CN104725201A - Method for adsorption, membrane separation and dehydration of polyoxymethylene dimethyl ether - Google Patents
Method for adsorption, membrane separation and dehydration of polyoxymethylene dimethyl ether Download PDFInfo
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- CN104725201A CN104725201A CN201510066015.2A CN201510066015A CN104725201A CN 104725201 A CN104725201 A CN 104725201A CN 201510066015 A CN201510066015 A CN 201510066015A CN 104725201 A CN104725201 A CN 104725201A
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Abstract
The invention discloses a method for adsorption, membrane separation and dehydration of polyoxymethylene dimethyl ether. The method comprises the following steps: introducing a gas phase material flow raw gas from the top of an adsorption tower I, and performing adsorption reaction in the adsorption tower I; putting a molecular sieve in the adsorption tower I into a regeneration stage after adsorption, and introducing the gas phase material flow raw gas into an adsorption tower II to perform adsorption reaction; at the regeneration stage, under the action of a vacuum pump, discharging a desorption gas from the top of the adsorption tower I, performing membrane separation treatment on the desorption gas, introducing the desorption gas into a raw gas pipeline, and performing adsorption deep dehydration in the next step; after the regeneration in the adsorption tower I, entering an adsorption state again; and after the adsorption in the adsorption tower II, entering the regeneration stage. By adopting the process, on the basis of ensuring the high purity of a product, a high yield is obtained, the desorption gas does not need to be returned to the previous stage distillation process for retreatment at the same time, and the complete independent running of a dehydration working section is realized, so that the method has obvious technical and economic advantages.
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, membrane sepn in conjunction with dewatering.
Background technology
Polymethoxy dimethyl ether (being called for short PODE or DMMn) has another name called polyoxymethylene dimethyl ether, polyoxymethylene dimethyl ethers, polymethoxy methylal, be a class take Methylal(dimethoxymethane) as parent, the sub-methoxyl group lower molecular weight acetals polymkeric substance that is main chain, its general formula is expressed as CH
3(CH
2o) nCH
3, wherein n be equal to or greater than 1 integer, general value is less than or equal to 8.Polymethoxy dimethyl ether is a kind of colourless or faint yellow volatile flammable liquid, has slight ethers smell.Be the derived product of methyl alcohol, main production process is by the compound providing paraformaldehyde (formaldehyde, trioxymethylene and paraformaldehyde etc.) and provides the compound of end-blocking methyl (methyl alcohol, dme and methylal etc.) to synthesize, and is methylal as n=1.Reaction equation is listed below:
2CH
3OH + nHCHO == CH
3O(CH
2O)
nCH
3+ H
2O
2CH
3OH +—(CH
2O)
3== CH
3O(CH
2O)
nCH
3+H
2O
2CH
3OH +HO(CH
2O)
nH == CH
3O(CH
2O)
nCH
3+H
2O
CH
3OCH
3+ HO(CH
2O)
nH == CH
3O(CH
2O)
nCH
3+H
2O
CH
3OCH
2OCH
3+ HO(CH
2O)
nH == CH
3O(CH
2O)
n+1CH
3+H
2O
With the development of Coal Chemical Industry, coal synthesizing methanol technology maturation, its output, well beyond demand, must develop the derived product of methyl alcohol to ensure the sound development of Coal Chemical Industry.On the other hand, with the development of automotive industry, energy consumption increases, and diesel combustion produces huge environmental issue simultaneously, and petroleum industry starts to be devoted to find additive to improve oil quality, and improve fuel performance, decreasing pollution thing discharges.
Polymethoxy dimethyl ether is the general designation of the linear many ether materials of a class, is the acetal similar with methylal.Because it has very high 16 octane values (>=30) and oxygen level (>=42.1%), and without sulphur without aromatic hydrocarbons, added in diesel oil and can significantly be improved diesel combustion characteristic, effectively improve thermo-efficiency, significantly reduce NO
xwith the discharge of particulate matter, be thus considered to the environmental protection type additive for diesel oil having application prospect.According to data, its addition in diesel oil can reach 15%, and annual requirement is more than 2,300 ten thousand tons, and year consumes methyl alcohol 2600 ~ 2,700 ten thousand tons, can effectively extend methanol industry chain and bring great economic benefit and environmental benefit, having great strategic significance and good economic worth.From in August, 2013 China first cover ton Methanol PODE3-8 device 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.In addition, this product also can be used as the properties-correcting agent of resol, solvent, softening agent and releasing agent etc., is widely used.
According to the study, the application of polymethoxy dimethyl ether on diesel-dope is based on n=3-8.Industrial production adopts the mode to mixture after reaction carries out rectifying to obtain PODE3-8 product, its gas gas-phase objects stream based on PODE2, containing the PODE3-8 of a small amount of methylal, unreacted material, water and trace.The front operation that can return gas gas-phase objects stream continues to produce, but water electrode facile hydrolysis target product acetal wherein, form hemiacetal, and acetal is close with hemiacetal boiling point, is difficult to effectively be separated and affect product quality.In 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 the moisture removed comparatively up hill and dale in polymethoxy dimethyl ether.
The patent No. is that the utility model patent of ZL201320077712.4 discloses a kind of methylal deep dehydration refining plant, and this device mainly adopts absorption/regenerator column, and binding molecule sieve, by the moisture removal in methylal.This patent simply show an apparatus structure, do not provide concrete processing condition, those skilled in the art is according to this apparatus structure, to realize effect that this apparatus structure wants to reach in fact, such dewatering unit is relatively common in this area in fact, and those skilled in the art knows, processing condition are very important design links, for different dehydration objects, need different technical process and processing condition, these be not those skilled in the art rule of thumb or limited number of time test can obtain.In addition, disclosed methylal deep dehydration refining plant for the treatment of mainly methylal, and the water content of methylal is very low, general about 0.5%, this is easy to its water content control below 0.05% concerning molecular sieve itself, such dewatering purifying equipment, for the larger gas gas-phase objects stream of water content, does not possess any reference value.
Summary of the invention
The object of the present invention is to provide the absorption of a kind of polymethoxy dimethyl ether, membrane sepn in conjunction with dewatering, the method can by the water content control of polymethoxy dimethyl ether below 0.05%, simultaneously, on the basis of guaranteeing quality of adsorption, effectively can also reduce energy consumption, improve the utilization ratio of sorbent material, can also yield be improved simultaneously, guaranteeing dehydration, workshop section is complete runs independently, prevents from occurring cross influence between operation.
The present invention for achieving the above object, realizes by the following technical solutions:
A kind of polymethoxy dimethyl ether absorption, membrane sepn, in conjunction with dewatering, comprise the following steps:
A the top of gas gas-phase objects stream unstripped gas from adsorption tower one is sent into by (), and absorption reaction is carried out in adsorption tower one, sorbent material in adsorption tower one is by the water adsorption in unstripped gas, do not discharged from the bottom of adsorption tower one by the gas adsorbed, enter in gas product storage tank, in unstripped gas, the volume percent content of each moiety is respectively: water is 2% ~ 10%, methyl alcohol is 3% ~ 5%, formaldehyde is 3% ~ 5%, PODE2 is 60% ~ 80%, remaining as PODE3 ~ 8, in the gas product obtained, the content of PODE2 ~ 8 is 99.95 ~ 99.99%;
B the sorbent material in () adsorption tower one completes absorption after, enter regeneration stage, meanwhile, gas gas-phase objects stream unstripped gas is sent into from the top of adsorption tower two, and absorption reaction is carried out in adsorption tower two, do not discharged from the bottom of adsorption tower two by the gas adsorbed, enter into gas product storage tank, in the gas product 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 the material after membrane sepn preliminary hydro-extraction process be incorporated to unstripped gas pipeline enter next step adsorption deeply dehydration;
D () adsorption tower one completes regeneration after, wait for and enter into adsorbed state; After adsorption tower two completes absorption, enter regeneration stage, meanwhile, adsorption tower one enters adsorbed state again;
E () is circulated above step, until the moisture content in gas gas-phase objects stream unstripped gas reaches requirement.
Further, preferably, the sorbent material in described step (a) is at least one in molecular sieve, silica gel, activated alumina, resin.
Further, preferably, the temperature in described adsorption tower one and adsorption tower two is 120 ~ 180 degrees Celsius, and keeps invariable in absorption phase and regeneration stage.
Further, preferably, in described step (b), the detailed process of regeneration stage is:
(b1) top inlet mouth and the base bleed mouth of adsorption tower one is closed;
(b2) vacuumize process by vacuum pump to adsorption tower one, the sorbent material in adsorption tower one realizes desorb, and obtains stripping gas;
(b3) stripping gas is extracted out from the top of adsorption tower one, material after membrane sepn preliminary hydro-extraction process turns back to unstripped gas pipeline and enters the dehydration of next step adsorption deeply, the moiety of stripping gas is: methyl alcohol and formaldehyde are 20% ~ 30%, PODE2 ~ 8 are 5% ~ 10%, and all the other are water.
Further, preferably, the time of described primary sorption and regeneration is 6 ~ 12 minutes.
Further, preferably, during regeneration stage, the vacuum tightness in adsorption tower one and adsorption tower two is-0.08 ~-0.06MPa.
Further, preferably, during regeneration stage, 0.5 minute was vacuumized every 1 minute.
Further, preferably, the time of described primary sorption is 2 times of the time of primary recycling.
The present invention compared with prior art, has the following advantages and beneficial effect:
(1) the present invention carries out circulation absorption, regeneration to polymethoxy dimethyl ether gaseous phase materials stream, on the basis realizing continuous adsorption, by the moisture controlled in gas gas-phase objects stream in satisfactory scope by the method for fractionation by adsorption; In addition, the gaseous products of the workshop section of production above carries out product depth dehydration without the need to entering pressure swing adsorption system through condensing heat-exchange, in the process of adsorbing and regenerate, do not change the temperature of adsorption tower, it is made to remain on an invariable state, greatly reduce the energy consumption that usual manner brings because desorb heats up, and also make the whole process time be reduced without the need to thermoregulator link, ensure that the continuity of technique.
(2) the present invention is when absorption phase, select to give vent to anger from the top air inlet of adsorption tower, bottom, select to carry out vacuumizing process bottom adsorption tower simultaneously, so not only be conducive to the absorption of unstripped gas, simultaneously also for desorb below provides conveniently, make the moisture in sorbent material etc. can by fast desorption out.
(3) the present invention is while accomplishing effectively to reduce the gaseous phase materials stream moisture content in polymethoxy dimethyl ether production process after rectifying, by membrane sepn, stripping gas is processed, stripping gas after process is directly incorporated into absorption unstripped gas and carries out adsorption deeply dehydration, and without the need to sending into leading portion rectification working process again, thus ensure that the complete independent operating of dehydration workshop section, prevent from occurring cross influence between operation, simultaneously, under the effect of membrane sepn, effectively improve the yield of unstripped gas.
Accompanying drawing explanation
Fig. 1 is process flow sheet 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 desorb vacuum tightness and energy consumption;
Fig. 4 is the graph of a relation of adsorption time and sorbent material utilization ratio.
Embodiment
Below in conjunction with embodiment, the present invention is described in further detail, but embodiments of the present invention are not limited thereto.
As shown in Figure 1, a kind of polymethoxy dimethyl ether absorption, membrane sepn, in conjunction with dewatering, comprise the following steps:
A volume percent content is respectively by (): water is 2% ~ 10%, methyl alcohol is 3% ~ 5%, formaldehyde is 3% ~ 5%, PODE2 is 60% ~ 80%, gas gas-phase objects stream unstripped gas remaining as PODE3 ~ 8 is sent into from the top of adsorption tower one, and absorption reaction is carried out in adsorption tower one, temperature in tower is 120 ~ 180 degrees Celsius, and keep invariable, sorbent material in adsorption tower one is by the water adsorption in unstripped gas, sorbent material can be molecular sieve, silica gel, activated alumina, in resin one or both or two or more, preferred molecular sieve, do not discharged from the bottom of adsorption tower one by the gas adsorbed, enter in gas product storage tank, in gas product, the content of PODE2 ~ 8 is 99.95 ~ 99.99%, all the other are methyl alcohol, the monomers such as formaldehyde,
B the sorbent material in () adsorption tower one completes absorption after, enter regeneration stage, meanwhile, gas gas-phase objects stream unstripped gas is sent into from the top of adsorption tower two, and absorption reaction is carried out in adsorption tower two, do not discharged from the bottom of adsorption tower two by the gas adsorbed, enter into gas product storage tank, in gas product, 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 after membrane separation, be incorporated into unstripped gas pipeline and enter the dehydration of next step adsorption deeply, in like manner, adsorption tower two is when carrying out adsorbent reactivation, identical with adsorption tower one principle;
D () adsorption tower one completes regeneration after, wait for and enter into adsorbed state; After adsorption tower two completes absorption, enter regeneration stage, meanwhile, adsorption tower one enters adsorbed state again; Any adsorption tower complete primary sorption start to the time of regeneration ending be 6 ~ 12 minutes;
E () is circulated above step, until the moisture content in gas gas-phase objects stream unstripped gas reaches requirement.
At present, in polymethoxy dimethyl ether dewatering process, the also not mentioned method relevant to membrane sepn, membrane sepn, by innovation, is incorporated into the dehydration of polymethoxy dimethyl ether by the present invention pioneeringly, and combine with adsorption dewatering, on the basis of guaranteeing high product purity, more obtaining high yield, making stripping gas again process without the need to getting back to leading portion rectification working process simultaneously, achieve 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 inlet mouth and the base bleed mouth of adsorption tower one, make adsorption tower one in air-tight state;
(b2) every 1 minute, vacuumize 0.5 minute by vacuum pump to adsorption tower one, make the vacuum tightness in adsorption tower one be-0.08 ~-0.06MPa, simultaneous temperature remains on 120 ~ 180 degrees Celsius, and the sorbent material in adsorption tower one realizes desorb with this understanding;
(b3) stripping gas is extracted out from the top of adsorption tower one, after membrane separation, is incorporated into unstripped gas pipeline and enters the dehydration of next step adsorption deeply, improve the utilization ratio of unstripped gas and the yield of product; In stripping gas, methyl alcohol and formaldehyde are 20% ~ 30%, PODE2 ~ 8 is 5% ~ 10%, and all the other are water.
In above-mentioned processing step, the main processing parameter optimized has: the temperature in desorption process, the vacuum tightness in desorption process, adsorption time.
An inventive point of the present invention is the temperature of adsorption tower in desorption process in optimization step (b2), temperature is higher, desorption effect is better, desorb is more thorough, is conducive to sorbent material and keeps higher adsorption effect when next time adsorbs, and the water content of namely adsorbing the product obtained next time is lower, but, temperature is higher, and energy consumption is also larger, and whole processing cost is also higher; And temperature is lower, although energy consumption is less, desorption effect is poorer, and pole affects the absorption again of sorbent material; Therefore, consider, select the desorption temperature that suitable, to obtain good desorption effect and lower energy consumption, the water content of again adsorbing the product obtained after the desorb of desorption effect sorbent material is weighed, and water content is lower, and desorption effect is better.
For obtaining a best desorption temperature, invention has been the impact of desorption temperature on product water content (again adsorbing the water content of the product obtained after desorb) and energy consumption to test, in experimentation, only change desorption temperature, other processing parameter remains unchanged, and desorption temperature is chosen for 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 respectively, experimental result is as shown in Fig. 2 and table one.
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 increases gradually, and when desorption temperature changes between 120 DEG C ~ 150 DEG C, the increase tendency of energy consumption is relatively mild, and when desorption temperature is more than 150 DEG C, energy consumption increases suddenly; As can be seen from table one, along with the rising of desorption temperature, product water content (again adsorbing the water content of the product obtained after desorb) reduces gradually, when desorption temperature changes between 120 DEG C ~ 150 DEG C, the reduction trend of product water content (again adsorbing the water content of the product obtained after desorb) clearly, when desorption temperature changes between 150 DEG C ~ 180 DEG C, the reduction trend of product water content (again adsorbing the water content of the product obtained after desorb) is very mild.Therefore, comprehensive energy consumption and product water content, the present invention is best, and desorption temperature is 150 DEG C, under this desorption temperature, energy consumption can be made lower, make product water content lower simultaneously.
Another inventive point of the present invention is the vacuum tightness of adsorption tower in desorption process in optimization step (b2), vacuum tightness higher (namely pressure is less), desorption effect is better, desorb is more thorough, is conducive to sorbent material and keeps higher adsorption effect when next time adsorbs, and the water content of namely adsorbing the product obtained next time is lower, but, vacuum tightness is higher, and energy consumption is also larger, and whole processing cost is also higher; And vacuum tightness is lower, although energy consumption is less, desorption effect is poorer, and pole affects the absorption again of sorbent material; Therefore, consider, select the desorb vacuum tightness that one suitable, to obtain good desorption effect and lower energy consumption, the water content of again adsorbing the product obtained after the desorb of desorption effect sorbent material is weighed, and water content is lower, and desorption effect is better.
For obtaining a best desorb vacuum tightness, invention has been the impact of desorb vacuum tightness on product water content (again adsorbing the water content of the product obtained after desorb) and energy consumption to test, in experimentation, only change desorb vacuum tightness, other processing parameter remains unchanged, and desorb vacuum tightness is chosen for-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 respectively, experimental result is as shown in Fig. 3 and table two.
Product water content under the different desorb vacuum tightness of table two
| Vacuum tightness (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 tightness, energy consumption increases gradually, and when vacuum tightness changes between-0.070 ~-0.060MPa, the increase tendency of energy consumption is relatively mild, and when desorb vacuum tightness exceedes-0.070MPa, energy consumption increases suddenly; As can be seen from table two, along with the rising of desorb vacuum tightness, product water content (again adsorbing the water content of the product obtained after desorb) reduces gradually, when desorb vacuum tightness changes between-0.070 ~-0.060MPa, the reduction trend of product water content (again adsorbing the water content of the product obtained after desorb) clearly, when desorb vacuum tightness changes between-0.080 ~-0.070MPa, the reduction trend of product water content (again adsorbing the water content of the product obtained after desorb) is very mild.Therefore, comprehensive energy consumption and product water content, the present invention is best, and desorb vacuum tightness is-0.070MPa, under this desorb vacuum tightness, energy consumption can be made lower, make product water content lower simultaneously.
Another inventive point of the present invention is to optimize the absorption in step (c) and recovery time, the time sum completing primary sorption and primary recycling is limited to 6 ~ 12 minutes, the respective time is distributed simultaneously, preferably, adsorption time is arranged to the twice of recovery time, such as, if adsorb 4 minutes, then 2 minutes are regenerated; If adsorb 8 minutes, then regenerate 4 minutes.Adsorption time is longer, and the utilization ratio of sorbent material is higher, but the water content of product is also higher simultaneously; Otherwise adsorption time is shorter, the water content of product is lower, but the utilization ratio of sorbent material is also lower, therefore, consider, and selects the adsorption time that suitable, to make the water content of product lower, makes the utilization ratio of sorbent material higher simultaneously.
For obtaining a best adsorption time, invention has been the impact of adsorption time on product water content and sorbent material utilization ratio to test, in experimentation, only change adsorption time, other processing parameter remains unchanged, and desorb vacuum tightness is chosen for 4 minutes respectively, 4.5 minutes, 5 minutes, 5.5 minutes, 6 minutes, 6.5 minutes, 7 minutes, 7.5 minutes, 8 minutes, experimental result is as shown in Fig. 4 and table three.
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 ratio of sorbent material improves gradually, when adsorption time changed between 4 ~ 6 minutes, the utilization ratio rising tendency of sorbent material is obvious, and when adsorption time changed between 6 ~ 8 minutes, the utilization ratio of sorbent material increases relatively mild; As can be seen from table three, along with the growth of adsorption time, product water content constantly raises, when adsorption time changed between 4 ~ 6 minutes, it is comparatively mild that product water content raises trend, and when adsorption time changed between 6 ~ 8 minutes, it is fairly obvious that product water content raises trend; Therefore, the utilization ratio of comprehensive sorbent material and product water content, when adsorption time is 6 minutes, when now the recovery time is 3 minutes, can obtain higher sorbent material utilization ratio, make product water content lower simultaneously, within 6 minutes, is best adsorption time.
In addition, it should be noted that, the present invention is just described for double tower, and double tower is the condition at least guaranteeing continuous adsorption, when gas gas-phase objects stream treatment capacity is larger, can have multiple adsorption tower.
The above is only preferred embodiment of the present invention, and not do any pro forma restriction to the present invention, every any simple modification, equivalent variations done above embodiment according to technical spirit of the present invention, all falls within protection scope of the present invention.
Claims (8)
1. polymethoxy dimethyl ether absorption, membrane sepn, in conjunction with a dewatering, is characterized in that, comprise the following steps:
A the top of gas gas-phase objects stream unstripped gas from adsorption tower one is sent into by (), and absorption reaction is carried out in adsorption tower one, sorbent material in adsorption tower one is by the water adsorption in unstripped gas, do not discharged from the bottom of adsorption tower one by the gas adsorbed, enter in gas product storage tank, in unstripped gas, the volume percent content of each moiety is respectively: water is 2% ~ 10%, methyl alcohol is 3% ~ 5%, formaldehyde is 3% ~ 5%, PODE2 is 60% ~ 80%, remaining as PODE3 ~ 8, in the gas product obtained, the content of PODE2 ~ 8 is 99.95 ~ 99.99%;
B the sorbent material in () adsorption tower one completes absorption after, enter regeneration stage, meanwhile, gas gas-phase objects stream unstripped gas is sent into from the top of adsorption tower two, and absorption reaction is carried out in adsorption tower two, do not discharged from the bottom of adsorption tower two by the gas adsorbed, enter into gas product storage tank, in the gas product 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 the material obtained after membrane sepn preliminary hydro-extraction process is incorporated to unstripped gas pipeline enters adsorption tower deep dehydration;
D () adsorption tower one completes regeneration after, wait for and enter into adsorbed state; After adsorption tower two completes absorption, enter regeneration stage, meanwhile, adsorption tower one enters adsorbed state again;
E () is circulated above step, until the moisture content in gas gas-phase objects stream unstripped gas reaches requirement.
2. a kind of polymethoxy dimethyl ether absorption according to claim 1, membrane sepn are in conjunction with dewatering, it is characterized in that: the sorbent material in described step (a) is at least one in molecular sieve, silica gel, activated alumina, resin.
3. a kind of polymethoxy dimethyl ether absorption according to claim 1, membrane sepn are in conjunction with dewatering, it is characterized in that: the temperature in described adsorption tower one and adsorption tower two is 120 ~ 180 degrees Celsius, and keeps invariable in absorption phase and regeneration stage.
4. a kind of polymethoxy dimethyl ether absorption according to claim 1, membrane sepn are in conjunction with dewatering, it is characterized in that: in described step (b), the detailed process of regeneration stage is:
(b1) top inlet mouth and the base bleed mouth of adsorption tower one is closed;
(b2) vacuumize process by vacuum pump to adsorption tower one, the sorbent material in adsorption tower one realizes desorb, and obtains stripping gas;
(b3) stripping gas is extracted out from the top of adsorption tower one, material after membrane sepn preliminary hydro-extraction process is incorporated to unstripped gas pipeline and enters the dehydration of next step adsorption deeply, the moiety of stripping gas is: methyl alcohol and formaldehyde are 20% ~ 30%, PODE2 ~ 8 are 5% ~ 10%, and all the other are water.
5. a kind of polymethoxy dimethyl ether absorption according to claim 4, membrane sepn are in conjunction with dewatering, it is characterized in that: during regeneration stage, and the vacuum tightness in adsorption tower one and adsorption tower two is-0.08 ~-0.06MPa.
6. a kind of polymethoxy dimethyl ether absorption according to claim 4, membrane sepn are in conjunction with dewatering, it is characterized in that: during regeneration stage, vacuumize 0.5 minute every 1 minute.
7. a kind of polymethoxy dimethyl ether absorption according to claim 4, membrane sepn are in conjunction with dewatering, it is characterized in that: the time of described primary sorption and regeneration is 6 ~ 12 minutes.
8. a kind of polymethoxy dimethyl ether absorption according to claim 7, membrane sepn are in conjunction with dewatering, it is characterized in that: the time of described primary sorption is 2 times of the time of primary recycling.
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| CN106365960A (en) * | 2016-10-12 | 2017-02-01 | 江苏凯茂石化科技有限公司 | Device and method for removing formaldehyde in polyoxymethylene dimethyl ethers |
| CN107163005A (en) * | 2017-06-21 | 2017-09-15 | 武汉智宏思博化工科技有限公司 | A kind of film dehydration couples the industrial equipment for producing anhydrous THF with molecular sieve adsorption |
| CN111087286A (en) * | 2018-10-23 | 2020-05-01 | 中国石油化工股份有限公司 | Method for refining polymethoxy dimethyl ether dimer |
| CN111087288A (en) * | 2018-10-23 | 2020-05-01 | 中国石油化工股份有限公司 | Method for purifying dimeric methoxy dimethyl ether |
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