CN105461513A - Method for simultaneous preparation of low viscosity methoxyl magnesium ionic liquid and high-pressure hydrogen - Google Patents
Method for simultaneous preparation of low viscosity methoxyl magnesium ionic liquid and high-pressure hydrogen Download PDFInfo
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- CN105461513A CN105461513A CN201510784103.6A CN201510784103A CN105461513A CN 105461513 A CN105461513 A CN 105461513A CN 201510784103 A CN201510784103 A CN 201510784103A CN 105461513 A CN105461513 A CN 105461513A
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C29/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
- C07C29/68—Preparation of metal alcoholates
- C07C29/70—Preparation of metal alcoholates by converting hydroxy groups to O-metal groups
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B3/00—Hydrogen; Gaseous mixtures containing hydrogen; Separation of hydrogen from mixtures containing it; Purification of hydrogen
- C01B3/02—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen
- C01B3/22—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen by decomposition of gaseous or liquid organic compounds
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2203/00—Integrated processes for the production of hydrogen or synthesis gas
- C01B2203/02—Processes for making hydrogen or synthesis gas
- C01B2203/0266—Processes for making hydrogen or synthesis gas containing a decomposition step
- C01B2203/0272—Processes for making hydrogen or synthesis gas containing a decomposition step containing a non-catalytic decomposition step
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2203/00—Integrated processes for the production of hydrogen or synthesis gas
- C01B2203/06—Integration with other chemical processes
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2203/00—Integrated processes for the production of hydrogen or synthesis gas
- C01B2203/12—Feeding the process for making hydrogen or synthesis gas
- C01B2203/1205—Composition of the feed
- C01B2203/1211—Organic compounds or organic mixtures used in the process for making hydrogen or synthesis gas
- C01B2203/1217—Alcohols
- C01B2203/1223—Methanol
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- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a method for simultaneous preparation of low viscosity methoxyl magnesium ionic liquid and high-pressure hydrogen. The steps are as below: (1) adding magnesium powder and methanol into a reactor; (2) opening the heating switch of a reactor, heating to rise the temperature, switching off the heating switch when the temperature rises to a certain degree, and reacting magnesium powder and methanol for 1-6 h; (3) cooling the reactor reaction, discharging the hydrogen gas generated in the reaction until atmospheric pressure is reached in the reactor, discharging the material, taking a liquid product, distilling to remove excess methanol to obtain the remaining melt which is methoxyl magnesium ionic liquid. The method of the present invention simultaneously prepares low viscosity methoxyl magnesium ionic liquid and high pressure hydrogen, has the advantages of simple preparation process, simple device and high reaction conversion rate; the low viscosity methoxyl magnesium ionic liquid has viscosity of 10-30m Pa.S and is conducive to the application in catalyst and extraction. The prepared hydrogen haspressure up to 1.0-60.0 MPa, and purity of greater than 99.99%.
Description
Technical field
The invention belongs to chemical reaction engineering technical field, be specifically related to a kind of method simultaneously preparing low-viscosity magnesium methylate ionic liquid and high pressure hydrogen.
Background technology
Ionic liquid (ionicliquid), also known as ionic liquid at room temperature (roomtemperatureionicliquid), refers to the organic salt be made up of anions and canons completely in room temperature or near room temperature.Ionic liquid is compared with electrolyte solution with conventional organic solvents, possesses following particular advantages: the character that (1) is non-volatile, nonflammable, conduction, catalysis, separation, coordinating, chirality etc. are unique, is the special solvent of a class and functional materials; (2) high thermostability, wide liquid temperature scope, adjustable acid-basicity, polarity, coordination ability and the solvability to organism, inorganics, polymkeric substance, gas etc. make ionic liquid become excellent reaction medium and the catalyzer of catalyzed reaction and organic synthesis; (3) wide electrochemical stability window and high ionic conductivity, make ionic liquid become the ionogen of good properties and the medium of electrochemical synthesis in electrochemical applications; (4) adjustable polarity and solvability make ionic liquid also demonstrate unique advantage in metal separation, purify protein, gas adsorption field; (5) lower interfacial energy, interfacial tension and good solubility, make ionic liquid also be widely used in nano material synthesis field; (6) low, the environmental protection of toxicity and recoverable.And less to the related manufacturing processes report of ionic liquid in technology today, what relate to is mostly the edge researchs such as the polishing fluid of ionic liquid.As can be seen here, the research and development prepared of ionic liquid are very necessary.
Ionic-liquid catalyst of urea alcoholysis synthesizing diethyl carbonate and preparation method thereof (CN201210451580.7), provide a kind of technique dehydrated alcohol, urea and catalyst preparing being become ionic liquid-catalyzed urea alcoholysis synthesizing diethyl carbonate, catalyzer is imidazoles metallic salt ionic liquid.Between the reaction period, stir speed (S.S.) is 700 ~ 1000r/min, and temperature of reaction is 160 ~ 230 DEG C, and the reaction times is 4 ~ 10h.The advantages such as it is high that the method has repeating utilization factor, non-corrosiveness, but it is high to prepare temperature of reaction required in ionic-liquid catalyst process, and energy consumption is large, needs to stir in reaction process, there is the dynamic seal of equipment and the problem of power consumption.
About the preparation aspect of hydrogen, the hydrogen manufacturing level of China rests on the general hydrogen of low pressure always and produces, and the device for producing hydrogen that high-purity high pressure hydrogen is then for want of advanced, therefore can only dependence on import.
A kind of device (CN201310628587.6) utilizing metal hydride to prepare high pressure hydrogen, this disclosure of the invention belongs to a kind of device utilizing metal hydride to prepare high pressure hydrogen of the Static Compression technical field of hydrogen, device is made up of function unit, heating circuit, cooling loop, reaction bed etc., the metal hydrides such as employing Ti-Mn base, Ti-Cr base can by the hydrogen pressurization of 0.2MPa to 20MPa, rate of supercharging reaches 100, export gas purity and reach 99.999%, but this equipment is only limitted to hydrogen compression, and the input cost of equipment is higher." methyl alcohol on MgO carrier-borne transition metal catalysts cracking for hydrogen " research of Zhu Gang etc. shows, under catalyzer, methyl alcohol energy cracking is for hydrogen-rich gas, but temperature of reaction reaches 600 DEG C, higher to the requirement of equipment, energy consumption is large simultaneously, is unfavorable for prepared by industrial production.
The information being disclosed in this background technology part is only intended to increase the understanding to general background of the present invention, and should not be regarded as admitting or imply in any form that this information structure has been prior art that persons skilled in the art are known.
Summary of the invention
The object of the present invention is to provide a kind of method simultaneously preparing low-viscosity magnesium methylate ionic liquid and high pressure hydrogen, aim to provide the preparation method that a kind of technique is simple and direct, equipment is simple, reaction conversion ratio is high, products obtained therefrom quality is good.
For achieving the above object, technical scheme provided by the invention is as follows:
Prepare a method for low-viscosity magnesium methylate ionic liquid and high pressure hydrogen simultaneously, comprise following operation steps:
(1) magnesium powder and methyl alcohol are added in reactor, then to reactor process;
(2) open reactor heater switch, heat temperature raising, after temperature rises to 40 DEG C ~ 100 DEG C, close heater switch, in reactor, the reaction times of magnesium powder and methyl alcohol is 1h ~ 6h;
(3) release reaction after reactor cooling and generate gained hydrogen to reacting kettle inner pressure to normal pressure, discharging, get liquid product through being distilled to 60 DEG C ~ 90 DEG C distillation removing excessive methanols, institute is remaining that light yellow clear starchiness melts is magnesium methylate ionic liquid.
Preferably, the magnesium powder added in step (1) and methyl alcohol are magnesium powder according to mass ratio: methyl alcohol=1:2 ~ 1:10.
Preferably, the magnesium Powder Particle Size described in step (1) is 20 order ~ 200 orders.
Preferably, described in step (1), methyl alcohol is anhydrous methanol.
Preferably, described in step (1) to reactor process be: reactor vacuumizes, and then uses N
2air in reactor is replaced.
Preferably, the vacuum tightness vacuumized described in is 70.0kPa ~ 95.0kPa; N
2displacement number of times is 2 times ~ 5 times, replaces N used
2pressure is 0.1MPa/ time ~ 0.5MPa/ time.
Preferably, release reaction after the cooling of reactor described in step (3)≤30 DEG C and generate gained hydrogen.
Preferably, in step (3), the viscosity of gained magnesium methylate ionic liquid is 10mPaS ~ 30mPaS.
Preferably, in step (3), the pressure of gained hydrogen is 1.0MPa ~ 60.0MPa, and purity is greater than 99.99%.
The inventive method prepares the catalyzer that gained magnesium methylate ionic liquid physical efficiency is used as esterification, condensation, cracking and cyclization, and can also be used as inorganic sizing agent, glue shear-strength is 15.0MPa ~ 50.0MPa, and bonding strength is constant in organic solvent.
Compared with prior art, the present invention has following beneficial effect:
Preparation method of the present invention prepares low-viscosity magnesium methylate ionic liquid and high pressure hydrogen simultaneously, and preparation technology is simple and direct, equipment is simple, reaction conversion ratio is high.Special needs to be pointed out is, methyl alcohol and magnesium powder reactor do not need to install whipping appts, there is not the dynamic seal problem of reactor, are more conducive to the manufacture of high-tension apparatus, operation, maintenance and leakproof; The magnesium methylate ionic liquid of gained low-viscosity is conducive to the application in catalyzer and extraction, simultaneously gained magnesium methylate ionic liquid or a kind of excellent inorganic sizing agent.Prepare gained hydrogen pressure and can reach 1.0MPa ~ 60.0MPa, purity is greater than 99.99%.Further preparation method of the present invention, without any " three wastes " discharge, is a kind of green cleaner production process.
Embodiment
Be described in detail below in conjunction with embodiment, but be to be understood that protection scope of the present invention not by the restriction of embodiment.In embodiment, methyl alcohol used is commercial anhydrous methanol.
Embodiment 1
Be 1:2 in mass ratio by magnesium powder and anhydrous methanol, wherein magnesium powder is 50g, granularity is 20 orders; Anhydrous methanol 100g.Magnesium powder and anhydrous methanol are dropped in 2L autoclave, be evacuated to after vacuum tightness is 70.0kPa to autoclave, use N
2to air displacement in autoclave 2 times, the N of each displacement
2pressure be 0.1MPa, cause danger to prevent remaining oxygen in still.Open autoclave heater switch, heat temperature raising, heater switch is closed when temperature rises to 40 DEG C, continue intensification again by reaction liberated heat and carry out chemical reaction, make magnesium powder and methyl alcohol react 6h in autoclave, then autoclave is cooled to 30 DEG C, release the hydrogen that reaction generates and reach discharging after normal pressure, get liquid-phase reaction product at 60 DEG C, distill the excessive methyl alcohol of removing, remaining light yellow clear starchiness melts is magnesium methylate ionic liquid.The viscosity of gained magnesium methylate ionic liquid is 10mPaS.The hydrogen pressure that reaction generates is 1.0MPa, and its purity is 99.991%.
Embodiment 2
Be 1:10 in mass ratio by magnesium powder and anhydrous methanol, wherein magnesium powder is 50g, granularity is 200 orders; Anhydrous methanol 500g.Magnesium powder and anhydrous methanol are dropped in 2L autoclave, be evacuated to after vacuum tightness is 95.0kPa to autoclave, use N
2to air displacement in autoclave 5 times, the N of each displacement
2pressure be 0.5MPa, cause danger to prevent remaining oxygen in still.Open autoclave heater switch, heat temperature raising, heater switch is closed when temperature rises to 100 DEG C, continue intensification again by reaction liberated heat and carry out chemical reaction, make magnesium powder and methyl alcohol react 1h in autoclave, then autoclave is cooled to 30 DEG C, release the hydrogen that reaction generates and reach discharging after normal pressure, get liquid-phase reaction product at 90 DEG C, distill the excessive methyl alcohol of removing, remaining light yellow clear starchiness melts is magnesium methylate ionic liquid.The viscosity of gained magnesium methylate ionic liquid is 30mPaS.The hydrogen pressure that reaction generates is 60.0MPa, and its purity is 99.997%.
Embodiment 3
Be 1:4 in mass ratio by magnesium powder and anhydrous methanol, wherein magnesium powder is 50g, granularity is 30 orders; Anhydrous methanol 200g.Magnesium powder and anhydrous methanol are dropped in 2L autoclave, be evacuated to after vacuum tightness is 82.0kPa to autoclave, use N
2to air displacement in autoclave 2 times, the N of each displacement
2pressure be 0.2MPa, cause danger to prevent remaining oxygen in still.Open autoclave heater switch, heat temperature raising, heater switch is closed when temperature rises to 50 DEG C, continue intensification again by reaction liberated heat and carry out chemical reaction, make magnesium powder and methyl alcohol react 2h in autoclave, then autoclave is cooled to 25 DEG C, release the hydrogen that reaction generates and reach discharging after normal pressure, get liquid-phase reaction product at 70 DEG C, distill the excessive methyl alcohol of removing, remaining light yellow clear starchiness melts is magnesium methylate ionic liquid.The viscosity of gained magnesium methylate ionic liquid is 20mPaS.The hydrogen pressure that reaction generates is 20.0MPa, and its purity is 99.992%.
Embodiment 4
Be 1:8 in mass ratio by magnesium powder and anhydrous methanol, wherein magnesium powder is 50g, granularity is 120 orders; Anhydrous methanol 400g.Magnesium powder and anhydrous methanol are dropped in 2L autoclave, be evacuated to after vacuum tightness is 90.0kPa to autoclave, use N
2to air displacement in autoclave 4 times, the N of each displacement
2pressure be 0.4MPa, cause danger to prevent remaining oxygen in still.Open autoclave heater switch, heat temperature raising, heater switch is closed when temperature rises to 70 DEG C, continue intensification again by reaction liberated heat and carry out chemical reaction, make magnesium powder and methyl alcohol react 1h in autoclave, then autoclave is cooled to 28 DEG C, release the hydrogen that reaction generates and reach discharging after normal pressure, get liquid-phase reaction product at 70 DEG C, distill the excessive methyl alcohol of removing, remaining light yellow clear starchiness melts is magnesium methylate ionic liquid.The viscosity of gained magnesium methylate ionic liquid is 20mPaS.The hydrogen pressure that reaction generates is 40.0MPa, and its purity is 99.994%.
Embodiment 5
Be 1:6 in mass ratio by magnesium powder and anhydrous methanol, wherein magnesium powder is 50g, granularity is 90 orders; Anhydrous methanol 300g.Magnesium powder and anhydrous methanol are dropped in 2L autoclave, be evacuated to after vacuum tightness is 86.0kPa to autoclave, use N
2to air displacement in autoclave 4 times, the N of each displacement
2pressure be 0.3MPa, cause danger to prevent remaining oxygen in still.Open autoclave heater switch, heat temperature raising, heater switch is closed when temperature rises to 60 DEG C, continue intensification again by reaction liberated heat and carry out chemical reaction, make magnesium powder and methyl alcohol react 3h in autoclave, then autoclave is cooled to 20 DEG C, release the hydrogen that reaction generates and reach discharging after normal pressure, get liquid-phase reaction product at 80 DEG C, distill the excessive methyl alcohol of removing, remaining light yellow clear starchiness melts is magnesium methylate ionic liquid.The viscosity of gained magnesium methylate ionic liquid is 15mPaS.The hydrogen pressure that reaction generates is 30.0MPa, and its purity is 99.993%.
Embodiment 6
Be 1:9 in mass ratio by magnesium powder and anhydrous methanol, wherein magnesium powder is 50g, granularity is 160 orders; Anhydrous methanol 450g.Magnesium powder and anhydrous methanol are dropped in 2L autoclave, be evacuated to after vacuum tightness is 92.0kPa to autoclave, use N
2to air displacement in autoclave 5 times, the N of each displacement
2pressure be 0.5MPa, cause danger to prevent remaining oxygen in still.Open autoclave heater switch, heat temperature raising, heater switch is closed when temperature rises to 90 DEG C, continue intensification again by reaction liberated heat and carry out chemical reaction, make magnesium powder and methyl alcohol react 5h in autoclave, then autoclave is cooled to 23 DEG C, release the hydrogen that reaction generates and reach discharging after normal pressure, get liquid-phase reaction product at 80 DEG C, distill the excessive methyl alcohol of removing, remaining light yellow clear starchiness melts is magnesium methylate ionic liquid.The viscosity of gained magnesium methylate ionic liquid is 28mPaS.The hydrogen pressure that reaction generates is 50.0MPa, and its purity is 99.996%.
The viscosity that the present invention prepares gained magnesium methylate ionic liquid is 10mPaS ~ 30mPaS, and gained hydrogen pressure can reach 1.0MPa ~ 60.0MPa, and purity is greater than 99.99%.The autoclave adopted in the inventive method does not need to install whipping appts, there is not dynamic seal and the power consumption problem of autoclave, is more conducive to the manufacture of high-tension apparatus, operation, maintenance and leakproof.
The aforementioned description to concrete exemplary of the present invention is to illustrate and the object of illustration.These descriptions not want the present invention to be defined as disclosed precise forms, and obviously, according to above-mentioned instruction, can much change and change.The object selected exemplary embodiment and describe is to explain certain principles of the present invention and practical application thereof, thus those skilled in the art can be realized and utilize various different exemplary of the present invention and various different selection and change.Scope of the present invention is intended to limited by claims and equivalents thereof.
Claims (9)
1. prepare a method for low-viscosity magnesium methylate ionic liquid and high pressure hydrogen simultaneously, it is characterized in that, comprise following operation steps:
(1) magnesium powder and methyl alcohol are added in reactor, then to reactor process;
(2) open reactor heater switch, heat temperature raising, after temperature rises to 40 DEG C ~ 100 DEG C, close heater switch, the reaction times of magnesium powder and methyl alcohol is 1h ~ 6h;
(3) release reaction after reactor cooling and generate gained hydrogen to reacting kettle inner pressure to normal pressure, discharging, gets liquid product through being distilled to 60 DEG C ~ 90 DEG C to remove excessive methanol, and institute is remaining that melts is magnesium methylate ionic liquid.
2. method according to claim 1, is characterized in that: the magnesium powder added in step (1) and methyl alcohol are magnesium powder according to mass ratio: methyl alcohol=1:2 ~ 1:10.
3. method according to claim 1, is characterized in that: the magnesium Powder Particle Size described in step (1) is 20 order ~ 200 orders.
4. method according to claim 1, is characterized in that: described in step (1), methyl alcohol is anhydrous methanol.
5. method according to claim 1, is characterized in that: described in step (1) to reactor process be: reactor vacuumizes, and then uses N
2air in reactor is replaced.
6. method according to claim 6, is characterized in that: described in the vacuum tightness that vacuumizes be 70.0kPa ~ 95.0kPa; N
2displacement number of times is 2 times ~ 5 times, replaces N used
2pressure is 0.1MPa/ time ~ 0.5MPa/ time.
7. method according to claim 1, is characterized in that: release reaction after the cooling of reactor described in step (3)≤30 DEG C and generate gained hydrogen.
8. method according to claim 1, is characterized in that: in step (3), the viscosity of gained magnesium methylate ionic liquid is 10mPaS ~ 30mPaS.
9. method according to claim 1, is characterized in that: in step (3), the pressure of gained hydrogen is 1.0MPa ~ 60.0MPa.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510784103.6A CN105461513B (en) | 2015-11-16 | 2015-11-16 | Method that is a kind of while preparing low-viscosity magnesium methoxide ionic liquid and high pressure hydrogen |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201510784103.6A CN105461513B (en) | 2015-11-16 | 2015-11-16 | Method that is a kind of while preparing low-viscosity magnesium methoxide ionic liquid and high pressure hydrogen |
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| CN105461513A true CN105461513A (en) | 2016-04-06 |
| CN105461513B CN105461513B (en) | 2018-08-28 |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20020032354A1 (en) * | 2000-09-14 | 2002-03-14 | Degussa Ag | Process for manufacturing magnesium alkoxide |
| CN1349973A (en) * | 2001-09-03 | 2002-05-22 | 广西大学 | Method and apparatus for synthesizing dimethyl carbonate |
| CN1653092A (en) * | 2002-05-10 | 2005-08-10 | 出光兴产株式会社 | Solid catalyst component for olefin polymerization, catalyst for olefin polymerization, and process for producing olefin polymer |
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- 2015-11-16 CN CN201510784103.6A patent/CN105461513B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20020032354A1 (en) * | 2000-09-14 | 2002-03-14 | Degussa Ag | Process for manufacturing magnesium alkoxide |
| CN1349973A (en) * | 2001-09-03 | 2002-05-22 | 广西大学 | Method and apparatus for synthesizing dimethyl carbonate |
| CN1653092A (en) * | 2002-05-10 | 2005-08-10 | 出光兴产株式会社 | Solid catalyst component for olefin polymerization, catalyst for olefin polymerization, and process for producing olefin polymer |
Non-Patent Citations (1)
| Title |
|---|
| 桂新胜等: "超临界条件下二氧化碳与甲醇直接合成碳酸二甲醋", 《高校化学工程学报》 * |
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