filtrate, and recovering organic matters;
(6) Sulfuric acid recovery: concentrating the secondary separation filtrate under reduced pressure to obtain sulfuric acid, and recycling the sulfuric acid in the step (4);
the nitrifying reaction liquid obtained in the step (2) contains nitrobenzoic acid derivatives, and the nitrobenzoic acid derivatives have a structure shown in a chemical formula 1:
wherein R is a straight or branched hydrocarbon group of 1 to 8 carbon atoms; n is an integer of 0 to 4; m is an integer of 1 to 4, and the sum of n and m is not more than 5;
the pre-concentration treatment in the step (1) is carried out under normal pressure or reduced pressure;
the mass concentration of the pre-concentrated nitric acid solution in the step (1) is 50% -68%;
n in step (2) 2 O 5 The molar ratio of the benzoic acid derivative in the waste acid liquid in the step (1) is 1-2: 1, a step of;
the dehydrating agent in the step (4) is sulfuric acid with the mass fraction of 80-98%.
2. The method for recycling the waste acid liquid of the nitrobenzoic acid derivatives according to claim 1, which is characterized in that: in the step (4), the mass ratio of the dehydrating agent to the primary separation filtrate is 1.2-2.5: 1.
3. the method for recycling the waste acid liquid of the nitrobenzoic acid derivatives according to claim 1, which is characterized in that: the mass concentration of the finished nitric acid in the step (4) is 95-98%.
4. The method for recycling the waste acid liquid of the nitrobenzoic acid derivatives according to claim 1, which is characterized in that: the mass concentration of the recovered sulfuric acid in the step (6) is 80% -96%.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108128826A (en) * | 2017-12-28 | 2018-06-08 | 江苏吉华化工有限公司 | A kind of wastewater treatment equipment containing nitric acid and processing method |
| CN108218710A (en) * | 2017-12-13 | 2018-06-29 | 江西科苑生物药业有限公司 | A kind of method of comprehensive utilization of m-methyl benzoic acid nitration reaction solid waste |
| CN111620397A (en) * | 2020-06-24 | 2020-09-04 | 山东友道化学有限公司 | Treatment system and treatment method for nitric acid-containing system |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108218710A (en) * | 2017-12-13 | 2018-06-29 | 江西科苑生物药业有限公司 | A kind of method of comprehensive utilization of m-methyl benzoic acid nitration reaction solid waste |
| CN108128826A (en) * | 2017-12-28 | 2018-06-08 | 江苏吉华化工有限公司 | A kind of wastewater treatment equipment containing nitric acid and processing method |
| CN111620397A (en) * | 2020-06-24 | 2020-09-04 | 山东友道化学有限公司 | Treatment system and treatment method for nitric acid-containing system |
Non-Patent Citations (3)
| Title |
|---|
| 00Cr14Ni14Si4钢的焊接工艺性;文明;《金属加工（热加工）》;20171231(第2017年第S1期);第127-128页 * |
| 中华人民共和国劳动部职业安全卫生与锅炉压力容器监察局编.2.4.2 事故树分析法.《工业防爆实用技术手册》.辽宁科学技术出版社,1996,(第1996年1月第1版),第1132页. * |
| 吴鹏等主编.硝化.《化学工程与工艺》.中国矿业大学出版社,2013,(第2013年7月第1版),第254-255页. * |
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