CN104071940B - A kind for the treatment of process of octyl alconyl waste lye - Google Patents
A kind for the treatment of process of octyl alconyl waste lye Download PDFInfo
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Abstract
The present invention relates to a kind for the treatment of process of octyl alconyl waste lye; First the method adopts mineral acid to carry out acidification, by the pH regulator to 3 of waste lye ~ 4.5 to waste lye; Then the process of infiltrating and vaporizing membrane evaporation concentration is carried out to acidizing fluid, or, the process of infiltrating and vaporizing membrane evaporation concentration is carried out again after breaking milk and removing oil is carried out to acidizing fluid, evaporation concentration liquid crystallisation by cooling after oily water separation reclaims mineral acid sodium salt, crystallization kettle liquid then returns acidification reactor circular treatment, evaporation condensate carries out adsorption treatment, and absorption water part returns condensation device for configuring alkali lye, and rest part water outlet enters sewage farm and carries out biological treatment and qualified discharge; The organic resourcesization the method achieved in waste lye reclaims, and turns waste into wealth, and the inorganic salt that acidization produces can also be reclaimed as byproduct simultaneously; In addition, process water outlet can replace fresh de-salted water for configuring fresh alkali lye, recycles, saves certain production cost, environmental benefit and remarkable in economical benefits.
Description
Technical field
The present invention relates to a kind for the treatment of process of octyl alconyl waste lye, the method is also suitable for the saponification waste lye administering valeral condensation decyl alcohol waste lye, cyclohexane oxidation preparing cyclohexanone.
Background technology
The existing octyl alconyl production technique of China mainly propenecarbonyl synthesis method.The method first with propylene with synthetic gas for Material synthesis butyraldehyde, then under the katalysis of 2% sodium hydroxide, carry out condensation reaction generation octenal by butyraldehyde.Butyraldehyde and octenal generate butanols and octanol finally by hydrogenation.And butyraldehyde condensation, while generating octenal, cannizzaro reaction (CannizzaroReaction) also occurs, reaction formula is as follows respectively:
2CH
3CH
2CH
2CHO+NaOH→CH
3CH
2CH
2COONa+CH
3CH
2CH
2OH+H
2O（2）
From above-mentioned reaction formula, on the one hand, while n butyraldehyde aldolization generates octenal, generate the water of equimolar amount, on the other hand because the generation of side reaction consumes sodium hydroxide, intrasystem concentration of lye can be caused constantly to decline.Therefore in order to maintain the accumulation problem of carboxylic acid sodium useless in the constant of catalyst system naoh concentration and resolution system, the fresh alkali lye of a certain amount of higher concentration must be added, discharge a part of alkali lye simultaneously, produce octanol waste lye thus.
This waste lye generally has following three features: one is that alkalescence is strong, and alkali content is about about 1 ~ 2%; Two is that quantity discharged is smaller, generally only has about 1 ~ 2t/h; Three is that organic content is high, and composition is complicated, its chemical oxygen demand (COD
cr) general at about 40000 ~ 100000mg/L, primarily of butyric acid, butyraldehyde, butanols, octenal and C
8above component provides, and the side reaction simultaneously for other makes wherein with organism such as a small amount of aldehydes, alcohols.
Both at home and abroad for a large amount of method of harness and development of octanol waste lye, these methods mainly contain acidizing extraction method, acidifying-from extraction process, acidifying thermal separation method, acidifying-extraction-absorption method, acidifying-stepwise solvent extraction method, multiple-effect evaporation method of enrichment and complexing abstraction, decompression falling film concentration method and acidifying-rectifying-electrolytic process.
CN1220971A adopts acidifying-this waste lye of abstraction technique process.First the method adopts mineral acid by waste lye acidifying, carries out extraction treatment, can make the COD of waste lye with hydrocarbon polymer more than alcohol more than 8 carbon or 6 carbon for extraction agent to it
crconcentration is down to 35000 ~ 9400mg/L by 47000mg/L, COD
crclearance reaches 80%, and extraction phase carries out rectifying makes reuse after extractant regeneration, reclaims organic constituent simultaneously.But the extractant regeneration temperature of the method also correspondingly increases along with the increase of regeneration times, extraction agent has been recycled after 35 times, and its regeneration temperature has risen to 250 DEG C by initial 180 DEG C, therefore, extraction agent can not infinite loop use, and needs regularly to be changed.Meanwhile, the facility investment of wastewater treatment and working cost also higher.
Chinese patent CN1353089A employing acidifying-from abstraction technique process octanol waste lye.The pH of waste lye is adjusted to 2.0 ~ 4.5 by this technology mineral acid, and the organic phase separated out after waste lye acidifying is as extraction agent, and the volume ratio of extraction agent and acid waste water is 1:2.After the method process, oil and COD
crclearance reach more than 80% and 50% respectively, in alkali lye, most bio-refractory material is reclaimed with the form of organic phase, and after process, the biological degradation rate of liquid effluent brings up to more than 90% by 40% simultaneously.The advantage of the method is that extraction agent does not need regeneration just can directly reuse, the extracting and separating time is short, and technique is simple, investment and working cost all lower, and waste liquid after treatment directly enters wastewater treatment field and carries out biochemical treatment after neutralization, can not impact wastewater treatment field.The method successfully achieves industrial application in certain petro-chemical corporation of the north, obtains certain economic benefit and environmental benefit.The shortcoming of the method is COD
crclearance is lower.
Chinese patent CN1530334A adopts acidifying thermal Release Technology to administer octanol waste lye, waste lye is acidified to pH and is less than 4.5 by the method, the milk sap formed after heating acidifying is 95 ~ 100 DEG C to temperature, and heat-up time is less than 0.5h, then stratification, form water-oil phase, by arranging the outlet height of water-oil phase, realizing two-phase and being automatically separated, organic phase is recycled, the method does not need additional extraction agent, but COD
crclearance be only about 50%, and energy consumption is higher.
Chinese patent CN1462729A adopts " acidifying-waste heat is from extraction " and " charcoal absorption " processes waste lye.The method utilizes waste water residual heat; with mineral acid by waste lye acidifying; with product octanol for extraction agent; extracting phase granulated active carbon carries out adsorption treatment; adsorb saturated gac through cryogenic overheating water vapor desorption and hyperthermia and superheating steam activation recycling utilization; the rectifying tower simultaneously organic phase being incorporated to octanol synthesis technique system carries out rectifying and product separation reclaims, in water outlet alkali and the rear biochemical system that directly enters carry out process and reach emission standard.Adopt the method process waste lye, can COD be made
crconcentration is down to below 650mg/L from 42500mg/L, COD
crclearance reaches more than 98%.But the method complex process, flow process is longer, because additional gac need regenerate and distillation operation, so running cost is higher; And the method does not consider that the butyric acid component that in waste lye, content is higher reclaims problem, whether the rectifying tower that the organic phase reclaimed is incorporated to octanol synthesis technique system after merging carries out rectifying separation, have an impact can not determine the quality of plant running and main products.This technology, to realize industrialization, also needs further checking.
Chinese patent CN1403381A is in acidifying-develop acidifying-stepwise solvent extraction technology on the basis of abstraction technique, the method adopts C7 and above single methanol thereof as extraction agent, the acid waste water of acidifying after extraction treatment is extracted, reclaims butyric acid (or butyrates) wherein.Extraction phase adopts the basic oxide such as highly basic or the calcium oxide back extraction Posterior circle such as sodium hydroxide to utilize, and back extraction phase concentration and recovery Sodium propanecarboxylate, the butyric acid rate of recovery reaches more than 80%, makes the COD in waste water simultaneously
cralso about 6000mg/L is dropped to further.But the shortcoming of the method is the waste water COD after process
crstill higher, and the butyric acid rate of recovery is lower and Sodium propanecarboxylate quality is not high, and utility value is little.
Wang Junmin etc. (" containing the process of alkali waste water in Octanol production " [J]. Environmental science and technology, 2009,32 (6): 356 ~ 357) multiple-effect evaporation method of enrichment process octanol waste lye is adopted, first the steam stripped produced in concentration process is adopted to remove and reclaim alcohol, aldehyde and other organism wherein, then mainly send into two-effect evaporation device containing the organic waste water of sodium hydroxide and Sodium propanecarboxylate, evaporation concentration to Sodium propanecarboxylate mass content is about 40%, then discharges system by high alkali liquid transferpump.Sun Tao etc. (" Alkaline high-strength Technologies for Organic Wastewater Treatment and technical study " [J]. Shandong petrochemical complex, 2008,36 (2): 97 ~ 100) further concentrated solution acidifying is produced butyric acid and reclaim(ed) sulfuric acid sodium.
Chinese patent CN1065642A adopts reduction vaporization to concentrate Process Study of Treating Octanol, and after concentrated, alkaline waste water returns condensation system, again participates in reaction, evaporates the process of hydromining stripping process, COD
crbe down to below 1000mg/L, Vapor phase partial carries out chromatographic separation after condensation, removes organism.Commercial practice proves, because Sodium propanecarboxylate contained in waste lye does not remove by this technology, intrasystem butyric acid sodium salt is caused to get more and more, and final Crystallization Plugging pipeline, cause condensation reaction system normally not run, thus seriously constrain the application in the industry of this patented technology.
Chinese patent 201110288711.X(application number) adopt macroporous adsorbent resin to carry out adsorption treatment, COD as sorbent material to the acid aqueous phase after acidifying oil removing
crbe down to below 300mg/L, absorption water outlet fully utilizes or as discharge of wastewater, adsorb saturated resin needs to adopt organic solvent regeneration simultaneously, and desorption liquid rectifying separation reclaims desorbing agent and butyric acid, desorbing agent recycle.The method treatment effect is good, but resin demand is large, and organic solvent easily loses, and cost is higher.
US Patent No. 6193872 adopts acidifying-rectifying-electrolysis United Technologies process octanol waste lye, first the method adopts mineral acid that the pH value of waste lye is adjusted to less than 6, reclaim the organism of separating out, lower floor's aqueous phase sends into rectifying tower rectification process, the product of tower top is butyric acid azeotropic liquid, and substantially do not contain organic still liquid through electrolysis treatment, obtain mineral acid and sodium hydroxide solution, mineral acid returns treatment system recycle, be used for acidifying condensation system produce waste lye, sodium hydroxide solution then as catalyzer return condensation systemic circulation utilize.The method makes octanol waste lye thoroughly be processed, and achieves the object of resource utilization.But this technique initial cost is high, operational condition is complicated, running cost is high, also under test at present, have no the report of industrial application.
The gain and loss of the above method of comprehensive analysis, can find out, although at present the recycling processing method of octanol waste lye is a lot, and respectively has feature, also can not find a kind of environmental friendliness and all high treatment process of economic benefit.Although acidization is the most simple and economical effective means removing oily substance in octanol waste lye, be difficult to reclaim the butyric acid in waste lye with high added value, existing abstraction technique is also difficult to reach desirable effect; Although and multiple-effect evaporation method of enrichment and rectification method effect are better, processing cost is high, the Sodium propanecarboxylate inferior quality of method of enrichment recovery simultaneously, is difficult to purify; Rectification method only can obtain moisture for 81.4%(mass content) the butyric acid azeotropic liquid of left and right, at present also concentrated correlation technique report of purifying further; Acidifying-macroreticular resin absorbing method resin demand is large, and cost of investment is high, and easily loses as the organic solvent of desorbing agent.Therefore, can say that the resource utilization of the butyric acid in octanol waste lye reclaims, be the difficult point place that current this strand of waste lye is administered.
Summary of the invention
The object of this invention is to provide a kind for the treatment of process of octyl alconyl waste lye, solve the improvement difficult problem that octyl alconyl produces the waste lye discharged, the method adopts the process combination process octanol waste lyes such as acidifying, infiltrating and vaporizing membrane evaporation and absorption, thoroughly can reclaim organism wherein, wastewater discharge and fresh water consumption can be reduced simultaneously, reduce processing cost and production cost.
The treatment process of a kind of octyl alconyl waste lye of the present invention, comprises the following steps:
(1) acidification:
Adopt mineral acid to carry out acidification to octyl alconyl waste lye, in acidification reactor, regulate pH to 3 ~ 4.5 of waste lye.
Described mineral acid is the one in sulfuric acid, hydrochloric acid, phosphoric acid or nitric acid.
(2) infiltrating and vaporizing membrane evaporation concentration:
The acidizing fluid of infiltrating and vaporizing membrane to step (1) is adopted to carry out the process of infiltrating and vaporizing membrane evaporation concentration, or oil removal treatment is carried out to acidizing fluid and reclaims oil phase, oil removing can adopt the modes such as conventional settlement separate or centrifugation to carry out, and the lower floor after oil removing clarifies acid aqueous phase and carries out the process of infiltrating and vaporizing membrane evaporation concentration again.
It is the preferential water permeable membrane of infiltration evaporation that described infiltrating and vaporizing membrane evaporates the film adopted.
Described infiltrating and vaporizing membrane vaporization temperature is 20 ~ 90 DEG C, and cycles of concentration is 2 ~ 15 times.
In infiltrating and vaporizing membrane evaporating concentration process, the mineral acid sodium salt concentration in evaporative process produced by acidification reaction constantly increases, the organic concentrations such as the butyric acid in concentrated solution also correspondingly increase, due to the salting out of inorganic salt, organism (comprising butyric acid etc. soluble in water) in concentrated solution is separated out in large quantities from water, forms water-oil phase.Concentrated solution enters water-and-oil separator and carries out oily water separation process, and oil phase reclaims, and aqueous phase is sent in cooling crystallizer and carried out crystallisation by cooling process, and cooling temperature is 0 ~ 20 DEG C, and the inorganic salt crystallization of crystallization is reclaimed, and can be used as byproduct and sell after refining; Crystalline mother solution then returns acidification reactor, and its advantage makes full use of mineral acid excessive in crystalline mother solution, thus saves processing cost.
(3) adsorption treatment:
Carry out adsorption treatment to the infiltrating and vaporizing membrane evaporation condensate that step (2) produces, remove a small amount of organism wherein, the saturated rear employing steam desorption and regeneration of adsorbent, steam desorption and regeneration temperature is 100 ~ 150 DEG C; Desorption liquid returns the process of infiltrating and vaporizing membrane vaporization cycle; The COD of adsorption treatment water outlet
crbe less than 500mg/L, part returns Octanol production device and replaces fresh de-salted water to configure alkali lye, reduces production cost, and rest part enters sewage farm and carries out biological treatment and qualified discharge.
Described sorbent material is macroporous adsorbent resin or gac, is preferably macroporous adsorbent resin.
Described absorption adopts single stripper operation or double tower alternate run.
(4) useful component is reclaimed:
Carry out rectification process to the oil phase that step (3) reclaims, reclaim butyraldehyde, butanols, octenal and butyric acid and restructuring grade useful component, and butyraldehyde, butanols, the recycle of octenal return mechanism, butyric acid and heavy constituent are then sold as byproduct.
Method provided by the invention has following characteristics and advantage:
1. method treatment effect provided by the present invention is good, and the organic resourcesization achieved in waste lye reclaims, and turns waste into wealth, and the inorganic salt that acidization produces can also reclaim as byproduct by the method simultaneously; In addition, process water outlet can replace fresh de-salted water for configuring alkali lye, recycles, and reduces wastewater discharge, saves certain production cost, environmental benefit and remarkable in economical benefits.
2. the present invention has technical process simply, the advantages such as operational condition is gentle, stable, apparatus structure is compact, and floor space is little.
3. infiltrating and vaporizing membrane evaporation of the present invention can make full use of the heat of waste lye self waste heat and acidification reaction generation, and without the need to external heat source, thus energy consumption is lower, thus significantly reduces processing cost.
4. the present invention is compared with acidizing extraction method, acidifying rectification method, multiple-effect evaporation method of enrichment and acidifying-absorption with macroporous adsorbent resin method, has COD
crthe advantage that clearance is high, energy consumption is low, adsorbent amount is few.
Embodiment
Embodiment 1:
Get 5LCOD
crfor the waste lye of 106312mg/L, adopt 98% vitriol oil to carry out acidification to it, regulate pH=3, acidizing fluid leaves standstill 24h, profit layering, and recovery oily substance is 96mL, measures the COD of clarification aqueous phase
crfor 38521mg/L.Adopt infiltrating and vaporizing membrane evaporation to carry out concentration to clarification aqueous phase, infiltrating and vaporizing membrane is the preferential water permeable membrane of modified polyvinyl alcohol, and vaporization temperature is 45 DEG C, and cycles of concentration is 11 times, collects concentrated solution and evaporation condensate respectively.
Evaporation condensate COD
crfor 3548mg/L, with the adsorption column adsorption treatment of the flow velocity of 1BV/h by the macroporous adsorbent resin of filling 100mL, when absorption water outlet volume is resin volume 30 times, water outlet COD
crfor 251mg/L, after this water outlet COD
crincrease sharply, illustrate that resin has adsorbed saturated.Adopt 150 DEG C of steam to carry out desorption and regeneration to the saturated resin of absorption, collect desorption liquid.
After concentrated solution leaves standstill 2h, profit layering, recovery oily substance is 117mL, and aqueous phase is cooled to 0 DEG C of crystallization, obtains 215g sodium sulfate crystal.
Embodiment 2:
Get 5LCOD
crfor the waste lye of 106312mg/L, adopt 98% vitriol oil to carry out acidification to it, regulate pH=4.5, acidizing fluid leaves standstill 24h, profit layering, and recovery oily substance is 95mL, measures the COD of clarification aqueous phase
crfor 39549mg/L.Mixed with the desorption liquid that embodiment 1 is collected by clarification aqueous phase, adopt infiltrating and vaporizing membrane evaporation to carry out concentration to mixed solution, infiltrating and vaporizing membrane is Nafion film, and vaporization temperature is 45 DEG C, and cycles of concentration is 13 times, collects concentrated solution and evaporation condensate respectively.Evaporation condensate COD
crfor 2362mg/L, with the absorption with macroporous adsorbent resin post adsorption treatment of the flow velocity of 1BV/h by embodiment 1 desorption and regeneration, when absorption water outlet volume is resin volume 32 times, water outlet COD
crfor 245mg/L, after this water outlet COD
crincrease sharply, illustrate that resin has adsorbed saturated.
Concentrated solution is left standstill 2h, profit layering, recovery oily substance is 129mL, and aqueous phase is cooled to 0 DEG C of crystallization, obtains 217g sodium sulfate crystal.
Claims (4)
1. a treatment process for octyl alconyl waste lye, is characterized in that: its operation steps is as follows:
(1) acidification:
First adopt mineral acid to carry out acidification to octyl alconyl waste lye, in acidification reactor, regulate pH to 3 ~ 4.5 of waste lye;
Described mineral acid is the one in sulfuric acid, hydrochloric acid, phosphoric acid or nitric acid;
(2) infiltrating and vaporizing membrane evaporation concentration process:
The process of infiltrating and vaporizing membrane evaporation concentration is carried out to the acidizing fluid that step (1) produces, or first oil removal treatment is carried out to acidizing fluid and reclaim oil phase, and then acid aqueous phase is clarified to the lower floor after oil removing carry out the process of infiltrating and vaporizing membrane evaporation concentration;
Described infiltrating and vaporizing membrane vaporization temperature is 20 ~ 90 DEG C, and cycles of concentration is 2 ~ 15 times; Concentrated solution enters water-and-oil separator to carry out oily water separation process and reclaims oil phase, and aqueous phase is then sent in cooling crystallizer and carried out crystallisation by cooling process, and cooling temperature is 0 ~ 20 DEG C; Reclaim the mineral acid sodium salt of crystallization; Crystalline mother solution then returns acidification reactor circular treatment;
(3) adsorption treatment:
Carry out adsorption treatment to the infiltrating and vaporizing membrane evaporation condensate that step (2) produces, remove a small amount of organism wherein, the saturated rear employing steam desorption and regeneration of adsorbent, desorption liquid then returns the process of infiltrating and vaporizing membrane vaporization cycle; Absorption water part returns condensation cell location alkali lye, and rest part enters sewage farm and carries out biological treatment and qualified discharge;
Described sorbent material steam desorption and regeneration temperature is 100 ~ 150 DEG C;
(4) useful component is reclaimed
Rectification process is carried out to the oil phase that step (2) reclaims, reclaims butyraldehyde, butanols, octenal and butyric acid and heavy constituent; Butyraldehyde, butanols, the recycle of octenal return mechanism, butyric acid and heavy constituent then reclaim as byproduct.
2. the treatment process of octyl alconyl waste lye according to claim 1, is characterized in that: the film that step (2) infiltrating and vaporizing membrane evaporative process adopts is the preferential water permeable membrane of infiltration evaporation.
3. the treatment process of octyl alconyl waste lye according to claim 2, is characterized in that: the preferential water permeable membrane of infiltration evaporation is acrylonitrile compolymer acrylic film, modified PVA membrane, cross-linking polyvinyl alcohol film, sodium polyacrylate/polydivinylbenezene film, asymmetric polyimide film, polyaniline blend film, vinylchlorid/polyacrylonitrile film, Nafion film, modification Nafion film or silica film one wherein.
4. the treatment process of octyl alconyl waste lye according to claim 1, is characterized in that: the sorbent material described in step (3) is macroporous adsorbent resin or gac.
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| CN106927596A (en) * | 2015-12-30 | 2017-07-07 | 中国石油天然气股份有限公司 | The processing method of octanol waste lye |
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| CN109912072A (en) * | 2019-03-14 | 2019-06-21 | 北京诚益通控制工程科技股份有限公司 | It is a kind of to extract the method and recovery system that sec-octyl alcohol is recycled in waste liquid from lincomycin |
| KR20210134922A (en) * | 2019-03-29 | 2021-11-11 | 도요보 가부시키가이샤 | water treatment system |
| CN110282798B (en) * | 2019-06-14 | 2022-03-25 | 广东省科学院化工研究所 | Treatment method of organic wastewater for synthesizing substituted benzimidazole |
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| EP0838435A1 (en) * | 1996-10-25 | 1998-04-29 | Kvaerner Process Technology Limited | Process and plant for treating an aqueous waste stream containing alkali metal carboxylates |
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