CN102910757A - Treatment technique of waste water generated in production of o-nitrophenol - Google Patents
Treatment technique of waste water generated in production of o-nitrophenol Download PDFInfo
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- CN102910757A CN102910757A CN201210373446XA CN201210373446A CN102910757A CN 102910757 A CN102910757 A CN 102910757A CN 201210373446X A CN201210373446X A CN 201210373446XA CN 201210373446 A CN201210373446 A CN 201210373446A CN 102910757 A CN102910757 A CN 102910757A
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Abstract
The invention discloses treatment technique of waste water generated in production of o-nitrophenol. The treatment technique comprises the following steps: firstly, pretreating waste water, entering a resin adsorption column for adsorption, desorbing the resin by adopting NaOH solution after the resin adsorption is saturated, adding acid into high-concentration desorption solution for acidizing so as to recover o-nitrophenol, wherein a low-concentration desorption solution sleeve is used for desorption, distilling and purifying the recovered o-nitrophenol, conducting hydrogenation and catalysis to produce o-nitrophenol; carrying out ozone oxidation, neutralization and decoloration on the waste water after being subjected to adsorption treatment, thereby becoming qualified salt water. After the technique is adopted, organic pollution of the waste water to water environment is lightened, the resource utilization can be realized, and the treatment technique has great economic values and practical values in treating the waste water generated in production of o-nitrophenol.
Description
Technical field
The present invention relates to a kind of waste water treatment process, be specifically related to a kind of disposal and utilization of o-NP saliferous factory effluent.
Background technology
O-NP is a kind of important organic intermediate, is widely used in the industry such as dyestuff, medicine, also can be used as analytical reagent, can be used to make oxine, chloro sulphur phenol S, Ortho-Aminophenol etc.
There are a lot of reports the treatment technology aspect of relevant o-NP factory effluent, such as iron carbon reduction+anaerobism+oxygen consumption, and extraction treatment method, active carbon adsorption, magnetic strength sodium hypochlorite oxidization, sulfonation matchmaker absorption method, resin adsorption method etc.Some only is confined to bibliographical information and laboratory experiment, and the working cost that has is too high.Resin adsorption method is processed this waste water effect and is better than additive method, and the method not only can reduce COD, can also reclaim o-NP, and the o-NP of recovery can directly return production workshop section.The method has not only been administered waste water, and has improved the product yield of o-NP.
In recent years, adopt the example of resin adsorption method Phenol-Containing Wastewater Treatment more both at home and abroad, but the resinous type that adopts differ greatly.For example, China Jiangsu chemical enterprise has just adopted the macroporous resin device to process the waste water that contains o-NP.Its waste water mainly is to separate the waste water that acidified mother liquor produces in the o-NP production process, and generation is 5439.8t/a, mainly contains part o-NP, sodium-chlor and hydrochloric acid in the waste water, and COD is about 8000-10000mg/L.Above-mentioned waste water is processed through macroporous resin adsorption device, deliver to its company's sewage works and process with macroporous resin regeneration, washes, reached preferably treatment effect, but because its saltiness still is difficult to reach re-set target, treatment effect is not obvious.
Summary of the invention
The present inventor is for waste water in the existing o-NP production process, particularly separate the waste water that acidified mother liquor produces, a kind of brand-new technique of utilizing resin to process is provided, alleviated the organic contamination of waste water to water surrounding, realize simultaneously the utilization of resources, in the processing of o-NP factory effluent, had great economic worth and practical value.
A kind of o-NP production wastewater treatment technique, concrete steps comprise:
(1) Wastewater Pretreatment: waste water enters the Waste Water Centralized pond lowers the temperature and sedimentation, reaches normal temperature, then enters the baffling tank, and to remove degreasing, waste water enters the strainer filtration behind the baffling;
(2) pretreated waste water enters resin absorbing column absorption;
(3) resin after absorption in the step (2) is saturated adopts the sodium hydroxide solution desorption;
(4) high concentration desorption liquid that gets off from step (3) desorption adopts hydrochloric acid soln to carry out acidifying and reclaims o-NP, and the light concentration desorption liquid cover is used for desorption process;
(5) after the liquid after the resin absorbing column absorption is through peroxidation, neutralization, except ammonia, decolouring, obtain sodium chloride brine.
Wherein, because this waste water mainly is the acid mother liquid in the o-NP salt acidifying process, the pH value is about 2～3, and temperature is higher, contain some oils, can damage resin, so can not directly adsorb it with resin, must carry out pre-treatment to it, namely described step (1).
The resin that adopts in the described step (2) is the XDA-1 resin, directly buied by market, it is a kind of high-specific surface area macroporous adsorbent resin, p-nitrophenol class material has efficient adsorption selectivity, and the XDA-1 resin is the resin that a kind of antipollution is strong, suction phenol amount is large, desorption is not affected by salt easily.
Adsorption rate is 1～20BV/h in the described step (2), and is best in this scope internal adsorption effect, with a collection of waste water ratio, if adsorption rate is lower than 1BV/h, can prolong adsorption time, make the wastewater treatment overlong time, production cost increases, and can not satisfy industrial requirement; If be higher than 20BV/h, the too fast meeting of adsorption rate is so that absorption is incomplete, and residual o-NP in the waste water does not reach the expection purpose of wastewater treatment.
Desorption temperature is 30～100 ℃ in the described step (3), owing to produce sodium onitrophenol in the desorption process, if desorption temperature is lower than 30 ℃, sodium onitrophenol crystallization meeting occluding device and pipeline; If be higher than 100 ℃, higher to equipment and requirements for pipes, increased cost for wastewater treatment.
Desorption rate is 1～20BV/h in the described step (3), if desorption rate is excessively slow, can prolong desorption time, the wastewater treatment overlong time, and production cost increases, and can not satisfy need of production; If desorption rate is too fast, then cause desorption not thorough, the o-NP rate of recovery is low, and can reduce the processing power of resin.
Sodium hydroxide solution in the described step (3), with this as desorbing agent, this is because in the actual production, need to reclaim sodium chloride brine, in order not bring other impurity into, thereby select NaOH solution as desorbing agent, after o-NP is reclaimed, do not contain other impurity in the sodium chloride brine, can be back to chlor-alkali production; If select other alkali lye, then can introduce impurity, impurity need to be disposed and just sodium chloride brine can be obtained, be back to the production of chlor-alkali, can increase wastewater treatment step and processing cost like this.
The massfraction of sodium hydroxide solution is 1～10% in the described step (3), if the massfraction of sodium hydroxide solution is excessively low, then can bring a large amount of water into to wastewater treatment, increased wastewater flow rate, reduced the concentration of recuperable sodium chloride brine, treatment effect is bad; If too high, local sodium onitrophenol excessive concentration, easily Crystallization Plugging equipment and pipeline in the time of can causing desorption.
So under such desorption conditions, the complete desorption of the o-NP of resin absorption gets off, so that being able to reprocessing cycle, uses resin, reduced production cost; The sodium chloride brine that finally obtains enters electrolyzer and produces caustic soda as electrolytic solution, with this as the raw material of producing o-NP, thereby realize the harmless treatment of whole waste water, and realized the recycle of resource.
Adopt hydrochloric acid soln to carry out acidifying in the described step (4), this is because in the actual production, needs to reclaim sodium chloride brine, in order not bring other impurity into, thereby select hydrochloric acid soln to carry out acidifying, and do not contain other impurity in the sodium chloride brine that recovery obtains like this, can be back to chlor-alkali production; If select other acid solutions, then can introduce impurity, need to dispose impurity and just can obtain sodium chloride brine, thereby be back to the production of chlor-alkali, can increase wastewater treatment step and processing cost like this.
The massfraction of hydrochloric acid soln is 5%-35% in the described step (4), if the excessive concentration of hydrochloric acid soln, hydrochloric acid volatilizees easily, and cost improves; If concentration is excessively low, can in N-process, bring a large amount of water into, increased wastewater flow rate, and poor processing effect.
Described step (4) middle and high concentration desorption liquid refers to the sodium hydroxide massfraction greater than 5% solution, and light concentration desorption liquid refers to that the sodium hydroxide massfraction is less than 5% solution.The sodium onitrophenol that the reaction of sodium hydroxide and o-NP generates in the high concentration desorption liquid that like this step (3) desorption is got off is near saturated, thereby the employing massfraction is the hydrochloric acid soln of 5%-35% carries out acidifying, recovery obtains o-NP, after passing through distilation again, but hydrogenation catalyst is for the production of Ortho-Aminophenol; Contain completely sodium hydroxide solution of unreacted in the light concentration desorption liquid, can continue and the o-NP reaction, so use when the light concentration desorption liquid cover is used for desorption, realized like this having reduced production cost by resource circulation utilization.
In the described step (5) in the oxidising process used oxygenant be a kind of in clorox, ozone, the potassium permanganate, be preferably ozone.If can there be free chlorine in the employing hypochlorite oxidation, needs could be with the sodium chloride brine reuse after blowing down and processing; If adopt potassium permanganate then can produce solid impurity, need to increase step and the expense of processing solid waste; Why selecting ozone to make oxygenant, is because in oxidising process, can not produce other by products except water and sodium-chlor, introduces other impurity can for the waste water of handling well.
So adopt the o-NP in the ozone oxidation waste water, in and waste water in acidic substance, remove the ammonia nitriding compound, and the processing of decolouring, do not produce other by products and become qualified sodium chloride brine, enter electrolyzer and produce caustic soda as electrolytic solution, with this raw material as the production o-NP, thereby realize the harmless treatment of whole waste water, and realized the recycle of resource.
The present invention at first to the o-NP factory effluent lower the temperature, sedimentation processes, reach normal temperature, then enter the baffling tank, remove oily substance in the waste water, enter the absorption of XDA-1 resin absorbing column through pretreated waste water, adsorption column adopts two posts series connection absorption, when the one-level adsorption column adsorbs near after saturated, make original secondary pillar become the one-level pillar by valve, change original main adsorption column with the 3rd pillar, namely adsorbed saturated one-level adsorption column, do the secondary absorption post, multistage like this continuous adsorption, then absorption is more complete; If it is saturated that the one-level adsorption column has adsorbed, then stop absorption, carry out desorption manipulation, simultaneously the secondary absorption post becomes again the one-level adsorption column, and with the 3rd adsorption column, the i.e. adsorption column of desorption end, the beginning secondary absorption, three posts like this recycle, but operate continuously reduces cost.
For protection of the environment; and saving cost; form the recycle of resource; adopt NaOH solution that resin is carried out desorption; the content of the waste water total ammonia nitrogen after the gained desorption is processed is less than 4ppm; sodium chloride content is about 12%; through ozone oxidation o-NP wherein, in and the acidic substance in the waste water, remove the ammonia nitriding compound; and the processing of decolouring; can become qualified sodium chloride brine, enter electrolyzer and produce caustic soda as electrolytic solution, with this raw material as the production o-NP; thereby realize the harmless treatment of whole waste water, and realized the recycle of resource.
After adopting this treatment process, alleviate the organic contamination of waste water to water surrounding, realized simultaneously the recycle of resource, reduced production cost, in the processing of o-NP factory effluent, had great economic worth and practical value.
Description of drawings
Fig. 1 is the schema of waste water treatment process of the present invention.
Embodiment
Embodiment 1
(1) Wastewater Pretreatment: waste water enters the Waste Water Centralized pond lowers the temperature and sedimentation, reaches normal temperature and then enters the baffling tank, and to remove degreasing, waste water enters strainer behind the baffling, and preprocessing process finishes;
(2) with pretreated 20m
3Waste water enters the absorption of XDA-1 resin absorbing column, and adsorption column adopts Φ 1000 * 5200 specifications, in-built XDA-1 resin 5m
3, adsorption rate is 1BV/h;
(3) the saturated rear resin of absorption in the step (2) being adopted massfraction is that 10% sodium hydroxide solution is made desorbing agent, under 30 ℃ with the speed desorption of 1BV/h;
(4) it is that o-NP is reclaimed in 30% hydrochloric acid soln acidifying that the high concentration desorption liquid that gets off from step (3) desorption adds massfraction, and the light concentration desorption liquid cover is used for desorption process, reclaims altogether o-NP 50.1Kg, and its rate of recovery is 83.5%;
(5) obtain sodium chloride brine after the liquid after the resin absorbing column absorption is through peroxidation, neutralization, except ammonia, decolouring, mass content is 11.48%.
Embodiment 2
(1) Wastewater Pretreatment: waste water enters the Waste Water Centralized pond lowers the temperature and sedimentation, reaches normal temperature and then enters the baffling tank, and to remove degreasing, waste water enters strainer behind the baffling, and preprocessing process finishes;
(2) pretreated 20m
3Waste water enters the absorption of XDA-1 resin absorbing column, and adsorption column adopts Φ 1000 * 5200 specifications, in-built XDA-1 resin 5m
3, adsorption rate is 20BV/h;
(3) the saturated rear resin of absorption in the step (2) is adopted 1% sodium hydroxide solution make desorbing agent, under 100 ℃ with the speed desorption of 20BV/h;
(4) it is that 20% hydrochloric acid soln acidifying is recovered to o-NP that the high concentration desorption liquid that gets off from step (3) desorption adds massfraction, and the light concentration desorption liquid cover is used for desorption process, reclaims altogether o-NP 49.9Kg, and the rate of recovery is 83.2%;
(5) obtain sodium chloride brine after the liquid after the resin absorbing column absorption is through peroxidation, neutralization, except ammonia, decolouring, mass content is 11.49%.
Embodiment 3
(1) Wastewater Pretreatment: waste water enters the Waste Water Centralized pond lowers the temperature and sedimentation, reaches normal temperature and then enters the baffling tank, and to remove degreasing, waste water enters strainer behind the baffling, and preprocessing process finishes;
(2) pretreated 20m
3Waste water enters the absorption of XDA-1 resin absorbing column, and adsorption column adopts Φ 1000 * 5200 specifications, in-built XDA-1 resin 5m
3, adsorption rate is 12BV/h;
(3) the saturated rear resin of absorption in the step (2) being adopted massfraction is that 7% sodium hydroxide solution is made desorbing agent, under 70 ℃ with the speed desorption of 15BV/h;
(4) it is that 5% hydrochloric acid soln acidifying is recovered to o-NP that the high concentration desorption liquid that gets off from step (3) desorption adds massfraction, and the light concentration desorption liquid cover is used for desorption process, reclaims altogether o-NP 51.8Kg, and the rate of recovery is 86.3%;
(5) obtain sodium chloride brine after the liquid after the resin absorbing column absorption is through peroxidation, neutralization, except ammonia, decolouring, mass content is 12.00%.
Embodiment 4
(1) Wastewater Pretreatment: waste water enters the Waste Water Centralized pond lowers the temperature and sedimentation, reaches normal temperature, then enters the baffling tank, and to remove degreasing, waste water enters strainer behind the baffling, and preprocessing process finishes;
(2) pretreated 20m
3Waste water enters the absorption of XDA-1 resin absorbing column, and adsorption column adopts Φ 1000 * 5200 specifications, in-built XDA-1 resin 5m
3, adsorption rate is 8BV/h;
(3) the saturated rear resin of absorption in the step (2) being adopted massfraction is that 4% sodium hydroxide solution is made desorbing agent, under 80 ℃ with the speed desorption of 10BV/h;
(4) it is that o-NP is reclaimed in 35% hydrochloric acid soln acidifying that the high concentration desorption liquid that gets off from step (3) desorption adds massfraction, and the light concentration desorption liquid cover is used for desorption process, reclaims altogether o-NP 59.3Kg, and its rate of recovery is 98.8%;
(5) obtain sodium chloride brine after the liquid after the resin absorbing column absorption is through peroxidation, neutralization, except ammonia, decolouring, mass content is 12.03%.
Can find out that from embodiment 1-4 the rate of recovery of o-NP is more than 83%, pass through distilation again after, but hydrogenation catalyst is for the production of Ortho-Aminophenol; The sodium chloride brine that obtains after the o-NP production wastewater treatment, mass content is about 12%, can enter electrolyzer and produce caustic soda as electrolytic solution, with this raw material as the production o-NP, thereby realize the harmless treatment of whole waste water, and realized the recycle of resource, reduced production cost.
Comparative example
Utilize the sodium chloride brine after treatment process of the present invention is processed embodiment 1-4 gained to compare with processing front waste water, see Table 1:
Before the table 1 o-NP production wastewater treatment and the result after processing relatively
As can be seen from the comparative examples, after utilizing the present invention to process the o-NP factory effluent, the mass content of total ammonia nitrogen is less than 4ppm in the sodium chloride brine that obtains, the mass content of o-NP is less than 1ppm, and the mass content of sodium-chlor is about 12%, can enter electrolyzer and produce caustic soda as electrolytic solution, with this raw material as the production o-NP, thereby realize the harmless treatment of whole waste water, and realized the recycle of resource, reduced production cost.
Claims (8)
1. o-NP production wastewater treatment technique, it is characterized in that: concrete steps comprise:
(1) Wastewater Pretreatment: waste water enters the Waste Water Centralized pond lowers the temperature and sedimentation, reaches normal temperature, then enters the baffling tank, and to remove degreasing, waste water enters the strainer filtration behind the baffling;
(2) pretreated waste water enters resin absorbing column absorption;
(3) resin after absorption in the step (2) is saturated adopts the sodium hydroxide solution desorption;
(4) high concentration desorption liquid that gets off from step (3) desorption adopts hydrochloric acid soln to carry out acidifying and reclaims o-NP, and the light concentration desorption liquid cover is used for desorption process;
(5) after the liquid after the resin absorbing column absorption is through peroxidation, neutralization, except ammonia, decolouring, obtain sodium chloride brine.
2. o-NP production wastewater treatment technique according to claim 1 is characterized in that: the resin that adopts in the described step (2) is the XDA-1 resin.
3. o-NP production wastewater treatment technique according to claim 1 is characterized in that: adsorption rate is 1～20BV/h in the described step (2).
4. o-NP production wastewater treatment technique according to claim 1 is characterized in that: desorption temperature is 30～100 ℃ in the described step (3).
5. o-NP production wastewater treatment technique according to claim 1 is characterized in that: desorption rate is 1～20BV/h in the described step (3).
6. o-NP production wastewater treatment technique according to claim 1 is characterized in that: the massfraction of sodium hydroxide solution is 1%～10% in the described step (3).
7. o-NP production wastewater treatment technique according to claim 1 is characterized in that: the massfraction of hydrochloric acid soln is 5%-35% in the described step (4).
8. o-NP production wastewater treatment technique according to claim 1 is characterized in that: in the described step (5) in the oxidising process used oxygenant be ozone.
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| CN104193071A (en) * | 2014-09-27 | 2014-12-10 | 安徽金禾实业股份有限公司 | Treating method of high-ammonia-nitrogen mother liquor wastewater in MCP (methyl cyclopentenolone) production |
| CN106630297A (en) * | 2017-01-18 | 2017-05-10 | 上海应用技术大学 | Wet-method catalytic oxidation treatment method of vanillin production wastewater |
| CN106865805A (en) * | 2017-03-31 | 2017-06-20 | 莱特莱德（北京）纯水设备技术股份有限公司 | A kind of organic phenols wastewater non-waste-emission device |
| CN107129078A (en) * | 2017-04-28 | 2017-09-05 | 南京环保产业创新中心有限公司 | O-aminophenol wastewater treatment and method of resource |
| CN108002622A (en) * | 2017-11-16 | 2018-05-08 | 王小军 | A kind of method administered with remanufacture benzofuraxan waste liquid |
| CN108046454A (en) * | 2017-12-29 | 2018-05-18 | 南通波涛化工有限公司 | A kind of resin adsorption method pre-processes waster water process containing phenol |
| CN108129271A (en) * | 2018-01-09 | 2018-06-08 | 江苏振方生物化学有限公司 | A kind of method of the chloro- 3,5- dinitro-p-trifluorotoluenes waste water acidification recycling phenol of 4- |
| CN108178364A (en) * | 2017-11-27 | 2018-06-19 | 上海化学工业区中法水务发展有限公司 | The method handled organic matter in high salinity industrial wastewater |
| CN108793493A (en) * | 2018-06-22 | 2018-11-13 | 西安蓝深环保科技有限公司 | O-aminophenol recovery and treatment method in a kind of strong brine |
| CN109081494A (en) * | 2018-09-21 | 2018-12-25 | 宁夏大学 | The device of organic macromolecule in a kind of removal industrial wastewater |
| CN110980864A (en) * | 2019-12-25 | 2020-04-10 | 湖北鸿鑫化工有限公司 | Method for treating o-nitrophenol production wastewater |
| CN114291916A (en) * | 2021-12-31 | 2022-04-08 | 天富凯业(辽宁)新材料有限公司 | System and method for recycling o-aminophenol from o-aminophenol acidification wastewater |
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| CN104193071A (en) * | 2014-09-27 | 2014-12-10 | 安徽金禾实业股份有限公司 | Treating method of high-ammonia-nitrogen mother liquor wastewater in MCP (methyl cyclopentenolone) production |
| CN106630297A (en) * | 2017-01-18 | 2017-05-10 | 上海应用技术大学 | Wet-method catalytic oxidation treatment method of vanillin production wastewater |
| CN106865805B (en) * | 2017-03-31 | 2020-10-27 | 莱特莱德（北京）纯水设备技术股份有限公司 | Organic phenol waste water does not have useless discharging equipment |
| CN106865805A (en) * | 2017-03-31 | 2017-06-20 | 莱特莱德（北京）纯水设备技术股份有限公司 | A kind of organic phenols wastewater non-waste-emission device |
| CN107129078A (en) * | 2017-04-28 | 2017-09-05 | 南京环保产业创新中心有限公司 | O-aminophenol wastewater treatment and method of resource |
| CN108002622A (en) * | 2017-11-16 | 2018-05-08 | 王小军 | A kind of method administered with remanufacture benzofuraxan waste liquid |
| CN108178364A (en) * | 2017-11-27 | 2018-06-19 | 上海化学工业区中法水务发展有限公司 | The method handled organic matter in high salinity industrial wastewater |
| CN108046454A (en) * | 2017-12-29 | 2018-05-18 | 南通波涛化工有限公司 | A kind of resin adsorption method pre-processes waster water process containing phenol |
| CN108129271A (en) * | 2018-01-09 | 2018-06-08 | 江苏振方生物化学有限公司 | A kind of method of the chloro- 3,5- dinitro-p-trifluorotoluenes waste water acidification recycling phenol of 4- |
| CN108793493A (en) * | 2018-06-22 | 2018-11-13 | 西安蓝深环保科技有限公司 | O-aminophenol recovery and treatment method in a kind of strong brine |
| CN109081494A (en) * | 2018-09-21 | 2018-12-25 | 宁夏大学 | The device of organic macromolecule in a kind of removal industrial wastewater |
| CN110980864A (en) * | 2019-12-25 | 2020-04-10 | 湖北鸿鑫化工有限公司 | Method for treating o-nitrophenol production wastewater |
| CN114291916A (en) * | 2021-12-31 | 2022-04-08 | 天富凯业(辽宁)新材料有限公司 | System and method for recycling o-aminophenol from o-aminophenol acidification wastewater |
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| CN114772774B (en) * | 2022-02-21 | 2024-05-28 | 安徽东至广信农化有限公司 | Nitrochlorobenzene production wastewater treatment method |
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