CN104628539A - Method and system for separating polyoxymethylene dimethyl ether - Google Patents
Method and system for separating polyoxymethylene dimethyl ether Download PDFInfo
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- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C41/00—Preparation of ethers; Preparation of compounds having groups, groups or groups
- C07C41/48—Preparation of compounds having groups
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Abstract
The invention discloses a method and a system for separating polyoxymethylene dimethyl ether (DMMn). The separation method comprises the following steps: (1) inputting the materials containing DMMn into a pretreatment unit filled with alkaliferous solids to remove the solid impurities, the acid, the water and the formaldehyde in the materials; (2) inputting the pretreated materials into an alkali auxiliary pressure swing distillation unit, performing pressure-swing separation on the light and heavy components of the materials in a rectifying tower under an alkali environment, preferably, the step (2) comprises: controlling the pressure of the rectifying tower to 0.0002-0.2 MPa, in each partitioning cycle, reducing the pressure of the rectifying tower from a relative high pressure to a relative low pressure, after finishing each partitioning cycle, recovering the pressure of the rectifying tower to a relative high pressure, and processing a next partitioning cycle. The separation system comprises a pretreatment unit and an alkali auxiliary pressure swing distillation unit and the like. By means of the separation method provided by the invention, the single components of the DMMn can be effectively separated, and the process is simple and controllable and can be long-term stably operated; besides, the adopted equipment is simple, easy to operate, green and environmentally friendly.
Description
Technical field
The present invention be more particularly directed to separating technology and the system of a kind of polymethoxy dimethyl ether (DMMn).
Background technology
Polymethoxy dimethyl ether CH
3o (CH
2o)
ncH
3(3≤n≤8, also known as DMMn) is a kind of novel diesel-dope of clean environment firendly, due to its physico-chemical property and traditional diesel oil very close, itself and diesel oil blending are burnt, effectively can improve efficiency of combustion, and reduce the discharge of soot.The blending performance of polymethoxy dimethyl ether and diesel oil is good, can dissolve each other, and has self lubricity, can extend diesel oil mechanical life.
DMMn also can as a kind of novel Alternative Diesel Fuel simultaneously.The patent documentations such as US7235113B2, EP1422285B1 propose, with polymethoxy dimethyl ether absolutely complete diesel oil substitute, it can be used as a kind of novel alternative fuel, by carrying out a certain proportion of composite to the acetal of different polymerization degree, obtaining the alternative fuel that can be directly used in oil engine.When the fuel of composition below using:
DMM2, CH
3o (CH
2o)
2cH
3: 45% (massfraction)
DMM3, CH
3o (CH
2o)
3cH
3: 28% (massfraction)
DMM4, CH
3o (CH
2o)
4cH
3: 15% (massfraction)
DMM5, CH
3o (CH
2o)
5cH
3: 8% (massfraction)
DMM6, CH
3o (CH
2o)
6cH
3: 4% (massfraction)
When motor speed is 500rpm, NOx discharge is: 1.2g/kwh; Particulate matter (PM) quantity discharged is: 0.001g/kwh; Hydrocarbon polymer: 0.3g/kwh, content is lower than Europe V standard (Euro V limit).
In order to adapt to the blending of different ratio or composite practical situation, need the DMM that the polymerization degree is different
nproduct, therefore to DMM
nit is necessary for carrying out plant-scale separation.And the product of different polymerization degree can also as synthetic intermediate, special solvent etc., thus good separating technology has great importance for follow-up application.
Refer to table 1, DMM
nproduct is the homologue dissolved each other that a series of polymerization degree is different, and they have very wide distribution on boiling point.Wherein, DMM1 is easy to volatilization, and more than DMM5 then has higher boiling point.And because DMMn is under acidity or micro-sour situation, can depolymerization reaction be occurred during heating and may, with the generation of white polymer solid, separation can not be carried out.Thus, industry thirsts for the separating technology developing a kind of efficient, stable polymethoxy dimethyl ether for a long time always.
Table 1DMM
nthe character such as molten, boiling point
| Compound | Fusing point/DEG C | Boiling point/DEG C | Cetane value | Oxygen level % |
| DMM1 | -105 | 42 | 29 | 42.1 |
| DMM2 | -69.7 | 105 | 63 | 45.3 |
| DMM3 | -42.5 | 156 | 78 | 47.1 |
| DMM4 | -9.8 | 202 | 90 | 48.2 |
| DMM5 | 18.3 | 242 | 100 | 48.5 |
Summary of the invention
Main purpose of the present invention is the separation method providing a kind of efficient, stable polymethoxy dimethyl ether, to overcome the deficiencies in the prior art.
For realizing aforementioned invention object, the technical solution used in the present invention comprises:
A kind of separation method of polymethoxy dimethyl ether (DMMn), comprising:
(1) the material input pretreatment unit be filled with containing alkali solid containing DMMn is carried out pre-treatment, at least to remove solid impurity in described material, acid, water and formaldehyde;
(2) assist variable-pressure rectification unit to carry out rectifying in material input alkali after pretreatment, with the rectifying tower of alkali environment, the light constituent in material is separated with heavy constituent transformation.
Further, the alkali solid that contains loaded in pretreatment unit comprises NaOH, Na
2cO
3, KOH, CaO, Na
2sO
3, K
2cO
3, the combination of any one or more in gac, but to be not limited thereto.
Comparatively preferred, the described alkali solid that contains comprises CaO and/or Na
2sO
3.
Further, step (2) comprising: material input alkali after pretreatment is assisted variable-pressure rectification unit, and contact with the column plate of the basic filler in rectifying tower or alkalinisation treatment, after multistage vapor-liquid separation, at the bottom of rectifying tower tower top, tower, obtain light constituent, heavy constituent respectively at various pressures.
Further, for forming described basic filler or the alkali for carrying out alkalinisation treatment to column plate comprises NaOH, Na
2cO
3, KOH, K
2cO
3, Ca (OH)
2, CaO, CaCO
3in the combination of any one or more, but to be not limited thereto.
Comparatively preferred, described basic filler is at least selected from the Na primarily of Stainless Steel Cloth and granulation
2cO
3, CaO, CaCO
3what one or more in particle were formed loads in mixture filler, with containing the dumped packing of the solution of any one or more coating in Na, K, Ca or structured packing.
As one of comparatively preferred embodiment, step (2) comprising: the pressure controlled in rectifying tower is 0.0002MPa-0.2MPa, and at least one partitioning cycle, make the pressure in rectifying tower drop to relatively low pressure from relatively high pressure, and after this at least one partitioning cycle terminates, by the pressure recovery in rectifying tower to relatively high pressure, then carry out next partitioning cycle.
Particularly preferred, step (2) comprising: the pressure controlled in rectifying tower is 0.0005MPa-0.1MPa.
As one of comparatively preferred embodiment, described separation method also can comprise further: again participate in building-up reactions in synthesis system part light constituent isolated in step (2) and/or heavy constituent being circulated to polymethoxy dimethyl ether according to actual production demand.
As one of comparatively preferred embodiment, described separation method also can comprise further: by the alkali manipulation of regeneration in alkali cycling element adopted in preprocessing process and rectifying, and is back to pretreatment unit and alkali assists variable-pressure rectification unit to reuse.
Present invention also offers a kind of polymethoxy dimethyl ether separation system being applied to aforementioned separation method, it comprises:
Be filled with the pretreatment unit containing alkali solid, at least for carrying out pre-treatment to the material containing DMMn, at least to remove solid impurity in described material, acid, water and formaldehyde;
The alkali comprising the rectifying tower of alkali environment assists variable-pressure rectification unit, at least for carrying out rectifying, to be separated with heavy constituent transformation by the light constituent in material to pretreated material input.
As one of comparatively preferred embodiment, described separation system also can comprise alkali cycling element, in order to will be back to pretreatment unit after the alkali adopted in preprocessing process and rectifying manipulation of regeneration and alkali assists variable-pressure rectification unit to reuse.
In the separation method of polymethoxy dimethyl ether of the present invention, by introducing alkali in sepn process, the decomposition of DMMn can be suppressed, and destroy the azeotropic of constituent part, it is easier to make to be separated, meanwhile, by adopting transformation process, the various ingredients of wide boiling spread can be isolated, and heat sensitive components can be distillated at low pressures.
Compared with prior art, the present invention at least tool has the following advantages: the separation method of this polymethoxy dimethyl ether can isolate the single component of DMMn efficiently, and technique is simply controlled, and can steady in a long-termly run, the equipment simultaneously adopted is simple, is easy to manipulation, environmental protection.
Accompanying drawing explanation
In order to be illustrated more clearly in the technical scheme in the embodiment of the present invention, below the accompanying drawing used required in describing embodiment is briefly described, apparently, accompanying drawing for the present invention in the following describes is only some embodiments of the present invention, for those of ordinary skill in the art, not paying under the prerequisite creating work, other accompanying drawing can also be obtained according to these accompanying drawings.
Fig. 1 is the separating technology schematic diagram of a kind of polymethoxy dimethyl ether among the present invention one typical embodiments;
Fig. 2 is the structural representation of the separation system of a kind of polymethoxy dimethyl ether among the better case study on implementation of the present invention one.
Embodiment
As previously mentioned, in view of prior art exists many deficiencies, inventor, through studying for a long period of time and putting into practice in a large number, is proposed technical scheme of the present invention, is illustrated as follows.
One aspect of the present invention mainly provides a kind of efficient, stable polymethoxy dimethyl ether separating technology, more precisely, is a kind of DMMn isolation technique.
Consult shown in Fig. 1, among a typical embodiments of the present invention, the separating technology of this polymethoxy dialkyl ether DMMn can comprise the steps:
(1) material of DMMn is contained after reaction after pretreatment unit, except components such as disacidify, water, formaldehyde;
Further, in pretreatment unit, process is as follows: the pretreater of streams through being filled with alkali containing DMMn after reaction can remove major part acid, water, formaldehyde.Next unit is entered after removing solid impurity.
Further, what use in pretreatment unit can be NaOH, Na containing alkali solid
2cO
3, KOH, CaO, Na
2sO
3, K
2cO
3, gac or containing the mixture of above-mentioned substance.Optimize, the alkali wherein adopted is CaO and Na
2sO
3.
(2) pretreated material enters alkali and assists variable-pressure rectification unit (Alkali Aided Variable Pressure Rectification, AAVPR), and in the rectifying tower of alkali environment, transformation isolates light constituent and heavy constituent.Comparatively preferred, wherein part is light, heavy constituent can according to production actual cycle to reactor secondary response again;
Further, alkali is assisted in variable-pressure rectification unit, and pretreated material enters rectifying tower, contacts with the column plate of the basic filler in tower or alkalinisation treatment, after multi-stage gas-liquid is separated, obtains light constituent from tower top, at the bottom of tower, obtain heavy constituent at various pressures.
Further, can be NaOH, Na for basic filler or for the alkali of alkalinisation treatment
2cO
3, KOH, K
2cO
3, Ca (OH)
2, CaO, CaCO
3.Comparatively preferably, for the filler of rectifying be the Na of Stainless Steel Cloth and granulation
2cO
3, CaO, CaCO
3particle loads in mixture filler, or with the conventional dumped packing applied containing Na, K, Ca solution or structured packing.
Preferably, rectifying tower internal pressure P
absfor 0.0002MPa-0.2MPa, drop to relatively low pressure from relatively high pressure, after a partitioning cycle terminates, return to relatively high pressure again, then enter next circulation.Further, more excellent pressure range is 0.0005MPa-0.1MPa.
(3) alkali used in process uses by alkali cycling element reprocessing cycle.
In pre-treatment and in rectifying, the alkali that uses is regenerated at alkali cycling element, and returns pre-treatment and rectification cell reuses.
Another aspect of the present invention provides a kind of separation system of polymethoxy dimethyl ether, and main cooperation with aforementioned separation method implements, and it can comprise pretreatment unit, alkali assists variable-pressure rectification unit, alkali cycling element etc.
Below in conjunction with some embodiments and accompanying drawing, technical scheme of the present invention is described in further detail.
Embodiment 1 refers to shown in Fig. 2, and the present embodiment system a kind of DMMn alkali assists the concrete enforcement example of variable-pressure rectification separation process scheme system.
Specifically, this technical process can comprise: first, material to be separated to be inputted in pretreater through pipeline 2 by pump P1 through pipeline 1 from raw material storage tank and processes, removing moisture, acid, formaldehyde, filling sodium sulphite anhydrous 99.3 in pretreater and anhydrous calcium oxide, after treatment, acid content is lower than 0.001%, water-content is lower than 0.1%, and formaldehyde is lower than 0.1% (massfraction).Material after process enters alkali through pipeline 3 and assists rectifying in variable-pressure rectification AAVPR unit, obtains the lighter fraction of DMMn after rectifying from tower top (pipeline 5), and heavy constituent is by (pipeline 6) discharge at the bottom of tower.The S-WAT loaded in pretreater and calcium oxide, input moisture eliminator through pipeline 7 and enter alkali revivifier through pipeline 8 and regenerated after using for some time.Alkali assists the partial alkaline component in variable-pressure rectification AAVPR unit to be regenerated in alkali revivifier after also drying device drying.
In the present embodiment, alkali assists in variable-pressure rectification AAVPR unit the stainless steel woven wire and the CaO-CaCO through granulation that adopt and load in mixture
3particle, rectifying tower inner member is also through Ca (OH)
2coating.Unit and pipeline, except raw material storage tank and pump P1, need to adopt alkali resistant materials manufacture.When rectifying tower internal pressure Pabs drops to 0.001MPa process can isolate DMM1, DMM2...DMM7 successively from tower top from 0.1MPa, heavy constituent DMMn can be discharged at the bottom of tower, n >=8.
Embodiment 2 pre-treatment example
10L is contained massfraction for acid 0.01%, water 1.5%, the material of the DMMn of formaldehyde 5.3% flows through the pretreater being filled with anhydrous CaO, gac with the speed of 100mL/min after, cross elimination solid impurity, after testing, acid content is lower than 0.001%, and water-content is lower than 0.015%, and formaldehyde is lower than 0.1% (massfraction).
Embodiment 3 pre-treatment example
10L is contained massfraction for acid 0.015%, water 1.0%, the material of the DMMn of formaldehyde 2.8% flows through with the speed of 100mL/min and is filled with anhydrous CaO, anhydrous Na
2sO
3, K
2cO
3, NaOH pretreater after, cross elimination solid impurity, after testing, acid content is lower than 0.001%, and water-content is lower than 0.01%, and formaldehyde is lower than 0.1% (massfraction).
Embodiment 4 pre-treatment example
10L is contained massfraction for acid 0.015%, water 1.0%, the material of the DMMn of formaldehyde 2.8% flows through with the speed of 100mL/min and is filled with KOH, anhydrous Na
2sO
3, K
2cO
3pretreater after, cross elimination solid impurity, after testing, acid content is lower than 0.001%, and water-content is lower than 0.01%, and formaldehyde is lower than 0.1% (massfraction).
Embodiment 5 rectifying example
Pretreated material (composition is in table 2) enters alkali and assists variable-pressure rectification tower, and tower inner member is with Ca (OH)
2logical N after slurries coating
2blow away powder and drying, in tower, load CaO, CaCO of Stainless Steel Cloth and granulation
3particle loads in mixture filler, and equivalent stage number is about 50.Control tower pressure is 0.1MPa, reboiler heating and temperature control at 60 DEG C, top gas phase temperature 30 DEG C, condensing temperature is 2 DEG C, and control of reflux ratio is 2, and the purity that under this condition, tower top distillates DMM1 can reach 98.5%.
Table 2DMMn feed composition
| DMM1 | DMM2 | DMM3 | DMM4 | DMM5 | DMM6 | DMM7 | DMM8 |
| 35.1％ | 26.0％ | 17.1％ | 10.2％ | 5.8％ | 3.2％ | 1.6％ | 0.8％ |
Embodiment 6 rectifying example
Rectifying tower inner member is with Ca (OH)
2, KOH and Na
2cO
3logical N after slurries coating
2blow away powder and drying, in tower, load CaO, CaCO of Stainless Steel Cloth and granulation
3, Na
2cO
3particle loads in mixture filler, and equivalent stage number is about 50.The basis of embodiment 5 reduces pressure tower, controls at 0.04MPa, reboiler heating and temperature control is at 80 DEG C, and top gas phase temperature 30 DEG C, condensing temperature is 5 DEG C, and control of reflux ratio is 3, and the purity that under this condition, tower top distillates DMM2 can reach 99.0%.
Embodiment 7 rectifying example
Stainless steel θ ring is immersed in containing Ca (OH)
2, NaOH, CaCO
3with Na
2cO
3slurries in, dry after hanging, be filled in rectifying tower, equivalent stage number is about 60, purge with inert nitrogen in tower, the basis of embodiment 6 reduces pressure tower, controls at 0.01MPa, reboiler heating and temperature control is at 150 DEG C, top gas phase temperature 65 DEG C, condensing temperature is 10 DEG C, and control of reflux ratio is 3, and the purity that under this condition, tower top distillates DMM3 can reach 99.9%.
Embodiment 8 rectifying example
Metal perforated plate perforated plate corrugated filler is immersed in containing Ca (OH)
2, CaCO
3with K
2cO
3slurries in, dry after hanging, be filled in rectifying tower, equivalent stage number is about 30, purge with inert nitrogen in tower, the basis of embodiment 7 reduces pressure tower, controls at 0.005MPa, reboiler heating and temperature control is at 185 DEG C, top gas phase temperature 100 DEG C, condensing temperature is 20 DEG C, and control of reflux ratio is 5, and the purity that under this condition, tower top distillates DMM4 can reach 99.9%.
Embodiment 9 rectifying example
Stainless steel θ ring is immersed in containing Ca (OH)
2, NaOH, CaCO
3with Na
2cO
3slurries in, dry after hanging, be filled in rectifying tower, equivalent stage number is about 60, purge with inert nitrogen in tower, the basis of embodiment 8 reduces pressure tower, controls at 0.002MPa, reboiler heating and temperature control is at 250 DEG C, top gas phase temperature 120 DEG C, condensing temperature is 20 DEG C, and control of reflux ratio is 5, and the purity that under this condition, tower top distillates DMM5 can reach 99.9%.
Embodiment 10 rectifying example
Stainless steel θ ring is immersed in containing Ca (OH)
2, NaOH, CaCO
3with Na
2cO
3slurries in, dry after hanging, be filled in rectifying tower, equivalent stage number is about 60, purge with inert nitrogen in tower, the basis of embodiment 9 reduces pressure tower, controls at 0.0015MPa, reboiler heating and temperature control is at 320 DEG C, top gas phase temperature 170 DEG C, condensing temperature is 30 DEG C, and control of reflux ratio is 2, and the purity that under this condition, tower top distillates DMM6 can reach 99.5%.
Embodiment 11 rectifying example
Stainless steel θ ring is immersed in containing Ca (OH)
2, NaOH, CaCO
3with Na
2cO
3slurries in, dry after hanging, be filled in rectifying tower, equivalence stage number is about 60, purges, the basis of embodiment 10 reduces pressure tower in tower with inert nitrogen, control at 0.0005MPa, reboiler heating and temperature control, at 360 DEG C, pushes up gas phase temperature 200 DEG C, and condensation column cap is incubated, control of reflux ratio is 2, the purity that under this condition, tower top distillates DMM7 can reach 99.2%, and discharging at the bottom of tower is DMM8, and purity is 98.0%.
Embodiment 12 alkali collection example
The CaO declined by certain batch of operating performance, Mixture of Activated Carbon unload, and after CaO, gac screening, CaO, after 110 DEG C of dry 24h, carries out calcining 6h, and temperature is set as 900 DEG C.By restorability after gac 100 DEG C of vacuum-drying 50h.
Comparative example 1
With the rectifying tower (equivalent stage number is about 60) that stainless steel θ ring is loaded, after purging with inert nitrogen in tower, the material to be separated (material composition is in table 3) not through pretreater is directly inputted in rectifying tower and carries out rectifying.Control tower pressure is 0.1MPa, and reboiler heating and temperature control, at 60 DEG C, pushes up gas phase temperature 30 DEG C, condensing temperature is 2 DEG C, and control of reflux ratio is 2, after cutting out partial DMM1, muddy as seen at the bottom of tower.Adularescent solid condensation in overhead condenser, is difficult to continue to be separated DMM2-8 component below.
The feed composition of table 3 comparative example 1
| Formaldehyde | Water | Acid | DMM1 | DMM2 | DMM3 | DMM4 | DMM5 | DMM6 | DMM7 | DMM8 |
| 2.8％ | 1.0％ | 0.01％ | 33.8％ | 25.0％ | 16.4％ | 9.9％ | 5.6％ | 3.1％ | 1.5％ | 0.77％ |
Comparative example 2
With the rectifying tower (equivalent stage number is about 60) that stainless steel θ ring is loaded, after purging with inert nitrogen in tower, will be input in rectifying tower through the pretreated material of pretreater (composition is shown in table 2 in embodiment 5) and carry out rectifying.Control tower pressure is 0.1MPa, and reboiler heating and temperature control is at 60 DEG C, and top gas phase temperature 30 DEG C, condensing temperature is 2 DEG C, and control of reflux ratio is 2.Can isolate DMM1 from tower top, purity is greater than 98.5%.But continue to run, after tower top cutting out partial DMM2, become muddy at the bottom of tower, and the mill base liquid that finally bleaches.Be difficult to be separated follow-up DMM3-8 component.
Summarize it, DMMn separating technology of the present invention at least has following beneficial effect: (1) transformation process can adapt to the various ingredients of wide boiling spread; (2) thermolysis of high boiling component is avoided; (4) alkali assists rectifying to inhibit the acid of DMMn in rectifying to decompose; (5) this technique isolated DMMn purity is very high; (6) alkali can regenerate rear reuse, environmental protection.
To those skilled in the art, obviously the invention is not restricted to the details of above-mentioned one exemplary embodiment, and when not deviating from spirit of the present invention or essential characteristic, the present invention can be realized in other specific forms.Therefore, no matter from which point, all should embodiment be regarded as exemplary, and be nonrestrictive, scope of the present invention is limited by claims instead of above-mentioned explanation, and all changes be therefore intended in the implication of the equivalency by dropping on claim and scope are included in the present invention.
In addition, be to be understood that, although this specification sheets is described according to embodiment, but not each embodiment only comprises an independently technical scheme, this narrating mode of specification sheets is only for clarity sake, those skilled in the art should by specification sheets integrally, and the technical scheme in each embodiment also through appropriately combined, can form other embodiments that it will be appreciated by those skilled in the art that.
Claims (10)
1. a separation method for polymethoxy dimethyl ether, is characterized in that comprising:
(1) the material input pretreatment unit be filled with containing alkali solid containing DMMn is carried out pre-treatment, at least to remove solid impurity in described material, acid, water and formaldehyde;
(2) assist variable-pressure rectification unit to carry out rectifying in material input alkali after pretreatment, with the rectifying tower of alkali environment, the light constituent in material is separated with heavy constituent transformation.
2. the separation method of polymethoxy dimethyl ether according to claim 1, is characterized in that loading comprise NaOH, Na containing alkali solid in pretreatment unit
2cO
3, KOH, CaO, Na
2sO
3, K
2cO
3, the combination of any one or more in gac; Preferably, the described alkali solid that contains comprises CaO and/or Na
2sO
3.
3. the separation method of polymethoxy dimethyl ether according to claim 1, it is characterized in that step (2) comprising: material input alkali after pretreatment is assisted variable-pressure rectification unit, and contact with the column plate of the basic filler in rectifying tower or alkalinisation treatment, after multistage vapor-liquid separation, at the bottom of rectifying tower tower top, tower, obtain light constituent, heavy constituent respectively at various pressures.
4. the separation method of polymethoxy dimethyl ether according to claim 3, is characterized in that for forming described basic filler or the alkali for carrying out alkalinisation treatment to column plate comprises NaOH, Na
2cO
3, KOH, K
2cO
3, Ca (OH)
2, CaO, CaCO
3in the combination of any one or more; Preferably, described basic filler is at least selected from the Na primarily of Stainless Steel Cloth and granulation
2cO
3, CaO, CaCO
3what one or more in particle were formed loads in mixture filler, with containing the dumped packing of the solution of any one or more coating in Na, K, Ca or structured packing.
5. the separation method of polymethoxy dimethyl ether according to any one of claim 1-4, it is characterized in that step (2) comprising: the pressure controlled in rectifying tower is 0.0002MPa-0.2MPa, and at least one partitioning cycle, make the pressure in rectifying tower drop to relatively low pressure from relatively high pressure, and after this at least one partitioning cycle terminates, by the pressure recovery in rectifying tower to relatively high pressure, then carry out next partitioning cycle.
6. the separation method of polymethoxy dimethyl ether according to claim 5, is characterized in that step (2) comprising: the pressure controlled in rectifying tower is 0.0005MPa-0.1MPa.
7. the separation method of polymethoxy dimethyl ether according to claim 1, is characterized in that comprising further: again participate in building-up reactions in synthesis system part light constituent isolated in step (2) and/or heavy constituent being circulated to polymethoxy dimethyl ether according to actual production demand.
8. the separation method of polymethoxy dimethyl ether according to any one of claim 1-4,6, it is characterized in that comprising further: by the alkali manipulation of regeneration in alkali cycling element adopted in preprocessing process and rectifying, and be back to pretreatment unit and alkali assists variable-pressure rectification unit to reuse.
9. be applied to the separation system of the polymethoxy dimethyl ether of method according to any one of claim 1-8, it is characterized in that comprising:
Be filled with the pretreatment unit containing alkali solid, at least for carrying out pre-treatment to the material containing DMMn, at least to remove solid impurity in described material, acid, water and formaldehyde;
The alkali comprising the rectifying tower of alkali environment assists variable-pressure rectification unit, at least for carrying out rectifying, to be separated with heavy constituent transformation by the light constituent in material to pretreated material input.
10. the separation system of polymethoxy dimethyl ether according to claim 9, is characterized in that comprising:
Alkali cycling element, in order to will be back to pretreatment unit after the alkali adopted in preprocessing process and rectifying manipulation of regeneration and alkali assists variable-pressure rectification unit to reuse.
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| CN109096064A (en) * | 2017-06-21 | 2018-12-28 | 中国石油化工股份有限公司 | The refining methd of polyoxymethylene dimethyl ethers |
| CN109096063A (en) * | 2017-06-21 | 2018-12-28 | 中国石油化工股份有限公司 | The method for purifying polyoxymethylene dimethyl ethers |
| CN109096065A (en) * | 2017-06-21 | 2018-12-28 | 中国石油化工股份有限公司 | The method of purification of polyoxymethylene dimethyl ethers |
| CN109096065B (en) * | 2017-06-21 | 2021-07-30 | 中国石油化工股份有限公司 | Purification method of polyoxymethylene dimethyl ether |
| CN109096064B (en) * | 2017-06-21 | 2021-09-03 | 中国石油化工股份有限公司 | Refining method of polyoxymethylene dimethyl ether |
| CN109096063B (en) * | 2017-06-21 | 2021-11-30 | 中国石油化工股份有限公司 | Method for purifying polyoxymethylene dimethyl ether |
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| CN116147286A (en) * | 2022-12-05 | 2023-05-23 | 广钢气体(广州)有限公司 | High-purity oxygen rectification control method and device thereof |
| CN116147286B (en) * | 2022-12-05 | 2024-01-12 | 广钢气体(广州)有限公司 | High-purity oxygen rectification control method and device thereof |
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