CN101362694A - Method for separating methanol and dimethyl carbonate azeotropic mixture - Google Patents
Method for separating methanol and dimethyl carbonate azeotropic mixture Download PDFInfo
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- CN101362694A CN101362694A CNA2008101452918A CN200810145291A CN101362694A CN 101362694 A CN101362694 A CN 101362694A CN A2008101452918 A CNA2008101452918 A CN A2008101452918A CN 200810145291 A CN200810145291 A CN 200810145291A CN 101362694 A CN101362694 A CN 101362694A
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- methanol
- screen membrane
- molecular screen
- methyl alcohol
- azeotropic mixture
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- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 title claims abstract description 161
- 238000000034 method Methods 0.000 title claims abstract description 37
- 239000000203 mixture Substances 0.000 title claims abstract description 21
- IEJIGPNLZYLLBP-UHFFFAOYSA-N dimethyl carbonate Chemical compound COC(=O)OC IEJIGPNLZYLLBP-UHFFFAOYSA-N 0.000 title claims description 15
- 239000012528 membrane Substances 0.000 claims abstract description 40
- 238000000926 separation method Methods 0.000 claims abstract description 39
- CXHHBNMLPJOKQD-UHFFFAOYSA-M methyl carbonate Chemical compound COC([O-])=O CXHHBNMLPJOKQD-UHFFFAOYSA-M 0.000 claims abstract description 29
- 239000002808 molecular sieve Substances 0.000 claims abstract description 16
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 claims abstract description 16
- 230000004087 circulation Effects 0.000 claims abstract description 6
- 239000011259 mixed solution Substances 0.000 claims abstract description 5
- 238000003795 desorption Methods 0.000 claims abstract description 3
- 238000011144 upstream manufacturing Methods 0.000 claims abstract description 3
- 238000009834 vaporization Methods 0.000 claims abstract description 3
- 230000008016 vaporization Effects 0.000 claims abstract description 3
- 239000000243 solution Substances 0.000 claims description 25
- 239000002243 precursor Substances 0.000 claims description 16
- 230000008595 infiltration Effects 0.000 claims description 11
- 238000001764 infiltration Methods 0.000 claims description 11
- 238000002156 mixing Methods 0.000 claims description 11
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 8
- 238000009833 condensation Methods 0.000 claims description 5
- 239000008367 deionised water Substances 0.000 claims description 5
- 229910021641 deionized water Inorganic materials 0.000 claims description 5
- 238000007789 sealing Methods 0.000 claims description 5
- 238000013019 agitation Methods 0.000 claims description 4
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 4
- 229910052782 aluminium Inorganic materials 0.000 claims description 4
- 239000004411 aluminium Substances 0.000 claims description 4
- 230000005494 condensation Effects 0.000 claims description 4
- 229910052710 silicon Inorganic materials 0.000 claims description 4
- 239000010703 silicon Substances 0.000 claims description 4
- 239000011734 sodium Substances 0.000 claims description 4
- 238000003786 synthesis reaction Methods 0.000 claims description 4
- 229910004298 SiO 2 Inorganic materials 0.000 claims description 3
- 230000032683 aging Effects 0.000 claims description 3
- 238000002425 crystallisation Methods 0.000 claims description 3
- 230000008025 crystallization Effects 0.000 claims description 3
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 3
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 3
- 235000019353 potassium silicate Nutrition 0.000 claims description 3
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 claims description 3
- ANBBXQWFNXMHLD-UHFFFAOYSA-N aluminum;sodium;oxygen(2-) Chemical compound [O-2].[O-2].[Na+].[Al+3] ANBBXQWFNXMHLD-UHFFFAOYSA-N 0.000 claims description 2
- 239000012153 distilled water Substances 0.000 claims description 2
- 229910001388 sodium aluminate Inorganic materials 0.000 claims description 2
- 230000008901 benefit Effects 0.000 abstract description 4
- 238000005265 energy consumption Methods 0.000 abstract description 4
- 239000000126 substance Substances 0.000 abstract description 4
- 238000009776 industrial production Methods 0.000 abstract description 2
- 239000012466 permeate Substances 0.000 abstract description 2
- 238000002360 preparation method Methods 0.000 abstract description 2
- 239000000463 material Substances 0.000 abstract 1
- 238000001704 evaporation Methods 0.000 description 7
- 230000008020 evaporation Effects 0.000 description 7
- 239000007788 liquid Substances 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 4
- 239000000047 product Substances 0.000 description 4
- 229910052680 mordenite Inorganic materials 0.000 description 3
- NIQCNGHVCWTJSM-UHFFFAOYSA-N Dimethyl phthalate Chemical compound COC(=O)C1=CC=CC=C1C(=O)OC NIQCNGHVCWTJSM-UHFFFAOYSA-N 0.000 description 2
- YGYAWVDWMABLBF-UHFFFAOYSA-N Phosgene Chemical compound ClC(Cl)=O YGYAWVDWMABLBF-UHFFFAOYSA-N 0.000 description 2
- 238000009835 boiling Methods 0.000 description 2
- 238000004364 calculation method Methods 0.000 description 2
- 238000007906 compression Methods 0.000 description 2
- 230000006835 compression Effects 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000004821 distillation Methods 0.000 description 2
- 239000003814 drug Substances 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 238000003912 environmental pollution Methods 0.000 description 2
- 238000000605 extraction Methods 0.000 description 2
- 239000012530 fluid Substances 0.000 description 2
- 230000004907 flux Effects 0.000 description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Natural products C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
- 238000005832 oxidative carbonylation reaction Methods 0.000 description 2
- 230000000149 penetrating effect Effects 0.000 description 2
- 235000021419 vinegar Nutrition 0.000 description 2
- 239000000052 vinegar Substances 0.000 description 2
- 239000003643 water by type Substances 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 241000370738 Chlorion Species 0.000 description 1
- QNLVXLJTOLHAMA-UHFFFAOYSA-N N=NC=NN.N=NC=NN.C(O)(O)=O Chemical compound N=NC=NN.N=NC=NN.C(O)(O)=O QNLVXLJTOLHAMA-UHFFFAOYSA-N 0.000 description 1
- TYUPOOPGJSZJAN-UHFFFAOYSA-N N=NC=NN.N=NC=NN.S(O)(O)(=O)=O Chemical compound N=NC=NN.N=NC=NN.S(O)(O)(=O)=O TYUPOOPGJSZJAN-UHFFFAOYSA-N 0.000 description 1
- 239000004809 Teflon Substances 0.000 description 1
- 229920006362 Teflon® Polymers 0.000 description 1
- 239000003905 agrochemical Substances 0.000 description 1
- 238000010533 azeotropic distillation Methods 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 125000002915 carbonyl group Chemical group [*:2]C([*:1])=O 0.000 description 1
- 230000006315 carbonylation Effects 0.000 description 1
- 238000005810 carbonylation reaction Methods 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000018044 dehydration Effects 0.000 description 1
- 238000006297 dehydration reaction Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- FBSAITBEAPNWJG-UHFFFAOYSA-N dimethyl phthalate Natural products CC(=O)OC1=CC=CC=C1OC(C)=O FBSAITBEAPNWJG-UHFFFAOYSA-N 0.000 description 1
- 229960001826 dimethylphthalate Drugs 0.000 description 1
- ROORDVPLFPIABK-UHFFFAOYSA-N diphenyl carbonate Chemical compound C=1C=CC=CC=1OC(=O)OC1=CC=CC=C1 ROORDVPLFPIABK-UHFFFAOYSA-N 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000004134 energy conservation Methods 0.000 description 1
- 239000012847 fine chemical Substances 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 238000004508 fractional distillation Methods 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 238000004817 gas chromatography Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 238000002955 isolation Methods 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 238000006198 methoxylation reaction Methods 0.000 description 1
- 125000005911 methyl carbonate group Chemical group 0.000 description 1
- XMJHPCRAQCTCFT-UHFFFAOYSA-N methyl chloroformate Chemical group COC(Cl)=O XMJHPCRAQCTCFT-UHFFFAOYSA-N 0.000 description 1
- 238000007069 methylation reaction Methods 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 238000005373 pervaporation Methods 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 231100000004 severe toxicity Toxicity 0.000 description 1
- 229920002379 silicone rubber Polymers 0.000 description 1
- 239000004945 silicone rubber Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 229920001169 thermoplastic Polymers 0.000 description 1
- 239000004416 thermosoftening plastic Substances 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
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- Separation Using Semi-Permeable Membranes (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention provides a new method for separating azeotropic mixture of methanol and methyl carbonate. The invention is characterized in that the mixed solution of methanol and methyl carbonate is supplied in circulation at the upstream side of molecular sieve membrane, and the downstream side of the molecular sieve membrane is connected to a vacuum system. As the molecular sieve membrane has the very high permselectivity for methanol, methanol in mixed solution preferentially permeates through the molecular sieve membrane, and vaporization and desorption are carried out at the downstream side of membrane, and then methanol is condensed and collected by the vacuum system. After multiple circulations, the mixed solution can achieve the complete separation of methanol and methyl carbonate. Compared with the traditional rectification method, the method of the invention has advantages of low energy consumption, no pollution, compact device, high separation efficiency, and the like, and has a very important meaning for industrial production of methyl carbonate and the preparation of other organic chemical materials by using methyl carbonate.
Description
Technical field
The invention provides the novel method of a kind of separation of methanol and dimethyl carbonate azeotropic mixture, belong to the separation technology field of methylcarbonate
Background technology
Carbonic acid diformazan vinegar (dimethyl carbonate, be called for short DMC) be a kind of novel green Chemicals of domestic and international chemical circles extensive concern over past ten years, can utilize it to carry out carbonylation, carbonyl methoxylation and methylation reaction, can replace widely used hypertoxicity phosgene, chloroformic acid methyl alcohol and sulfuric acid diformazan vinegar, be called as the new matrix of field " 21 century organic synthesis ".It all has extensive use in agricultural chemicals, medicine, Polymer Synthesizing, fuel dope and solvent.Early stage methylcarbonate (DMC) mainly is synthetic by phosgene route, because the corrodibility of unstripped gas severe toxicity and chlorion has limited scale operation and the application of DMC.The industrial process of carbon current dimethyl phthalate mainly adopts liquid phase oxidative carbonylation of methanol method, gas-phase methanol oxidative carbonylation method and ester-interchange method etc.But no matter adopt which kind of method, initial resulting thick product is the mixture of DMC-MeOH.Because methyl alcohol and methylcarbonate form binary azeotrope, common separation method is difficult to reach the requirement of product separation, and the separation of DMC directly affects the economic benefit of whole factory, and is therefore particularly important to the research of DMC-MeOH azeotrope separation method.The method of the separation DMC-MeOH binary azeotrope of having reported has the crystallizing process under low temperature, membrane separation process, azeotropic distillation, compression rectification method and extraction fractional distillation etc.At present external manufacturer separates DMC-MeOH azeotrope by extracting rectifying or compression rectification.Rectificating method is used for the separation of azeotropic mixture, has that energy consumption height, operating unit are many, the adding of extraction agent and entrainer causes quality product to reduce and problems such as environmental pollution easily.
Infiltration evaporation (Pervaporation is called for short PV) is a kind of new membrane isolation technique, and it is the novel process of a kind of high-level efficiency, less energy-consumption, less investment.Its separation principle is not subjected to the restriction of thermodynamic(al)equilibrium, depends primarily on the interaction between film and the penetrant component, is particularly suitable for that distillation method is difficult to separate or the separation of indissociable nearly boiling point, constant boiling mixture and isomers.Separate with traditional rectification method and to compare, the infiltration evaporation membrane separation process can energy-conservation 1/2～1/3, process cost is 50% of traditional rectification method technology, and can avoid product and environmental pollution, have significantly economically separating of organism and organic mixture removing in dehydration of organic solvent, the water, in the environmental protection and technical advantage.Have broad application prospects and market potential at industrial circles such as petrochemical complex, medicine, food, environmental protection, fine chemicals, be acknowledged as 21st century one of the most promising new and high technology.
Summary of the invention
The object of the present invention is to provide the novel method of a kind of separation of methanol and dimethyl carbonate azeotropic mixture, compare with traditional rectification method, this method has that energy consumption is low, pollution-free, compact, the separation efficiency advantages of higher of device.
The invention provides the novel method of a kind of separation of methanol and dimethyl carbonate azeotropic mixture, it is characterized in that the mixing solutions of methyl alcohol and methylcarbonate is supplied with in the upstream side circulation of molecular screen membrane, the downstream side of molecular screen membrane links to each other with vacuum system.Because molecular screen membrane has very high permselective property to methyl alcohol, molecular screen membrane is passed through in the preferential infiltration of the methyl alcohol in the mixing solutions, and at the downstream side of film vaporization desorption, reclaims through the vacuum system condensation.Mixing solutions is through repeatedly reaching separating fully of methyl alcohol and methylcarbonate after the circulation.
Said molecular screen membrane can be that all have optionally molecular screen membrane of penetrated preferably to methyl alcohol in the separation method provided by the invention, as NaY, NaX, T type, Mordenite, ZSM-5 types and Beta type etc., NaY contains the Na molecular screen membrane for the Y type, and NaX is for the X type contains the Na molecular screen membrane, Mordenite is a mordenite.
Said molecular screen membrane can be a tubulose in the separation method provided by the invention, also can be tabular.
Said NaY molecular screen membrane can prepare by the following method in the separation method provided by the invention:
(1) sodium aluminate, sodium hydroxide are dissolved in the precursor solution that obtains aluminium in the deionized water;
(2) water glass solution is mixed the precursor solution that obtains silicon with deionized water;
(3) under the high degree of agitation, the precursor solution of aluminium is added drop-wise in the precursor solution of silicon, obtains the precursor colloidal sol of NaY molecular sieve, the mole of each component consists of: Na
2O:Al
2O
3: SiO
2: H
2O=22:1:25:990 handles this precursor colloidal sol ageing at room temperature 12 hours;
(4) with pre-coated NaY molecular sieve kind crystalline porous α-Al
2O
3Film pipe vertical fixing is in synthesis reaction vessel, and the two ends of film pipe are with the sealing of PTFE band, to prevent the growth of molecular sieve in the film pipe.The molecular sieve precursor colloidal sol of (3) gained is poured in the reactor, and sealing back crystallization in 100 ℃ of air dry ovens was handled 5 hours.After the molecular screen membrane pipe taking-up that obtains, fully wash to neutrality with distilled water, promptly get the molecular screen membrane of falling NaY 60 ℃ of dried overnight.
In the separation method provided by the invention in said methyl alcohol and the methylcarbonate mixing solutions content of methyl alcohol can be 1%-95%wt.
The temperature of said methyl alcohol and methylcarbonate mixed solution can be 25-75 ℃ in the separation method provided by the invention.
The vacuum tightness in said molecular screen membrane downstream side can be 200-400Pa in the separation method provided by the invention.
Methyl alcohol provided by the invention is compared with traditional distillation/rectificating method with the separation method of methylcarbonate, and it is outstanding to be characterised in that separation is not subjected to vapour-liquid equilibrated restriction, can realize separating fully of methyl alcohol and methylcarbonate.For the industrial production of methylcarbonate and prepare other Organic Chemicals such as diphenyl carbonate etc. by methylcarbonate and all have very important significance.
Description of drawings
Fig. 1 is the synoptic diagram of methyl alcohol provided by the invention and methylcarbonate infiltration evaporation tripping device
Fig. 2 is the infiltration evaporation separating resulting of methyl alcohol and methylcarbonate (50%/50%) mixture under the differing temps
Embodiment
Separation method to methyl alcohol of the present invention and methylcarbonate is elaborated by the following examples
The preparation of embodiment 1 NaY molecular screen membrane
With 38.01 gram sodium hydroxide and 8.54 gram NaAlO
2Be dissolved in the 236.9 gram deionized waters, obtain solution A; With 188.55 gram water glass (SiO
2Content 27.3%) mix with 245.7 gram deionized waters, obtain solution B.Under high degree of agitation, solution A is dripped in the solution B, obtain the precursor colloidal sol of NaY molecular sieve.Continue high degree of agitation after 2 hours, ageing at room temperature 12 hours.With the α-Al of precoating with NaY molecular sieve crystal seed
2O
3Film pipe (external diameter 13mm, wall thickness 2mm, length 35cm, mean pore size 1.0 μ m, porosity 38%) two ends are vertically fixed in the synthesis reaction vessel after with PTFE band sealing, and molecular sieve precursor colloidal sol is transferred in the reactor, and crystallization was handled 5 hours in preheating 100 ℃ air dry oven.After reaction finishes, the molecular screen membrane pipe is taken out, to neutral, be drying to obtain the molecular screen membrane of falling NaY at 60 ℃ at last with the deionized water thorough washing.
Embodiment 2 methyl alcohol separate with the infiltration evaporation of methylcarbonate
Figure one is methyl alcohol and the isolating infiltration evaporation tripping device of the methylcarbonate synoptic diagram among the present invention.NaY molecular screen membrane pipe places stainless assembly, and an end links to each other with a bit of teflon rod, and the other end links to each other with vacuum system, and two ends seal successively with silicone rubber tube and thermoplastic tube respectively, the outer wrap heating zone of assembly.The stock liquid that is heated to 50 ℃ in thermostatic bath is by the liquor pump supply that circulates in assembly, infiltration steam liquid N
2Condensation is reclaimed, and two cold-traps switch use to guarantee continuously measured.The penetrating fluid scales/electronic balance weighing that condensation is collected, the concentration of stock liquid and penetrating fluid is used the gas-chromatography detection by quantitative respectively.Separation performance is mainly by permeation flux Q (kg/m
2H) and separation factor α represent that wherein permeation flux Q represents the size by the infiltration capacity of film, method of calculation are quality/(unit time * membrane area) of the penetrant that the per-meate side condensation is collected in the unit time.Separation factor is represented the height of the separation efficiency of methyl alcohol and methylcarbonate, and method of calculation are α=(Y
CH3OH/ Y
DMC)/(X
CH3OH/ X
DMC), wherein Y and X represent the mass concentration of methyl alcohol and methylcarbonate in penetrant and the stock liquid respectively.Separate the methyl alcohol and the methylcarbonate mixing solutions of different concns with the NaY molecular screen membrane of embodiment 1 gained, separating resulting is as shown in table 1.Methyl alcohol and methylcarbonate (50/50wt%) mixing solutions separating resulting is seen figure two under the differing temps.As can be seen, by NaY molecular sieve film pervasion vaporescence, can well realize separating of methyl alcohol and dimethyl carbonate azeotropic mixture.
The infiltration evaporation separating resulting of table one, different concns methyl alcohol and methylcarbonate mixing solutions
Claims (8)
1. the method for separation of methanol and dimethyl carbonate azeotropic mixture is characterized in that the mixing solutions of methyl alcohol and methylcarbonate is supplied with in the upstream side circulation of molecular screen membrane, and the downstream side of molecular screen membrane links to each other with vacuum system; Because molecular screen membrane has very high permselective property to methyl alcohol, molecular screen membrane is passed through in the preferential infiltration of the methyl alcohol in the mixing solutions, and at the downstream side of film vaporization desorption, reclaims through the vacuum system condensation; Mixing solutions is through repeatedly reaching separating fully of methyl alcohol and methylcarbonate very soon after the circulation.
2. according to the method for described separation of methanol of claim 1 and dimethyl carbonate azeotropic mixture, it is characterized in that
Molecular screen membrane can be that all have optionally molecular screen membrane of penetrated preferably to methyl alcohol.
3. according to the method for described separation of methanol of claim 1 and dimethyl carbonate azeotropic mixture, it is characterized in that molecular screen membrane is NaA, NaY, NaX, T, Mordernite, ZSM-5 or Beta molecular screen membrane.
4. according to the method for described separation of methanol of claim 1 and dimethyl carbonate azeotropic mixture, it is characterized in that molecular screen membrane is tubulose or tabular.
5. according to the method for described separation of methanol of claim 1 and dimethyl carbonate azeotropic mixture, the mass content that it is characterized in that methyl alcohol in methyl alcohol and the methylcarbonate mixing solutions is 5%-95%.
6. according to the method for described separation of methanol of claim 1 and dimethyl carbonate azeotropic mixture, it is characterized in that the temperature of methyl alcohol and methylcarbonate mixed solution is 25-75 ℃.
7. according to the method for described separation of methanol of claim 1 and dimethyl carbonate azeotropic mixture, the vacuum tightness in the molecular screen membrane downstream side that it is characterized in that is 200-400Pa.
8. according to the method for described separation of methanol of claim 3 and dimethyl carbonate azeotropic mixture, it is characterized in that the NaY molecular screen membrane can prepare by the following method:
(1) sodium aluminate, sodium hydroxide are dissolved in the precursor solution that obtains aluminium in the deionized water;
(2) water glass solution is mixed the precursor solution that obtains silicon with deionized water;
(3) under the high degree of agitation, the precursor solution of aluminium is added drop-wise in the precursor solution of silicon, obtains the precursor colloidal sol of NaY molecular sieve, the mole of each component consists of: Na
2O:Al
2O
3: SiO
2: H
2O=22:1:25:990 handles this precursor colloidal sol ageing at room temperature 12 hours;
(4) with pre-coated NaY molecular sieve kind crystalline porous α-Al
2O
3Film pipe vertical fixing is in synthesis reaction vessel, and the two ends of film pipe are with the sealing of PTFE band, to prevent the growth of molecular sieve in the film pipe; The molecular sieve precursor colloidal sol of (3) gained is poured in the reactor, and sealing back crystallization in 100 ℃ of air dry ovens was handled 5 hours; After the molecular screen membrane pipe taking-up that obtains, fully wash to neutrality with distilled water, promptly get the molecular screen membrane of falling NaY 60 ℃ of dried overnight.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2008101452918A CN101362694A (en) | 2007-08-03 | 2008-08-01 | Method for separating methanol and dimethyl carbonate azeotropic mixture |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200710049675.5 | 2007-08-03 | ||
| CN200710049675 | 2007-08-03 | ||
| CNA2008101452918A CN101362694A (en) | 2007-08-03 | 2008-08-01 | Method for separating methanol and dimethyl carbonate azeotropic mixture |
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|---|---|
| CN101362694A true CN101362694A (en) | 2009-02-11 |
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ID=40389327
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102921313A (en) * | 2012-11-05 | 2013-02-13 | 上海师范大学 | Hollow fiber composite film used for separating carbinol/ dimethyl carbonate mixture and preparation method and application thereof |
| CN103084076A (en) * | 2013-01-30 | 2013-05-08 | 上海师范大学 | Organic and inorganic hybrid hollow fiber pervaporation membrane for separating methanol/dimethyl carbonate mixture |
| CN103495342A (en) * | 2013-09-25 | 2014-01-08 | 北京钟华鼎盛节能技术有限公司 | Method for separating MEOH-DMC (methanol-dimethyl carbonate) through vapor permeation |
| CN103772202A (en) * | 2014-01-27 | 2014-05-07 | 南京工业大学 | Method for separating methanol-dimethyl carbonate azeotropic liquid |
| CN109053448A (en) * | 2018-10-19 | 2018-12-21 | 中国科学院山西煤炭化学研究所 | Separation method for pure and mild dimethyl carbonate mixture |
| CN111170863A (en) * | 2020-03-16 | 2020-05-19 | 天津市新天进科技开发有限公司 | Energy-saving process method and device for purifying dimethyl carbonate by adopting four-tower heat integration |
| CN111454152A (en) * | 2020-06-22 | 2020-07-28 | 东营市海科新源化工有限责任公司 | Preparation method and preparation device of electronic grade dimethyl carbonate |
| CN113634138A (en) * | 2021-08-23 | 2021-11-12 | 华东理工大学 | Dynamic hydrothermal synthesis hollow fiber outer wall SUZ-4 type molecular sieve pervaporation membrane and method for removing methanol by using solvent thereof |
| CN115572215A (en) * | 2022-10-24 | 2023-01-06 | 浙江汇甬新材料有限公司 | Separation method of methanol and dimethyl carbonate azeotrope by membrane separation coupled rectification |
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Cited By (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102921313A (en) * | 2012-11-05 | 2013-02-13 | 上海师范大学 | Hollow fiber composite film used for separating carbinol/ dimethyl carbonate mixture and preparation method and application thereof |
| CN102921313B (en) * | 2012-11-05 | 2015-07-15 | 上海师范大学 | Hollow fiber composite film used for separating carbinol/ dimethyl carbonate mixture and preparation method and application thereof |
| CN103084076A (en) * | 2013-01-30 | 2013-05-08 | 上海师范大学 | Organic and inorganic hybrid hollow fiber pervaporation membrane for separating methanol/dimethyl carbonate mixture |
| CN103084076B (en) * | 2013-01-30 | 2014-12-10 | 上海师范大学 | Organic and inorganic hybrid hollow fiber pervaporation membrane for separating methanol/dimethyl carbonate mixture |
| CN103495342B (en) * | 2013-09-25 | 2016-01-20 | 北京钟华鼎盛节能技术有限公司 | A kind of Steam soak is separated the method for MEOH-DMC |
| CN103495342A (en) * | 2013-09-25 | 2014-01-08 | 北京钟华鼎盛节能技术有限公司 | Method for separating MEOH-DMC (methanol-dimethyl carbonate) through vapor permeation |
| CN103772202A (en) * | 2014-01-27 | 2014-05-07 | 南京工业大学 | Method for separating methanol-dimethyl carbonate azeotropic liquid |
| CN109053448A (en) * | 2018-10-19 | 2018-12-21 | 中国科学院山西煤炭化学研究所 | Separation method for pure and mild dimethyl carbonate mixture |
| CN111170863A (en) * | 2020-03-16 | 2020-05-19 | 天津市新天进科技开发有限公司 | Energy-saving process method and device for purifying dimethyl carbonate by adopting four-tower heat integration |
| CN111454152A (en) * | 2020-06-22 | 2020-07-28 | 东营市海科新源化工有限责任公司 | Preparation method and preparation device of electronic grade dimethyl carbonate |
| CN113634138A (en) * | 2021-08-23 | 2021-11-12 | 华东理工大学 | Dynamic hydrothermal synthesis hollow fiber outer wall SUZ-4 type molecular sieve pervaporation membrane and method for removing methanol by using solvent thereof |
| CN113634138B (en) * | 2021-08-23 | 2023-01-24 | 华东理工大学 | Dynamic hydrothermal synthesis hollow fiber outer wall SUZ-4 type molecular sieve pervaporation membrane and method for removing methanol by using solvent thereof |
| CN115572215A (en) * | 2022-10-24 | 2023-01-06 | 浙江汇甬新材料有限公司 | Separation method of methanol and dimethyl carbonate azeotrope by membrane separation coupled rectification |
| CN115572215B (en) * | 2022-10-24 | 2024-04-30 | 浙江汇甬新材料有限公司 | Separation method of methanol and dimethyl carbonate azeotrope through coupling and rectification of membrane separation |
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