CN102815844B - Method for pretreating coal chemical industry production waste water and recycling resources of waste water - Google Patents
Method for pretreating coal chemical industry production waste water and recycling resources of waste water Download PDFInfo
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Abstract
The invention discloses a method for pretreating coal chemical industry production waste water and recycling resources of the waste water. According to the technical scheme, the method comprises the following steps of: (1) performing rectification, deacidification and deamination, namely feeding the coal chemical industry waste water into a rectification, deacidification and deamination tower, transferring ammonia and carbon dioxide in the waste water from a liquid phase to a gas phase, and respectively recycling 15 to 20 percent of ammonia water and ammonium bicarbonate; and (2) performing complexing extraction and recycling phenolic substances, namely adjusting the pH of the rectified residual solution in a kettle to be less than 3 by acid, adding a prepared oil phase according to a certain proportion, performing complexing extraction, after extraction is balanced, obtaining a load oil phase and pretreated waste water, performing reverse extraction on the load oil phase by sodium hydroxide solution serving as an extraction agent to obtain a concentrated sodium phenolate solution and a regenerated oil phase, acidifying the sodium phenolate to obtain crude phenol, and recycling the regenerated oil phase. Compared with the prior art, the method has the advantages that the technical flow is simple; the equipment investment is small, the energy consumption is low, the efficiency is high, and the phenol recycling rate is high; harmlessness and reclamation of the waste water are realized; and the method is obvious in economical and environmental benefits.
Description
Technical field
The invention belongs to water-treatment technology field, be specifically related to the pre-treatment of a kind of Coal Chemical Industry factory effluent and resource recycle method thereof.
Background technology
Coal Chemical Industry is the basis and one of main pillar of China's chemical industry.Coal chemical industrial waste water is the high concentrated organic wastewater producing in coal coke processed, gas purification and coke chemicals removal process.The source of coal chemical industrial waste water mainly contains gasification waste water, gelatin liquefaction waste water, dry distillation of coal waste water (coking chemical waste water or blue charcoal waste water).Coal chemical industrial waste water contains the hazardous and noxious substances such as a large amount of phenols, alkanes, arene, heterocyclic and ammonia nitrogen.The bottleneck of restriction China Developing Coal Chemical Industry is not only in the processing of coal chemical industrial waste water, is also a great problem of domestic and international Chemical Industry facing.
Chinese patent application CN100484894C has introduced a kind of method of single tower compression rectification gas treatment waste water.The method divides hot and cold two strands from the rectifier with lateral line withdrawal function and middle and upper part, to enter in tower coal gasification waste water, from tower top rectifying, go out gas mixture through phase-splitting, washing and isolate light oil, acid gas etc., from side line extraction ammoniacal liquor gas through two-stage fractional condensation, the refining liquefied ammonia that to obtain, from still liquid and organic solvent counter-current extraction, the rectifying separation of extraction at the bottom of tower, go out crude phenols and organic solvent, extracting phase reclaims organic solvent through the rectifying of solvent distillation tower.
Chinese patent application CN102180569A has introduced a kind of blue charcoal Waste Water Treatment.This system comprises strengthening pre-treatment and comprehensive treating process.Strengthening pretreatment system comprises adjusting, oil removing, dephenolize, desulfurization, five unit of ammonia still process, and total system mainly adopts A2/O2 biochemical process.
Chinese patent application CN101781067B has introduced a kind of coking waste water treatment method.The method mainly adopts iron carbon-Fenton reagent oxide compound technique to carry out pre-treatment to waste water.The method can not be recycled resource, processing cost is high.
In aforesaid method, all have following problem: 1) deacidifying process is unreasonable, make the sour gas such as carbonic acid gas, hydrogen sulfide of the ionic state of dissolving in waste water can not be converted into cost-effectively free state, the residual quantity of sour gas is too high.The separation of ammonia, phenol is not thorough, causes in ammonolysis product phenol content and content of acid gas very high, deamination workshop section, reclaims solvent workshop section and need under higher temperature, pressure, carry out, and the preparation difficulty of by product is strengthened; 2) when the ammonia content in waste water is high, the fluctuation of service of deammoniation tower, in part flow process, adopts the complicated tower stripping ammonia with lateral line withdrawal function, when ammonia concentration is high, because extracted amount, the internal circulating load of ammonia are large, often causes deammoniation tower tower to be pressed unstable, the ammonia content of purifying waste water fluctuation; 3) owing to can not effectively solving the problem that volatile phenol affects ammonia quality, some technique takes first to extract the technique of deamination again, thereby the pH in when extraction is higher.When pH > 8, phenol mainly exists with ionic state in water and wetting ability improves greatly, and the efficiency of extracting and dephenolizing is significantly reduced; 4) extraction agent used water-soluble large, with water azeotropic, adopt rectificating method it can not be reclaimed completely; 5) after pre-treatment, wastewater biochemical feasibility is poor, processes water outlet and does not reach emission standard; 6) various, the complicated operation of strengthening pretreatment system engineering structure, and dephenolize unit adopts chemical subsidiary logos; 7) energy consumption is large, investment cost is high.
Summary of the invention
The pre-treatment of Coal Chemical Industry factory effluent and the resource recycle method thereof of a kind of environmental benefit, remarkable in economical benefits have been the object of the present invention is to provide, it has obtained having the bicarbonate of ammonia using in fertilizer, starter, printing and dyeing in treating processes, simplified the step of deamination, sour gas simultaneously, and reached in efficient processing waste water the clearance of total phenol and COD, to solve problems of the prior art.
Technical solution of the present invention is as follows:
A coal chemical industrial waste water pretreatment process, mainly comprises the following steps: 1) rectifying depickling deamination; 2) complexometric extraction reclaims aldehydes matter; 3) reclaim phase acid out.
Technical scheme of the present invention is carried out according to following concrete operation step:
1) rectifying depickling deamination:
The operation of rectifying depickling deamination is that those of ordinary skill in the art is familiar with.
Coal chemical industrial waste water is directly sent into rectifying tower, and tower reactor waste water is heated to boiling, makes ammonia in wastewater and carbonic acid gas enter gas phase by liquid phase, from gas mixture minute condensed in two stages under normal pressure of overhead extraction.One-level condensing temperature is controlled at 35-45 ℃, and reflux ratio is 5-10, and Produced Liquid is 15-20% ammoniacal liquor, and produced quantity accounts for wastewater volume 1-3%.B-grade condensation temperature is controlled at 20-30 ℃, makes the ammonia and the carbonic acid gas direct effect that are not condensed generate solid ammonium bicarbonate, and gained solid accounts for the 0.5-1.5% of wastewater quality.This step gained ammoniacal liquor, bicarbonate of ammonia all can be used as by-product and sell outward.
2) complexometric extraction recovery aldehydes matter mainly comprises the following steps:
A. prepare oil phase: complexing extractant and thinner are made into oil phase, and wherein complexing extractant consumption accounts for the 30-50% of oil phase cumulative volume.In complexometric extraction operation, the consumption of oil phase is the 10-20% of the wastewater volume that is extracted.
B. complexometric extraction: by still raffinate after rectifying with inorganic acid for adjusting pH to 1-3, then under agitation condition, add oil phase, control rotating speed is 100-150 rev/min, extraction 30-60 minute, stratification, the aldehydes matter in waste water enters upper oil phase (also claiming load oil phase); Lower floor's water is through pretreated factory effluent, delivers to biochemical treatment system.
C. liquid caustic soda back extraction: adding massfraction to the load oil phase obtaining after complexometric extraction is that 15-30% sodium hydroxide solution is stripped, stir 30-60 minute, stratification, separates oil phase and reclaims phase (being phenol sodium water solution), and oil phase returns to complexometric extraction step cycle and applies mechanically.The add-on of reextraction operation alkali lye is the 15-30% of load oil phase volume.
3) reclaim phase acid out:
In reclaiming mutually, drip behind 98% sulfuric acid acid for adjusting pH value to 1～3, stratification, upper strata is the mixed phenol of separating out, the amount of separating out accounts for the 12-20% that reclaims phase volume, wherein phenol accounts for 50-55%, ortho-methyl phenol accounts for 20-25%, and p-methyl phenol accounts for 9-12%, and directly export trade is to phenols production of articles enterprise; Lower floor's acid out mother liquor returns to complexometric extraction step process.
The present invention prepares oil phase complexing extractant used and is selected from one or both mixtures in alkyl tertiary amine N235, tri-n-octyl amine (TOA), trioctylphosphine oxide (TOPO) (TOPO); Thinner used is selected from one or more mixtures in aviation kerosene, sulfonated kerosene, n-Octanol, dimethylbenzene.
The preferred vitriol oil of complexometric extraction step of the present invention mineral acid used, concentrated hydrochloric acid or both mixtures.
Coal Chemical Industry factory effluent pretreatment process tool provided by the invention has the following advantages:
1. toxic pollutant clearance is high.Ammonia nitrogen removal frank is greater than 99%, and total phenol clearance is up to 99%.
2. after this combination technique is processed, COD clearance is greater than 95%, significantly improves biodegradability, can guarantee the discharge of waste water stably reaching standard.
3. realize utilization of wastewater resource.Rectifying depickling deamination step gained strong aqua, solid ammonium bicarbonate, and reclaim phase acid out step gained mixed phenol and can be used as by-product and sell outward, obvious economic benefit there is.
4. compared with the prior art, rectifying depickling deamination step operates under normal pressure, 90-100 ℃ condition, and energy consumption is little, cost is low.
5. the complexing extractant of selecting is water-soluble low, and cycle loss is less than 0.1%, processes coal chemical industrial waste water cost per ton and is less than 20 yuan (not comprising recovery value).
Therefore, Coal Chemical Industry factory effluent pretreatment process provided by the invention is easy and simple to handle, be easy to industrial application, has obvious environmental benefit, economic benefit and social benefit.
Accompanying drawing explanation
Fig. 1 is coal chemical industrial waste water pretreatment technology schema of the present invention.
Embodiment
By following examples, the present invention is further described in detail.But the present invention only limits to absolutely not this.The present invention's rectifying tower diameter used 400mm, tower height 1000mm, in-built stainless steel ripple filler, the high 900mm of filler.
Embodiment 1
This example is used waste water to take from Yulin Mou Lantan manufacturer, and water quality situation is as follows: COD is 25000mg/L, and total phenol concentration is 8428mg/L, and ammonia nitrogen concentration is 3214mg/L, IC(inorganic carbon) concentration 1200 is mg/L, pH value is 9.
Get 500mL coal chemical industrial waste water and send into rectifying depickling deammoniation tower, tower reactor waste water is heated to boiling, and ammonia and carbonic acid gas in waste water are transferred to gas phase by liquid phase, from the gas mixture of overhead extraction, divide condensed in two stages.One-level condensing temperature is controlled at 45 ℃, and controlling reflux ratio is 5, obtains distillate, and volume is 2.5mL, and wherein ammoniacal liquor mass concentration is 15%.B-grade condensation temperature is controlled at 20 ℃, makes to generate solid ammonium bicarbonate without ammonia and the carbonic acid gas direct effect of condensation, and gained solid weight in wet base is 4.0g.
Measure 25mL extraction agent TOA, 25mL kerosene, mix and be made into oil phase.Get still raffinate after 475mL rectifying, add the 0.3mL98% vitriol oil and regulate pH to 3, the oil phase that adds 48mL to prepare under agitation condition, controlling rotating speed is 100 revs/min, extracts 60 minutes, stratification, aldehydes matter in waste water enters upper oil phase (also claiming load oil phase), and volume is 50mL; Lower floor's water is through pretreated factory effluent, delivers to biochemical treatment system.
To the load oil phase obtaining after complexometric extraction, adding 10mL massfraction is that 30% sodium hydroxide solution is stripped, stir 60 minutes, stratification, separates 47.5mL oil phase, 12mL reclaims phase (being phenol sodium water solution), and oil phase returns to complexometric extraction step cycle and applies mechanically.
In reclaiming mutually, drip after 0.5mL98% sulfuric acid acid for adjusting pH value to 3, stratification, upper strata is the mixed phenol of separating out, volume is 3.6mL, and wherein phenol accounts for 50%, and ortho-methyl phenol accounts for 25%, p-methyl phenol accounts for 9%, and directly export trade is to phenols production of articles enterprise; Lower floor's acid out mother liquor returns to complexometric extraction step process.
After pre-treatment, waste water quality situation sees the following form:
Embodiment 2
Wastewater source is same as embodiment 1.
Get 500mL coal chemical industrial waste water and send into rectifying depickling deammoniation tower, tower reactor waste water is heated to boiling, and ammonia and carbonic acid gas in waste water are transferred to gas phase by liquid phase, from the gas mixture of overhead extraction, divide condensed in two stages.One-level condensing temperature is controlled at 35 ℃, and wherein a part of phlegma is sent into rectifying tower as phegma, and reflux ratio is 10, the direct extraction of another part phlegma, and volume is 7.5mL, wherein ammonia concn is 20%.B-grade condensation temperature is controlled at 30 ℃, makes to generate solid ammonium bicarbonate without ammonia and the carbonic acid gas direct effect of condensation, and gained solid weight in wet base is 4.2g.
Measure 30mL extraction agent TOPO, 70mL n-Octanol, mix and be made into oil phase.Get still raffinate after 492mL rectifying, add the 0.5mL98% vitriol oil and regulate pH to 2.5, the oil phase that adds 98mL to prepare under agitation condition, controlling rotating speed is 150 revs/min, extract 30 minutes, stratification, the aldehydes matter in waste water enters upper oil phase (also claiming load oil phase), and volume is 100mL; Lower floor's water is through pretreated factory effluent, delivers to biochemical treatment system.
To the load oil phase obtaining after complexometric extraction, adding 30mL massfraction is that 20% sodium hydroxide solution is stripped, stir 30 minutes, stratification, separates 96.5mL oil phase, 32L reclaims phase (being phenol sodium water solution), and oil phase returns to complexometric extraction step cycle and applies mechanically.
In reclaiming mutually, drip after 2mL98% sulfuric acid acid for adjusting pH value to 2, stratification, upper strata is the mixed phenol of separating out, volume is 4.2mL, and wherein phenol accounts for 53%, and ortho-methyl phenol accounts for 20%, p-methyl phenol accounts for 12%, and directly export trade is to phenols production of articles enterprise; Lower floor's acid out mother liquor returns to complexometric extraction step process.
After pre-treatment, waste water quality situation sees the following form:
Embodiment 3
This example is used waste water to take from Inner Mongol Mou Lantan manufacturer, and water quality situation is as follows: COD is 28560mg/L, and total phenol concentration is 8300mg/L, and ammonia nitrogen concentration is 7100mg/L, IC(inorganic carbon) concentration 2500 is mg/L, pH value is 9.5.
Get 800mL coal chemical industrial waste water and send into rectifying depickling deammoniation tower, tower reactor waste water is heated to boiling, and ammonia and carbonic acid gas in waste water are transferred to gas phase by liquid phase, from the gas mixture of overhead extraction, divide condensed in two stages.One-level condensing temperature is controlled at 40 ℃, and wherein a part of phlegma is sent into rectifying tower as phegma, and reflux ratio is 8, the direct extraction of another part phlegma, and volume is 8mL, wherein ammonia concn is 18%.B-grade condensation temperature is controlled at 25 ℃, makes to generate solid ammonium bicarbonate without ammonia and the carbonic acid gas direct effect of condensation, and gained solid weight in wet base is 10g.
Measure 40mL extraction agent TOA, 60mL kerosene, mix and be made into oil phase.Get still raffinate after 792mL rectifying, add the 1.1mL98% vitriol oil and regulate pH to 2, the oil phase that adds 100mL to prepare under agitation condition, controlling rotating speed is 120 revs/min, extract 45 minutes, stratification, the aldehydes matter in waste water enters upper oil phase (also claiming load oil phase), and volume is 103mL; Lower floor's water is through pretreated factory effluent, delivers to biochemical treatment system.
To the load oil phase obtaining after complexometric extraction, adding 50mL massfraction is that 15% sodium hydroxide solution is stripped, stir 40 minutes, stratification, separates 98mL oil phase, 53mL reclaims phase (being phenol sodium water solution), and oil phase returns to complexometric extraction step cycle and applies mechanically.
In reclaiming mutually, drip after 4.2mL98% sulfuric acid acid for adjusting pH value to 1, stratification, upper strata is the mixed phenol of separating out, volume is 6.4mL, and wherein phenol accounts for 55%, and ortho-methyl phenol accounts for 21%, p-methyl phenol accounts for 8%, and directly export trade is to phenols production of articles enterprise; Lower floor's acid out mother liquor returns to complexometric extraction step process.
After pre-treatment, waste water quality situation sees the following form:
Embodiment 4
This example is used waste water to take from Harbin gasification plant, and water quality situation is as follows: COD is 21000mg/L, and total phenol concentration is 5500mg/L, and ammonia nitrogen concentration is 7679mg/L, IC(inorganic carbon) concentration 2470 is mg/L, pH value is 9.
Rectifying depickling deamination step is with embodiment 3.
In complexometric extraction operation, oil phase consumption is 80mL, and in the operation of stripping, 15% sodium hydroxide concentration is 30L, and all the other operational conditions are same as embodiment 1.Finally separate oil phase 78.5mL, reclaim phase 32mL.Oil phase returns to complexometric extraction step cycle and applies mechanically.
In reclaiming mutually, drip after 1.6mL98% sulfuric acid acid for adjusting pH value to 2, stratification, upper strata is the mixed phenol of separating out, volume is 8mL, and wherein phenol accounts for 52%, and ortho-methyl phenol accounts for 23%, p-methyl phenol accounts for 10%, and directly export trade is to phenols production of articles enterprise; Lower floor's acid out mother liquor returns to complexometric extraction step process.
After pre-treatment, waste water quality situation sees the following form:
Claims (4)
1. the pre-treatment of Coal Chemical Industry factory effluent and a resource recycle method thereof, is characterized in that comprising the following steps:
1) rectifying depickling deamination
Coal chemical industrial waste water is directly sent into rectifying tower, and tower reactor waste water is heated to boiling, makes ammonia in wastewater and carbonic acid gas enter gas phase by liquid phase, from gas mixture minute condensed in two stages under normal pressure of overhead extraction; One-level condensing temperature is controlled at 35-45 ℃, and reflux ratio is 5-10, and Produced Liquid is 15-20% ammoniacal liquor, and produced quantity accounts for wastewater volume 1-3%; B-grade condensation temperature is controlled at 20-30 ℃, makes to generate solid ammonium bicarbonate without ammonia and the carbonic acid gas direct effect of condensation, and gained solid accounts for the 0.5-1.5% of wastewater quality;
2) complexometric extraction recovery aldehydes matter mainly comprises the following steps:
A. prepare oil phase: complexing extractant and thinner are made into oil phase, and wherein complexing extractant consumption accounts for the 30-50% of oil phase cumulative volume, in complexometric extraction operation, the consumption of oil phase is the 10-20% of the wastewater volume that is extracted;
B. complexometric extraction: by still raffinate after rectifying with inorganic acid for adjusting pH to 1-3, then under agitation condition, add oil phase, control rotating speed is 100-150 rev/min, extraction 30-60 minute, stratification, the aldehydes matter in waste water enters upper oil phase, and upper oil phase also claims load oil phase; Lower floor's water is through pretreated factory effluent, delivers to biochemical treatment system;
C. liquid caustic soda back extraction: adding massfraction to the load oil phase obtaining after complexometric extraction is that 15-30% sodium hydroxide solution is stripped, stir 30-60 minute, stratification, separates oil phase and reclaims phase, reclaiming is phenol sodium water solution mutually, and oil phase returns to complexometric extraction step cycle and applies mechanically; The add-on of reextraction operation alkali lye is the 15-30% of load oil phase volume;
3) reclaim phase acid out
In reclaiming mutually, drip behind 98% sulphur acid for adjusting pH value to 1～3, stratification, upper strata is the mixed phenol of separating out, the amount of separating out accounts for the 12-20% that reclaims phase volume, wherein phenol accounts for 50-55%, ortho-methyl phenol accounts for 20-25%, and p-methyl phenol accounts for 9-12%, and lower floor's acid out mother liquor returns to complexometric extraction step process.
2. the method for claim 1, the complexing extractant that it is characterized in that preparing described in oil phase is selected from one or both mixtures in alkyl tertiary amine N235, tri-n-octyl amine (TOA), trioctylphosphine oxide (TOPO) (TOPO).
3. the method for claim 1, is characterized in that described thinner is selected from one or more mixtures in aviation kerosene, sulfonated kerosene, n-Octanol, dimethylbenzene.
4. the method for claim 1, is characterized in that described mineral acid is selected from the vitriol oil, concentrated hydrochloric acid or both mixtures.
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| CN107176722A (en) * | 2017-07-26 | 2017-09-19 | 江苏道明化学有限公司 | A kind of method of Wastewater Pretreatment |
| CN109384346A (en) * | 2017-08-07 | 2019-02-26 | 吕素慧 | A kind of processing method of the waste water containing high-concentration phenol |
| CN108706825A (en) * | 2018-05-31 | 2018-10-26 | 华南理工大学 | A method of processing coal chemical industrial waste water containing phenol |
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