CN104725201B - A kind of polymethoxy dimethyl ether absorption, membrance separation combine dewatering - Google Patents
A kind of polymethoxy dimethyl ether absorption, membrance separation combine dewatering Download PDFInfo
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Abstract
The invention discloses a kind of polymethoxy dimethyl ether absorption, membrance separation combines dewatering, comprises the following steps: sent into from the top of adsorption tower one by gas gas-phase objects stream unstripped gas, and carry out adsorption reaction in adsorption tower one；After molecular sieve in adsorption tower one completes absorption, entering regeneration stage, gas gas-phase objects stream unstripped gas carries out adsorption reaction in sending into adsorption tower two；During regeneration stage, under the effect of vacuum pump, stripping gas is discharged from the top of adsorption tower one, and after membrane separation, is incorporated into unstripped gas pipeline and enters the dehydration of next step adsorption deeply；After adsorption tower one completes regeneration, it is re-introduced into adsorbed state；After adsorption tower two completes absorption, enter regeneration stage.The present invention uses above-mentioned technique, on the basis of guaranteeing high product purity, more obtain high yield, make stripping gas again process without returning to leading portion rectification working process simultaneously, achieve the complete independent operating of dehydration workshop section, there is obvious technology and advantage economically.
Description
Technical field
The present invention relates to polymethoxy dimethyl ether production field, be specifically related to the absorption of a kind of polymethoxy dimethyl ether, film divides
From combining dewatering.
Background technology
Polymethoxy dimethyl ether (being called for short PODE or DMMn) has another name called polyoxymethylene dimethyl ether, polyoxymethylene dimethyl ethers, poly-first
Epoxide dimethoxym ethane, is the low-molecular-weight acetals polymer that a class is with dimethoxymethane as parent, methylene epoxide is as main chain, its
Formula is expressed as CH3(CH2O) nCH3, wherein n is the integer equal to or more than 1, and general value is less than or equal to 8.Polymethoxy two
Methyl ether is a kind of colourless or faint yellow volatile flammable liquid, has slight ethers abnormal smells from the patient.It is the downstream product of methanol, mainly gives birth to
Product method is by providing the compound (formaldehyde, metaformaldehyde and paraformaldehyde etc.) of paraformaldehyde and providing the chemical combination of end-blocking methyl
Thing (methanol, dimethyl ether and dimethoxym ethane etc.) synthesizes, and is dimethoxym ethane as n=1.Reaction equation is listed below:
2CH3OH + nHCHO == CH3O(CH2O)nCH3 + H2O
2CH3OH +—(CH2O)3 == CH3O(CH2O)nCH3 +H2O
2CH3OH +HO(CH2O)nH == CH3O(CH2O)nCH3 +H2O
CH3OCH3 + HO(CH2O)nH == CH3O(CH2O)nCH3 +H2O
CH3OCH2OCH3 + HO(CH2O)nH == CH3O(CH2O)n+1CH3 +H2O
With the development of Coal Chemical Industry, coal synthesizing methanol technology maturation, its yield is well beyond demand, it is necessary under exploitation methanol
Trip product is to ensure the sound development of Coal Chemical Industry.On the other hand, with the development of auto industry, energy resource consumption increases, diesel oil simultaneously
Burning produces huge environmental issue, and petroleum industry starts to be devoted to find additive to improve oil quality, improves aviation fuel
Can, reduce pollutant emission.
Polymethoxy dimethyl ether is the general designation of the linear many ether materials of class, is the acetal similar with dimethoxym ethane.Due to it
There are the highest 16 octane numbers (>=30) and oxygen content (>=42.1%), and without sulfur without aromatic hydrocarbons, being added in diesel oil can be notable
Improve diesel combustion characteristic, be effectively improved the thermal efficiency, NO is greatly reducedxWith the discharge of particulate matter, thus it is considered as great
The environmental protection type additive for diesel oil of application prospect.According to data, its addition in diesel oil is up to 15%, and annual requirement is more than 2300
Ten thousand tons, year consumes methanol 2600 ~ 27,000,000 tons, can effectively extend methanol industry chain and bring great economic benefit and environmental protection effect
Benefit, has great strategic significance and good economic worth.Ton methanol PODE3-8 device is overlapped from August, 2013 China head
Since Heze City, Shandong Province is gone into operation, all parts of the country fall over each other to start to develop PODE3-8 project.It addition, this product also acts as phenolic aldehyde tree
The modifying agent of fat, solvent, plasticizer and releasing agent etc., be widely used.
It was found that the application that polymethoxy dimethyl ether is on diesel fuel additives is based on n=3-8.Commercial production uses instead
The mode of rectification should be carried out obtain PODE3-8 product by mixture afterwards, its gas gas-phase objects stream based on PODE2, containing a small amount of dimethoxym ethane,
The PODE3-8 of unreacted material, water and trace.Gas gas-phase objects stream can return to front operation and continues to produce, but the water electrode Yishui River therein
Solve target product acetal, form hemiacetal, and acetal is close with hemiacetal boiling point, it is difficult to efficiently separate and affect product quality.
It addition, the boiling point of PODE2 is 105 degrees Celsius, with the boiling point of water closely, therefore, general azeotropic distillation mode is difficult to relatively
For removing the moisture in polymethoxy dimethyl ether up hill and dale.
The utility model patent of Patent No. ZL201320077712.4 discloses a kind of dimethoxym ethane deep dehydration and purifies dress
Putting, this device mainly uses absorption/regenerator, and binding molecule sieve, by the moisture removal in dimethoxym ethane.This patent is only given
One apparatus structure, does not provide concrete process conditions, and those skilled in the art, according to this apparatus structure, is in fact
Cannot realize the effect that this apparatus structure wants to reach, such dehydration device is relatively common in this area in fact, and
Those skilled in the art both knows about, and process conditions are very important design links, for different dehydration objects, needs not
Same technological process and process conditions, these are not that rule of thumb or limited number of time test is obtained in that those skilled in the art
's.It addition, disclosed dimethoxym ethane deep dehydration purifier is for the mainly dimethoxym ethane processed, and the water content of dimethoxym ethane
The lowest, probably about 0.5%, this is easy to for molecular sieve itself by its water content control below 0.05%,
Such dewatering purifying equipment, for the gas gas-phase objects stream that water content is bigger, does not possess any reference value.
Summary of the invention
It is an object of the invention to provide a kind of polymethoxy dimethyl ether absorption, membrance separation combines dewatering, the method
Can be by the water content control of polymethoxy dimethyl ether below 0.05%, meanwhile, on the basis of guaranteeing quality of adsorption, moreover it is possible to
Effectively reduce energy consumption, improve the utilization rate of adsorbent, yield can also be improved simultaneously, it is ensured that dehydration workshop section completely operates independently from,
Prevent from occurring between operation cross influence.
The present invention for achieving the above object, realizes by the following technical solutions:
A kind of polymethoxy dimethyl ether absorption, membrance separation combine dewatering, comprise the following steps:
A gas gas-phase objects stream unstripped gas is sent into by () from the top of adsorption tower one, and carry out adsorption reaction in adsorption tower one,
Water adsorption in unstripped gas, gas not to be adsorbed are discharged from the bottom of adsorption tower one, are entered by the adsorbent in adsorption tower one
Enter in product gas storage tank, in unstripped gas the volume percent content of each constituent be respectively as follows: water be 2% ~ 10%, methanol be 3% ~
5%, formaldehyde be 3% ~ 5%, PODE2 be 60% ~ 80%, remaining as PODE3 ~ 8, in the product gas obtained, the content of PODE2 ~ 8 is
99.95~99.99%；
B the adsorbent in () adsorption tower one completes absorption after, enter regeneration stage, meanwhile, gas gas-phase objects stream raw material
Gas is sent into from the top of adsorption tower two, and carries out adsorption reaction in adsorption tower two, and gas not to be adsorbed is from adsorption tower two
Bottom is discharged, and enters in product gas storage tank, and in the product gas obtained, the content of PODE2 ~ 8 is 99.95 ~ 99.99%；
C, during () regeneration stage, under the effect of vacuum pump, stripping gas is discharged from the top of adsorption tower one, and divides through film
Material after preliminary hydro-extraction processes is incorporated to unstripped gas pipeline and enters the dehydration of next step adsorption deeply；
D () adsorption tower one completes regeneration after, wait and enter into adsorbed state；After adsorption tower two completes absorption, enter regeneration
In the stage, meanwhile, adsorption tower one is again introduced into adsorbed state；
E () circulation above step, until the moisture in gas gas-phase objects stream unstripped gas reaches requirement.
Further, preferably, the adsorbent in described step (a) be molecular sieve, silica gel, activated alumina,
At least one in resin.
Further, preferably, the temperature in described adsorption tower one and adsorption tower two is 120 ~ 180 degrees Celsius,
And keep invariable in absorption phase and regeneration stage.
Further, preferably, in described step (b), the detailed process of regeneration stage is:
(b1) top air inlet and the base bleed mouth of adsorption tower one are closed；
(b2) by vacuum pump, adsorption tower one being carried out evacuation process, the adsorbent in adsorption tower one realizes desorbing, and
Obtain stripping gas；
(b3) stripping gas is extracted out from the top of adsorption tower one, and the material after membrance separation preliminary hydro-extraction processes returns to raw material
Gas pipeline enters the dehydration of next step adsorption deeply, and the constituent of stripping gas is: methanol and formaldehyde are 20% ~ 30%, PODE2 ~ 8 are
5% ~ 10%, remaining is water.
Further, preferably, the time of described primary sorption and regeneration is 6 ~ 12 minutes.
Further, preferably, during regeneration stage, the vacuum in adsorption tower one and adsorption tower two is-0.08
~-0.06MPa。
Further, preferably, during regeneration stage, every 1 minute evacuation 0.5 minute.
Further, preferably, the time of described primary sorption is 2 times of time of primary recycling.
The present invention compared with prior art, has the following advantages and beneficial effect:
(1) present invention carries out circulation absorption, again by the method for adsorbing separation to polymethoxy dimethyl ether gaseous phase materials stream
Raw, on the basis of realizing absorption continuously, by the moisture Control in gas gas-phase objects stream in the range of meeting the requirements；It addition, it is front
Look unfamiliar produce workshop section gaseous products need not move through condensing heat-exchange enter pressure swing adsorption system carry out product depth dehydration, absorption and
During regeneration, do not change the temperature of adsorption tower so that it is be maintained at an invariable state, greatly reduce routine side
The energy consumption that formula is brought because desorbing heats up, and also make the whole process time be reduced without thermoregulator link, it is ensured that
The seriality of technique.
(2) present invention is when absorption phase, selects to give vent to anger from top air inlet, the bottom of adsorption tower, selects from absorption simultaneously
Tower bottom carries out evacuation process, so not only contributes to the absorption of unstripped gas, the most also provides conveniently for desorbing below,
Make the moisture in adsorbent etc. can by fast desorption out.
(3) present invention divides accomplishing effectively to reduce in polymethoxy dimethyl ether production process the gaseous phase materials flowing water after rectification
While content, being processed stripping gas by membrance separation, the stripping gas after process is directly incorporated into absorption unstripped gas and inhales
Attached deep dehydration, and without being re-fed into leading portion rectification working process, ensure that the complete independent operating of dehydration workshop section, prevent operation
Between cross influence occurs, meanwhile, under the effect of membrance separation, be effectively increased the yield of unstripped gas.
Accompanying drawing explanation
Fig. 1 is the process chart of the present invention；
Fig. 2 is the graph of a relation of desorption temperature and energy consumption；
Fig. 3 is the graph of a relation of desorbing vacuum and energy consumption；
Fig. 4 is the graph of a relation of adsorption time and adsorbent utilization rate.
Detailed description of the invention
Below in conjunction with embodiment, the present invention is described in further detail, but embodiments of the present invention are not limited to this.
As it is shown in figure 1, a kind of polymethoxy dimethyl ether adsorbs, membrance separation combines dewatering, comprise the following steps:
(a) volume percent content is respectively as follows: water be 2% ~ 10%, methanol be 3% ~ 5%, formaldehyde be 3% ~ 5%, PODE2 be
60% ~ 80%, the gas gas-phase objects stream unstripped gas remaining as PODE3 ~ 8 is sent into from the top of adsorption tower one, and enters in adsorption tower one
Row adsorption reaction, the temperature in tower is 120 ~ 180 degrees Celsius, and keeps invariable, and the adsorbent in adsorption tower one is by raw material
Water adsorption in gas, adsorbent can be one or both or two kinds in molecular sieve, silica gel, activated alumina, resin with
On, preferred molecular sieve, gas not to be adsorbed is discharged from the bottom of adsorption tower one, enters in product gas storage tank, in product gas
The content of PODE2 ~ 8 is 99.95 ~ 99.99%, and remaining is the monomer such as methanol, formaldehyde；
B the adsorbent in () adsorption tower one completes absorption after, enter regeneration stage, meanwhile, gas gas-phase objects stream raw material
Gas is sent into from the top of adsorption tower two, and carries out adsorption reaction in adsorption tower two, and gas not to be adsorbed is from adsorption tower two
Bottom is discharged, and enters in product gas storage tank, and in product gas, the content of PODE2 ~ 8 is 99.95 ~ 99.99%；
C, during () regeneration stage, under the effect of vacuum pump, stripping gas is discharged from the top of adsorption tower one, and divides through film
After processing, being incorporated into unstripped gas pipeline and enter the dehydration of next step adsorption deeply, in like manner, adsorption tower two is carrying out adsorbent reactivation
Time, identical with adsorption tower one principle；
D () adsorption tower one completes regeneration after, wait and enter into adsorbed state；After adsorption tower two completes absorption, enter regeneration
In the stage, meanwhile, adsorption tower one is again introduced into adsorbed state；Any adsorption tower completes primary sorption and starts the time to regeneration ending
It it is 6 ~ 12 minutes；
E () circulation above step, until the moisture in gas gas-phase objects stream unstripped gas reaches requirement.
At present, in polymethoxy dimethyl ether dewatering process, the most not mentioned method relevant to membrance separation, the present invention passes through
Innovation, is incorporated into membrance separation the dehydration of polymethoxy dimethyl ether pioneeringly, and combines with adsorption dewatering, guaranteeing
On the basis of high product purity, more obtain high yield, make stripping gas carry out again without returning to leading portion rectification working process simultaneously
Process, it is achieved that the complete independent operating of dehydration workshop section, there is obvious technology and advantage economically.
In the present embodiment, in step (b), the detailed process of regeneration stage is:
(b1) close top air inlet and the base bleed mouth of adsorption tower one, make adsorption tower one in air-tight state；
(b2) every 1 minute, by vacuum pump to adsorption tower one evacuation 0.5 minute, the vacuum in adsorption tower one is made
For-0.08 ~-0.06MPa, temperature is maintained at 120 ~ 180 degrees Celsius simultaneously, and the adsorbent in adsorption tower one realizes with this understanding
Desorbing；
(b3) stripping gas is extracted out from the top of adsorption tower one, after membrane separation, is incorporated into unstripped gas pipeline and enters
Next step adsorption deeply is dehydrated, and improves utilization rate and the yield of product of unstripped gas；In stripping gas methanol and formaldehyde be 20% ~
30%, PODE2 ~ 8 are 5% ~ 10%, and remaining is water.
In above-mentioned processing step, the main technological parameter optimized has: the temperature in desorption process, the vacuum in desorption process
Degree, adsorption time.
One inventive point of the present invention is adsorption tower temperature in desorption process in optimization step (b2), and temperature is more
Height, desorption effect is the best, and desorbing is the most thorough, and beneficially adsorbent keeps higher adsorption effect, i.e. next time when next time adsorbs
The water content of the product that absorption obtains is the lowest, but, temperature is the highest, and energy consumption is the biggest, and whole processing cost is the highest；And temperature
The lowest, although energy consumption is the least, but desorption effect is the poorest, and pole affects the absorption again of adsorbent；Therefore, consider, choosing
Selecting a suitable desorption temperature, to obtain preferable desorption effect and relatively low energy consumption, desorption effect is with after adsorbent desorbing
The water content again adsorbing the product obtained is weighed, and water content is the lowest, and desorption effect is the best.
For obtaining an optimal desorption temperature, the present invention has done desorption temperature and (after desorbing has again inhaled product water content
The water content of the attached product obtained) and the impact experiment of energy consumption, in experimentation, only changing desorption temperature, other technique is joined
Number keep constant, and desorption temperature be chosen for respectively 120 DEG C, 125 DEG C, 130 DEG C, 135 DEG C, 140 DEG C, 145 DEG C, 150 DEG C, 155
DEG C, 160 DEG C, 165 DEG C, 170 DEG C, 175 DEG C, 180 DEG C, experimental result is as shown in Fig. 2 and Biao mono-.
Product water content under the different desorption temperature of table one
| Desorption temperature (DEG C) | 120 | 125 | 130 | 135 | 140 | 145 | 150 | 155 | 160 | 165 | 170 | 175 | 180 |
| Product water content (%) | 0.050 | 0.047 | 0.044 | 0.041 | 0.035 | 0.031 | 0.025 | 0.022 | 0.019 | 0.017 | 0.015 | 0.012 | 0.010 |
As seen from Figure 2, along with the continuous rising of desorption temperature, energy consumption is gradually increased, when desorption temperature 120 DEG C ~
Between 150 DEG C during change, the increase tendency of energy consumption is relatively mild, and when desorption temperature is more than 150 DEG C, energy consumption increases suddenly；By
Table one is it can be seen that along with the rising of desorption temperature, product water content (adsorbs the water content of the product obtained) again after desorbing
Being gradually lowered, when desorption temperature changes between 120 DEG C ~ 150 DEG C, product water content (adsorbs the product obtained again after desorbing
The water content of product) reduction trend it is obvious that when desorption temperature changes between 150 DEG C ~ 180 DEG C, product water content (desorbing
After again adsorb the water content of the product obtained) reduction trend the mildest.Therefore, from the point of view of comprehensive energy consumption and product water content,
The optimal desorption temperature of the present invention is 150 DEG C, under this desorption temperature, it is possible to make energy consumption relatively low, makes product water content relatively low simultaneously.
Another inventive point of the present invention is adsorption tower vacuum in desorption process, vacuum in optimization step (b2)
Spending the highest (i.e. pressure is the least), desorption effect is the best, and desorbing is the most thorough, and beneficially adsorbent keeps higher when next time adsorbs
The water content of adsorption effect, the i.e. next time product that absorption obtains is the lowest, but, vacuum is the highest, and energy consumption is the biggest, whole process
Cost is the highest；And vacuum is the lowest, although energy consumption is the least, but desorption effect is the poorest, and pole affects the absorption again of adsorbent；
Therefore, to consider, select a suitable desorbing vacuum, to obtain preferable desorption effect and relatively low energy consumption, solve
The water content again adsorbing the product obtained after inhaling effect adsorbent desorbing is weighed, and water content is the lowest, and desorption effect is the best.
For obtaining an optimal desorbing vacuum, the present invention has done desorbing vacuum to product water content (after desorbing again
The water content of the product that secondary absorption obtains) and the impact experiment of energy consumption, in experimentation, only change desorbing vacuum, other
Technological parameter keep constant, and desorbing vacuum be chosen for respectively-0.060MPa ,-0.062 MPa ,-0.064 MPa ,-0.066
MPa ,-0.070 MPa ,-0.072 MPa ,-0.074 MPa ,-0.076 MPa ,-0.078 MPa ,-0.080 MPa, experiment knot
Fruit is as shown in Fig. 3 and Biao bis-.
Product water content under the different desorbing vacuum of table two
| Vacuum (MPa) | -0.060 | -0.062 | -0.064 | -0.066 | -0.068 | -0.070 | -0.072 | -0.074 | -0.076 | -0.078 | -0.080 |
| Product water content (%) | 0.05 | 0.048 | 0.045 | 0.042 | 0.037 | 0.028 | 0.024 | 0.020 | 0.016 | 0.013 | 0.010 |
As seen from Figure 3, along with the continuous rising of vacuum, energy consumption is gradually increased, when vacuum-0.070 ~-
Between 0.060MPa during change, the increase tendency of energy consumption is relatively mild, when desorbing vacuum exceedes-0.070MPa, and energy
Consumption is steep to be increased；By table two it can be seen that along with the rising of desorbing vacuum, product water content (adsorbs the product obtained again after desorbing
The water content of product) it is gradually lowered, when desorbing vacuum changes between-0.070 ~-0.060MPa, product water content (desorbing
After again adsorb the water content of the product obtained) reduction trend it is obvious that when desorbing vacuum is at-0.080 ~-0.070MPa
Between change time, the reduction trend of product water content (again adsorbing the water content of the product obtained after desorbing) is the mildest.Therefore,
From the point of view of comprehensive energy consumption and product water content, the present invention optimal desorbing vacuum is-0.070MPa, under this desorbing vacuum, and energy
Enough make energy consumption relatively low, make product water content relatively low simultaneously.
Another inventive point of the present invention is absorption and the recovery time optimizing in step (c), will complete once to inhale
The time sum echoing primary recycling is limited to 6 ~ 12 minutes, is allocated the respective time, it is preferred that when will adsorb simultaneously
Between be arranged to the twice of recovery time, such as, if absorption 4 minutes, then regeneration 2 minutes；If adsorbing 8 minutes, then regeneration 4 minutes.
Adsorption time is the longest, and the utilization rate of adsorbent is the highest, but the water content of product is the highest simultaneously；Otherwise, adsorption time is the shortest,
The water content of product is the lowest, but the utilization rate of adsorbent is the lowest, therefore, consider, and selects a suitable suction
The attached time, so that the water content of product is relatively low, the utilization rate simultaneously making adsorbent is higher.
For obtaining an optimal adsorption time, the present invention has done adsorption time to product water content and adsorbent utilization rate
Impact experiment, in experimentation, only change adsorption time, other technological parameter keeps constant, and desorbing vacuum is respectively
It is chosen for 4 minutes, 4.5 minutes, 5 minutes, 5.5 minutes, 6 minutes, 6.5 minutes, 7 minutes, 7.5 minutes, 8 minutes, experimental result
As shown in Fig. 4 and Biao tri-.
Product water content under the different adsorption time of table three
| Adsorption time (minute) | 4 | 4.5 | 5 | 5.5 | 6 | 6.5 | 7 | 7.5 | 8 |
| Product water content (%) | 0.01 | 0.012 | 0.015 | 0.018 | 0.022 | 0.030 | 0.036 | 0.044 | 0.05 |
As seen from Figure 4, along with the continuous growth of adsorption time, the utilization rate of adsorbent gradually steps up, when absorption
Between between 4 ~ 6 minutes during change, the utilization rate growth trend of adsorbent is obvious, and when adsorption time became between 6 ~ 8 minutes
During change, the utilization rate of adsorbent increases the mildest；By table three it can be seen that along with the growth of adsorption time, product water content
Constantly raising, when adsorption time changed between 4 ~ 6 minutes, it is more mild that product water content raises trend, and when absorption
Between between 6 ~ 8 minutes change time, product water content raise trend fairly obvious；Therefore, the utilization rate of comprehensive adsorbent and product
From the point of view of product water content, when adsorption time is 6 minutes, when now the recovery time is 3 minutes, it is possible to obtain higher adsorbent and utilize
Rate, makes product water content relatively low simultaneously, within 6 minutes, is optimal adsorption time.
In addition, it is necessary to special instruction, the present invention simply illustrates as a example by double tower, and double tower is to ensure that absorption continuously
Condition at least, when gas gas-phase objects stream treating capacity is bigger, can have multiple adsorption tower.
The above, be only presently preferred embodiments of the present invention, and the present invention not does any pro forma restriction, every depends on
Any simple modification of being made above example according to the technical spirit of the present invention, equivalent variations, each fall within the protection of the present invention
Within the scope of.
Claims (8)
1. a polymethoxy dimethyl ether absorption, membrance separation combine dewatering, it is characterised in that comprise the following steps:
A gas gas-phase objects stream unstripped gas is sent into by () from the top of adsorption tower one, and carry out adsorption reaction in adsorption tower one, absorption
Water adsorption in unstripped gas, gas not to be adsorbed are discharged by the adsorbent in tower one from the bottom of adsorption tower one, enter and produce
In product gas storage tank, in unstripped gas the volume percent content of each constituent be respectively as follows: water be 2% ~ 10%, methanol be 3% ~ 5%, first
Aldehyde is 3% ~ 5%, PODE2 is 60% ~ 80%, remaining as PODE3 ~ 8, in the product gas obtained, the content of PODE2 ~ 8 is 99.95 ~
99.99%；
Adsorbent in (b) adsorption tower one complete absorption after, enter regeneration stage, meanwhile, gas gas-phase objects stream unstripped gas from
The top of adsorption tower two is sent into, and carries out adsorption reaction in adsorption tower two, and gas not to be adsorbed is from the bottom of adsorption tower two
Discharging, enter in product gas storage tank, in the product gas obtained, the content of PODE2 ~ 8 is 99.95 ~ 99.99%；
C, during () regeneration stage, under the effect of vacuum pump, stripping gas is discharged from the top of adsorption tower one, and through at the beginning of membrance separation
The material obtained after step processed is incorporated to unstripped gas pipeline and enters adsorption tower deep dehydration；
D () adsorption tower one completes regeneration after, wait and enter into adsorbed state；After adsorption tower two completes absorption, enter regeneration stage,
Meanwhile, adsorption tower one is again introduced into adsorbed state；
E () circulation above step, until the moisture in gas gas-phase objects stream unstripped gas reaches requirement.
A kind of polymethoxy dimethyl ether absorption the most according to claim 1, membrance separation combine dewatering, and its feature exists
In: the adsorbent in described step (a) is at least one in molecular sieve, silica gel, activated alumina, resin.
A kind of polymethoxy dimethyl ether absorption the most according to claim 1, membrance separation combine dewatering, and its feature exists
In: the temperature in described adsorption tower one and adsorption tower two is 120 ~ 180 degrees Celsius, and keeps perseverance in absorption phase and regeneration stage
Fixed constant.
A kind of polymethoxy dimethyl ether absorption the most according to claim 1, membrance separation combine dewatering, and its feature exists
In: in described step (b), the detailed process of regeneration stage is:
(b1) top air inlet and the base bleed mouth of adsorption tower one are closed；
(b2) by vacuum pump, adsorption tower one being carried out evacuation process, the adsorbent in adsorption tower one realizes desorbing, and obtains
Stripping gas；
(b3) stripping gas is extracted out from the top of adsorption tower one, and the material after membrance separation preliminary hydro-extraction processes is incorporated to raw material trachea
Line enters the dehydration of next step adsorption deeply, and the constituent of stripping gas is: methanol and formaldehyde are 20% ~ 30%, PODE2 ~ 8 be 5% ~
10%, remaining is water.
A kind of polymethoxy dimethyl ether absorption the most according to claim 4, membrance separation combine dewatering, and its feature exists
In: during regeneration stage, the vacuum in adsorption tower one and adsorption tower two is-0.08 ~-0.06MPa.
A kind of polymethoxy dimethyl ether absorption the most according to claim 4, membrance separation combine dewatering, and its feature exists
In: during regeneration stage, every 1 minute evacuation 0.5 minute.
A kind of polymethoxy dimethyl ether absorption the most according to claim 4, membrance separation combine dewatering, and its feature exists
In: the time of described primary sorption and regeneration is 6 ~ 12 minutes.
A kind of polymethoxy dimethyl ether absorption the most according to claim 7, membrance separation combine dewatering, and its feature exists
In: the time of described primary sorption is 2 times of the time of primary recycling.
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| CN107163005B (en) * | 2017-06-21 | 2023-09-12 | 武汉智宏思博化工科技有限公司 | Industrial equipment for producing anhydrous THF by coupling membrane dehydration and molecular sieve adsorption |
| CN111087288B (en) * | 2018-10-23 | 2023-05-02 | 中国石油化工股份有限公司 | Purification method of dimeric methoxy dimethyl ether |
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| CN102976893B (en) * | 2013-01-05 | 2015-11-25 | 四川亚连科技有限责任公司 | A kind of flushing-free circulation manufactures the method for dehydrated alcohol |
| CN102992954B (en) * | 2013-01-05 | 2015-09-09 | 四川亚连科技有限责任公司 | A kind of high yield prepares the technique of dehydrated alcohol |
| CN203060888U (en) * | 2013-02-19 | 2013-07-17 | 西安超滤化工有限责任公司 | Methylal deep dehydration purifying device |
| CN103360224A (en) * | 2013-07-31 | 2013-10-23 | 东营市润成碳材料科技有限公司 | Combined process for preparing poly methoxy-dimethyl ether |
| CN103848730B (en) * | 2014-01-09 | 2015-06-17 | 东营市润成碳材料科技有限公司 | Production device system and production process for polymethoxy dimethyl ether (PODE) |
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