CN1234619C - Method for treating wastewater generated from fabricating nitrophenol as well as for reclaiming and using resources - Google Patents
Method for treating wastewater generated from fabricating nitrophenol as well as for reclaiming and using resources Download PDFInfo
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- CN1234619C CN1234619C CN 200410014570 CN200410014570A CN1234619C CN 1234619 C CN1234619 C CN 1234619C CN 200410014570 CN200410014570 CN 200410014570 CN 200410014570 A CN200410014570 A CN 200410014570A CN 1234619 C CN1234619 C CN 1234619C
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- activated carbon
- carbon fiber
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- nitrophenol
- waste water
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Abstract
The present invention discloses a method for treating waste water of p-nitrophenol production as well as recovering and utilizing resources. The present invention comprises the following technological processes: pretreatment, adsorption of p-nitrophenol in waste water, sodium chloride recovery and utilization, and desorption of adsorbed p-nitrophenol. The present invention is characterized in that the recovery rate of the p-nitrophenol is approximate to 100%, and recovered p-nitrophenol can be reused in a work section. A large amount of sodium chloride in the waste water is utilized to produce sodium hydroxide and hydrochloric acid, the sodium hydroxide and the hydrochloric acid which are used for producing the p-nitrophenol can be cyclically used, and thus, nearly no waste is generated during the production, and the purpose of clean production is achieved.
Description
One, technical field
The present invention relates to the improvement of p-NP factory effluent of industries such as a kind of fine chemistry industry, pharmacy discharging and the method for resource recycling.
Two, background technology
P-NP is a kind of important medicine, agricultural chemicals, dyestuff intermediate.One of its production technique is to be raw material with the p-Nitrophenyl chloride, and is synthetic through reactions such as hydrolysis one acidifyings.P-NP is the priority pollutants in China's water pollution control.P-NP factory effluent pH value is generally 1～2, COD
Cr(chemical aerobic amount) 10000～15000mg/L, p-NP 3000-8000mg/L, sodium-chlor mass concentration 14～15%.P-NP method for treating wastewater to high density mainly contains chemical oxidization method, extraction process, absorption method.Adopt extraction process at present mostly, but still higher through p-NP concentration in the water outlet behind the multi-stage solvent extraction, owing to existing to carry secretly with extraction agent, liquid-liquid extraction in water, dissolves again, contain the extraction agent of a certain amount of loss in the extraction back water outlet, cause secondary pollution.
In existing these methods, the technical process of absorption method and operation are simpler.Sorbing material commonly used has gac, silica gel, activated alumina etc.The report that adsorbents adsorb p-NPs such as flyash, organobentonite and resin have been arranged.But because the absorption property (comprising loading capacity, absorption and desorption rate, work-ing life etc.) of these materials is not ideal enough, make that the sorbent material consumption is big, adsorption tower equipment is huge, investment and working cost be higher.
Activated carbon fiber is the third generation activated carbon product after powdered carbon and granulated active carbon, is a kind of new carbon of getting up along with the carbon fiber industrial development.Because activated carbon fiber has flourishing micropore and huge specific surface area, make that the absorption property of activated carbon fiber is excellent especially, loading capacity is big, and absorption, desorption rate are fast.Adopt activated carbon fiber to make sorbent material, can reduce the consumption of sorbent material and the volume of adsorption tower.
Three, summary of the invention
The object of the invention provides a kind ofly both can effectively administer p-NP waste water, can reclaim simultaneously p-NP wherein, and utilize in the waste water a large amount of sodium-chlor to produce caustic soda and hydrochloric acid, the caustic soda and the hydrochloric acid that need in the p-NP production are recycled, thereby in make producing almost no waste produce, reach the purpose of real cleaner production.
Technical scheme of the present invention is as follows:
A kind of improvement of p-NP factory effluent and the method for resource recycling is characterized in that its technological process is as follows:
A) pre-treatment: the p-NP factory effluent is filtered, get filtrate;
B) p-NP in the absorption waste water: is under the condition of 2～40BV/h at 0～35 ℃ with flow velocity with the filtrate temperature, and flowing through is filled with the adsorption tower of activated carbon fiber, and p-NP is adsorbed on the activated carbon fiber, absorption effluent;
C) recycle sodium-chlor: after adding alkali and transferring to neutrality, adopt electrolytic process to recycle wherein sodium-chlor;
D) the adsorbed p-NP of desorption: with mass concentration is that 0.5～10% aqueous sodium hydroxide solution and water are made desorbing agent, the activated carbon fiber desorption and regeneration of p-NP in the waste water will have been adsorbed, eluting temperature is 30～100 ℃, and the desorbing agent flow velocity is 1～30BV/h.
Pre-treatment described in the steps A, elder generation refilters after the p-NP factory effluent is cooled to 0～30 ℃, reclaims wherein part p-NP.
Activated carbon fiber is 0.2～0.6g p-NP/g to the adsorptive capacity of p-NP in the waste water among the step B; Filtrate temperature described in the step B is controlled at 10～30 ℃, and flow velocity is 5～15BV/h.
Alkali described in the step C is sodium hydroxide, yellow soda ash or sodium bicarbonate.
Described in the step D in the desorbing agent consumption of sodium hydroxide be 0.4～1: 1 with the ratio that has been adsorbed on the p-NP on the activated carbon fiber; Eluting temperature described in the step D is 60～100 ℃, and the desorbing agent flow velocity is 3～10BV/h.
To select model for use be the activated carbon fiber of A10, A12, YT-1000, YT-1300, YT-1600 to activated carbon fiber in the technology, and preferably model is the activated carbon fiber of A10, A12 or YT-1300.
Desorption is an aqueous sodium hydroxide solution desorption of using higher concentration earlier, water wash-out again, the high density elutriant (referring to the elutriant with the aqueous sodium hydroxide solution desorption) that will contain p-NP returns production workshop section and does the raw material use, light concentration desorption liquid preparation next batch desorbing agent, unnecessary light concentration desorption liquid returns the p-NP wastewater disposal basin.
The improvement of p-NP factory effluent of the present invention and the absorption of the p-NP of resource utilization and desorption can adopt the adsorption method of double-column in series absorption and single tower desorption.I, II, three adsorption towers of III promptly are set, earlier with I, the series connection of II tower, the I tower is a first step adsorption tower, and the II tower is a second stage adsorption tower, after the absorption of I tower is saturated, switch to II, III tower series connection absorption, the II tower is a first step adsorption tower, and the III tower is a second stage adsorption tower, and the I tower carries out desorption and regeneration simultaneously, so circulation can make the entire treatment system move continuously.
Beneficial effect of the present invention:
The improvement of p-NP factory effluent of the present invention and resource recycling technology can make the p-NP factory effluent after the present invention handles, the water outlet water white transparency, and the clearance of p-NP and total organic carbon is all near 100%; The rate of recovery of p-NP is near 100%; A large amount of sodium-chlor makes almost no waste discharge of whole production in the waste water as producing the raw material of caustic soda and hydrochloric acid, reaches cleaner production and resource circulation utilization.
Four, embodiment
Embodiment 1:
With pH be about 1～2, the factory effluent of the about 5741mg/L of p-NP, total organic carbon 3326mg/L, sodium-chlor 14% is through overcooling and filtration, recovery part p-NP crystal, pH be about 1～2, the filtrate of p-NP 4395mg/L, total organic carbon 2500mg/L, sodium-chlor mass concentration 14%.
Is the 4g model that the activated carbon fiber (sky, Shenyang scavenging material factory) of A12 is packed into that (15 * 200mm), the activated carbon fiber admission space is 25cm in the glass adsorption column that has chuck
3With filtrate at normal temperatures, flow through activated carbon fiber with the 250mL/h flow velocity and fill bed, wastewater treatment capacity 400mL, the absorption effluent water white transparency, wherein the clearance of p-NP is near 100%, total organic carbon＜20mg/L.
Absorption effluent is regulated about pH to 7 through hydro-oxidation sodium, send diaphragm process chlor-alkali workshop salt refining workshop section, but preparation electrolytic chlorination sodium solution, and work is produced the raw material of caustic soda and hydrochloric acid.
Earlier in chuck about logical hot water heat activated charcoal fiber adsorption layer to 90 ℃, be that 4% aqueous sodium hydroxide solution and the hot water of 75mL are made desorbing agent with the 25mL concentration of heat successively then, desorption temperature is 90 ± 5 ℃, carry out desorption respectively with the activated carbon fiber packed bed of flowing through under the 100mL/h flow velocity, desorption rate＞99% of p-NP behind twice desorption.The high concentration desorption liquid of 25mL directly send acidifying workshop section to carry out reuse before collecting; Light concentration desorption liquid preparation next batch desorbing agent, redundance returns the p-NP wastewater disposal basin.
Embodiment 2:
Change the activated carbon of sorbent fiber among the embodiment 1 into activated carbon fiber that model is models such as A10, YT-1000, YT-1300, YT-1600 respectively, other processing modes are with embodiment 1.Its result is except every batch of wastewater treatment capacity changes to some extent, and other remain unchanged substantially as adsorption effect, desorption rate.
Embodiment 3:
Other conditions among the embodiment 1 are constant, and wastewater treatment capacity is 180mL; With the 25mL concentration of heat is that 2% aqueous sodium hydroxide solution and the hot water of 75mL are made desorbing agent, and its adsorption effect is fine, desorption rate remains unchanged substantially.
Embodiment 4:
Other conditions among the embodiment 1 are constant, and wastewater treatment capacity is 450mL; With the 25mL concentration of heat is that 8% aqueous sodium hydroxide solution and the hot water of 75mL are made desorbing agent, and its adsorption effect better, desorption rate remains unchanged substantially.
Embodiment 5:
A) pre-treatment.With pH be about 1～2, the factory effluent of the about 5741mg/L of p-NP, total organic carbon 3326mg/L, sodium-chlor 14% is through overcooling and filtration, recovery part p-NP crystal, pH be about 1～2, the filtrate of p-NP 4395mg/L, total organic carbon 2500mg/L, sodium-chlor mass concentration 14%.
B) p-NP in the absorption waste water.Select three adsorption towers for use, every tower internal diameter 300mm, tower height 1800mm, 20 kilograms of the activated carbon fiber that every tower filling model is A12, the activated carbon fiber admission space is 0.125m
320 ± 5 ℃ filtrate is delivered into adsorption tower, and the method for I, the absorption of II double-column in series adverse current is adopted in absorption, and absorption flow is 1.25m
3/ h, every batch processing amount 2m
3Waste water is p-NP＜3mg/L after treatment, total organic carbon＜20mg/L.
C) recycle sodium-chlor.It is about 7 that absorption effluent transfers to pH through hydro-oxidation sodium, send diaphragm process chlor-alkali workshop salt refining workshop section to make the raw material of electrolysis production caustic soda and hydrochloric acid.
D) the adsorbed p-NP of desorption.Adsorption treatment 2m
3I adsorption tower aqueous sodium hydroxide solution desorption.Earlier I adsorption tower raffinate is drained,, use 0.125m more respectively afterwards with 100 ℃ hot water adverse current injection adsorption tower and left standstill 20 minutes
34% sodium hydroxide solution and 0.375m
3Water following current desorption, desorption temperature is 90 ± 5 ℃, flow velocity is 0.5m
3/ h.With preceding 0.125m
3High concentration desorption liquid and the back 0.375m
3It is stand-by that light concentration desorption liquid is put into two storage tanks respectively.
High concentration desorption liquid directly send acidifying workshop section to carry out reuse; Light concentration desorption liquid is used to prepare the next batch desorbing agent, and redundance returns the p-NP wastewater disposal basin.
Embodiment 6:
In embodiment 5, in absorption waste water, in the p-NP, adopt winter the method for naturally cooling that the filtrate temperature is controlled at about 5 ℃, flow rate control is at 0.625m
3/ h; Recycle in the sodium-chlor, to transfer to pH be about 7 to absorption effluent through adding yellow soda ash; In the desorption, be that 1% sodium hydroxide and water are made desorbing agent with mass concentration, eluting temperature is about 90 ℃, and the desorption flow velocity is 0.375m
3/ h, other condition is constant.Its result is except every batch of wastewater treatment capacity changes to some extent, and its adsorption effect, desorption rate remain unchanged substantially.
Embodiment 7:
In embodiment 5, in absorption waste water, in the p-NP, adopt the method for naturally cooling that the filtrate temperature is controlled at about 20 ℃ in spring, autumn, flow rate control is at 1.875m
3/ h; Recycle in the sodium-chlor, to transfer to pH be about 7 to absorption effluent through adding sodium bicarbonate; In the desorption, be that 10% sodium hydroxide and water are made desorbing agent with mass concentration, eluting temperature is about 60 ℃, and the desorption flow velocity is 1.25m
3/ h, other condition is constant.Its result is except every batch of wastewater treatment capacity changes to some extent, and its adsorption effect, desorption rate remain unchanged substantially.
Embodiment 8:
In embodiment 5, in absorption waste water, in the p-NP, adopt summer the method for naturally cooling that the filtrate temperature is controlled at about 30 ℃, flow rate control is at 3.75m
3/ h; Recycle in the sodium-chlor, to transfer to pH be about 7 to absorption effluent through adding yellow soda ash; In the desorption, be that 4% sodium hydroxide and water are made desorbing agent with mass concentration, eluting temperature is about 70 ℃, and the desorption flow velocity is 1.875m
3/ h, other condition is constant.Its result is except every batch of wastewater treatment capacity changes to some extent, and its adsorption effect, desorption rate remain unchanged substantially.
Claims (10)
1. the method for the improvement of a p-NP factory effluent and resource recycling is characterized in that its technological process is as follows:
A) pre-treatment: the p-NP factory effluent is filtered, get filtrate;
B) p-NP in the absorption waste water: is under the condition of 2～40BV/h at 0～35 ℃ with flow velocity with the filtrate temperature, and flowing through is filled with the adsorption tower of activated carbon fiber, and p-NP is adsorbed on the activated carbon fiber, absorption effluent;
C) recycle sodium-chlor: after adding alkali and transferring to neutrality, adopt electrolytic process to recycle wherein sodium-chlor;
D) the adsorbed p-NP of desorption: with mass concentration is that 0.5～10% aqueous sodium hydroxide solution and water are made desorbing agent, the activated carbon fiber desorption and regeneration of p-NP in the waste water will have been adsorbed, eluting temperature is 30～100 ℃, and the desorbing agent flow velocity is 1～30BV/h.
2. method according to claim 1 is characterized in that the pre-treatment described in the steps A, and elder generation refilters after the p-NP factory effluent is cooled to 0～30 ℃, reclaims wherein part p-NP.
3. method according to claim 1 is characterized in that activated carbon fiber among the step B is 0.2～0.6g p-NP/g to the adsorptive capacity of p-NP in the waste water.
4. method according to claim 1 is characterized in that the filtrate temperature described in the step B is controlled at 10～30 ℃, and flow velocity is 5～15BV/h.
5. method according to claim 1 is characterized in that the alkali described in the step C is sodium hydroxide, yellow soda ash or sodium bicarbonate.
6. method according to claim 1 is characterized in that described in the step D that the consumption of sodium hydroxide is 0.4～1: 1 with the ratio that has been adsorbed on the p-NP on the activated carbon fiber in the desorbing agent.
7. method according to claim 1 is characterized in that the eluting temperature described in the step D is 60～100 ℃, and the desorbing agent flow velocity is 3～10BV/h.
8. method according to claim 1 is characterized in that the model of activated carbon fiber used in the technology is selected A10, A12, YT-1000, YT-1300, YT-1600 for use.
9. method according to claim 8, the model that it is characterized in that used activated carbon fiber is A10, A12 or YT-1300.
10. method according to claim 1 is characterized in that adopting double-column in series to adsorb in the technology and the adsorption method of single tower desorption.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN 200410014570 CN1234619C (en) | 2004-04-06 | 2004-04-06 | Method for treating wastewater generated from fabricating nitrophenol as well as for reclaiming and using resources |
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| CN 200410014570 CN1234619C (en) | 2004-04-06 | 2004-04-06 | Method for treating wastewater generated from fabricating nitrophenol as well as for reclaiming and using resources |
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| CN1234619C true CN1234619C (en) | 2006-01-04 |
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| CN100352770C (en) * | 2006-01-23 | 2007-12-05 | 南京大学 | Integrated process for treating waste water of p-aminophenol production and resource recovery method |
| CN101514070B (en) * | 2009-04-07 | 2011-11-09 | 达斯玛环境科技（北京）有限公司 | Disposal technique of nitrobenzene-containing sewage |
| CN102464373A (en) * | 2011-10-20 | 2012-05-23 | 常州亚环环保科技有限公司 | Method for removing benzopyrene from drinking water |
| CN102617354B (en) * | 2012-03-07 | 2014-01-01 | 安徽海华科技股份有限公司 | Refining process of o-nitrophenol |
| CN102910757B (en) * | 2012-09-27 | 2013-11-27 | 新泰昊原化工有限责任公司 | Treatment technique of waste water generated in production of o-nitrophenol |
| CN103848472B (en) * | 2014-01-13 | 2016-03-09 | 洛阳智方环保技术有限公司 | A kind of phenolic wastewater removes device and removing process thereof |
| CN103936207B (en) * | 2014-05-15 | 2015-06-10 | 山东大学 | Method for treating nitrophenol wastewater |
| CN106622152A (en) * | 2016-10-20 | 2017-05-10 | 东南大学 | A preparing method and applications of a humic acid-activated charcoal composite adsorbent |
| CN107055899A (en) * | 2017-02-27 | 2017-08-18 | 广东工业大学 | A kind of processing method of the waste water containing high-concentration phenol |
| CN107117749A (en) * | 2017-05-17 | 2017-09-01 | 浙江奇彩环境科技股份有限公司 | A kind of para-aminophenol produces the recycling processing method of waste water |
| US20190003978A1 (en) * | 2017-06-28 | 2019-01-03 | Uop Llc | Process and apparatus to detect mercaptans in a caustic stream |
| CN114873689B (en) * | 2022-04-24 | 2023-07-18 | 河北海力恒远新材料股份有限公司 | Treatment method for waste brine generated in preparation of sodium paranitrophenolate |
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