CN104326594A - Catalysis-loading conjointing method and device for purifying water quality of methanol-to-olefin (MTO) process quenched water - Google Patents
Catalysis-loading conjointing method and device for purifying water quality of methanol-to-olefin (MTO) process quenched water Download PDFInfo
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- CN104326594A CN104326594A CN201410541502.5A CN201410541502A CN104326594A CN 104326594 A CN104326594 A CN 104326594A CN 201410541502 A CN201410541502 A CN 201410541502A CN 104326594 A CN104326594 A CN 104326594A
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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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- 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
Abstract
The invention discloses a catalysis-loading conjointing method and device for purifying water quality of methanol-to-olefin (MTO) process quenched water. A dual-function catalytic-settlement assistant agent is introduced, one function of the dual-function catalytic-settlement assistant agent is catalytic effect to promote denaturation and destabilization of impurities, the impurities are changed into alumen ustum which is easy to remove and conductive to follow-up flocculation reaction; the other function of the dual-function catalytic-settlement assistant agent is to be used as co-sedimentation matters, a co-sedimentation matter (a conjointing matter) which is heavy in weight, high in density and easy to separate is formed by the co-sedimentation matters and the impurities, and the problems of slow sedimentation or floating of alum floc in the follow-up flocculation process. The catalysis-loading conjointing method and device have good treatment effect, the quality of treated water is clear and transparent, and the device has the advantages of small occupation area. Through arrangement of a catalysis-settlement assistant agent separation and recovery system, the catalytic-settlement assistant agent recovery rate can reach 99.5%, and the catalytic-settlement assistant agent can be recycled in the system.
Description
Technical field
The present invention relates to a kind of chimeric method of catalysis-loading and the device that purify MTO technique quenched water water quality.Also can be used for dyeing waste water, paper waste, pharmacy waste water, basic chemical industry waste water, coal chemical industrial waste water, refinery water and petrochemical wastewater pre-treatment or advanced treatment.
Background technology
Along with the day by day exhaustion of petroleum resources, oil price progressively rises, and make the cost of the oil vapour producing ethylene by cracking taking petroleum naphtha as raw material more and more higher, the price of downstream derivative product increases, and competitive power is more and more weak.Therefore, people transfer searching substitute technology to, to reduce the production cost of ethene, thus the Technology such as Methanol ethene, coal ethene and lighter hydrocarbons ethene is developed thereupon, and handling object of the present invention is exactly the quenched water of Methanol ethene (MTO) process.
In the technological process of Methanol ethene and coal ethene, the reaction heat of generation is taken away by quenched water usually, and reclaims this part heat by series of heat exchangers, for heating other processing medium.Quenched water is actually and recycles between quench tower and interchanger.
Generate at methanol dehydration in the process of ethene, also occur with a large amount of side reactions simultaneously.The by product turbidity that these side reactions generate is large, and viscosity is high; Add in catalyzer use procedure and powder phenomenon-tion can occur, produce a large amount of finely divided particulates, suspended particle in quenched water and organic by-products content very high, and constantly accumulate in working cycle, cause quench tower and the frequent fouling and clogging of heat exchanger, device is had to process of often stopping, and causes the cycle of operation of whole device shorter.
Two kinds of measures are mainly taked to maintain quenched water water conditioning at present:
(1) filtered by part quenched water, the filtrate after filtration returns quench water system again;
(2) while part quenched water filters, the fresh quenched water of part is added, the quenched water decontaminated water Treatment stations of same quantity of simultaneously will draining.
There is following shortcoming in filtration method:
Due to the restriction of the factors such as filtering material, processing power, the cleaning frequency and purchase cost, the filtering material such as screen cloth or very thin filter cloth that order number is very high can not be used.Therefore strainer is caused to there is the following problem that cannot overcome:
1) poor filtration effect.Because catalyst fines particle diameter is too thin and emulsus organic waste cannot filter, filtrate is still very muddy, and still containing a large amount of fine particle and emulsus organic waste in quenched water, quench tower and heat exchanger fouling and clogging problem can not be solved;
2) processing power is unstable.After strainer cleaning, initial stage processing power is strong, along with the prolongation processing power of working time can progressively decline, until can not meet processing requirement to switch cleaning;
3) strainer must frequently be cleared up, and not only labour intensity is large, and impacts equipment life;
4) quenched water temperature is high, and the organic steam that contains a large amount of during cleaning evaporate in environment, causes severe operational environment;
5) strainer needs to clear up weekly once, and cleaning up cost is high.
Because traditional method exists the problems referred to above, so MTO purifying process water problem is never resolved.
Summary of the invention
The object of the invention is:
1) catalyst fines particle and emulsus organic waste in effective elimination Methanol ethene (MTO) quenched water, solve device blockage, the problem that fundamentally thoroughly the solution quenched water water quality impact plant running cycle is short;
2) the present invention is separated impurities in water and can realizes automatically removing continuously, avoid labour intensity that labor cleaning brings greatly, the problem such as severe operational environment.
3) process costs such as equipment cleaning are reduced.
The present invention adopts following technical scheme:
The concrete steps of the chimeric method of catalysis-loading of purification MTO technique quenched water water quality of the present invention are as follows:
(1) quenched water come from Methanol ethylene process is sent into pre-reactor, and add catalysis-settling agent and auxiliary agent in pre-reactor, then mix;
(2) enter the first reactor from pre-reactor quenched water out, and add in the first reactor and become owner of sinking agent, then stir, make main sinking agent and the raw aggregation of the abundant hybrid concurrency of quenched water, at this residence time 2-5 minute;
(3) the second reactor is entered from the first reactor quenched water out, catalysis-the settling agent reclaimed from " block polymer-impurity " separation system is added in second reactor, then mix, with impurity, chimeric reaction occurs, at this residence time 2-5 minute;
(4) enter the 3rd reactor from the second reactor quenched water out, add in the 3rd reactor and help sinking agent, under agitation make it mix with quenched water, make wadding spend rapid increase, at this residence time 2-5 minute;
(5) settling tank is entered from the 3rd reactor quenched water out, purify waste water from settling tank top and discharge in upper strata, gravity flow enters water purification holding tank, and then turn back to quench water system through force (forcing) pump, the block polymer with catalysis-settling agent is discharged bottom settling tank;
(6) block polymer bottom settling tank, will wherein a part directly be turned back in pre-reactor by transferpump, continue to play its katalysis; Another part is delivered to " block polymer-impurity " separation and recovery system;
(7) the isolated impurity of " block polymer-impurity " separation and recovery system is discharged to sludge treating system, and the catalysis-settling agent separated is got back to the second reactor and played a role at this as cosedimentation thing;
(8) for preventing oxygen from dissolving in quenched water, in above-mentioned decontamination process and precipitate and separate process, inert gas seal measure is all adopted.
In step (1), the Titanium series catalyst that catalysis-settling agent is is carrier with iron powder powder, iron powder is a kind of powdered iron ore, granularity 80-180 object mixture; Synthetic method is as follows:
95% iron powder+5% titanium dioxide powder also fully mixes, and then add the epoxy resin binder of 50%, abundant stirring and evenly mixing, dry at 75 DEG C of temperature, ball milling becomes granularity to be 100-160 order; The add-on of catalysis-settling agent is the 1-6% of process water weight.
In step (1), auxiliary agent is sodium hydroxide, adds sodium hydroxide and makes the pH of quenched water be greater than 7.5.
In step (2), main sinking agent is the one in polymerize aluminum chloride, bodied ferric sulfate, polyaluminium sulfate, iron trichloride, and the add-on of main sinking agent is the concentration making it in water is 100-800mg/L.
In step (3), from catalysis-settling agent that " block polymer-impurity " separator reclaims, its add-on is the 30-70% of settling tank output, and settling tank output is the 10-30% of the process water yield.
In step (4), help sinking agent to be fire resistant polypropylene amides, adaptive temperature is greater than 75 DEG C; Helping the add-on of sinking agent to be the concentration making it in process water is 5-25mg/L.
In step (5), in settling tank, be provided with bridge breaker, prevent the delay of block polymer from blocking.
In step (6), " block polymer-impurity " separation and recovery system forms by by broken embedding device, magnet rotary drum and stripper, broken embedding device block polymer structure is broken from, iron powder by the iron powder sucking-off in block polymer, then can be unloaded magnet rotary drum by stripper by magnet rotary drum.
The chimeric high-efficiency water purifying treatment device of catalysis-loading of the present invention is by pre-reactor, the first reactor, the second reactor, the 3rd reactor, and settling tank and " block polymer-impurity " separation and recovery system composition, they are connected by pipeline successively.
Invention introduces " catalysis-help sinking agent " with dual-use function: one of its function is katalysis, promote that impurity sex change is de-steady, become the alumen ustum easily removed, favourable follow-up flocculation reaction; Its another function is the cosedimentation thing as impurity, forms that density is large, quality weight together with impurity, the cosedimentation thing (block polymer) that free settling is separated, and solves the slow or On The Floating of settling of floccus in follow-up flocculation process.Not only plant area is little, and after process, water quality is as clear as crystal.
The design of the present invention to " catalysis-settling agent " is very ingenious, the katalysis of this agent, cosedimentation effect is integrated, and devises unique way of recycling: a part is recycled directly to toss area, plays its katalysis simultaneously; Another part, turns back to system after being reclaimed by " block polymer-impurity " separation and recovery system, continues its cosedimentation thing and utilizes; " block polymer-impurity " separation recovery efficiencies is high, and the rate of recovery of catalysis-settling agent reaches more than 99.5%.
In a word, expensive catalyzer can be made not only to play a dual role but also can not run off.
The present invention can solve a MTO Water warfare industry difficult problem, and at present, Methanol ethene (MTO) is the emerging production technique of ethene, and its advantage is that production cost reduces greatly.But the impurity in quenched water does not have good purifying method, impurity can only circulate in systems in which and accumulate, so often cause equipment to block, have a strong impact on the cycle of operation of device, this has become the technical bottleneck of MTO industry development.Technique quenched water, after process of the present invention, fundamentally can solve device blockage.
Existing processing scheme more problems: first filtration method decontamination effect improving is bad, the ultra-fine grain in water and cotton-shaped organic filtration not out, can not thoroughly be dealt with problems; Strainer still often can produce blocking, brings that labour intensity is large, the problem such as bad environments and environmental pollution; Equipment cleaning is very large on impact equipment life.
Advantage of the present invention:
1) treatment effect is good: the present invention by adding one " catalysis-settling agent " and auxiliary agent in water, its katalysis, suspended substance and colloidal materials can be made de-steady rapidly, and make some dissolved matter sex change, form the alumen ustum easily removed, its treatment effect is good especially, and the water quality after process is as clear as crystal.
2) plant area is little: " catalysis-settling agent " in invention has two kinds of functions, except its katalysis, a function is the cosedimentation thing as impurity in addition, effect due to it makes that the cosedimentation amount of formation is heavy, density is large, settling velocity is fast, solves traditional water treatment pollutent impurity floating or not settlement issues.So taking up an area little is another advantage of the present invention, the occupation of land of this technique accounts for 1/10th of traditional technology.
3) the present invention is simple to operate, easy to maintenance.
4) the present invention is shock-resistant, and suspended contamination change in concentration affects treatment effect hardly.
Accompanying drawing explanation
Fig. 1 is the process flow sheet of method of the present invention;
In figure: 1 pre-reactor, 2 first reactors, 3 second reactors, 4 the 3rd reactors, 5 settling tanks, 6 water purification pots, 7 " block polymer-impurity " separation and recovery system, 8 sludge treating systems.
Embodiment
The following examples describe in further detail of the present invention.
The chimeric high-efficiency water purifying treatment device of catalysis-loading of the present invention is made up of pre-reactor, the first reactor, the second reactor, the 3rd reactor, settling tank and water purification pot, " block polymer-impurity " separation and recovery system, sludge treating system, and they are connected by pipeline successively.
Embodiment 1 process MTO of the present invention device technique quenched water
1) from the quenched water of MTO device interchanger quenched water return water pipe, by sending into quenched water refining plant of the present invention after a reducing valve decompression.
2) add the catalysis-settling agent and auxiliary agent with katalysis at pre-reactor, mix through mixing tank.The effect of catalyzer is that suspended substance, turbidity and other pollutent (being referred to as impurity) in accelerating auxiliaries and water reacts, and makes impurities in water generation sex change de-steady, becomes the material easily removed.In operational process, catalysis-settling agent mainly by directly returning bottom settling tank, and back amount is the 70-30% of settling tank output, and settling tank output is the 10-30% of the process water yield, adds time not enough at this.
3) quenched water of above-mentioned (2) enters the first reactor.Add at this and become owner of sinking agent.This reactor is provided with agitator, and winner's sinking agent is fully mixed with the quenched water of above-mentioned (2).Impurity in main sinking agent and water reacts, and makes impurity particle become large.
4) quenched water of above-mentioned (3) is from flowing into the second reactor.Add at this catalysis-settling agent reclaimed from " block polymer-impurity " separator, the effect of catalysis-settling agent is mutually entrenched togather with impurity, forms the block polymer of the large easily sedimentation of density.
5) the quenched water gravity flow of above-mentioned (4) enters the 3rd reactor.3rd reactor is also provided with agitator.Add at this and high temperature resistantly help sinking agent, under the effect of agitator, help sinking agent that the block polymer in water is increased further, form the macrobead block polymer easily removed.
6) the quenched water gravity flow of above-mentioned (5) enters precipitate and separate system.Quenched water after this completes purification is separated with impurity.Purify waste water from settling tank top and discharge in upper strata, gravity flow enters water purification holding tank, then turns back to quench water system through force (forcing) pump.Block polymer with catalysis-settling agent is discharged bottom settling tank.
7) in order to prevent the delay of block polymer from blocking, have also been devised bridge breaker at this.
8) block polymer bottom settling tank, wherein a part will directly turn back to catalysis-settling agent toss area (before static mixer) by transferpump, continue to play its katalysis; Another part is delivered to " block polymer-impurity " separation and recovery system.
9) the isolated impurity of " block polymer-impurity " separator is discharged to sludge treating system, and the catalysis-settling agent separated is got back to the second reactor and played a role at this as cosedimentation thing.
10) for preventing oxygen from dissolving in quenched water, reactive system and the precipitate and separate system of device all adopt inert gas seal measure.Before and after the process of MTO technique quenched water, leading indicator data are in table 1.
Table 1 " catalysis-loading is fitted together to " purifying treatment MTO technique quenched water catalog data
| Leading indicator | Measure unit | Before process | After process | Clearance (%) |
| CODcr | mg/L | 3650 | 1320 | 63.8 |
| Suspended substance | mg/L | 299 | 15.6 | 95 |
| Turbidity | NTU | 238 | 0.5 | 99.8 |
Embodiment 2. adopts advanced treatment refinery water data of the present invention in table 2.
Table 2 " catalysis-loading is fitted together to " purifying treatment refinery water catalog data
| Leading indicator | Measure unit | Before process | After process | Clearance (%) |
| CODcr | mg/L | 120 | 60 | 50 |
| Suspended substance | mg/L | 80 | 20 | 75 |
| Turbidity | NTU | 45 | 0.5 | 99 |
Embodiment 3. adopts process basic chemical industry (white dyes) waste water data of the present invention in table 3.
Table 3 " catalysis-loading is fitted together to " purifying treatment white dyes waste water catalog data
| Leading indicator | Measure unit | Before process | After process | Clearance (%) |
| CODcr | mg/L | 700 | 250 | 60 |
| Suspended substance | mg/L | 68 | 15 | 78 |
| Fluorescence | Absorbance Unit, writes a Chinese character in simplified form A.U. | 0.9 | 0.01 | 90 |
Although illustrate and describe embodiments of the invention, for the ordinary skill in the art, be appreciated that and can carry out multiple change, amendment, replacement and modification to these embodiments without departing from the principles and spirit of the present invention, scope of the present invention is by claims and equivalents thereof.
Claims (9)
1. purify the chimeric method of catalysis-loading of MTO technique quenched water water quality, it is characterized in that: the concrete steps of described method are as follows:
(1) quenched water come from Methanol ethylene process is sent into pre-reactor, and add catalysis-settling agent and auxiliary agent in pre-reactor, then mix;
(2) enter the first reactor from pre-reactor quenched water out, and add in the first reactor and become owner of sinking agent, then stir, make main sinking agent and the raw aggregation of the abundant hybrid concurrency of quenched water, at this residence time 2-5 minute;
(3) the second reactor is entered from the first reactor quenched water out, catalysis-the settling agent reclaimed from " block polymer-impurity " separator is added in second reactor, then mix, with impurity, chimeric reaction occurs, at this residence time 2-5 minute;
(4) enter the 3rd reactor from the second reactor quenched water out, add in the 3rd reactor and help sinking agent, under agitation make it mix with quenched water, make wadding spend rapid increase, at this residence time 2-5 minute;
(5) settling tank is entered from the 3rd reactor quenched water out, purify waste water from settling tank top and discharge in upper strata, gravity flow enters water purification holding tank, and then turn back to quench water system through force (forcing) pump, the block polymer with catalysis-settling agent is discharged bottom settling tank;
(6) block polymer bottom settling tank, will wherein a part directly be turned back in pre-reactor by transferpump, continue to play its katalysis; Separation system that another part is delivered to " block polymer-impurity ";
(7) the isolated impurity of " block polymer-impurity " separation system is discharged to sludge treating system, and the catalysis-settling agent separated is got back to the second reactor and played a role at this as cosedimentation thing;
(8) for preventing oxygen from dissolving in quenched water, in above-mentioned decontamination process and precipitate and separate process, inert gas seal measure is all adopted.
2. the chimeric method of catalysis-loading of purification MTO technique quenched water water quality as claimed in claim 1, it is characterized in that: in step (1), the Titanium series catalyst that catalysis-settling agent is is carrier with iron powder powder, iron powder is a kind of powdered iron ore, granularity 80-180 object mixture; Synthetic method is as follows: the titanium dioxide powder of 95% iron powder+5% fully mixes, then adds the epoxy resin binder of 50%, stirs and fully mixes, dry at 75 DEG C of temperature, and ball milling becomes granularity to be
100-160 order; The add-on of catalysis-settling agent is the 1-6% of process water weight, in operational process, catalysis-settling agent mainly by directly returning bottom settling tank, back amount is the 70-30% of settling tank output, and settling tank output is the 10-30% of the process water yield, adds time not enough at this.
3. the chimeric method of catalysis-loading of purification MTO technique quenched water water quality as claimed in claim 1, is characterized in that: in step (1), auxiliary agent is sodium hydroxide, adds sodium hydroxide and make the pH of quenched water be greater than 7.5.
4. the chimeric method of catalysis-loading of purification MTO technique quenched water water quality as claimed in claim 1, it is characterized in that: in step (2), main sinking agent is the one in polymerize aluminum chloride, bodied ferric sulfate, polyaluminium sulfate, iron trichloride, and the add-on of main sinking agent is the concentration making it in water is 100-800mg/L.
5. the chimeric method of catalysis-loading of purification MTO technique quenched water water quality as claimed in claim 1, it is characterized in that: in step (3), from catalysis-settling agent that " block polymer-impurity " separator reclaims, its add-on is the 30-70% of settling tank output, and settling tank output is the 10-30% of the process water yield.
6. the chimeric method of catalysis-loading of purification MTO technique quenched water water quality as claimed in claim 1, it is characterized in that: in step (4), help sinking agent to be fire resistant polypropylene amides, adaptive temperature is greater than 75 DEG C; Helping the add-on of sinking agent to be the concentration making it in process water is 5-25mg/L.
7. the chimeric method of catalysis-loading of purification MTO technique quenched water water quality as claimed in claim 1, is characterized in that: in step (5), be provided with bridge breaker in settling tank, prevents the delay of block polymer from blocking.
8. the chimeric method of catalysis-loading of purification MTO technique quenched water water quality as claimed in claim 1, it is characterized in that: in step (6), " block polymer-impurity " separation and recovery system by: broken embedding device, magnet rotary drum and stripper form, broken embedding device effect destroys block polymer structure to be convenient to reclaim, catalysis-settling agent sucking-off that magnet in block polymer with iron powder can will be carrier, stripper is that iron powder is unloaded magnet rotary drum.
9. one kind purifies the device of MTO technique quenched water water quality, it is characterized in that: described device by: pre-reactor, the first reactor, the second reactor, the 3rd reactor, settling tank, water purification pot, " block polymer-impurity " separation and recovery system and sludge treating system form, and they are connected by pipeline successively.
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Citations (3)
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| US4940550A (en) * | 1989-05-02 | 1990-07-10 | The Curators Of The University Of Missouri | Multi-step process for concentrating magnetic particles in waste sludges |
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| CN102716605A (en) * | 2012-07-10 | 2012-10-10 | 上海华畅环保设备发展有限公司 | Method and device for comprehensive utilization of reaction product quenching wastewater generated in preparing isobutene by dehydrogenating isobutane |
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2014
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4940550A (en) * | 1989-05-02 | 1990-07-10 | The Curators Of The University Of Missouri | Multi-step process for concentrating magnetic particles in waste sludges |
| CN201152925Y (en) * | 2008-01-04 | 2008-11-19 | 青岛弘国工贸有限公司 | Magnetic powder recovering device |
| CN102716605A (en) * | 2012-07-10 | 2012-10-10 | 上海华畅环保设备发展有限公司 | Method and device for comprehensive utilization of reaction product quenching wastewater generated in preparing isobutene by dehydrogenating isobutane |
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| 鲁风芹等: "加载嵌合技术深度处理炼油废水的中试研究", 《青岛科技大学学报（自然科学版）》 * |
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