CN106588658A - Method of synthesizing dimethyl carbonate - Google Patents
Method of synthesizing dimethyl carbonate Download PDFInfo
- Publication number
- CN106588658A CN106588658A CN201611028332.6A CN201611028332A CN106588658A CN 106588658 A CN106588658 A CN 106588658A CN 201611028332 A CN201611028332 A CN 201611028332A CN 106588658 A CN106588658 A CN 106588658A
- Authority
- CN
- China
- Prior art keywords
- graphene oxide
- dimethyl carbonate
- catalyst
- synthesis
- methyl alcohol
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- IEJIGPNLZYLLBP-UHFFFAOYSA-N dimethyl carbonate Chemical compound COC(=O)OC IEJIGPNLZYLLBP-UHFFFAOYSA-N 0.000 title claims abstract description 32
- 238000000034 method Methods 0.000 title claims abstract description 21
- 230000002194 synthesizing effect Effects 0.000 title abstract 2
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims abstract description 46
- 239000003054 catalyst Substances 0.000 claims abstract description 37
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 32
- 229910021389 graphene Inorganic materials 0.000 claims abstract description 24
- KMTRUDSVKNLOMY-UHFFFAOYSA-N Ethylene carbonate Chemical compound O=C1OCCO1 KMTRUDSVKNLOMY-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000002041 carbon nanotube Substances 0.000 claims abstract description 13
- 229910021393 carbon nanotube Inorganic materials 0.000 claims abstract description 13
- 239000002994 raw material Substances 0.000 claims abstract description 3
- 230000015572 biosynthetic process Effects 0.000 claims description 17
- 238000003786 synthesis reaction Methods 0.000 claims description 17
- XTXRWKRVRITETP-UHFFFAOYSA-N Vinyl acetate Chemical compound CC(=O)OC=C XTXRWKRVRITETP-UHFFFAOYSA-N 0.000 claims description 12
- -1 carbon nano tube modified graphene Chemical class 0.000 claims description 12
- 238000006243 chemical reaction Methods 0.000 claims description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 11
- 229910052596 spinel Inorganic materials 0.000 claims description 7
- 239000011029 spinel Substances 0.000 claims description 7
- 238000006555 catalytic reaction Methods 0.000 claims description 6
- 239000008367 deionised water Substances 0.000 claims description 6
- 229910021641 deionized water Inorganic materials 0.000 claims description 6
- 229910052799 carbon Inorganic materials 0.000 claims description 3
- 239000003795 chemical substances by application Substances 0.000 claims description 3
- 230000035484 reaction time Effects 0.000 claims description 2
- 238000005034 decoration Methods 0.000 claims 2
- 239000002071 nanotube Substances 0.000 claims 1
- 238000004519 manufacturing process Methods 0.000 abstract description 4
- 229910002092 carbon dioxide Inorganic materials 0.000 description 11
- WQDUMFSSJAZKTM-UHFFFAOYSA-N Sodium methoxide Chemical group [Na+].[O-]C WQDUMFSSJAZKTM-UHFFFAOYSA-N 0.000 description 8
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 7
- 238000013019 agitation Methods 0.000 description 5
- 238000005119 centrifugation Methods 0.000 description 5
- 238000006073 displacement reaction Methods 0.000 description 5
- 239000000047 product Substances 0.000 description 5
- 238000010792 warming Methods 0.000 description 5
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 229910002804 graphite Inorganic materials 0.000 description 3
- 239000010439 graphite Substances 0.000 description 3
- 238000000926 separation method Methods 0.000 description 3
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 2
- 229960004424 carbon dioxide Drugs 0.000 description 2
- 230000003197 catalytic effect Effects 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 239000012065 filter cake Substances 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 150000003839 salts Chemical class 0.000 description 2
- 229910000029 sodium carbonate Inorganic materials 0.000 description 2
- VWDWKYIASSYTQR-UHFFFAOYSA-N sodium nitrate Chemical compound [Na+].[O-][N+]([O-])=O VWDWKYIASSYTQR-UHFFFAOYSA-N 0.000 description 2
- 238000000967 suction filtration Methods 0.000 description 2
- 231100000419 toxicity Toxicity 0.000 description 2
- 230000001988 toxicity Effects 0.000 description 2
- 238000002604 ultrasonography Methods 0.000 description 2
- 239000002699 waste material Substances 0.000 description 2
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- 241000446313 Lamella Species 0.000 description 1
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 description 1
- YGYAWVDWMABLBF-UHFFFAOYSA-N Phosgene Chemical compound ClC(Cl)=O YGYAWVDWMABLBF-UHFFFAOYSA-N 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 229910052783 alkali metal Inorganic materials 0.000 description 1
- 150000008044 alkali metal hydroxides Chemical class 0.000 description 1
- 229910000272 alkali metal oxide Inorganic materials 0.000 description 1
- 150000001340 alkali metals Chemical class 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000000903 blocking effect Effects 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 229910002090 carbon oxide Inorganic materials 0.000 description 1
- SIXOAUAWLZKQKX-UHFFFAOYSA-N carbonic acid;prop-1-ene Chemical compound CC=C.OC(O)=O SIXOAUAWLZKQKX-UHFFFAOYSA-N 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000013064 chemical raw material Substances 0.000 description 1
- 239000007809 chemical reaction catalyst Substances 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 235000009508 confectionery Nutrition 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 150000002148 esters Chemical group 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- 239000005457 ice water Substances 0.000 description 1
- 239000011229 interlayer Substances 0.000 description 1
- 150000002576 ketones Chemical class 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- CXHHBNMLPJOKQD-UHFFFAOYSA-M methyl carbonate Chemical compound COC([O-])=O CXHHBNMLPJOKQD-UHFFFAOYSA-M 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 150000007530 organic bases Chemical class 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 238000000066 reactive distillation Methods 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 239000002893 slag Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 239000004317 sodium nitrate Substances 0.000 description 1
- 235000010344 sodium nitrate Nutrition 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000002910 solid waste Substances 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 1
- 230000002459 sustained effect Effects 0.000 description 1
- 238000001291 vacuum drying Methods 0.000 description 1
- 239000003643 water by type Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C68/00—Preparation of esters of carbonic or haloformic acids
- C07C68/06—Preparation of esters of carbonic or haloformic acids from organic carbonates
- C07C68/065—Preparation of esters of carbonic or haloformic acids from organic carbonates from alkylene carbonates
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J21/00—Catalysts comprising the elements, oxides, or hydroxides of magnesium, boron, aluminium, carbon, silicon, titanium, zirconium, or hafnium
- B01J21/18—Carbon
- B01J21/185—Carbon nanotubes
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Nanotechnology (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Low-Molecular Organic Synthesis Reactions Using Catalysts (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention relates to a method of synthesizing dimethyl carbonate, wherein graphene oxide modified by carbon nano tubes is used as a catalyst and ethylene carbonate and methanol are used as raw material. The method is carried out in a high-pressure kettle at certain temperature and under certain pressure. The method has simple operation and high catalyst efficiency, is good in catalyst repeatability and can effectively reduce production cost of the dimethyl carbonate.
Description
Technical field
The present invention relates to the synthesis field of dimethyl carbonate, more particularly to a kind of CNT modified with graphene oxide
As the method for catalyst Synthesis of dimethyl carbonate.
Background technology
Dimethyl carbonate (Dimethyl Carbonate, DMC), is a kind of water white transparency, slightly smell, micro- sweet during normal temperature
Liquid, be insoluble in water, but can be with the almost all of immiscible organic solvent such as alcohol, ether, ketone.DMC toxicity was very low, in 1992
Just non-toxic product is classified as by Europe, is a kind of environmental protective type chemical raw material for meeting modern cleaning procedure requirement, therefore the synthesis of DMC
Technology receives the extensive attention of domestic and international chemical circles.
DMC initial production method is phosgenation, is succeeded in developing in 1918, but the toxicity of phosgene and corrosivity are limited
The application of this method, in particular with environmental protection by whole world attention degree increasingly raising, phosgenation is eliminated.
It is the most frequently used route of current industry by ethylene carbonate and methyl alcohol ester exchange Synthesis of dimethyl carbonate.Ester exchange
The catalyst system and catalyzing of reaction can be divided into homogeneous catalytic reaction and heterogeneous catalytic reaction, and at present both at home and abroad synthesis DMC is mainly logical
Homogeneous catalytic reaction system is crossed, reaction catalyst used has：Alkali metal oxide, alkali metal hydroxide, alkali metal alcoholates,
Alkali carbonate, alkaline metal oxalate, quaternary ammonium halides salt and organic base etc..Industrially by propene carbonate and methanol-fueled CLC
Catalyst used by dimethyl carbonate is sodium methoxide, but the use of sodium methoxide catalyst, there are many shortcomings, can summarize such as
Under：(1) consumption of catalyst is big, now industrial often to produce 1 ton of dimethyl carbonate, needs weight/mass percentage composition 25-30%'s
Sodium methoxide 80-110kg or so；(2) substantial amounts of waste residue is produced after catalyst failure, causes environmental pollution；(3) it is solid in catalysis system
The precipitation of body affects system quantity-produced stability, blocking pipeline and equipment, has a strong impact on the continuity of production；(4) into work
Skill is complicated, and in order to catalyst waste slag is removed from reaction mass system, solid waste is separated out when preventing rectifying, is attached to heat exchange
Device tubulation inner wall surface and it is attached on filler, adds desalted water from reactive distillation column tower reactor heavy constituent out and be passed through two
Carbonoxide, to make, then remaining catalyst sodium methoxide failure is changed into NaOH and carbon dioxide reaction is changed into inorganic salts carbon
Sour sodium, then sodium carbonate is filtered out by filter, this causes production technology extremely complex；(5) catalyst is unable to reuse, due to urging
Sodium carbonate inorganic salts are generated after agent failure, catalytic action is there is no longer.
Therefore, develop a kind of simple to operate, product and catalyst convenient separation, products obtained therefrom purity is high, and catalyst is reclaimed
And the method for the good Synthesis of dimethyl carbonate of multiplexing performance is highly significant.However, up to the present with graphene oxide as catalysis
Agent Synthesis of dimethyl carbonate is also without document report.
The content of the invention
The technical problem to be solved in the present invention is for current ethylene carbonate and methyl alcohol ester exchange Synthesis of dimethyl carbonate
During the catalyst usage amount that occurs it is big and separation and recovery of catalyst is difficult, the yield of product methyl-carbonate is more low to ask
Topic, there is provided a kind of simple to operate, catalyst efficiency is higher, product and catalyst convenient separation, catalyst is reclaimed and multiplexing performance
The method of good Synthesis of dimethyl carbonate.
In order to solve the above problems, following technical scheme is present invention employs：
Synthesis DMC methods of the present invention with carbon nano tube modified graphene oxide as catalyst, with ethylene carbonate
It is raw material with methyl alcohol, is reacted in autoclave.
Carbon nano tube modified graphene oxide catalyst is adopted and prepared with the following method：Graphene oxide and CNT are added
Enter in deionized water in room temperature ultrasound 2h, graphene oxide mass concentration in deionized water is 1%, is subsequently filtered, and is done
Dry, wherein graphene oxide and the mass ratio of CNT are 1:1-4:1.
The synthesis of dimethyl carbonate is carried out as follows：Sequentially add in autoclave a certain amount of methyl alcohol,
Ethylene carbonate and carbon nano tube modified graphene oxide, carbon nano tube modified graphene oxide catalyst amount is material carbon
The 1-3% of vinyl acetate quality, oxide spinel vinyl acetate is 1 with the mol ratio of methyl alcohol:2-1:10, use CO2In displacement autoclave
Air 2 times, then fill CO2To 0.5-1Mpa, magnetic agitation heating, 100-120 DEG C is warming up to, 4-6h is reacted at this temperature.Drop
To room temperature, centrifugation is extracted reaction solution, analyzed.
Wherein, described catalyst graphene oxide can be carried out in accordance with the following methods in the lab：
In ice-water bath, 5g crystalline flake graphites and 2.5g sodium nitrate are well mixed with the concentrated sulfuric acid of 115mL, it is slow in stirring
Add 15gKMnO4, less than 2 DEG C sustained responses 1h are kept, 35 DEG C of water-bath 30min are transferred them to, it is gradually added 250mL
Deionized water, temperature rises to 98 DEG C and continues to react after 1h, can substantially observe mixture by brown stain into glassy yellow.Further
Continuously it is diluted with water, and with the H of mass fraction 30%2O2Solution process.By above-mentioned solution suction filtration, washed with 5%HCl solution to
Neutrality, is put into filter cake in baking oven 80 DEG C and is fully drying to obtain graphite oxide.Take 0.1g graphite oxides and be put into 50mL deionized waters
In, ultrasonically treated 1.5h (180W, 60Hz) subsequently carries out suction filtration, filter cake is put into into 40 DEG C (10Pa) in vacuum drying oven and is dried 6h
Obtain final product required graphene oxide.
After above-mentioned technical scheme, the present invention achieves the effect of highly significant, with carbon nano tube modified oxidation
Graphene is catalyst, and energy consumption and cost are greatlyd save in the building-up process of dimethyl carbonate, and the reaction time shortens, reaction temperature
Degree is reduced, and catalyst amount is reduced.Graphene oxide interlayer compared with simple graphene oxide, Jing after carbon nano tube modified
Distance is substantially improved so that the oxygen-containing functional group of surface of graphene oxide be completely exposed with reaction system, therefore catalytic efficiency
It is substantially improved.Trace it to its cause, be because CNT is entered in the lamella of graphene oxide during modification.
Specific embodiment
The present invention will be described further with regard to following examples, however, it should be noted that these embodiments are only to illustrate
It is used, and is not necessarily to be construed as the restriction of present invention enforcement.
Carbon nano tube modified graphene oxide catalyst is prepared first：By graphene oxide and CNT be added to from
In room temperature ultrasound 2h in sub- water, graphene oxide mass concentration in deionized water is 1%, is subsequently filtered, and is dried, wherein oxygen
Graphite alkene is 1 with the mass ratio of CNT:1-4:1.Obtained catalyst is used in following specific embodiments.
Embodiment 1
Methyl alcohol, ethylene carbonate, wherein carbon nano tube modified graphene oxide, carbonic acid are sequentially added in autoclave
Vinyl acetate is 1 with the mol ratio of methyl alcohol:10, graphene oxide and the mass ratio of CNT are 1 in catalyst:1, catalyst is used
Measure as the 1% of oxide spinel vinyl acetate quality, use CO2Air 2 times in displacement autoclave, then fill CO2To 0.5Mpa, magnetic agitation
Heating, is warming up to 100 DEG C, and 6h is reacted at this temperature.Room temperature is down to, centrifugation is extracted reaction solution, is analyzed.Ethylene carbonate turns
Rate 82%, dimethyl carbonate selective 99%.
Embodiment 2
Methyl alcohol, ethylene carbonate, wherein carbon nano tube modified graphene oxide, carbonic acid are sequentially added in autoclave
Vinyl acetate is 1 with the mol ratio of methyl alcohol:10, graphene oxide and the mass ratio of CNT are 4 in catalyst:1, catalyst is used
Measure as the 3% of oxide spinel vinyl acetate quality, use CO2Air 2 times in displacement autoclave, then fill CO2To 1Mpa, magnetic agitation adds
Heat, is warming up to 100 DEG C, and 4h is reacted at this temperature.Room temperature is down to, centrifugation is extracted reaction solution, is analyzed.Ethylene carbonate is converted
Rate 85%, dimethyl carbonate selective 99%.
Embodiment 3
Methyl alcohol, ethylene carbonate, wherein carbon nano tube modified graphene oxide, carbonic acid are sequentially added in autoclave
Vinyl acetate is 1 with the mol ratio of methyl alcohol:2, graphene oxide and the mass ratio of CNT are 2 in catalyst:1, catalyst is used
Measure as the 2% of oxide spinel vinyl acetate quality, use CO2Air 2 times in displacement autoclave, then fill CO2To 1Mpa, magnetic agitation adds
Heat, is warming up to 120 DEG C, and 4h is reacted at this temperature.Room temperature is down to, centrifugation is extracted reaction solution, is analyzed.Ethylene carbonate is converted
Rate 90%, dimethyl carbonate selective 99%.
Embodiment 4
Methyl alcohol, ethylene carbonate, wherein carbon nano tube modified graphene oxide, carbonic acid are sequentially added in autoclave
Vinyl acetate is 1 with the mol ratio of methyl alcohol:8, graphene oxide and the mass ratio of CNT are 2 in catalyst:1, catalyst is used
Measure as the 2% of oxide spinel vinyl acetate quality, use CO2Air 2 times in displacement autoclave, then fill CO2To 1Mpa, magnetic agitation adds
Heat, is warming up to 120 DEG C, and 6h is reacted at this temperature.Room temperature is down to, centrifugation is extracted reaction solution, is analyzed.Ethylene carbonate is converted
Rate 94%, dimethyl carbonate selective 99%.
With the above-mentioned desirable embodiment according to the present invention as enlightenment, by above-mentioned description, relevant staff is complete
Entirely various change and modification can be carried out in the range of without departing from this invention technological thought.The technology of this invention
Property scope is not limited to the content on specification, it is necessary to its technical scope is determined according to right.
Claims (5)
1. a kind of method of Synthesis of dimethyl carbonate, it is characterised in that the method is with carbon nano tube modified graphene oxide as catalysis
Agent, with ethylene carbonate and methyl alcohol as raw material, is reacted in autoclave.
2. the method for a kind of Synthesis of dimethyl carbonate according to claim 1, it is characterised in that described CNT is repaiied
Decorations graphene oxide catalyst is adopted and prepared with the following method：Graphene oxide and CNT are added in deionized water in room temperature
Ultrasonic 2h, graphene oxide mass concentration in deionized water is 1%, is subsequently filtered, and is dried, wherein graphene oxide and carbon
The mass ratio of nanotube is 1:1-4:1.
3. the method for a kind of Synthesis of dimethyl carbonate according to claim 1, it is characterised in that described CNT is repaiied
Decorations graphene oxide catalyst amount is the 1-3% of oxide spinel vinyl acetate quality.
4. the method for a kind of Synthesis of dimethyl carbonate according to claim 1, it is characterised in that oxide spinel vinyl acetate with
The mol ratio of methyl alcohol is 1:2-1:10.
5. the method for a kind of Synthesis of dimethyl carbonate according to claim 1, it is characterised in that described reaction temperature is
100-120 DEG C, reaction atmosphere is CO2, initial pressure is 0.5-1Mpa, and the reaction time is 4-6 hours.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611028332.6A CN106588658B (en) | 2016-11-18 | 2016-11-18 | Method for synthesizing dimethyl carbonate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611028332.6A CN106588658B (en) | 2016-11-18 | 2016-11-18 | Method for synthesizing dimethyl carbonate |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN106588658A true CN106588658A (en) | 2017-04-26 |
| CN106588658B CN106588658B (en) | 2020-06-26 |
Family
ID=58592493
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201611028332.6A Active CN106588658B (en) | 2016-11-18 | 2016-11-18 | Method for synthesizing dimethyl carbonate |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN106588658B (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108579789A (en) * | 2018-05-07 | 2018-09-28 | 常州大学 | A kind of preparation method for synthesizing ethylene carbonate process solid catalyst |
| CN109438409A (en) * | 2018-12-05 | 2019-03-08 | 常州大学 | A kind of method of synthesizing annular carbonate |
| CN109608337A (en) * | 2019-01-21 | 2019-04-12 | 山西大学 | A kind of the alcoholysis process intensifying device and method of ethylene carbonate |
| CN110304996A (en) * | 2019-06-28 | 2019-10-08 | 浙江锦润生物科技有限公司 | A kind of removal methods of base catalyst |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20070083062A1 (en) * | 2005-10-07 | 2007-04-12 | Darbha Srinivas | Process for the preparation of dialkyl carbonate |
| CN104072377A (en) * | 2014-06-24 | 2014-10-01 | 常州大学 | Method for synthesizing linear carbonic ester through exchange reaction of cyclic carbonate and alcohol ester |
| CN104383951A (en) * | 2014-10-31 | 2015-03-04 | 常州大学 | Catalyst for synthesis of linear carbonate by virtue of transesterification of cyclic carbonate and alcohol and preparing method of catalyst |
| CN104447312A (en) * | 2014-11-21 | 2015-03-25 | 常州大学 | Dimethyl carbonate synthesis method |
| WO2015114474A1 (en) * | 2014-01-30 | 2015-08-06 | Indian Oil Corporation Limited | Single-pot synthesis of dialkyl carbonates using catalyst from natural resource |
-
2016
- 2016-11-18 CN CN201611028332.6A patent/CN106588658B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20070083062A1 (en) * | 2005-10-07 | 2007-04-12 | Darbha Srinivas | Process for the preparation of dialkyl carbonate |
| WO2015114474A1 (en) * | 2014-01-30 | 2015-08-06 | Indian Oil Corporation Limited | Single-pot synthesis of dialkyl carbonates using catalyst from natural resource |
| CN104072377A (en) * | 2014-06-24 | 2014-10-01 | 常州大学 | Method for synthesizing linear carbonic ester through exchange reaction of cyclic carbonate and alcohol ester |
| CN104383951A (en) * | 2014-10-31 | 2015-03-04 | 常州大学 | Catalyst for synthesis of linear carbonate by virtue of transesterification of cyclic carbonate and alcohol and preparing method of catalyst |
| CN104447312A (en) * | 2014-11-21 | 2015-03-25 | 常州大学 | Dimethyl carbonate synthesis method |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108579789A (en) * | 2018-05-07 | 2018-09-28 | 常州大学 | A kind of preparation method for synthesizing ethylene carbonate process solid catalyst |
| CN108579789B (en) * | 2018-05-07 | 2021-06-01 | 常州大学 | Application of carbon nitride/graphene oxide composite material |
| CN109438409A (en) * | 2018-12-05 | 2019-03-08 | 常州大学 | A kind of method of synthesizing annular carbonate |
| CN109608337A (en) * | 2019-01-21 | 2019-04-12 | 山西大学 | A kind of the alcoholysis process intensifying device and method of ethylene carbonate |
| CN109608337B (en) * | 2019-01-21 | 2020-04-17 | 山西大学 | Device and method for reinforcing alcoholysis process of ethylene carbonate |
| CN110304996A (en) * | 2019-06-28 | 2019-10-08 | 浙江锦润生物科技有限公司 | A kind of removal methods of base catalyst |
| CN110304996B (en) * | 2019-06-28 | 2022-02-11 | 浙江锦润生物科技有限公司 | Method for removing alkali catalyst |
Also Published As
| Publication number | Publication date |
|---|---|
| CN106588658B (en) | 2020-06-26 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN105344341B (en) | A kind of preparation method of solid catalyst for Synthesis of dimethyl carbonate | |
| CN104447312B (en) | A kind of method of Synthesis of dimethyl carbonate | |
| CN106588658A (en) | Method of synthesizing dimethyl carbonate | |
| CN109134231B (en) | Device and process for continuously producing chloroacetic acid by differential circulation | |
| CN108610324B (en) | Preparation method of vinyl sulfate | |
| CN106631776A (en) | Green preparation process for synthesizing 12-carbon alcohol ester by double catalytic system | |
| CN107243345A (en) | A kind of O composite metallic oxide catalyst that ethylene glycol co-producing dimethyl carbonate is prepared for ester exchange reaction | |
| CN105503544A (en) | Method for catalytically synthesizing propylene glycol methyl ether by adopting solid base catalyst KF/ZrO2-SiO2 | |
| CN106588657A (en) | Method for synthesizing dimethyl carbonate | |
| CN105879892A (en) | Solid base catalyst for synthesizing dimethyl carbonate through transesterification method and preparation method and application | |
| CN103360287B (en) | MethyIsuIfino benzaldehyde preparation method | |
| CN108976108A (en) | A method of synthesis pseudo ionone | |
| CN102850223A (en) | Method for synthesizing methylethyl carbonate | |
| CN100513370C (en) | Process for improving product quality and yield of propanediol and glycol | |
| CN102786427B (en) | Synthetic method of bis-(2-dimethylaminoethyl)ether | |
| CN110013875A (en) | A kind of preparation method of fluorine richness molecular sieve FER | |
| CN103506126B (en) | A kind of preparation method of copper radical synthesizing methanol catalyst | |
| CN115894433A (en) | Process for continuously synthesizing vinyl sulfate crude product | |
| CN104030893A (en) | Method for preparing 4-methyl catechol | |
| CN103435463A (en) | Method for preparing 9-fluorenone via four-phase transfer catalysis | |
| CN102850185A (en) | Method for synthesizing isopropanol by using cation exchange resin as catalyst | |
| GB1563598A (en) | Manufacture of lactones of the triphenylmethane series | |
| CN105037113A (en) | Synthesis method of carbonic acid ortho-ester | |
| CN103709004A (en) | Preparation method of 1, 3-propanediol | |
| CN112552210A (en) | Method for preparing N, N' -dicyclohexylcarbodiimide by using co-reactor |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| TR01 | Transfer of patent right | ||
| TR01 | Transfer of patent right |
Effective date of registration: 20240423 Address after: Room 303-21579, No. 304, South Community A, Binhe Street, Pinggu District, Beijing, 101200 Patentee after: BEIJING ZHITOUJIA INTELLECTUAL PROPERTY OPERATION CO.,LTD. Country or region after: China Address before: Gehu Lake Road Wujin District 213164 Jiangsu city of Changzhou province No. 1 Patentee before: CHANGZHOU University Country or region before: China |