CN101376550B - Method for processing process waste water of dimethyl ether preparation by dehydrating methyl alcohol - Google Patents
Method for processing process waste water of dimethyl ether preparation by dehydrating methyl alcohol Download PDFInfo
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Abstract
The invention provides a method of treating the process effluent of dimethyl ether synthesis via methanol dehydration. The method at least comprises the following three steps: the first step, the process effluent is divided into two flows through the evaporation, wherein one flow is rich in organic substances and the other flow is poor in organic substances; the second step, the flow rich in organic substances is subjected to the membrane separation, the organic substances in the concentrate is recovered, and the water phase is reutilizes; and the third step, the flow poor in organic substances is subjected to the biochemical treatment so that the water quality meets the requirements on reclaimed water. Optionally, the method further comprises the fourth step, that is, the reclaimed water is treated by the water quality stabilization technology to meet the reclaimed water treatment requirement on the production equipment. The method can recycle the whole effluent after treatment and reclaim the organic substances in the effluent, and achieves the effect of resource utilization of the process effluent and the organic substances in the process effluent.
Description
Technical field
The present invention relates to the treatment process of process waste water of dimethyl ether preparation by dehydrating methyl alcohol.
Background technology
Dme claims wooden ether again, is a kind of emerging basic chemical raw materials, because it has good easy compression, condensation, vaporizing property, the purposes of many uniquenesses is arranged in chemical industry such as pharmacy, fuel, agricultural chemicals.Along with the in short supply and price increase of petroleum resources, going deep into of clean environment firendly theory widelyd popularize as the clean fuel-dme of diesel oil alternate resources, and progressed into domestic fuel market and automobile fuel market.In the long run, the dme market outlook are wide, are the Chaoyang Chemicals that emerging rapidly in the world wide.
The production method of dme mainly contains three kinds of traditional method, single stage method and two-step approachs.Traditional method is to adopt an acidic catalyst, and methyl alcohol liquid phase or gas-phase dehydration are produced dme; Single stage method is raw material with the synthetic gas, and direct dimethyl ether synthesis on the composite catalyst of and methanol dehydration synthetic at methyl alcohol is purified and obtained product; Two-step approach is to make methyl alcohol with synthetic gas, and methyl alcohol dewaters under the solid catalyst effect and makes dme then.No matter take which kind of method, water all is that methyl alcohol passes through one of dehydration dimethyl ether-preparing technological process primary product, when obtaining dme, produces a large amount of processing wastewaters.Contain a large amount of unreacted methanol, formic acid, a part of dme etc. in the processing wastewater.If adopt conventional sewage treatment facility to handle, not only increase the burden of Sewage treatment systems greatly, and cause the waste of contained large amount of organic in the waste water.Therefore, being necessary the waste water that the dme production process produces is effectively handled and utilization rationally, when producing good social benefit and environmental benefit, also is that enterprise creates good economic benefit.
The processing wastewater that the dme production process produces, its water quality depends on catalyst type and processing condition such as temperature, the pressure etc. that reaction is adopted to a great extent, principal pollutant are oxygen-bearing hydrocarbons, as methyl alcohol, methyl ether etc., have COD content height, inorganic salt content is low, temperature is high and the water yield is big characteristics.
The processing wastewater treatment project example of production dme generation seldom at present.But become the focus in the industry widely paid close attention to because the preparing dimethyl ether from methanol technical development is rapid recent years, therefore presses for the research and development processing wastewater and handle and reuse technology.
Consulted the U.S. chemical abstract database at interior domestic and international 10 patents, bibliographic data base,, do not seen relevant direct reuse method as yet at process waste water of dimethyl ether preparation by dehydrating methyl alcohol from the information that obtains.All only relate in the document and processing wastewater is drained into waste water disposal facility handle, for example:
CN 2621179Y proposes a kind of methanol liquid-phase dehydration and produces fuel grade dimethyl ether plant effluent treatment unit, has a upflow anaerobic sludge blanket reactor, the aeration ditch of filler is housed around the up-flow anaerobic sludge blanket setting, this aeration ditch outlet is by pipe connection one compound membrane filtration baffled reactor, and treatment effect can reach national grade one discharge standard.Though manufacturing cost and processing cost are all lower, organism discharges in a large number in the water, causes the wasting of resources.
" environmental science and technology " in March, 2003, " engineering bacteria is handled the research of a high-purity dimethyl ether factory effluent " literary composition synthesized chemical plant high-purity dimethyl ether factory effluent at Wu County, Jiangsu, adopted secondary oxidation technology, used engineering bacteria LEY
7Handle this waste water, improved the degradation rate of biochemistry pool sewage.Water outlet COD is below 100mg/L, and system reaches more than 90% the COD clearance.Processing intent also is a qualified discharge, does not relate to the reuse problem of organic recovery and water in the literary composition.
" Jiangsu chemical industry " April calendar year 2001, one step of the synthetic gas preparing dimethy ether novel process and the U.S. air Products Co., Ltd liquid phase production dme novel process of Denmark Haldor Topsoe company reported in " one-step method from syngas preparing dimethy ether technical progress " literary composition.All be that reaction product methyl alcohol/dme/water mixture is at first sent into the dme tower in the two technical process, overhead product is the dme product.The bottomsstream is sent into methanol column, at this methyl alcohol is told from cat head, and water is then delivered to wastewater treatment equipment at the bottom of the tower.Processing intent is qualified discharge equally, does not relate to the reuse problem of organic recovery and water.
Summary of the invention
The present invention is directed to the defective that prior art exists, a kind of treatment process of process waste water of dimethyl ether preparation by dehydrating methyl alcohol is provided, make the waste water fully recovering after the processing, the organism in the waste water obtains reclaiming, and realizes organic recycling in processing wastewater and the waste water.
Process waste water of dimethyl ether preparation by dehydrating methyl alcohol treatment process provided by the invention comprises following three technique units at least:
First technique unit is divided into processing wastewater by evaporative process and is rich in organism and poorly contains organic two strands of current;
Second technique unit carries out membrane sepn to being rich in organic current, the organism in the concentrated solution is reclaimed the water reuse;
The 3rd technique unit contains organic waste water and carries out biochemical treatment poor, makes water quality reach the requirement of reuse recirculated water;
According to method provided by the invention, can also comprise the 4th technique unit, promptly adopt Stability Technique of Water Quality that reuse recirculated water is handled, make it satisfy production equipment to the circulating water treatment effect of requirement.
In first technique unit, by evaporative process processing wastewater is divided into and is rich in organism and poorly contains organic two strands of current, be that boiling point is lower than 100 ℃ organism such as methyl alcohol, dme etc. and separates from waste water, organic wastewater is rich in formation, and this strand current account for 10～30% (weight) of processing wastewater total amount; The current that account for Total Water about 70～90% (weight) are the poor organism current that contain, and only contain organic matters.
According to the present invention, the relevant device of evaporative process is simple distillation system, multi-effect evaporation system, stripping system etc.For Distallation systm, can control the amount of steaming by the control temperature out, evaporation section does not enter next processing unit.For multi-effect evaporation system, generally form by 2～10 vaporizers, connect flow process between effect and can be following current, adverse current, advection or mixed flow.Preferred flow is the downflow system multiple-effect evaporator, finally evaporates raffinate and enters next processing unit.
In second technique unit, carry out membrane sepn to being rich in organic current, membrane sepn adopts reverse osmosis membrane assembly and supporting pre-treatment facility such as ultrafiltration etc.The organism that the concentrated solution of membrane sepn promptly reclaims can be back to the dimethyl ether preparation by dehydrating methyl alcohol production technique or separate the purification post-treatment and become variant production.Reclaim water COD behind the organism when higher (generally being higher than 100mg/L), contain the organism current with the 3rd technique unit poor and merge and handle.When water COD concentration is about 20-100mg/L, after can handling further removal organism by two-pass reverse osmosis, make in the water COD concentration less than 20mg/L, the pH value is between 7.0-8.0, total dissolved solidss (TDS) content is less than 100mg/L, turbidity satisfies the water quality requirement of boiler feed water less than 1.0NTU, can be back to the water wash column water that the technology process is done in boiler or reuse.When water COD is low (generally being lower than 20mg/L), direct reuse is done the water wash column water of technology process in boiler or reuse.
In the 3rd technique unit, poorly contain organic low concentration of water COD and generally be higher than 500mg/L, remove most organic by the biochemical treatment process, make water outlet COD less than 60mg/L, reach the requirement that is back to recirculated water.
Said biochemical treatment process comprises at least a in anaerobic treatment and the aerobic treatment, anaerobic treatment process can adopt flow lifting type anaerobic sludge layer reactor (UASB), internal-circulation anaerobic reactor (IC), anaerobic filter, anaerobic fluidized bed reactor (AFBR), membrane bioreactor etc.Aerobic treatment process can adopt activated sludge process, BAF (BAF), bio-contact oxidation, membrane bioreactor, blodisc, trickling filter, fluidized-bed reactor etc.
At the 4th technique unit, said Stability Technique of Water Quality is to wait by interpolation alkaline matter and/or inhibiter, Scale inhibitors and/or biocide to satisfy the requirement that reuse water is used for recirculated water.Alkaline matter can be lithium, sodium and potassium oxide compound, oxyhydroxide, carbonate or supercarbonate with and composition thereof; Inhibiter can be organophosphate and metal oxide, organophosphate such as 1-hydroxyethyl-1,1-bisphosphate, Amino Trimethylene Phosphonic Acid, ethylene diamine tetramethylene phosphonic acid, 2-hydroxyl phosphino-acetate etc. and composition thereof, metal oxide such as zinc chloride, zinc sulfate, zinc oxide, molybdate, tungstate, silicate etc. and composition thereof; Dirt dispersion agent can be the sodium polyacrylate that is applicable to water treatment, acrylic acid/esters multipolymer, sodium acrylate/2-methyl-2 '-acrylamido-propene sulfonic acid multipolymer, poly-epoxy succinic acid, the acid of poly-asparagus fern peace etc. and composition thereof; Biocide can be the compound that discharges hypochlorite in chlorine, hypochlorite and the use thereof, smell oxygen, dioxide peroxide, quaternary ammonium salt, quaternary alkylphosphonium salt, glutaraldehyde, isothiazolinone, dibromo Malonamide nitrile etc. and composition thereof.
The scope of application of the present invention comprises: traditional methanol vapor phase or liquid-phase dehydration are produced the processing of processing wastewater in the dme technology; The processing of one step of synthetic gas preparing dimethy ether processing wastewater; And two step method is promptly first by the synthetic gas synthesizing methanol, and then the processing of process waste water of dimethyl ether preparation by dehydrating.
The present invention possesses following outstanding advantage:
A, compared with former method of wastewater treatment, a whole set of processing scheme provided by the invention can make the process waste water of dimethyl ether preparation by dehydrating methyl alcohol fully recovering in production, realizes processing wastewater reuse truly.
B, present method can be carried out most of organism in the waste water trans-utilization or directly be reclaimed, and realize the recycling of refuse.
Embodiment
Embodiment 1:
Wastewater source: methanol liquid-phase dehydration is produced process waste water of dimethyl ether.
A, employing 8 single-effect evaporators distill waste water, and phlegma accounts for about 30% of Total Water, and phlegma COD is about 3.5 ten thousand mg/L, and vinasse accounts for about 70% of Total Water, and COD is about 800mg/L.
B, phlegma described in a is carried out reverse osmosis membrane separation.The organism that reclaims becomes variant production by separating purification processing.Water COD higher (being about 200mg/L) merges processing with vinasse.
C, adopt the conventional combined treatment process be followed successively by two-stage UASB anaerobic reactor, aerobic activated sludge process, bio-contact oxidation, sand filtration to handle to vinasse described in the above a.Water outlet COD is less than 60mg/L.The biogas that anaerobic process produce can be as the raw material of synthetic gas after purifying purification.
D, water outlet described in the above c added alkaline matter make its pH value reach 9.5-14, and suitably add inhibiter, Scale inhibitors and sterilant etc., be back to circulating water system.Under this condition of water quality, erosion rate≤0.10mm/a, adhesion speed≤15mg/ (cm
2.month), total plate count≤1 * 10
5Individual/mL, and cycles of concentration reaches about 6, satisfied the water quality requirement of recirculated water.
Embodiment 2:
Wastewater source: methanol gas phase dewatering preparing is got process waste water of dimethyl ether.
A, employing simple distillation system distill waste water, and phlegma accounts for about 20% of Total Water, and COD is about 1.5 ten thousand mg/L in the phlegma.Vinasse accounts for about 80% of Total Water, and COD is about 1000mg/L.
B, adopt purification process to carry out deep purifying based on membrane sepn to phlegma described in the above a.The concentrated solution of membrane sepn is can be back to the dimethyl ether preparation by dehydrating methyl alcohol production technique after organism reclaims or separate purification processing by alternate manner to become variant production.Water outlet COD is less than 20mg/L, and the pH value is between 7.0-8.0, and total dissolved solidss (TDS) content is less than 100mg/L, and turbidity satisfies the water quality requirement of boiler feed water less than 1.0NTU.
C, adopt the biochemical processing process be followed successively by two-stage internal-circulation anaerobic reactor, TSA biological filter to handle to vinasse described in the above a.Water outlet COD is less than 60mg/L.The biogas that anaerobic process produce can be as the raw material of synthetic gas after purifying purification.
D, water outlet described in the above c added alkaline matter make its pH value reach 9.5-14, and suitably add inhibiter, Scale inhibitors and sterilant etc., be back to circulating water system.Under this condition of water quality, erosion rate≤0.10mm/a, adhesion speed≤15mg/ (cm
2.month), total plate count≤1 * 10
5Individual/mL, and cycles of concentration reaches about 6, satisfied the water quality requirement of recirculated water.
Embodiment 3:
Wastewater source: one-step method from syngas is produced process waste water of dimethyl ether.
A, employing 2 single-effect evaporators evaporate water outlet described in the above a, and phlegma accounts for about 10% of Total Water, and phlegma COD is about 20,000 mg/L.Vinasse accounts for about 90% of Total Water, and COD is about 2000mg/L.
B, adopt purification process to carry out deep purifying based on membrane sepn to phlegma described in the above a.Can be back to the dimethyl ether preparation by dehydrating methyl alcohol production technique after organism reclaims or separate purification processing and become variant production by alternate manner.Water COD lower (being about 25mg/L), but direct reuse is in boiler.
C, adopt the conventional combined treatment process be followed successively by two-stage UASB anaerobic reactor, aerobic activated sludge process, bio-contact oxidation, sand filtration to handle to vinasse described in the above a.Water outlet COD is less than 60mg/L.The biogas that anaerobic process produce can have been realized most of organic trans-utilization as the raw material of synthetic gas after purifying purification.
D, water outlet described in the above c added alkaline matter make its pH value reach 9.5-14, and suitably add inhibiter, Scale inhibitors and sterilant etc., be back to circulating water system.Under this condition of water quality, erosion rate≤0.10mm/a, adhesion speed≤15mg/ (cm
2.month), total plate count≤1 * 10
5Individual/mL, and cycles of concentration reaches about 6, satisfies the water quality requirement of recirculated water.
Embodiment 4:
Wastewater source: use the synthetic gas two step method to produce process waste water of dimethyl ether.
A, employing 4 are imitated evaporation technologies waste water are distilled.Phlegma accounts for about 20% of Total Water, and phlegma COD is about 20,000 mg/L.Vinasse accounts for about 80% of Total Water, and COD is about 1500mg/L.
B, adopt purification process to carry out deep purifying based on membrane sepn to phlegma described in the above a.Can be back to the dimethyl ether preparation by dehydrating methyl alcohol production technique after organism reclaims or separate purification processing and become variant production by alternate manner.Water outlet COD is less than 10mg/L, and the pH value is between 7.0-8.0, and total dissolved solidss (TDS) content is less than 100mg/L, and turbidity satisfies the water quality requirement of boiler feed water less than 1.0NTU.
C, adopt the biochemical processing process be followed successively by two-stage internal-circulation anaerobic reactor, TSA biological filter to handle to vinasse described in the above a.Water outlet COD is less than 60mg/L.The biogas that anaerobic process produce can have been realized most of organic trans-utilization as the raw material of synthetic gas after purifying purification.
D, water outlet described in the above c added alkaline matter make its pH value reach 9.5-14, and suitably add inhibiter, Scale inhibitors and sterilant etc., be back to circulating water system.Under this condition of water quality, erosion rate≤0.10mm/a, adhesion speed≤15mg/ (cm
2.month), total plate count≤1 * 10
5Individual/mL, and cycles of concentration reaches about 6, satisfies the water quality requirement of recirculated water.
Embodiment 5:
Wastewater source: use the synthetic gas two step method to produce process waste water of dimethyl ether.
A, employing stripping process carry out stripping to waste water.Phlegma accounts for about 20% of Total Water, and phlegma COD is about 30,000 mg/L.The stripping raffinate accounts for about 80% of Total Water, and COD is about 1200mg/L.
B, adopt purification process to carry out deep purifying based on membrane sepn to phlegma described in the above a.Can be back to the dimethyl ether preparation by dehydrating methyl alcohol production technique after organism reclaims or separate purification processing and become variant production by alternate manner.Water outlet COD is about 80mg/L, further handles by the two-pass reverse osmosis device, makes water outlet COD less than 20mg/L, and the pH value is between 7.0-8.0, and total dissolved solidss (TDS) content is less than 100mg/L, and turbidity satisfies the water quality requirement of boiler feed water less than 1.0NTU.
C, adopt the biochemical processing process be followed successively by two-stage internal-circulation anaerobic reactor, TSA biological filter to handle to vinasse described in the above a.Water outlet COD is less than 60mg/L.The biogas that anaerobic process produce can have been realized most of organic trans-utilization as the raw material of synthetic gas after purifying purification.
D, water outlet described in the above c added alkaline matter make its pH value reach 9.5-14, and suitably add inhibiter, Scale inhibitors and sterilant etc., be back to circulating water system.Under this condition of water quality, erosion rate≤0.10mm/a, adhesion speed≤15mg/ (cm
2.month), total plate count≤1 * 10
5Individual/mL, and cycles of concentration reaches about 6, satisfies the water quality requirement of recirculated water.
Claims (13)
1. process waste water of dimethyl ether preparation by dehydrating methyl alcohol treatment process comprises following three technique units at least:
First technique unit is divided into processing wastewater and is rich in organism and poorly contains organic two strands of current by evaporative process;
Second technique unit carries out membrane sepn to being rich in organic current, the organism in the concentrated solution is reclaimed the water reuse;
The 3rd technique unit contains organic waste water and carries out biochemical treatment poor, makes water quality reach the requirement of reuse recirculated water.
2. in accordance with the method for claim 1, it is characterized in that, also comprise the 4th technique unit, promptly adopt Stability Technique of Water Quality that reuse recirculated water is handled, make it satisfy production equipment the circulating water treatment effect of requirement.
3. in accordance with the method for claim 1, it is characterized in that, in first technique unit, be rich in 10～30% (weight) that organic current account for the processing wastewater total amount, poorly contain 70～90% (weight) that the organism current account for the processing wastewater total amount.
4. in accordance with the method for claim 1, it is characterized in that the relevant device of evaporative process is simple distillation system, multi-effect evaporation system or stripping system.
5. in accordance with the method for claim 1, it is characterized in that in second technique unit, membrane sepn adopts reverse osmosis membrane assembly and supporting pre-treatment facility.
6. in accordance with the method for claim 1, it is characterized in that in second technique unit, the organism of recovery is back to production technique or separates the purification post-treatment and becomes product.
7. in accordance with the method for claim 1, it is characterized in that, when reclaiming water COD behind the organism and being higher than 100mg/L, contain the organism current with the 3rd technique unit poor and merge and handle.
8. in accordance with the method for claim 1, it is characterized in that, in second technique unit, when the water COD behind the recovery organism is lower than 100mg/L, handle further removal organism, make water outlet COD further reduce to below the 20mg/L by two-pass reverse osmosis, the pH value is between 7.0-8.0, total dissolved solid content is less than 100mg/L, and turbidity is back to the water wash column water that the technology process is done in boiler or reuse less than 1.0NTU.
9. in accordance with the method for claim 1, it is characterized in that, in the 3rd technique unit, contain organic low concentration of water stream by biochemical treatment process removal most organic, make water outlet COD, reach the requirement that is back to recirculated water less than 60mg/L to poor.
10. in accordance with the method for claim 1, it is characterized in that said biochemical treatment process comprises at least a in anaerobic treatment and the aerobic treatment.
11. in accordance with the method for claim 10, it is characterized in that anaerobic treatment process adopts flow lifting type anaerobic sludge layer reactor, internal-circulation anaerobic reactor, at least a in anaerobic filter, anaerobic fluidized bed reactor or the membrane bioreactor.
12. in accordance with the method for claim 10, it is characterized in that aerobic treatment process adopts at least a in activated sludge process, BAF, biological contact oxidation process, membrane bioreactor, blodisc, trickling filter or the fluidized-bed reactor
13. in accordance with the method for claim 2, it is characterized in that at the 4th technique unit, said Stability Technique of Water Quality is to satisfy the requirement that reuse water is used for recirculated water by adding alkaline matter or inhibiter, Scale inhibitors and/or biocide.
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Families Citing this family (7)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101962235B (en) * | 2009-07-24 | 2013-05-01 | 中国石油化工股份有限公司 | Method for high temperature wastewater treatment and reuse in MTO process |
| CN102442744B (en) * | 2010-09-30 | 2013-07-03 | 中国石油化工股份有限公司 | Treatment method of high-concentration process waste water during methanol-to-olefin process |
| CN103102004A (en) * | 2011-11-10 | 2013-05-15 | 中国石油化工股份有限公司 | Industrial circulation water treatment method |
| CN104556541B (en) * | 2013-10-22 | 2017-03-01 | 中国石油化工股份有限公司 | A kind of processing method of preparing gasoline by methanol Process Production water |
| CN105330086B (en) * | 2014-06-18 | 2018-03-02 | 中国石油化工股份有限公司 | A kind of processing method of methanol-to-olefins waste water |
| CN110950476A (en) * | 2019-12-03 | 2020-04-03 | 广东益诺欧环保股份有限公司 | Treatment method and treatment system for high-salinity wastewater containing methanol |
| CN114656116B (en) * | 2022-04-25 | 2023-04-07 | 倍杰特集团股份有限公司 | Alcohol ester wastewater recycling device and method |
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| EP1484288A2 (en) * | 2003-06-02 | 2004-12-08 | Institut Francais Du Petrole | Process for purifying waste water that is polluted with MTBE or TAME by using the strain Mycobacterium Austroafricanum I-2562, which is fixed on a mineral support comprising perlite |
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