CN107445330A - A kind of handling process of inexpensive MTO alkali cleanings zero discharged waste alkali liquid - Google Patents
A kind of handling process of inexpensive MTO alkali cleanings zero discharged waste alkali liquid Download PDFInfo
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- CN107445330A CN107445330A CN201610377730.2A CN201610377730A CN107445330A CN 107445330 A CN107445330 A CN 107445330A CN 201610377730 A CN201610377730 A CN 201610377730A CN 107445330 A CN107445330 A CN 107445330A
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- spent lye
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F9/00—Multistage treatment of water, waste water or sewage
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/34—Chemical or biological purification of waste gases
- B01D53/96—Regeneration, reactivation or recycling of reactants
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2251/00—Reactants
- B01D2251/30—Alkali metal compounds
- B01D2251/304—Alkali metal compounds of sodium
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2251/00—Reactants
- B01D2251/60—Inorganic bases or salts
- B01D2251/604—Hydroxides
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/40—Devices for separating or removing fatty or oily substances or similar floating material
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/52—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/58—Treatment of water, waste water, or sewage by removing specified dissolved compounds
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2301/00—General aspects of water treatment
- C02F2301/08—Multistage treatments, e.g. repetition of the same process step under different conditions
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- Oil, Petroleum & Natural Gas (AREA)
- Chemical Kinetics & Catalysis (AREA)
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Abstract
The present invention provides a kind of handling process of inexpensive MTO alkali cleanings zero discharged waste alkali liquid, and the handling process comprises the following steps:(1) oil wash deaerates:MTO spent lyes are washed using washing oil, it is preliminary to remove entrained oil class in spent lye, reduced pressure treatment is carried out afterwards;(2) storage tank is stood:Spent lye after preliminary removing oils and reduced pressure treatment, is stood in storage tank by stopping, and oil slick is further removed after profit layering;(3) carbonate is removed:Carbonate deposition agent is added in the spent lye after standing oil removing and carries out precipitation reaction, the precipitation in spent lye is removed after stratification;(4) alkali liquid regeneration:Sodium hydroxide is added into the spent lye for removing carbonate, carries out alkali liquid regeneration.By the handling process of the present invention, sodium hydroxide reproducible utilization, the zero-emission of spent lye processing is realized, greatly reduce alkali lye dosage, mitigate environmental protection pressure.
Description
Technical field
The present invention relates to petrochemical wastewater process field, more particularly, to a kind of inexpensive MTO
The handling process of alkali cleaning zero discharged waste alkali liquid.
Background technology
Contain CO in MTO device product gas2Deng sour gas, technological process requirement is by product gas
CO2It is removed to 10-6(VOL) below.Current widely used setting caustic wash tower, passes through NaOH solution
The method of cleaning product gas removes CO2.In washing process, with NaOH chemistry occurs for sour gas
React and remove, while produce spent lye.
From ethylene unit caused by spent lye it is different, not sulfur-bearing in MTO spent lyes, but contain diformazan
The organic oxygen compounds such as ether, methanol.The presence of organic matter can cause spent lye COD very high, and rear
In continuous processing procedure, such organic oxygen compound of degrading is difficult to using traditional biochemical sewage processing, to dress
Put operation and bring very big environmental protection pressure.If the organic matter in spent lye can be removed to reduce COD,
It then can directly neutralize the sewage plant processing of Hou Songquan factories.
At present, the processing method of domestic spent lye (slag) mainly includes burning method, neutralisation, oxidation
Method and the major class of biological treatment four.
Burning method belongs to direct facture, organic matter is generated CO under high temperature and normal pressure2And H2O,
NaOH changes into Na2CO3, sulfate and carbonate are remained dissolved in treated waste liquid.The method
It is a kind of feasible processing method, it is simple to operate.Its shortcoming is that energy consumption is big, and running cost is high;Meanwhile
The sodium carbonate that burning is formed at high temperature can be serious to refractory corrosion in stove, also easily in fast cooling device
With fouling in pipeline.This method needs to set up a whole set of complicated fume treatment flow, to meet flue gas
Qualified discharge requirement.Therefore, the use of burning method is restricted.
Neutralisation is with concentrated sulfuric acid neutralisation and CO2Neutralisation is representative.Sulfuric acid disappears in concentrated sulfuric acid neutralisation
Consumption is big, and financial cost is high, serious to equipment corrosion.CO2Neutralisation needs stable CO2Gas
Source, general petrochemical plant are not easy to provide.
Oxidizing process includes wet oxidation (WAO) and CWO (CWAO);MTO salkali waste
Not sulfur-bearing in liquid, therefore, when handling MTO spent lyes, WAO and CWAO are inapplicable.
Biological treatment is with QBR (Quick Bioreactor) high-concentration sewage disposal technologies and South Korea SK
Biological reinforcing technology is representative, is a kind of biological oxidation technology.Biological treatment inevitably has
Have that long flow path, floor space are big, treatment effeciency is low, operating cost (needing regular replenishment strain) is higher
The shortcomings of, the application of bioanalysis is limited to a certain extent.Meanwhile one can be produced using bioanalysis
Quantitative sludge, the processing to sludge are also increasingly restricted.
To sum up analyze, for MTO spent lyes, current various processing methods exist it is inapplicable,
The problems such as investment is big, operating cost is high, efficiency is low.
The content of the invention
It is an object of the invention to provide a kind of handling process of inexpensive MTO alkali cleanings zero discharged waste alkali liquid,
For MTO spent lyes not sulfur-bearing, the features such as content of organics is high, in efficient, inexpensive reduction MTO
In spent lye while content of organics, it is acid to continue on for caustic wash tower removing by regeneration for spent lye
Gas, realize the efficient of MTO spent lyes, zero discharge treatment and recycle.
To achieve these goals, the present invention provides a kind of inexpensive MTO alkali cleanings zero discharged waste alkali liquid
Handling process, the handling process comprise the following steps:
(1) oil wash deaerates:MTO spent lyes are washed using washing oil, tentatively remove spent lye
Middle entrained oil class;Reduced pressure treatment is carried out to the spent lye after oil wash, reduces to its pressure
0.15MPaG~flare pressure;
(2) storage tank is stood:Spent lye after preliminary removing oils and reduced pressure treatment, passes through in storage tank
Stop and stand, oil slick is further removed after profit layering;
(3) carbonate is removed:Carbonate deposition agent is added in the spent lye after standing oil removing to be precipitated
Reaction, stratification remove the precipitation in spent lye afterwards;
(4) alkali liquid regeneration:Sodium hydroxide is added into the spent lye for removing carbonate, carries out alkali lye again
It is raw.
In step (1), described oil wash is directed to inject washing oil in spent lye, utilizes washing oil and salkali waste
Liquid tentatively dissolves into the oils in spent lye to being present in the different solubility of the oils in spent lye
In washing oil, by stratification, washing oil and spent lye are separated, reach the purpose of spent lye de-oiling.
According to handling process provided by the invention, it is preferable that in step (1), the washing oil is containing benzene
Gasoline.
Spent lye comes from caustic wash tower, and pressure is about 0.5-1.8MPaG, according to processing work provided by the invention
Skill, it is preferable that in step (1), reduced pressure treatment is carried out to the spent lye after oil wash, makes its pressure
Reduce to 0.08MPaG~flare pressure (about 0.05MPaG).Pressure reduces, and hydro carbons is in spent lye
Solubility reduces, and can remove the gaseous hydrocarbons of dissolving, while the organic oxygen compound that annoying proposition is a small amount of.
Deaerated by oil wash, the content of organics in spent lye can be reduced to about by about 6000-10000mg/l
2000-4500mg/l。
In step (2), spent lye needs to stand in storage tank stops time enough, is layered profit
So as to remove free oils.The standing residence time except considering profit layering, it is also necessary to consider MTO
The buffer time of operational load fluctuation and the waste alkali liquor treatment device maintenance of agent set.According to this hair
The handling process of bright offer, it is preferable that in step (2), stop of the spent lye in storage tank is stood
Time is 5-10 days, more preferably 6-8 days.
In order that oil particulates small in spent lye are fully gathered into compared with larger oil droplet, to ensure deoiling effect,
According to handling process provided by the invention, it is preferable that in step (2), spent lye is oily in storage tank
Free oils is further removed by coalescer after water separation.
In step (3), in the spent lye after stewing process inorganic matter substantially only containing NaOH and
Na2CO3, carbonate can not only be removed by adding carbonate deposition agent, and can also improve NaOH's
Concentration.In step (3), it is preferable that carbonate deposition agent is selected from calcium oxide and/or calcium hydroxide.
According to Na2CO3Concentration determines to add the amount of calcium oxide or calcium hydroxide, sodium carbonate and calcium hydroxide reaction
Generation sodium hydroxide and precipitation of calcium carbonate, carbonate clearance can reach more than 99%.Reaction equation
For:
Na2CO3+Ca(OH)2→2NaOH+CaCO3↓。
In step (4), remove inorganic matter in the spent lye of carbonate and only contain NaOH, other inorganic matters
Micro presence, do not interfere with the use after alkali liquid regeneration.Now, solid hydrogen is added into spent lye
Sodium oxide molybdena or certain density fresh sodium hydroxide solution, it is dense that control regenerates sodium hydroxide in spent lye
Spend consistent with the concentration that caustic wash tower needs.The naoh concentration needed in caustic wash tower is 5-15wt%,
Caused regeneration sodium hydroxide solution can continue on for the caustic wash tower of upstream, and realization recycles.
Because the spent lye crossed by the PROCESS FOR TREATMENT can recycle, even if containing few in spent lye
The organic oxygen compound of amount, caustic wash tower butter may be produced, but because Matter Transfer, accumulation
Certain density organic oxygen compound can be removed in step (1) by oil wash, finally realize organic oxidation
Thing content is balanced, and butter is also constantly discharged because alkali lye circulates.
The beneficial effect that technical scheme is brought is:
1st, after present invention process is handled, sodium hydroxide can be realized at spent lye with regeneration
The zero-emission of reason, alkali lye dosage is greatly reduced, mitigate environmental protection pressure;
What the 2nd, the present invention can be achieved to be not required to MTO device caustic wash units adds fresh alkali lye, is not required to phase
Equipment facility is closed, investment is reduced and takes up an area;
3rd, subsidiary conditions used in the present invention are common washing oil, steam, nitrogen etc., and regular chemical plant holds
Be easy to get to;
4th, process condition relaxes, and equipment and materials is carbon steel or stainless steel, and cost is low;
5th, calcium carbonate caused by spent lye is solid waste, and processing is relatively easy;
6th, acid-base neutralization process is not required to, avoids use and the equipment corrosion of sulfuric acid hazardous chemical.
Brief description of the drawings
Fig. 1 shows the processing technological flow figure of inexpensive MTO alkali cleanings zero discharged waste alkali liquid.
Label is described as follows in figure:
1- oil washes deaerate;2- storage tanks are stood;3- removes carbonate;4- alkali liquid regenerations.
Embodiment
The preferred embodiment of the present invention is more fully described below with reference to accompanying drawings.Although show in accompanying drawing
The preferred embodiment of the present invention is shown, however, it is to be appreciated that may be realized in various forms the present invention
Without should be limited by embodiments set forth herein.
Embodiment 1
The spent lye of one MTO caustic wash towers bottom discharge, wherein:COD is 8000mg/l, Na2CO3
Concentration is 7.6wt%, NaOH concentration 1.6wt%, and free oils is 250mg/l, methanol concentration
0.03mol%, dimethyl ether con 0.01mol%.
It is as follows using the processing technological flow figure shown in Fig. 1, the treatment process steps:
(1) oil wash deaerates:Using the difference of solubility, MTO spent lyes are washed using washing oil
Wash, by stratification, washing oil and spent lye are separated, it is preliminary to remove entrained oil in spent lye
Class;Reduced pressure treatment is carried out to the spent lye after oil wash, its pressure is reduced to by 1.4MPaG
0.05MPaG;Deaerated by oil wash, the content of organics of oil content and dissolving in spent lye reduces
To about 4000mg/l;
(2) storage tank is stood:By the spent lye after preliminary removing oils and reduced pressure treatment, enter in storage tank
Row, which stops, to be stood, and stop time of repose of the spent lye in storage tank is 6 days;After profit layering, lead to
Cross oil skimming and further remove oil slick;
(3) carbonate is removed:According to Na2CO3Concentration, added in the spent lye after standing oil removing
Calcium oxide carries out precipitation reaction, removes the precipitation in spent lye after stratification, sodium hydroxide it is dense
Degree, which can be improved to 6wt%, carbonate clearance, can reach more than 99%;
(4) alkali liquid regeneration:20wt% fresh sodium hydroxide is added into the spent lye for removing carbonate
Solution, alkali liquid regeneration is carried out, control naoh concentration and caustic wash tower needs in the spent lye of regeneration
10wt% concentration is consistent.
By the PROCESS FOR TREATMENT, even if containing organic oxygen compound in spent lye, caustic wash tower butter may be made
Produce, but because Matter Transfer, the certain density organic oxygen compound of accumulation can be in step (1)
Removed by oil wash, finally realize that organic oxygen compound content balances, butter is also continuous because alkali lye circulates
Discharge.It can realize that alkali lye recycles.
Embodiment 2
The spent lye of one MTO caustic wash towers bottom discharge, wherein:COD is 15000mg/l, Na2CO3
Concentration is 6.7wt%, NaOH concentration 1.5wt%, free oil 1000mg/l, methanol concentration
0.04mol%, dimethyl ether con 0.02mol%.
It is as follows using the processing technological flow figure shown in Fig. 1, the treatment process steps:
(1) oil wash deaerates:Using the difference of solubility, MTO spent lyes are washed using washing oil
Wash, by stratification, washing oil and spent lye are separated, it is preliminary to remove entrained oil in spent lye
Class;Reduced pressure treatment is carried out to the spent lye after oil wash, its pressure is reduced to by 1.3MPaG
0.05MPaG;Deaerated by oil wash, the content of organics of oil content and dissolving in spent lye reduces
To about 4000mg/l;
(2) storage tank is stood:By the spent lye after preliminary removing oils and reduced pressure treatment, enter in storage tank
Row, which stops, to be stood, and stop time of repose of the spent lye in storage tank is 8 days;After profit layering, lead to
Cross oil skimming and remove oil slick;
(3) carbonate is removed:According to Na2CO3Concentration, added in the spent lye after standing oil removing
Calcium hydroxide carries out precipitation reaction, and the precipitation in spent lye is removed after stratification, sodium hydroxide
Concentration can improve to 5wt%, carbonate clearance and can reach more than 99%;
(4) alkali liquid regeneration:20wt% fresh sodium hydroxide is added into the spent lye for removing carbonate
Solution, alkali liquid regeneration is carried out, control naoh concentration and caustic wash tower needs in the spent lye of regeneration
10wt% concentration is consistent.
By the PROCESS FOR TREATMENT, even if containing organic oxygen compound in spent lye, caustic wash tower butter may be made
Produce, but because Matter Transfer, the certain density organic oxygen compound of accumulation can be in step (1)
Removed by oil wash, finally realize that organic oxygen compound content balances, butter is also continuous because alkali lye circulates
Discharge.It can realize that alkali lye recycles.
Embodiment 3
The spent lye of one MTO caustic wash towers bottom discharge, wherein:COD is 8000mg/l, Na2CO3
Concentration is 7.6wt%, NaOH concentration 1.6wt%, and free oils is 250mg/l, methanol concentration
0.03mol%, dimethyl ether con 0.01mol%.
It is as follows using the processing technological flow figure shown in Fig. 1, the treatment process steps:
(1) oil wash deaerates:Using the difference of solubility, MTO spent lyes are washed using washing oil
Wash, by stratification, washing oil and spent lye are separated, it is preliminary to remove entrained oil in spent lye
Class;Reduced pressure treatment is carried out to the spent lye after oil wash, its pressure is reduced to by 1.4MPaG
0.1MPaG;Deaerated by oil wash, the content of organics of oil content and dissolving in spent lye is reduced to
About 5000mg/l;
(2) storage tank is stood:By the spent lye after preliminary removing oils and reduced pressure treatment, enter in storage tank
Row, which stops, to be stood, and stop time of repose of the spent lye in storage tank is 6 days;After profit layering, lead to
Cross oil skimming and remove oil slick;
(3) carbonate is removed:According to Na2CO3Concentration, added in the spent lye after standing oil removing
Calcium oxide carries out precipitation reaction, removes the precipitation in spent lye after stratification, sodium hydroxide it is dense
Degree, which can be improved to 5wt%, carbonate clearance, can reach more than 99%;
(4) alkali liquid regeneration:20wt% fresh sodium hydroxide is added into the spent lye for removing carbonate
Solution, alkali liquid regeneration is carried out, control naoh concentration and caustic wash tower needs in the spent lye of regeneration
10wt% concentration is consistent.
Comparative example 1
The spent lye of one MTO caustic wash towers bottom discharge, wherein:COD is 8000mg/l, Na2CO3
Concentration is 7.6wt%, NaOH concentration 1.6wt%, and free oils is 250mg/l, methanol concentration
0.03mol%, dimethyl ether con 0.01mol%.
It is as follows using the processing technological flow figure shown in Fig. 1, the treatment process steps:
(1) deaerate:Reduced pressure treatment is carried out to spent lye, its pressure is reduced to by 1.4MPaG
0.05MPaG;By degassing, the content of organics of oil content and dissolving in spent lye is reduced to about
7000mg/l;
(2) storage tank is stood:By the spent lye after reduced pressure treatment, stop standing is carried out in storage tank, is given up
Stop time of repose of the alkali lye in storage tank is 6 days;After profit layering, oil slick is removed by oil skimming;
(3) carbonate is removed:According to Na2CO3Concentration, added in the spent lye after standing oil removing
Calcium oxide carries out precipitation reaction, removes the precipitation in spent lye after stratification, sodium hydroxide it is dense
Degree, which can be improved to 6wt%, carbonate clearance, can reach more than 99%;
(4) alkali liquid regeneration:20wt% fresh sodium hydroxide is added into the spent lye for removing carbonate
Solution, alkali liquid regeneration is carried out, control naoh concentration and caustic wash tower needs in the spent lye of regeneration
10wt% concentration is consistent.
The spent lye of comparative example 1 is handled according to the handling process of embodiment 1, unlike, do not select
Oil wash step.After processing, content of organics is removed to below 7000mg/l, sodium hydroxide in spent lye
Concentration can reach the 10wt% of caustic wash tower needs concentration.But without oil wash step, in spent lye
It can be accumulated containing organic oxygen compound, while caustic wash tower can be promoted to produce a large amount of butter, organic matter and butter are equal
It is unable to discharge system.It is thus impossible to realize that alkali lye recycles, it is impossible to reach zero-emission.
Various embodiments of the present invention are described above, described above is exemplary, and exhaustive
Property, and it is also not necessarily limited to disclosed each embodiment.In the model without departing from illustrated each embodiment
Enclose and spirit in the case of, many modifications and changes for those skilled in the art
It will be apparent from.
Claims (7)
1. a kind of handling process of inexpensive MTO alkali cleanings zero discharged waste alkali liquid, it is characterised in that should
Handling process comprises the following steps:
(1) oil wash deaerates:MTO spent lyes are washed using washing oil, tentatively remove spent lye
Middle entrained oil class;Reduced pressure treatment is carried out to the spent lye after oil wash, reduces to its pressure
0.15MPaG~flare pressure;
(2) storage tank is stood:Spent lye after preliminary removing oils and reduced pressure treatment, passes through in storage tank
Stop and stand, oil slick is further removed after profit layering;
(3) carbonate is removed:Carbonate deposition agent is added in the spent lye after standing oil removing to be precipitated
Reaction, stratification remove the precipitation in spent lye afterwards;
(4) alkali liquid regeneration:Sodium hydroxide is added into the spent lye for removing carbonate, carries out alkali lye again
It is raw.
2. the handling process of inexpensive MTO alkali cleanings zero discharged waste alkali liquid according to claim 1,
Wherein, in step (1), reduced pressure treatment is carried out to the spent lye after oil wash, reduces to its pressure
0.08MPaG~flare pressure.
3. the processing work of inexpensive MTO alkali cleanings zero discharged waste alkali liquid according to claim 1
Skill, wherein, in step (2), spent lye enters one after water-oil separating in storage tank by coalescer
Step removes free oils.
4. the processing work of inexpensive MTO alkali cleanings zero discharged waste alkali liquid according to claim 1
Skill, wherein, in step (2), stop time of repose of the spent lye in storage tank is 5-10 days.
5. the processing work of inexpensive MTO alkali cleanings zero discharged waste alkali liquid according to claim 4
Skill, wherein, in step (2), stop time of repose of the spent lye in storage tank is 6-8 days.
6. the inexpensive MTO alkali cleanings zero discharged waste alkali liquid according to any one of claim 1-5
Handling process, wherein, in step (1), the washing oil is the gasoline containing benzene.
7. the inexpensive MTO alkali cleanings zero discharged waste alkali liquid according to any one of claim 1-5
Handling process, wherein, in step (3), carbonate deposition agent is selected from calcium oxide and/or hydroxide
Calcium.
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Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN202497742U (en) * | 2012-03-02 | 2012-10-24 | 江苏克莱斯克能源装备有限公司 | Waste alkali oil-water separating coalescer |
CN104609623A (en) * | 2013-11-05 | 2015-05-13 | 中国石油化工股份有限公司 | Ethylene alkaline cleaning waste liquid processing method |
CN105217830A (en) * | 2014-06-25 | 2016-01-06 | 中国石油化工股份有限公司 | A kind of method for oxidation of methanol-to-olefins waste lye |
-
2016
- 2016-05-31 CN CN201610377730.2A patent/CN107445330B/en active Active
Patent Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN202497742U (en) * | 2012-03-02 | 2012-10-24 | 江苏克莱斯克能源装备有限公司 | Waste alkali oil-water separating coalescer |
CN104609623A (en) * | 2013-11-05 | 2015-05-13 | 中国石油化工股份有限公司 | Ethylene alkaline cleaning waste liquid processing method |
CN105217830A (en) * | 2014-06-25 | 2016-01-06 | 中国石油化工股份有限公司 | A kind of method for oxidation of methanol-to-olefins waste lye |
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