CN101353187A - MTO prewhirl flow type reaction waste vapor stripping purifying method and apparatus - Google Patents
MTO prewhirl flow type reaction waste vapor stripping purifying method and apparatus Download PDFInfo
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- CN101353187A CN101353187A CNA2008100427158A CN200810042715A CN101353187A CN 101353187 A CN101353187 A CN 101353187A CN A2008100427158 A CNA2008100427158 A CN A2008100427158A CN 200810042715 A CN200810042715 A CN 200810042715A CN 101353187 A CN101353187 A CN 101353187A
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Abstract
The invention provides a method for stripping and purifying MTO prerotation flow pattern reaction wastewater. The method comprises that micro rotational flow separation is carried out on the MTO reaction wastewater to remove the contained catalyzer particles thereof. A device for stripping and purifying MTO prerotation flow pattern reaction wastewater is also provided by the invention.
Description
Technical field
The invention belongs to coal transformation technology field, relate to and remove the method and apparatus that enters the minor amount of catalyst particles that exists in the preceding reaction waste of stripping tower in the MTO technological process, be suitable for handling the heterogeneous sepn process of solid-liquid that comprises MTO technological reaction waste water.Specifically, the invention provides a kind of MTO prewhirl flow type reaction waste vapor stripping purifying method and device.
Background technology
MTO is the abbreviation of Methane To Olefin, that is, and and methanol-to-olefins.The methanol-to-olefins technology mainly was divided into for two steps: at first be by the Sweet natural gas synthetic coarse methanol, methyl alcohol is converted into the alkene based on ethene and propylene more then.The ethene that different technology generates is different with the ratio of propylene.Representative MTO technology has at present: the Technology of UOP, UOP/Hydro, ExxonMobil and the Dalian Chemistry and Physics Institute.Along with the national economic development and day by day riseing to the low-carbon alkene demand, be faced with more and more serious short situation as raw material resources such as the petroleum naphtha of ethylene production raw material, solar oils, therefore, the industrial application problem of quickening methanol-to-olefins technology has caused the attention of each side.
Unreacted portion methyl alcohol and reaction gas enter quench tower after leaving reactor together in MTO technology, and water is that liquid separates with olefin product with methanol condensed in quench tower.The reaction waste that is dissolved with methyl alcohol is sent to stripping in the stripping tower, with methyl alcohol and water sepn.Stripping is one of method of parting liquid phase mixture, and steam stripped cardinal principle is exactly to utilize the phase equilibrium relationship between gas-liquid two-phase that volatile components is transferred to the gas phase from liquid phase.In the technology that the present invention relates to, be to discharge from cat head after methyl alcohol is transferred to gas phase by water, contained the water of methyl alcohol at the bottom of the tower hardly.
Because also contain minor amount of catalyst particles in the reaction waste, and granules of catalyst enters into the stable operation that stripping tower can influence gas stripping column, in order to guarantee the stripping tower long-term operation, preferred plan is before reaction waste enters stripping tower it to be carried out denitrating catalyst to handle, and meanwhile reduces the pollution of granules of catalyst to the downstream material.The separation of reaction waste catalyzer belongs to heterogeneous solid-liquid and separates, and current traditional physics solid-liquid isolation technique mainly can be divided into several classes: filtration, sedimentation, electrostatic separation, centrifugation, membrane sepn etc.According to separation principle, membrane separation technique also belongs to the category of filtering separation.
Liquid takes off the adoptable equipment of thin granules of catalyst accurate filter, magnetic separator, membrane separation apparatus, cyclone separator etc.Their use occasion difference, effect also difference are very big.Accurate filter and membrane separation apparatus exist mainly that cost is too high, maintenance cost also compares higher, and pressure drop is excessive after easily stopping up, stopping up, result of use is good under the little situation of low discharge, catalyst content, but under the bigger situation of big flow, catalyst content the bad problem of result of use.Magnetic separator need be selected design according to the character of catalyzer own, and the liquid that contains granules of catalyst is by a high gradient magnetic separator, and catalyzer is subjected to very strong magnetic field force effect, is captured and holds back, and realizes the separation of catalyzer; This technology application surface is narrow, and magnetic field needs to produce with electric field, and energy consumption is bigger, effect and bad under the situation of the big little content of flow.
Chinese patent application CN 1942558A discloses the recovery method of discharging reactor catalyst in a kind of one or more solid-liquid cyclonic separators that adopt a cover serial or parallel connection combined running or the hydrocyclone recycle oxygenate-to-olefin process, and catalyzer reclaims use after separating.The conventional solid-liquid cyclone separator or the separation accuracy of wet cyclone are the 5-10 micron, but several vapor-solid cyclonic separation in reactor, have been passed through from the product stream that reactor is discharged, very little (the 1-20 micron of the particle diameter of granules of catalyst in the reaction waste, 80% below 10 microns), therefore conventional solid-liquid cyclone separator or wet cyclone can not play effective separating effect.
In addition, although also adopt the method that one or more gas-solid separating devices are installed at the fluidized-bed reactor top in the prior art, but go out in the reaction product stream of reactor and still carry the little amount of catalyst fine particle, these catalyst particles leave quench tower with reaction waste in quench tower, cause the stripping reaction waste to contain to be difficult on a small quantity the solid particulate of removing.
Therefore, this area presses for a kind of method that can more effectively remove minor amount of catalyst particles in the MTO reaction waste of developing.
Summary of the invention
The invention provides a kind of new, remove the method and the device that enter the minor amount of catalyst particles that exists in the reaction waste before the stripping tower in the MTO technological process, overcome the defective that prior art exists.
On the one hand, the invention provides a kind of MTO prewhirl flow type reaction waste vapor stripping purifying method, this method comprises:
The MTO reaction waste is carried out little cyclonic separation, to remove the granules of catalyst that wherein contains.
One preferred embodiment in, the working temperature of described MTO reaction waste is 95-115 ℃, catalyst content is 30-400mg/L, catalyst particle size is the 1-10 micron, density of catalyst is 1300-1500kg/m
3
Another preferred embodiment in, after having carried out described little cyclonic separation, catalyst content is below the 30mg/L.
Another preferred embodiment in, the density of described MTO reaction waste is 900-930kg/m
3, viscosity is the 0.15-0.35 centipoise.
Another preferred embodiment in, described little cyclonic separation is to use little cyclone separator to carry out.
Another preferred embodiment in, described little cyclone separator is made up of eddy flow core pipe.
On the other hand, the invention provides a kind of MTO prewhirl flow type reaction waste vapor stripping refining plant, this device comprises:
Be connected with quench tower, be used for the MTO reaction waste is carried out little cyclonic separation, to remove little cyclone separator of the granules of catalyst that wherein contains.
One preferred embodiment in, described little cyclone separator is made up of eddy flow core pipe.
Another preferred embodiment in, the pressure-losses of described little cyclone separator is 0.2-0.5MPa.
Another preferred embodiment in, the inlet velocity of described little cyclone separator is the 8-15 meter per second, the water inlet gauge pressure is 0.9-1.3MPa.
Description of drawings
Fig. 1 is the synoptic diagram according to the little cyclonic separation purification process of MTO technology stripping reaction waste of one embodiment of the present invention.
Embodiment
The present inventor finds through after the extensive and deep research, little cyclone separator has separation efficiency height, reliability height, advantage such as applied widely, be applied to remove granules of catalyst in the MTO reaction waste and can more effectively remove and enter the minor amount of catalyst particles that exists in the reaction waste before the stripping tower in the MTO technological process, overcome the defective that exists in the prior art.Based on above-mentioned discovery, the present invention is accomplished.
The reaction mechanism of MTO is that the dehydration of methyl alcohol elder generation generates dme, and the dehydration of the equilibrium mixture of dme and methyl alcohol is converted into low-carbon alkene and a small amount of stable hydrocarbon, the aromatic hydrocarbons etc. based on ethene, propylene then, has generated a large amount of water owing to dehydration reaction in the reaction process.Water and unreacted methanol are carried little amount of catalyst with the form of gas and are left reactor with product, and the logistics of discharging reactor is called reaction gas.After reaction gas entered quench tower and cools off, water vapour and methanol solution turned to liquid, and first alcohol and water soluble in water is discharged quench tower together, is called reaction waste.Most of reaction waste is extracted out from the middle and upper part of tower, because the position in quench tower is high more, granules of catalyst content is few more, claims that in order to distinguish this part reaction waste is reaction waste A; Remaining a part of reaction waste is discharged quench tower at the bottom of tower, be called water (reaction waste B) at the bottom of the quench tower.Being called chilling after reaction waste B separates through little cyclone separator purifies waste water, chilling is purified waste water and reaction waste B mixes a part of quench tower cooling reaction gas that returns again in back after the supercooler cooling, reached the recycle of water, a part is called the stripping reaction waste in addition, and the stripper stripping that degass is with separation of methanol.Separate the methyl alcohol that obtains and get back to reactor continuation reaction, and water is delivered to another device as the raw material that generates synthetic gas, has realized the efficient resource utilization of water.
Repeatedly partial gasification can obtain highly purified difficult volatiles in liquid phase in theory, repeatedly partial condensation can obtain highly purified volatile components in gas phase, and water and methyl alcohol boiling point difference are bigger, therefore can adopt the distillatory method to realize the separation of first alcohol and water in gas stripping column.Temperature increases at the bottom of from cat head to tower gradually in the tower, and tower top temperature is greatly about 100-130 ℃.
The catalyst content of reaction waste A lower (30-400mg/L), particle less (1-10 micron), the catalyst content that the chilling that the little cyclone separator purification of process obtains is purified waste water is lower than the catalyst content of reaction waste A especially, but the catalyst fines that they carry still can accumulate in gas stripping column, influence the operation of gas stripping column, in order to prolong the cycle of operation of stripping tower, the present inventor adopts little cyclone separator that the stripping reaction waste is carried out little cyclonic separation purifying treatment.Described little cyclone separator is made up of some eddy flow core pipes.It is little that little cyclone separator has the operation pressure drop, advantage of low energy consumption.
In a first aspect of the present invention, a kind of MTO prewhirl flow type reaction waste vapor stripping purifying method is provided, this method comprises:
To water at the bottom of the MTO technology quench tower, promptly reaction waste carries out little cyclonic separation, with remove granules of catalyst in the reaction waste (that is, and the granules of catalyst of carrying secretly in the reactor, its content is about 30-400mg/L, density is about 900-930kg/m
3, particle diameter is about the 1-10 micron).
Preferably, the working temperature of described reaction waste is about 95-115 ℃, and catalyst content is about 30-400mg/L, and catalyst particle size is about the 1-10 micron, and density of catalyst is about 1300-1500kg/m
3
Preferably, the density of described reaction waste is about 900-930kg/m
3, viscosity is about the 0.15-0.35 centipoise.
In a second aspect of the present invention, a kind of MTO prewhirl flow type reaction waste vapor stripping refining plant is provided, this device comprises:
Be connected with MTO reactor 1, the reaction gas that is used for reactor carries out chilling so that the alkene of product and water are able to isolating quench tower 2, and most of granules of catalyst enters in the water in quench tower; Be connected with described quench tower 2, be used for the stripping reaction waste is carried out solid-liquid separation to remove little cyclone separator 5-2 of stripping reaction waste catalyzer; Be connected with described little cyclone separator 5-2, be used for the stripping reaction waste after purifying is transported to the stripping water pump 3-2 of gas stripping column; Be connected with described stripping water pump 3-2, be used for the stripping after the purification that obtains through solid-liquid separation purified waste water and carry out steam stripped gas stripping column 6, in order to divide dried up in dissolved do not participate in the methyl alcohol of reaction.
Preferably, the pressure-losses of described little cyclone separator (that is the pressure difference between little cyclone separator inlet and the overflow port) is about 0.2-0.5MPa.
Preferably, the inlet velocity of described little cyclone separator is about the 8-15 meter per second, and the water inlet gauge pressure is about 0.9-1.3MPa.
Preferably, method and apparatus of the present invention also can be applied to the purification of MTP (preparing propylene from methanol) and OTO (producing lighter hydrocarbons from oxygenatedchemicals) technological reaction waste water.
Below referring to accompanying drawing.
Fig. 1 is the synoptic diagram according to the little cyclonic separation purification process of MTO technology stripping reaction waste of one embodiment of the present invention.As shown in Figure 1, methyl alcohol enters a series of dehydration reaction production of process under the effect of catalyzer of MTO reactor 1 back and meanwhile also generates a large amount of water based on the olefin product of ethene and propylene from reactor 1 bottom; Be present in reactant in the MTO reactor 1 and the product of not consumption leaves from the top of MTO reactor 1 with gas form; The reaction product and the unreacted reactant of part that come out from MTO reactor 1 cool off to quench tower 2, and water and methanol condensed are liquid phase in quench tower 2, separate with other reaction product, and olefin product leaves quench tower 2 to the washing of water wash column (not shown); A water that condensation is got off and a methyl alcohol part are discharged from the bottom of quench tower 2, are called reaction waste B, and a part is extracted out from the middle and upper part of quench tower 2 in addition, is called reaction waste A; Reaction waste B handles the back through little cyclone separator 5-1 cyclone de-solid and mixes with reaction waste B under the effect of chilling water pump 3-1, a mixed reaction waste part after supercooler 4 cooling as chilling agent return quench tower 2, another part enters the granules of catalyst that further removes among little cyclone separator 5-2 wherein once more; Water stripping after the purification is transported to gas stripping column 6 and removes wherein methyl alcohol under the effect of stripping water pump 3-2; The methyl alcohol that reclaims returns MTO reactor 1 and participates in reaction, and water is as the raw material of producing synthetic gas.
The separation test effect of little cyclone separator has been shown in the following table 1 under the different pressure-losseses.
Table 1
As can be seen, the pressure boost loss helps the raising of separation efficiency from last table 1, can increase the energy consumption of technology in the time of still because of the pressure boost loss, and therefore in the present invention, the pressure-losses of little cyclone separator is 0.2-0.5MPa preferably.
Having illustrated in the pressure-losses in the following table 2 is 0.30MPa, and import granules of catalyst concentration is under the condition of 218.44mg/L, the import and the overflow port size-grade distribution of stripping reaction waste catalyzer micro powder granule.
Table 2
As can be seen, 83.48% granules of catalyst particle diameter is arranged less than 10.257 microns in the stripping reaction waste from last table 2, therefore, want the separation efficiency that reaches good, conventional cyclonic separation equipment is difficult to realize.Separate through little cyclone separator, the particle greater than 10 microns in the treated water outlet (overflow port) has only 0.7%, and the separation efficiency of overall separation efficiency up to 88.95%, 5.506 micron is about 80.0%.
The major advantage of method and apparatus of the present invention is:
The present invention adopts little cyclone separator that MTO technology stripping reaction waste is carried out Removal of catalyst particle place Reason, equipment of the present invention is simple, separative efficiency is high, guaranteed the long-term operation of equipment.
All quote in this application as a reference at all documents that the present invention mentions, just as each piece document Quoted separately as a reference such. Should be understood that in addition after having read above-mentioned instruction content of the present invention, Those skilled in the art can make various changes or modifications the present invention, and these equivalent form of values fall within this Shen equally Please the appended claims limited range.
Claims (10)
1. MTO prewhirl flow type reaction waste vapor stripping purifying method, this method comprises:
The MTO reaction waste is carried out little cyclonic separation, to remove the granules of catalyst that wherein contains.
2. the method for claim 1 is characterized in that, the working temperature of described MTO reaction waste is 95-115 ℃, and catalyst content is 30-400mg/L, and catalyst particle size is the 1-10 micron, and density of catalyst is 1300-1500kg/m
3
3. method as claimed in claim 2 is characterized in that, after having carried out described little cyclonic separation, catalyst content is below the 30mg/L.
4. the method for claim 1 is characterized in that, the density of described MTO reaction waste is 900-930kg/m
3, viscosity is the 0.15-0.35 centipoise.
5. as each described method among the claim 1-4, it is characterized in that described little cyclonic separation is to use little cyclone separator to carry out.
6. method as claimed in claim 5 is characterized in that, described little cyclone separator is made up of eddy flow core pipe.
7. MTO prewhirl flow type reaction waste vapor stripping refining plant, this device comprises:
Be connected with quench tower (2), be used for the MTO reaction waste is carried out little cyclonic separation, to remove little cyclone separator (5-2) of the granules of catalyst that wherein contains.
8. device as claimed in claim 7 is characterized in that, described little cyclone separator is made up of eddy flow core pipe.
9. as claim 7 or 8 described devices, it is characterized in that the pressure-losses of described little cyclone separator is 0.2-0.5MPa.
10. as claim 7 or 8 described devices, it is characterized in that the inlet velocity of described little cyclone separator is the 8-15 meter per second, the water inlet gauge pressure is 0.9-1.3MPa.
Priority Applications (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2008100427158A CN101353187B (en) | 2008-09-10 | 2008-09-10 | MTO prewhirl flow type reaction waste vapor stripping purifying method and apparatus |
| EP09157758.5A EP2163310A3 (en) | 2008-09-10 | 2009-04-09 | Method for purifying quench water and scrubbing water from MTO (methanol-to-olefin process) by mini-hydrocyclone and apparatus used for same |
| US12/427,578 US8083951B2 (en) | 2008-09-10 | 2009-04-21 | Method for purifying quench water and scrubbing water from MTO by mini-hydrocyclone and apparatus used for same |
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|---|---|---|---|
| CN2008100427158A CN101353187B (en) | 2008-09-10 | 2008-09-10 | MTO prewhirl flow type reaction waste vapor stripping purifying method and apparatus |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102093153A (en) * | 2010-11-05 | 2011-06-15 | 华东理工大学 | Optimal combination method and device for purifying and separating MTO (Methanol To Olefins) reaction gas containing catalyst micropowder |
| 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 |
| CN104826670A (en) * | 2015-04-14 | 2015-08-12 | 华东理工大学 | Method and apparatus for removing oil pollutants contained in catalyst micro-powder in MTO quenching wastewater |
| CN104888984A (en) * | 2014-03-05 | 2015-09-09 | 中国石化工程建设有限公司 | Magnetic cyclone separator, separation apparatus and separation method |
| CN108373180A (en) * | 2018-04-19 | 2018-08-07 | 浙江兴兴新能源科技有限公司 | A kind of methanol-to-olefins sour water stripper and its sewage water treatment method |
-
2008
- 2008-09-10 CN CN2008100427158A patent/CN101353187B/en active Active
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102093153A (en) * | 2010-11-05 | 2011-06-15 | 华东理工大学 | Optimal combination method and device for purifying and separating MTO (Methanol To Olefins) reaction gas containing catalyst micropowder |
| CN102093153B (en) * | 2010-11-05 | 2014-04-09 | 华东理工大学 | Optimal combination method and device for purifying and separating MTO (Methanol To Olefins) reaction gas containing catalyst micropowder |
| 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 |
| CN104888984A (en) * | 2014-03-05 | 2015-09-09 | 中国石化工程建设有限公司 | Magnetic cyclone separator, separation apparatus and separation method |
| CN104826670A (en) * | 2015-04-14 | 2015-08-12 | 华东理工大学 | Method and apparatus for removing oil pollutants contained in catalyst micro-powder in MTO quenching wastewater |
| CN108373180A (en) * | 2018-04-19 | 2018-08-07 | 浙江兴兴新能源科技有限公司 | A kind of methanol-to-olefins sour water stripper and its sewage water treatment method |
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