CN104628539B - The separation method and system of polymethoxy dimethyl ether - Google Patents
The separation method and system of polymethoxy dimethyl ether Download PDFInfo
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- CN104628539B CN104628539B CN201510058475.0A CN201510058475A CN104628539B CN 104628539 B CN104628539 B CN 104628539B CN 201510058475 A CN201510058475 A CN 201510058475A CN 104628539 B CN104628539 B CN 104628539B
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- C07—ORGANIC CHEMISTRY
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- C07C41/00—Preparation of ethers; Preparation of compounds having groups, groups or groups
- C07C41/48—Preparation of compounds having groups
- C07C41/58—Separation; Purification; Stabilisation; Use of additives
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Abstract
A kind of polymethoxy dimethyl ether（DMMn）Separation method and system.The separation method includes：（1）Material input containing DMMn is filled with to the pretreatment unit of the solid containing alkali, to remove solid impurity, acid, water and the formaldehyde in the material；（2）By material after pretreatment input alkali auxiliary variable-pressure rectification unit, light, the heavy constituent transformation in material are separated in the rectifying column of alkali environment.Preferably, step（2）Including：It is 0.0002MPa 0.2MPa to control the pressure in rectifying column, and the pressure in rectifying column is set to drop to relatively low pressure from relatively high pressure in each separation circulation, and after each separation circulation terminates, the pressure in rectifying column is recovered to relatively high pressure, then carry out next separation circulation.The piece-rate system includes pretreatment unit, alkali auxiliary variable-pressure rectification unit etc..DMMn one pack system can be efficiently isolated by the present invention, and technique is simply controllable, can run steadily in the long term, while the equipment used is simple, is easily manipulated, it is green.
Description
Technical field
The present invention is more particularly directed to the separating technology and system of a kind of polymethoxy dimethyl ether (DMMn).
Background technology
Polymethoxy dimethyl ether CH3O(CH2O)nCH3(3≤n≤8, also known as DMMn) are a kind of new bavins of clean environment firendly
Oil additive, because its physicochemical property and traditional diesel oil are sufficiently close to, it is blended with diesel oil and burnt, combustion can be effectively improved
Efficiency is burnt, and reduces the discharge of soot.The blending performance of polymethoxy dimethyl ether and diesel oil is good, can dissolve each other, and has
Self lubricity, diesel oil mechanical life can be extended.
DMMn can also be as a kind of new Alternative Diesel Fuel simultaneously.US7235113B2, EP1422285B1 etc. are special
Sharp document proposes, with the complete diesel oil substitute of polymethoxy dimethyl ether a hundred per cent, as a kind of new alternative fuel, leads to
Cross and a certain proportion of compounding is carried out to the acetal of different polymerization degree, obtain can be directly used for the alternative fuel of internal combustion engine.Work as use
During the fuel of consisting of：
DMM2, CH3O(CH2O)2CH3：45% (mass fraction)
DMM3, CH3O(CH2O)3CH3：28% (mass fraction)
DMM4, CH3O(CH2O)4CH3：15% (mass fraction)
DMM5, CH3O(CH2O)5CH3：8% (mass fraction)
DMM6, CH3O(CH2O)6CH3：4% (mass fraction)
When engine speed is 500rpm, NOx discharge is:1.2g/kwh；Particulate matter (PM) discharge capacity is:0.001g/
kwh；Hydrocarbon:0.3g/kwh, content are less than Europe V standards (Euro V limit).
In order to adapt to the blending of different ratio or compound actual conditions, it is necessary to the different DMM of the degree of polymerizationnProduct, therefore
To DMMnIt is necessary to carry out plant-scale separation.And the product of different polymerization degree can also be used as synthetic intermediate, special type
Solvent etc., thus good separating technology has great importance for follow-up application.
Refer to table 1, DMMnProduct is a series of different homologue to dissolve each other of degree of polymerization, and they have very on boiling point
Wide distribution.Wherein, DMM1 is easy to volatilize, and more than DMM5 then has higher boiling point.And due to DMMn acid or
May occur in which under the slightly sour situation of person, during heating depolymerization reaction and may with the generation of white polymer solid, prevent separation from
Carry out.Thus, industry is thirsted for developing a kind of separating technology of efficient, stable polymethoxy dimethyl ether for a long time always.
Table 1DMMnThe property such as molten, boiling point
| Compound | Fusing point/DEG C | Boiling point/DEG C | Cetane number | Oxygen content % |
| 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 |
The content of the invention
It is a primary object of the present invention to provide it is a kind of efficiently, the separation method of stable polymethoxy dimethyl ether, with gram
Take the deficiencies in the prior art.
To realize aforementioned invention purpose, the technical solution adopted by the present invention includes：
A kind of separation method of polymethoxy dimethyl ether (DMMn), including：
(1) pretreatment unit that the material input containing DMMn is filled with to the solid containing alkali is pre-processed, at least to remove
Solid impurity, acid, water and the formaldehyde gone in the material；
(2) material after pretreatment input alkali auxiliary variable-pressure rectification unit is subjected to rectifying, with the rectifying column of alkali environment
Light component in material is separated with heavy constituent transformation.
Further, the solid containing alkali being filled in pretreatment unit includes NaOH, Na2CO3、KOH、CaO、Na2SO3、
K2CO3, any of activated carbon or two or more combinations, but not limited to this.
More preferable, the solid bag containing alkali contains CaO and/or Na2SO3。
Further, step (2) includes：By material after pretreatment input alkali auxiliary variable-pressure rectification unit, and with essence
The column plate contact of the alkaline filler or basification in tower is evaporated, after multistage vapor-liquid separation, is distinguished at various pressures
Light component, heavy constituent are obtained from rectifying column tower top, bottom of towe.
Further, for form the alkaline filler or for column plate carry out basification alkali include NaOH,
Na2CO3、KOH、K2CO3、Ca(OH)2、CaO、CaCO3Any of or two or more combinations, but not limited to this.
More preferable, the alkaline filler is at least selected from mainly by stainless steel cloth and the Na of granulation2CO3、CaO、
CaCO3One or both of particle it is formed above load in mixture filler, with molten containing any of Na, K, Ca or two or more
The dumped packing of liquid coating or structured packing.
As more one of preferred embodiment, step (2) includes：It is 0.0002MPa- to control the pressure in rectifying column
0.2MPa, and pressure in rectifying column is dropped to relatively low pressure from relatively high pressure, and
After at least one separation circulation terminates, the pressure in rectifying column is recovered to relatively high pressure, then carries out next separation circulation.
Particularly preferably, step (2) includes：It is 0.0005MPa-0.1MPa to control the pressure in rectifying column.
As more one of preferred embodiment, the separation method further may also include：It will be separated in step (2)
The part light component and/or heavy constituent gone out is recycled in the synthesis system of polymethoxy dimethyl ether again according to actual production demand
Secondary participation synthetic reaction.
As more one of preferred embodiment, the separation method further may also include：By preprocessing process and
The alkali used in distillation process regeneration treatment in alkali cycling element, and it is back to pretreatment unit and alkali auxiliary variable-pressure rectification list
Member reuses.
Present invention also offers a kind of polymethoxy dimethyl ether piece-rate system applied to foregoing separation method, it includes：
The pretreatment unit of the solid containing alkali is filled with, is at least used to pre-process the material containing DMMn, with least
Remove solid impurity, acid, water and the formaldehyde in the material；
Rectifying column comprising alkali environment alkali auxiliary variable-pressure rectification unit, at least be used for pretreated material is inputted into
Row rectifying, the light component in material is separated with heavy constituent transformation.
As more one of preferred embodiment, the piece-rate system may also include alkali cycling element, that will locate in advance
Pretreatment unit and alkali auxiliary variable-pressure rectification unit are back to after the alkali regeneration treatment used in reason process and distillation process again
Use.
In the separation method of the polymethoxy dimethyl ether of the present invention, by introducing alkali in separation process, it can suppress
DMMn decomposition, and destroy the azeotropic of constituent part so that separation is easier, meanwhile, by using transformation process, Ke Yifen
The various ingredients of wide boiling spread are separated out, and heat sensitive components are distillated at low pressures.
Compared with prior art, the present invention at least has the following advantages that：The separation method of the polymethoxy dimethyl ether can be with
The efficient one pack system for isolating DMMn, and technique is simply controllable, and can run steadily in the long term, while the equipment used is simple,
It is easily manipulated, it is green.
Brief description of the drawings
Technical scheme in order to illustrate the embodiments of the present invention more clearly, make required in being described below to embodiment
Accompanying drawing is briefly described, it should be apparent that, the accompanying drawing for the present invention in describing below is only the one of the present invention
A little embodiments, for those of ordinary skill in the art, can also be attached according to these on the premise of creation work is not paid
Figure obtains other accompanying drawings.
Fig. 1 is a kind of separating technology schematic diagram of polymethoxy dimethyl ether among a typical embodiments of the invention；
Fig. 2 is a kind of structural representation of the piece-rate system of polymethoxy dimethyl ether among a preferable case study on implementation of the invention
Figure.
Embodiment
As it was previously stated, in view of prior art has many deficiencies, inventor is able to through studying for a long period of time and largely putting into practice
Technical scheme is proposed, is illustrated as follows.
One aspect of the present invention mainly provides a kind of polymethoxy dimethyl ether separating technology efficiently, stable, more really
That cuts says, is a kind of DMMn isolations technique.
As shown in fig.1, among the typical embodiments of the present invention, polymethoxy dialkyl ether DMMn separation
Technique may include steps of：
(1) material containing DMMn removes the components such as acid, water, formaldehyde after pretreatment unit after reacting；
Further, process is as follows in pretreatment unit：The material containing DMMn, which flows through, after reaction is filled with the pre- of alkali
Processor can remove most of acid, water, formaldehyde.Enter next unit after removing solid impurity.
Further, the solid containing alkali used in pretreatment unit can be NaOH, Na2CO3、KOH、CaO、
Na2SO3、K2CO3, activated carbon or the mixture containing above-mentioned substance.Optimization, wherein the alkali used is CaO and Na2SO3。
(2) pretreated material enters alkali auxiliary variable-pressure rectification unit (Alkali Aided Variable
Pressure Rectification, AAVPR), transformation isolates light component and heavy constituent in the rectifying column of alkali environment.More
Preferably, which part is light, heavy constituent can be recycled to reactor secondary response again according to produce reality；
Further, alkali is aided in variable-pressure rectification unit, the alkalescence that pretreated material enters in rectifying column, with tower
Filler or the column plate of basification contact, after multi-stage gas-liquid separates, at various pressures from tower top obtain light component,
Heavy constituent is obtained from bottom of towe.
Further, can be NaOH, Na for alkaline filler or for the alkali of basification2CO3、KOH、
K2CO3、Ca(OH)2、CaO、CaCO3.More preferably, the filler for rectifying is stainless steel cloth and the Na of granulation2CO3、
CaO、CaCO3Particle loads in mixture filler, either with the conventional dumped packing coated containing Na, K, Ca solution or structured packing.
Preferably, rectifying tower pressure interior force PabsFor 0.0002MPa-0.2MPa, drop to relatively low pressure from relatively high pressure, one
After individual separation circulation terminates, relatively high pressure is returned to again, enters back into next circulation.Further, more excellent pressure limit is
0.0005MPa-0.1MPa。
(3) alkali used during can be used by alkali cycling element regeneration cycle.
The alkali used in pretreatment and in distillation process is regenerated in alkali cycling element, and returns to pretreatment and essence
Unit is evaporated to reuse.
Another aspect of the present invention provides a kind of piece-rate system of polymethoxy dimethyl ether, mainly with the foregoing side of separation
Method, which coordinates, to be implemented, and it can include pretreatment unit, alkali auxiliary variable-pressure rectification unit, alkali cycling element etc..
Technical scheme is described in further detail below in conjunction with some embodiments and accompanying drawing.
Embodiment 1 is referred to shown in Fig. 2, a kind of DMMn alkali auxiliary variable-pressure rectification separating technology flow system of the present embodiment system
Specific implementation example.
Specifically, the technological process can include：First, by material to be separated from raw material storage tank through pipeline 1 by pump P1
Input in preprocessor and handle through pipeline 2, remove moisture, acid, formaldehyde, the filling anhydrous sodium sulfite in preprocessor with it is anhydrous
Calcium oxide, after processing, acid content is less than 0.001%, and water content is less than 0.1%, and formaldehyde is less than 0.1% (mass fraction).Place
Material after reason enters rectifying in alkali auxiliary variable-pressure rectification AAVPR units through pipeline 3, is obtained after rectifying from tower top (pipeline 5)
DMMn lighter fraction, heavy constituent from bottom of towe (pipeline 6) by discharging.The sodium sulfite and calcium oxide loaded in preprocessor, warp
Regenerated using drier is inputted through pipeline 7 after a period of time by pipeline 8 into alkali regenerator.Alkali aids in variable-pressure rectification
Partial alkaline component in AAVPR units after drier is dried in alkali regenerator through also being regenerated.
In the present embodiment, it is granulated in alkali auxiliary variable-pressure rectification AAVPR units using the stainless steel steel wire loaded in mixture with passing through
CaO-CaCO3Particle, rectifying column inner member is also through Ca (OH)2Coating.Unit is with pipeline except raw material storage tank and pump P1
Outside, it is necessary to be manufactured using alkali resistant materials.Can be from during rectifying tower pressure interior force Pabs drops to 0.001MPa from 0.1MPa
Tower top isolates DMM1, DMM2...DMM7 successively, and heavy constituent DMMn, n >=8 can be discharged from bottom of towe.
Embodiment 2 pre-processes example
10L is contained into mass fraction for acid 0.01%, water 1.5%, the DMMn of formaldehyde 5.3% material is with 100mL/min
Speed flow through and be filled with the preprocessor of anhydrous CaO, activated carbon after, filter off solid impurity, after testing, acid content is less than
0.001%, water content is less than 0.015%, and formaldehyde is less than 0.1% (mass fraction).
Embodiment 3 pre-processes example
10L is contained into mass fraction for acid 0.015%, water 1.0%, the DMMn of formaldehyde 2.8% material is with 100mL/min
Speed flow through and be filled with anhydrous CaO, anhydrous Na2SO3、K2CO3, NaOH preprocessor after, filter off solid impurity, through inspection
Survey, acid content is less than 0.001%, and water content is less than 0.01%, and formaldehyde is less than 0.1% (mass fraction).
Embodiment 4 pre-processes example
10L is contained into mass fraction for acid 0.015%, water 1.0%, the DMMn of formaldehyde 2.8% material is with 100mL/min
Speed flow through and be filled with KOH, anhydrous Na2SO3、K2CO3Preprocessor after, filter off solid impurity, after testing, acid content
Less than 0.001%, water content is less than 0.01%, and formaldehyde is less than 0.1% (mass fraction).
The rectifying example of embodiment 5
Pretreated material (composition is shown in Table 2) enters alkali auxiliary variable-pressure rectification tower, and tower inner member is with Ca (OH)2Slurries apply
Lead to N after covering2Powder and drying are blown away, stainless steel cloth and CaO, CaCO for being granulated are loaded in tower3Particle loads in mixture filler, equivalent tower
Plate number is about 50.It is 0.1MPa to control pressure tower, and reboiler heating and temperature control pushes up 30 DEG C of gas phase temperature at 60 DEG C, condensation temperature
Spend for 2 DEG C, reflux ratio control is 2, and tower top distillates DMM1 purity up to 98.5% under the conditions of this.
Table 2DMMn feed compositions
| DMM1 | DMM2 | DMM3 | DMM4 | DMM5 | DMM6 | DMM7 | DMM8 |
| 35.1% | 26.0% | 17.1% | 10.2% | 5.8% | 3.2% | 1.6% | 0.8% |
The rectifying example of embodiment 6
Rectifying column inner member is with Ca (OH)2, KOH and Na2CO3Lead to N after slurries coating2Powder and drying are blown away, is loaded in tower
Stainless steel cloth and CaO, the CaCO being granulated3、Na2CO3Particle loads in mixture filler, and the equivalent number of plates is about 50.In the base of embodiment 5
Pressure tower is reduced on plinth, is controlled in 0.04MPa, reboiler heating and temperature control pushes up 30 DEG C of gas phase temperature, condensation temperature at 80 DEG C
For 5 DEG C, reflux ratio control is 3, and tower top distillates DMM2 purity up to 99.0% under the conditions of this.
The rectifying example of embodiment 7
Stainless steel θ rings are immersed in containing Ca (OH)2、NaOH、CaCO3With Na2CO3Slurries in, after hanging dry, fill out
Loading in rectifying column, the equivalent number of plates is about 60, is purged in tower with inert nitrogen, pressure tower is reduced on the basis of embodiment 6,
Control is in 0.01MPa, and reboiler heating and temperature control pushes up 65 DEG C of gas phase temperature at 150 DEG C, and condensation temperature is 10 DEG C, reflux ratio
Control as 3, tower top distillates DMM3 purity up to 99.9% under the conditions of this.
The rectifying example of embodiment 8
Metal perforated plate perforated plate corrugated filler is immersed in containing Ca (OH)2、CaCO3With K2CO3Slurries in, after hanging do
It is dry, it is filled into rectifying column, the equivalent number of plates is about 30, is purged in tower with inert nitrogen, tower is reduced on the basis of embodiment 7
Pressure, controlling in 0.005MPa, reboiler heating and temperature control pushes up 100 DEG C of gas phase temperature at 185 DEG C, and condensation temperature is 20 DEG C,
Reflux ratio control is 5, and tower top distillates DMM4 purity up to 99.9% under the conditions of this.
The rectifying example of embodiment 9
Stainless steel θ rings are immersed in containing Ca (OH)2、NaOH、CaCO3With Na2CO3Slurries in, after hanging dry, fill out
Loading in rectifying column, the equivalent number of plates is about 60, is purged in tower with inert nitrogen, pressure tower is reduced on the basis of embodiment 8,
Control is in 0.002MPa, and reboiler heating and temperature control pushes up 120 DEG C of gas phase temperature at 250 DEG C, and condensation temperature is 20 DEG C, backflow
It is 5 than control, tower top distillates DMM5 purity up to 99.9% under the conditions of this.
The rectifying example of embodiment 10
Stainless steel θ rings are immersed in containing Ca (OH)2、NaOH、CaCO3With Na2CO3Slurries in, after hanging dry, fill out
Loading in rectifying column, the equivalent number of plates is about 60, is purged in tower with inert nitrogen, pressure tower is reduced on the basis of embodiment 9,
Control is in 0.0015MPa, and reboiler heating and temperature control pushes up 170 DEG C of gas phase temperature at 320 DEG C, and condensation temperature is 30 DEG C, backflow
It is 2 than control, tower top distillates DMM6 purity up to 99.5% under the conditions of this.
The rectifying example of embodiment 11
Stainless steel θ rings are immersed in containing Ca (OH)2、NaOH、CaCO3With Na2CO3Slurries in, after hanging dry, fill out
Load in rectifying column, the equivalent number of plates is about 60, is purged in tower with inert nitrogen, and tower pressure is reduced on the basis of embodiment 10
Power, control in 0.0005MPa, reboiler heating and temperature control is pushed up 200 DEG C of gas phase temperature, condensation column cap insulation, returned at 360 DEG C
Stream is 2 than control, and tower top distillates DMM7 purity up to 99.2% under the conditions of this, and bottom of towe discharging is DMM8, purity 98.0%.
The alkali collection example of embodiment 12
The CaO of certain batch runnability decline, Mixture of Activated Carbon are unloaded, after CaO, activated carbon screening, CaO exists
After 110 DEG C of dry 24h, calcining 6h is carried out, temperature is set as 900 DEG C.Will be restorative after 100 DEG C of vacuum drying 50h of activated carbon
Energy.
Comparative example 1
The rectifying column (the equivalent number of plates is about 60) loaded with stainless steel θ rings, after being purged with inert nitrogen in tower, will not have
It is directly inputted to by the material to be separated (material composition is shown in Table 3) of preprocessor in rectifying column and carries out rectifying.Control pressure tower
For 0.1MPa, reboiler heating and temperature control pushes up 30 DEG C of gas phase temperature at 60 DEG C, condensation temperature is 2 DEG C, and reflux ratio control exists
2, after part DMM1 is isolated, the visible muddiness of bottom of towe.There is white solid condensation in overhead condenser, it is difficult to continue behind separation
DMM2-8 components.
The feed composition of the comparative example 1 of table 3
| 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
The rectifying column (the equivalent number of plates is about 60) loaded with stainless steel θ rings, after being purged with inert nitrogen in tower, it will pass through
The pretreated material of preprocessor (composition is shown in table 2 in embodiment 5), which is input in rectifying column, carries out rectifying.The pressure tower is controlled to be
0.1MPa, reboiler heating and temperature control push up 30 DEG C of gas phase temperature at 60 DEG C, and condensation temperature is 2 DEG C, and reflux ratio is controlled 2.Can
To isolate DMM1 from tower top, purity is more than 98.5%.But continue to run with, after tower top isolates part DMM2, bottom of towe becomes
Muddiness, and finally become stock white liquid.It is difficult to separate follow-up DMM3-8 components.
It is summarized, DMMn separating technologies of the invention at least have the advantages that：(1) transformation process is adapted to width
The various ingredients of boiling spread；(2) thermal decomposition of high boiling component is avoided；(4) rectifying of alkali auxiliary is inhibited in distillation process
DMMn acid decomposition；(5) the DMMn purity that the technique is isolated is very high；(6) reuse after alkali can regenerate, it is green.
It is obvious to a person skilled in the art that the invention is not restricted to the details of above-mentioned one exemplary embodiment, Er Qie
In the case of without departing substantially from spirit or essential attributes of the invention, the present invention can be realized in other specific forms.Therefore, no matter
From the point of view of which point, embodiment all should be regarded as exemplary, and be nonrestrictive, the scope of the present invention is by appended power
Profit requires rather than described above limits, it is intended that all in the implication and scope of the equivalency of claim by falling
Change is included in the present invention.
Moreover, it will be appreciated that although the present specification is described in terms of embodiments, not each embodiment is only wrapped
Containing an independent technical scheme, this narrating mode of specification is only that those skilled in the art should for clarity
Using specification as an entirety, the technical solutions in the various embodiments may also be suitably combined, forms those skilled in the art
It is appreciated that other embodiment.
Claims (9)
- A kind of 1. separation method of polymethoxy dimethyl ether, it is characterised in that including：(1) pretreatment unit that the material input containing DMMn is filled with to the solid containing alkali is pre-processed, at least to remove institute Solid impurity, acid, water and the formaldehyde in material are stated, the solid containing alkali is selected from NaOH, Na2CO3、KOH、CaO、Na2SO3、K2CO3 Any of or two or more combinations；(2) by material after pretreatment input alkali auxiliary variable-pressure rectification unit, and with the alkaline filler or alkali in rectifying column Change the column plate contact of processing, after multistage vapor-liquid separation, obtained gently from rectifying column tower top, bottom of towe respectively at various pressures Component, heavy constituent, the pressure wherein in rectifying column are controlled as 0.0002MPa-0.2MPa, and at least one separation circulation The pressure in rectifying column is inside set to drop to relatively low pressure from relatively high pressure, and after at least one separation circulation terminates, by essence The pressure evaporated in tower is recovered to relatively high pressure, then carries out next separation circulation.
- 2. the separation method of polymethoxy dimethyl ether according to claim 1, it is characterised in that：The solid containing alkali is selected from CaO and/or Na2SO3。
- 3. the separation method of polymethoxy dimethyl ether according to claim 1, it is characterised in that：Filled out for forming the alkalescence Material or the alkali for carrying out basification to column plate are selected from NaOH, Na2CO3、KOH、K2CO3、Ca(OH)2、CaO、CaCO3In Any one or more combinations.
- 4. the separation method of polymethoxy dimethyl ether according to claim 1, it is characterised in that：The alkaline filler is selected from master Will be by stainless steel cloth and the Na of granulation2CO3、CaO、CaCO3One or both of particle it is formed above load in mixture filler, or The dumped packing or structured packing that person coats containing any of Na, K, Ca or two or more solution.
- 5. the separation method of polymethoxy dimethyl ether according to claim 1, it is characterised in that step (2) includes：Control essence It is 0.0005MPa-0.1MPa to evaporate the pressure in tower.
- 6. the separation method of polymethoxy dimethyl ether according to claim 1, it is characterised in that also include：By in step (2) The part light component and/or heavy constituent isolated are recycled to the synthesis system of polymethoxy dimethyl ether according to actual production demand Synthetic reaction is inside participated in again.
- 7. according to the separation method of polymethoxy dimethyl ether any one of claim 1-6, it is characterised in that also include：Will The alkali used in preprocessing process and distillation process regeneration treatment in alkali cycling element, and it is back to pretreatment unit and alkali is auxiliary Variable-pressure rectification unit is helped to reuse.
- 8. the piece-rate system applied to the polymethoxy dimethyl ether of method any one of claim 1-7, it is characterised in that Including：The pretreatment unit of the solid containing alkali is filled with, is at least used to pre-process the material containing DMMn, at least to remove Solid impurity, acid, water and formaldehyde in the material；The alkali auxiliary variable-pressure rectification unit of rectifying column comprising alkali environment, is at least used to input pretreated material to carry out essence Evaporate, the light component in material is separated with heavy constituent transformation.
- 9. the piece-rate system of polymethoxy dimethyl ether according to claim 8, it is characterised in that including：Alkali cycling element, pretreatment unit will be back to after the alkali used in preprocessing process and distillation process regeneration treatment Reused with alkali auxiliary variable-pressure rectification unit.
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| 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 |
| 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 |
| CN108993497B (en) * | 2018-08-14 | 2021-05-28 | 中国科学院兰州化学物理研究所苏州研究院 | Nano ruthenium-carbon catalyst and preparation method and application thereof |
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| CN103772163B (en) * | 2012-10-18 | 2016-04-13 | 中国科学院兰州化学物理研究所 | The reactive system of continuous production polymethoxy dimethyl ether and processing method |
| 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) |
| CN203820659U (en) * | 2014-04-25 | 2014-09-10 | 北京旭阳化工技术研究院有限公司 | System for preparing polymethoxydimethyl ether |
| CN104003855B (en) * | 2014-05-21 | 2015-10-28 | 上海盘马化工工程技术有限公司 | Methyl alcohol is the system of initial reaction raw material continuous production polymethoxy dimethyl ether |
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