CN105016949B - A kind of method and device of the depth separating methanol of carbon four - Google Patents
A kind of method and device of the depth separating methanol of carbon four Download PDFInfo
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Abstract
The present invention relates to a kind of method and device of the depth separating methanol of carbon four.The treatment of separating methanol is carried out to the carbon four that azeotropic distillation tower top is extracted out, is divided into three steps：Pre- distribution extraction is carried out to carbon four using microfacies distribution technique first；Secondly reextraction is carried out to methyl alcohol in carbon four using micro- eddy flow abstraction technique, the carbon four after last fully extraction carries out carbon four and separated with the depth of extract with extract into modularization depth separator；Carbon four after being processed through separating methanol enters subsequent production device, and extract is reclaimed in returning to methanol distillation column.The present invention also provides a set of device for realizing the method, including extraction equipment and separator；Extraction equipment is divided into microfacies disperser and micro- eddy flow extraction equipment；Separator is coarse separation module and several parts such as corrugated plating reinforcing sedimentation, water bag, interfacial meter.Method of the present invention processing speed is fast, efficiency high, and methanol content is not more than 5ppm in the carbon four after treatment, so as to improve the performance of the follow-up deep processing device of carbon four.
Description
Technical field
The present invention relates to a kind of method of the depth separating methanol of carbon four, specifically, pre- point is carried out using microfacies distribution technique
Cloth extract, then using micro- eddy flow abstraction technique and Coalescence-separation Technology methyl alcohol in carbon four is carried out depth extract separated with depth,
Efficiently, the methyl alcohol in fast eliminating carbon four, improves the performance of the follow-up deep processing device of carbon four.
Background technology
Considerable amount of low molecular hydrocarbons quasi-molecule, such as the carbon fourth class can be generated in petroleum refining process；On the one hand they can be with
Directly burnt as fuel, but it is not high using them as fuel economy benefit, also without valency compared with the fuel such as natural gas
Lattice advantage；On the other hand due to being good organic synthesis raw material containing considerable amount of alkene, higher octane is produced with these alkene
The gasoline blend component of value and a series of petrochemical have at a relatively high economic benefit, and wherein alkylated reaction is place
Manage an important channel of carbon four.Sulfuric acid alkylation alkylate oil (isooctane) is to mix the iso-butane and butylene in carbon four
It is raw material, as catalyst, liquid phase reactor generates high octane gasoline component-alkylate oil to the sulfuric acid with 89-98% at low temperature
Machining process, sulfuric acid concentration directly affect alkyl oil yield, thus control sulfuric acid concentration it is most important.
The raw material of alkylated reaction is divided into two kinds, a kind of C-4-fraction in catalytic cracked gas, and this kind of raw material can be straight
Connect utilization；Another raw material be MTBE devices after ether after carbon four, for this raw material, due to being reacted in MTBE in need add
Methyl alcohol participates in reaction, so certainly existing excessive methyl alcohol after ether in carbon four, the carbon four containing high concentration methanol can not be direct
Enter alkyl plant as raw material, because methyl alcohol can directly occur esterification instead with the sulfuric acid catalyst in alkyl plant
Should, can cause increasing considerably and producing largely unnecessary spent acid for sulfuric acid catalyst consumption, thus must be to ether after
Carbon four carries out separating methanol treatment, and methanol content is down to below standard value in making carbon four.
The separating methanol of existing carbon four is most to be separated using methanol extraction tower (or being water scrubber) to the methyl alcohol in carbon four,
But most methanol extraction tower treatment effect is all bad, methanol content can still reach in the carbon four after being processed through methanol extraction tower
1000~3000ppm, it is impossible to meet the requirement of alkyl plant, operationally also there is tray brace summer corrosion in methanol extraction tower
And extraction tower such as blocks at the situation, methanol extraction tower now has been poorly suitable for the treatment of the separating methanol of carbon four, and urgent need will be to it
It is improved or a kind of new technology substitution methanol extraction tower.
The U of Chinese patent CN 203108398 disclose a kind of method for reducing desalination water consumption, this method solve reaction
Present in superfluous desalted water, by the adjustment of technological process, reduce the amount of useless desalted water in consersion unit, realize desalted water
Maximization degree is utilized, but this method does not solve the problems, such as that desalted water water consumption is big fundamentally, why methyl alcohol
Water scrubber washing amount is primarily due to be not fully contacted with the methyl alcohol in carbon four in desalted water, it is impossible to reach than larger
Fully the purpose of extraction, causes water scrubber to be necessarily required to excessive desalted water to participate in extraction, could be by the first in carbon four
Alcohol extraction as much as possible.
The method that the B of Chinese patent CN 102093176 disclose methanol extraction in a kind of dimethoxym ethane, the method is using continuous
Adverse current rotating disk is acted on, and will contain methyl alcohol dimethoxym ethane carries out multiple counter-current extraction process with extract so that as much as possible turn of methyl alcohol
In moving on to extract, but this method can be only done extraction of the particle diameter in the methyl alcohol drop of more than 10um, for particle diameter in 10um
Following methyl alcohol drop cannot then accomplish the process of extraction transfer so that still carry substantial amounts of methyl alcohol, this method in stoste secretly
In using the separating methanol of carbon four, can there is cumbersome technique, high energy consumption, extract incomplete shortcoming.
Chinese application number 201410472173.3 is disclosed a kind of realizes four chlorinations using the method for first extracting rectifying again
Carbon is separated with methyl alcohol, because carbon tetrachloride dissolves each other with carbon four, can be applied on the separating methanol of carbon four this method, but this
Kind of method has that an energy consumption is big, extraction is incomplete, so cause to separate incomplete, it is impossible to accomplish to be sufficiently separated.
Come this year more on the research report using methyl alcohol in molecular sieve adsorption carbon four, such as Chinese application number
200810145291.8 disclose a kind of method of utilization molecular sieve adsorption methyl alcohol, using adsorbent by the methanol adsorption in carbon four
In middle molecular sieve, so as to realize that carbon four is separated with methyl alcohol, but this technology needs to consume a large amount of adsorbents, may be only available for one
Under the conditions of some specific, so commercial Application does not have on a large scale.
Chinese application number 201410440054.X discloses a kind of method being improved to methanol extraction tower, from structure
And done beneficial improvement in technological process, but do not solve that methanol extraction column efficiency is low, water consumption is big fundamentally, deposit
The problems such as blocking and corrosion.
In the treatment of the current separating methanol of carbon four, it is badly in need of a kind of efficient, low energy consumption, the dress of the separating methanol of carbon four of easy care
Put.
The content of the invention
In order to overcome the above-mentioned deficiencies of the prior art, the invention provides a kind of method of the depth separating methanol of carbon four；To altogether
The carbon four that boiling distillation tower top is extracted out carries out the treatment of separating methanol, and the process is divided into three steps：Microfacies distribution technique is used first
Pre- distribution extraction is carried out to carbon four, part methyl alcohol contained in carbon four is transferred in extract；Secondly using the extraction of micro- eddy flow
Technology carries out reextraction to methyl alcohol in carbon four, and the carbon four after last fully extraction separates dress with extract into modularization depth
Putting carries out carbon four and is separated with the depth of extract；Carbon four after being processed through separating methanol enters subsequent production device, and extract is returned
Methanol Recovery is carried out in methanol distillation column.
Concrete technical scheme of the invention is as follows：
A kind of method of the depth separating methanol of carbon four, comprises the following steps：
(1) carbon four is tentatively extracted using microfacies portion of techniques, extract particle diameter model after the distribution of microfacies distributor
It is 3~15 μm to enclose, and is uniformly distributed；
Wherein, when the content of methyl alcohol in the carbon four is 0.01~1%, extract is the 0.1~3% of carbon four；Work as institute
When the content for stating methyl alcohol in carbon four is 1~5%, extract is the 1~5% of carbon four, and the percentage is volume ratio；
The process operation temperature is 30~40 DEG C；
(2) secondary deep extraction is carried out using micro- eddy flow extraction-isolation technics, the pressure drop of the process for 0.3~
0.10Mpa, the extraction residence time is 0.01~1s；
(3) carbon four after extracting twice enters back into modularization depth separator and carries out depth point with extraction liquid mixture
From the pressure drop of the process is 0.001~0.01Mpa；Carbon four after being processed through separating methanol enters subsequent production device, and extract enters
Entering methanol distillation column carries out Methanol Recovery.
Preliminary extraction process is carried out in microfacies disperser in step (1), and the average grain diameter of dispersed phase is 7~10 μm,
Two-phase flow velocity is 6~10m/s, and the extraction process time is 0.5~2s.
Extract described in step (1) is the desalted water that pH value is 7.5~8.5.
The inlet velocity of step (2) micro- eddy flow extraction is 4~7m/s.
Step (3) carries out carbon four and extract using the method described in Chinese patent application Publication No. CN103980934A
Depth separate, in the separation process flow velocity be 0.002~0.005m/s, the disengaging time be less than or equal to 60s.
The device of any of the above-described method is realized, described device includes extraction equipment and separator；The extraction equipment by
Microfacies disperser and micro- eddy flow extraction equipment are constituted；The separator includes coarse separation module, Shui Bao, interfacial meter.
Described device includes azeotrope tower 1, tower top delivery outlet and the input port phase of microfacies disperser 2 of azeotrope tower 1
Connection, the delivery outlet of water pot 7 is connected with the input port of microfacies disperser 2, so as to dispersed, dispersed phase of realizing carbon four and desalted water
Particle diameter is connected in below 10um, the delivery outlet of microfacies disperser 2 with micro- input port of eddy flow extractor 3, and carbon four mixes with desalted water
Liquid enters and is fully extracted in eddy flow extractor 3 in a subtle way, the methyl alcohol in carbon four is transferred in desalted water, micro- eddy flow extractor 3
Delivery outlet is connected with the input port of modularization depth separator 4, and carbon four enters with methanol aqueous solution in modularization depth separator 4
Row depth is separated；The delivery outlet of modularization depth separator 4 is connected with the input port of four processing unit (plant) of follow-up carbon 5, separating methanol carbon four
Industrial production, modularization depth separator delivery outlet 4 and the input port phase of methanol distillation column 6 are carried out into the processing unit (plant) of follow-up carbon four
Connection, the methanol aqueous solution after separation carries out methyl alcohol and is separated with desalted water into methanol distillation column, and the methyl alcohol after recovery is returned
MTBE devices are produced, and desalted water returns to water pot and is circulated utilization.
Compared with prior art, the method tool of the separating methanol of carbon provided by the present invention four has the advantage that：
(1) traditional water scrubber washing amount：The volume ratio 1 of carbon four：20, compared with traditional water scrubber, the side that the present invention is provided
Method water consumption is few, and extract (desalted water) loss is greatly lowered, and optimal inflow ratio is 2%；
(2) traditional water scrubber floor space, and technological requirement water scrubber is general higher, and volume exclusion is larger；And it is of the invention
The equipment of offer is small, with certain cost advantage；
(3) process of traditional water scrubber extraction is carbon four and extract counter-current extraction, and not exclusively, the present invention is carried effect of extracting
The method of confession can effectively solve to extract incomplete problem, and the spent acid amount of the residual in equipment is greatly lowered, and mitigation sets
Standby extent of corrosion；
(4) traditional water scrubber operating pressure is larger, and observable index is higher, and compared with traditional water scrubber, it is whole that the present invention is provided
Covering device energy consumption is relatively low, meets the promotion of current energy-conserving and environment-protective；
(5) traditional water scrubber is cumbersome, there is many safety factors in operation, compared with traditional water scrubber, the present invention
The method of offer is simple to operate, equipment safety, it is easier to safeguard；
(6) traditional water scrubber carbon four is separated with methanol aqueous solution and fully relies on Action of Gravity Field sedimentation separation, for particle diameter
Cannot be separated in the methanol aqueous solution drop of 10um or so, a large amount of methyl alcohol can be caused to be entrained disguising into alkyl in value carbon four
Put, compared with traditional water scrubber, the present invention provide method using microfacies distribution technique, micro- eddy flow extraction-isolation technics and
Coalescence-separation Technology, realizes that methyl alcohol fully extracts the process for depth separate；
(7) compared with traditional water scrubber, the method processing speed that the present invention is provided is fast, efficient, first in the carbon four after treatment
Alcohol content is not more than 5ppm, improves the performance of the deep processing device of follow-up carbon four.
Brief description of the drawings
Fig. 1 is to realize device of the invention and schematic flow sheet.
Symbol description
1st, azeotrope tower；2nd, microfacies disperser；3rd, micro- eddy flow extractor；
4th, modularization depth separator；5th, the processing unit (plant) of follow-up carbon four；6 methanol distillation columns；
7th, water pot；F1, carbon four；F2, desalted water；F3, mixing carbon four and desalted water；
Carbon four and methanol aqueous solution after F4, extraction；F5, separating methanol carbon four；F6, methanol aqueous solution.
Fig. 1 is referred to, to realize the device and flow chart of the inventive method.The device includes azeotrope tower 1, and azeotropic steams
The tower top delivery outlet for evaporating tower 1 is connected with the input port of microfacies disperser 2, and the delivery outlet of water pot 7 is connected with the input port of microfacies disperser 2
Connect, dispersed so as to realize carbon four and desalted water, Dispersed Phase Size is in below 10um, the delivery outlet of microfacies disperser 2 and micro- rotation
Stream extractor 3 input port is connected, carbon four and desalination water mixed liquid into fully being extracted in micro- eddy flow extractor 3, by carbon
Methyl alcohol in four is transferred in desalted water, and micro- delivery outlet of eddy flow extractor 3 is connected with the input port of modularization depth separator 4,
Carbon four carries out depth and separates with methanol aqueous solution in modularization depth separator 4；The delivery outlet of modularization depth separator 4 with it is rear
The input port of four processing unit (plant) of continuous carbon 5 is connected, and separating methanol carbon four carries out industrial production, modularization into the processing unit (plant) of follow-up carbon four
Depth separator delivery outlet 4 is connected with the input port of methanol distillation column 6, and the methanol aqueous solution after separation enters into methanol distillation column
Row methyl alcohol is separated with desalted water, and the methyl alcohol after recovery returns to MTBE devices and produced, and desalted water returns to water pot 7 and is circulated profit
With.
In flow charts, microfacies disperser 2 can be used individually with micro- eddy flow extractor 3, and 3 are used in experimentation
Individual combination is tested, and the advantage of microfacies extraction and depth separation coupling technology is further illustrated, according to combination
Form is 1.：The micro- eddy flow extractors 3 of microfacies disperser 2+；②：Microfacies disperser 2；③：Micro- eddy flow extractor 3；It is real to carry out contrast
Test analysis.
It is combined with corrugated plating reinforcing sedimentation techniques using Coalescence-separation Technology in modularization depth separator 4, to carbon
Less than 10 μm of methanol aqueous solution first carries out coalescence and grows up in four, then wakes up with a start gravitational settling point in corrugated plating reinforcing settling section
From to floating, the larger methanol aqueous solution of density is settled down to downwards water bag to the less aqueous solution of carbon four of density, and setting is wrapped in water
One piece of glass plate level gauge, observes the boundary position of carbon four and methanol aqueous solution at any time, and control methanol aqueous solution goes out valve switch degree.
Embodiment 1
Petro-chemical corporation is refined in Shandong somewhere, and methanol content is up to carbon four in carbon four after through the washing extraction of methyl alcohol water scrubber after ether
1000~3000ppm, badly influences the production of alkyl plant.Separating methanol treatment is carried out to the carbon four after methyl alcohol water scrubber,
Combining form is the micro- eddy flow extractors 3 of microfacies disperser 2+, is extracted completely, and it is carried out using one-level coarse separation module
Depth is separated, and experimental program is as shown in table 1 below：
Table 1
Carbon four separating methanol (after Methanol Wash Column) experimental record
Different desalted water inflows are matched according to different methanol contents, to reach optimal effect of extracting and minimum use
Water, mitigates methanol distillation column treating capacity, reducing energy consumption.
Experiment effect is proved, in below 5ppm, met subsequently by the methanol content after device of the invention treatment
The production requirement of the processing unit (plant) of carbon four, substantially reduces the consumption and plant energy consumption of sulfuric acid catalyst in alkyl plant and gives up
Acid amount, improves the performance of the follow-up processing of carbon four.When desalted water proportioning is 2%, separating effect is optimal, compared to traditional water scrubber
The water consumption of desalted water is greatlyd save, follow-up methanol distillation column operational load is reduced, the energy of whole technological process is reduced
Consumption.
Further to reduce energy consumption, efficiency is improved, carbon four is drawn before water scrubber, separating methanol treatment is carried out to carbon four, because
For the methanol content of carbon four is between 2~4% before water scrubber, content is higher, and one-level separator possibly cannot meet depth separation
Required precision, depth separation is carried out using two-stage tandem mode；Extraction combination is the micro- eddy flow extractions of microfacies disperser 2+
Device 3；Experimental program is as shown in table 2 below：
Table 2
Carbon four separating methanol (before Methanol Wash Column) experimental record
Experiment effect proves that the methanol content of carbon four after being processed through secondary separation device is in below 5ppm, primary outlet
Methanol content is higher may be too high due to material inlet methyl alcohol, may be entrained with by carbon four through coalescing rear portion methyl alcohol drop
Go, cause to separate not exclusively, separation accuracy requirement can be reached using the second-order separation.
Embodiment 2
For contrast whether there is the difference for extracting completely, this experiment extraction part individually uses microfacies disperser 2, by micro- cyclone
3 short circuits, separating methanol treatment is carried out to carbon after water scrubber four, and experimental program is as shown in table 3 below：
Table 3
Carbon four separating methanol (after Methanol Wash Column) experimental record table
The results show, is individually being extracted using microfacies disperser 2, is finally recovered effect and is unable to reach separation essence
Degree is required.
Embodiment 3
For contrast whether there is the difference for extracting completely, this experiment extraction part individually uses micro- eddy flow extractor 3, by microfacies point
The short circuit of device 2 is dissipated, separating methanol treatment is carried out to carbon after water scrubber four, experimental program is as shown in table 4 below：
Table 4
Carbon four separating methanol (after Methanol Wash Column) experimental record
The results show, is individually being extracted using microfacies disperser 3, is finally recovered effect and is unable to reach separation essence
Degree is required.
Three groups of Experimental comparisons explanation, in the processing procedure of the separating methanol of carbon four, extract with separating has together to treatment effect
The effect of sample, optimal experiment effect is the mode of extraction completely using the micro- eddy flow extractors 3 of microfacies disperser 2+, using modularization
Depth separator, extraction completely is carried out to it and depth is separated.
It is only in sum the preferred embodiment of invention, not for limiting practical range of the invention.It is i.e. all according to
The equivalence changes that the content of scope of the present invention patent is made and modification, all should be technology category of the invention.
Claims (5)
1. the method for the depth separating methanol of a kind of carbon four, it is characterised in that comprise the following steps：
（1）Carbon four is tentatively extracted using microfacies dispersion technology, particle size range is 3 after extract is distributed through microfacies distributor
~15 μm, it is uniformly distributed；
Wherein, when the content of methyl alcohol in the carbon four is 0.01~1%, extract is the 0.1~3% of carbon four；When the carbon
When the content of methyl alcohol is 1~5% in four, extract is the 1~5% of carbon four, and the percentage is volume ratio；
The process operation temperature is 30~40 DEG C；
（2）Secondary deep extraction is carried out using micro- eddy flow extraction-isolation technics, the pressure drop of the process is 0.3~0.10Mpa, extraction
The residence time is taken for 0.01~1s；
（3）Carbon four after extracting twice enters back into modularization depth separator with extraction liquid mixture to carry out depth and separates,
The pressure drop of the process is 0.001~0.01Mpa；Carbon four after being processed through separating methanol enters subsequent production device, and extract enters
Methanol distillation column carries out Methanol Recovery；
The device of use includes extraction equipment and separator；The extraction equipment is by microfacies disperser and micro- eddy flow extraction dress
Put composition；The separator includes coarse separation module, Shui Bao, interfacial meter；
The tower top delivery outlet that described device has azeotrope tower, azeotrope tower is connected with the input port of microfacies disperser,
The delivery outlet of water pot is connected with the input port of microfacies disperser；The delivery outlet of microfacies disperser is defeated with micro- eddy flow extractor
Entrance is connected；The delivery outlet of micro- eddy flow extractor is connected with the input port of modularization depth separator；Modularization depth
The delivery outlet of separator is connected with the input port of the processing unit (plant) of follow-up carbon four；The delivery outlet and first of modularization depth separator
The input port of alcohol recovery tower is connected.
2. method according to claim 1, it is characterised in that step（1）In preliminary extraction process be in microfacies disperser
In carry out, the average grain diameter of dispersed phase is 7~10 μm, and two-phase flow velocity is 6~10m/s, and the extraction process time is 0.5~2s.
3. method according to claim 1, it is characterised in that step（1）Described in extract be pH value be 7.5-8.5
Desalted water.
4. method according to claim 1, it is characterised in that step（2）The inlet velocity of the micro- eddy flow extraction for 4~
7m/s。
5. method according to claim 1, it is characterised in that step（3）The modularization depth separator is to use
Coalescence-separation Technology is combined with corrugated plating reinforcing sedimentation techniques, and the methanol aqueous solution to less than 10 μm in carbon four first gathers
Knot is grown up, and then carries out gravity settling separation in corrugated plating reinforcing settling section, and the less aqueous solution of carbon four of density is to floating, density
Larger methanol aqueous solution is settled down to downwards water bag, and one piece of glass plate level gauge of setting is wrapped in water, and carbon four and first are observed at any time
The boundary position of alcohol solution, control methanol aqueous solution goes out valve switch degree, and flow velocity is 0.002~0.005m/ in the separation process
S, the disengaging time is less than or equal to 60s.
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| CN108017516A (en) * | 2017-12-01 | 2018-05-11 | 宁夏宝塔化工中心实验室(有限公司) | A kind of method of etherification of olefine technique recycling methanol |
| CN108704672A (en) * | 2018-05-31 | 2018-10-26 | 上海华畅环保设备发展有限公司 | Ebullated bed wood tar adds the on-line regeneration method and apparatus of hydrogen decaying catalyst |
| CN108704673A (en) * | 2018-05-31 | 2018-10-26 | 上海华畅环保设备发展有限公司 | Ebullated bed wood tar adds the de-oiling method and device of the outer waste discharge catalyst of hydrogen |
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| CN104225955B (en) * | 2014-09-01 | 2016-06-22 | 宁波海越新材料有限公司 | Carbon four separating methanol technique after ether |
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