CN105254472A - Preparation method for low residual granular sodium alkoxide or potassium alcoholate - Google Patents
Preparation method for low residual granular sodium alkoxide or potassium alcoholate Download PDFInfo
- Publication number
- CN105254472A CN105254472A CN201510554885.4A CN201510554885A CN105254472A CN 105254472 A CN105254472 A CN 105254472A CN 201510554885 A CN201510554885 A CN 201510554885A CN 105254472 A CN105254472 A CN 105254472A
- Authority
- CN
- China
- Prior art keywords
- alcohol
- solvent
- potassium
- sodium
- sodium alkoxide
- 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.)
- Pending
Links
Classifications
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention provides a preparation method for low residual granular sodium alkoxide or potassium alcoholate. The method includes using sodium or potassium and alcohol as raw materials, mixing the mixture with a solvent, reacting in inert gas atmosphere by using a microwave heating method, and removing the residual alcohol and solvent in the presence of microwave after the reaction to get the granular sodium alkoxide or potassium alcoholate. The microwave frequency is 2450 +/- 50 MHz. The method can prepare sodium alkoxide or potassium alcoholate with low residual solvent, and the prepared sodium alkoxide or potassium alcoholate is large granular solid, so that the development from powdered product to granular product can be realized, and the problems of residual solvent and potential risk troubled human for a long time can be overcome.
Description
Technical field
The invention belongs to chemical field, relate to sodium alkoxide, potassium alcoholate, be specifically related to the preparation method of a kind of low residue particulate state sodium alkoxide or potassium alcoholate.
Background technology
Sodium alkoxide, potassium alcoholate are a kind of industrial chemicals very useful in fields such as medicine, agricultural chemicals, dyestuffs.Synthetic method about it mainly contains two kinds of methods according to main raw material classification used.The first is metal method, namely reacts with sodium Metal 99.5, potassium metal and corresponding alcohol and generates corresponding sodium alkoxide, potassium alcoholate; Second method is alkaline process, namely reacts to alcohol generate corresponding sodium alkoxide, potassium alcoholate with sodium hydroxide, potassium hydroxide, sodium amide, potassium amide and low-molecular-weight sodium alkoxide, potassium alcoholate.These two kinds of methods cut both ways, all industrially apply at present, maximum shortcoming is that solid sodium ethanol, potassium alcoholate dissolvent residual that two kinds of methods generate are higher, as produced sodium tert-butoxides by these two kinds of methods, potassium tert.-butoxide easily produces the trimethyl carbinol and sodium alkoxide, potassium alcoholate complex compound, be difficult to obtain pure sodium alkoxide, potassium alcoholate.In order to obtain the product of low residue, the methods such as the drying plant that people adopt high vacuum, high temperature, band to pulverize, although also can dissolvent residual be reduced but result in another one shortcoming, the solid sodium ethanol generated, potassium alcoholate are fine powdered, granularity is very little, about about 100 orders, easy generation dust, the respiratory tract of easy suction user, the eyes of easy injury user, due to its easier conglomeration in the chemical reaction of some thickness systems, be not easy to mix with system cause reacting not exclusively or reaction yield low.Along with people are to the strict demand of quality product, reaction yield, labour protection; high this two shortcomings also become sodium alkoxide, potassium alcoholate production industry pay much attention to the problem small in powder of dissolvent residual is sodium alkoxide, potassium alcoholate manufacturing enterprise pays close attention to and a difficult problem for research.
Summary of the invention
Based on low residue and granulating implacable contradiction therebetween in sodium alkoxide, potassium alcoholate production process in prior art; the invention provides the preparation method of a kind of low residue particulate state sodium alkoxide or potassium alcoholate; solve technique of the prior art to be difficult to prepare granular sodium alkoxide, potassium alcoholate, and the low residue problem of solvent in granulated product will be solved.
In order to solve the problems of the technologies described above, the application adopts following technical scheme to be achieved:
The preparation method of a kind of low residue particulate state sodium alkoxide or potassium alcoholate; the method with sodium or potassium and alcohol for raw material; with solvent; under protection of inert gas, adopt the mode of microwave heating to react; under microwave action, remove the remaining alcohol and solvent of reaction after reaction terminates, obtain particulate state sodium alkoxide, potassium alcoholate.
The present invention also has and distinguishes technical characteristic as follows:
Concrete, described alcohol is the alcohol of the alcohol of straight chain, the alcohol of side chain or ring-type.
Preferably, the alcohol of described straight chain is methyl alcohol, ethanol, propyl alcohol or butanols; The alcohol of described side chain is Virahol, 2-butanols, the trimethyl carbinol or tertiary amyl alcohol; The alcohol of described ring-type is hexalin.
Concrete, the mol ratio of described sodium, potassium and alcohol is 1:(1.05 ~ 30).
Concrete, described solvent is reaction raw materials alcohol itself or the varsol higher than alcohol boiling point, aromatic hydrocarbon solvent, organic amino kind solvent or ether solvent.
Preferably, described varsol is straight-chain paraffin, branched paraffin, cyclic alkane or unsaturated olefin; Described aromatic hydrocarbon solvent is benzene,toluene,xylene, trimethylbenzene, ethylbenzene, diethylbenzene or isopropyl benzene; Described organic amino kind solvent is primary amine, secondary amine, tertiary amine, ring-type secondary amine or cyclic tertiary amine; Described ether solvent is fatty alcohol-ether, fragrant alcohol ether, cyclic ethers or dioxy cyclic ethers.
Concrete, described rare gas element is nitrogen, argon gas.
Concrete, the mode of described employing microwave heating carries out adopting other type of heating to carry out boosting in the process of reacting.
Concrete, described temperature of reaction controls at 60 DEG C ~ 150 DEG C with the temperature removing alcohol and solvent; The described pressure-controlling removing alcohol and solvent is at-0.5mmHg ~ normal pressure.
Concrete, described microwave frequency is 2450 ± 50MHz.
Compared with prior art, useful technique effect is in the present invention:
Method of the present invention can realize low solvent residue sodium alkoxide, potassium alcoholate is produced; the sodium alkoxide generated, potassium alcoholate are large grained solids; achieve the leap from existing powdery product to granulated product, thus solve problem of solvent residual and the use safety potential problem of long-standing problem people simultaneously.
Method of the present invention adopts microwave heating, microwave on the one hand can from physical layer accelerated reaction, accelerate the escape velocity that newly-generated alkoxide leaves metallic surface, microwave chemically aspect can also decompose alcohol and sodium alkoxide on the other hand, the complex compound that potassium alcoholate is formed, interrupt alcohol and sodium alkoxide, the complex coordination key formed between potassium alcoholate, make alcohol and solvent can fast eliminating, and just can remove in the process forming granular product, and do not need that the crude product being enclosed with alcohol and solvent is carried out pulverizing and remove, changing heat transfer type makes drying process residual solvent be difficult to the present situation of convenient in rapid escape, thus generate low residue particulate state sodium alkoxide, potassium alcoholate, improve quality product, reduce sodium alkoxide, security risk in potassium alcoholate use procedure, technological process is simple, be very easy to industrially extensively promote, have easy to operate, environmental friendliness, production safety, the feature of less energy-consumption, sodium alkoxide will be promoted, there is revolutionary progress in potassium alcoholate industry.
Accompanying drawing explanation
Fig. 1 is the pattern comparison diagram of the sodium methylate adopting the method for embodiment 1 and adopt produced in conventional processes.
Below in conjunction with drawings and Examples, particular content of the present invention is described in more detail.
Embodiment
Defer to technique scheme, below provide specific embodiments of the invention, it should be noted that the present invention is not limited to following specific embodiment, all equivalents done on technical scheme basis all fall into protection scope of the present invention.Below in conjunction with embodiment, the present invention is described in further details.
Embodiment 1: the preparation of low residue particulate state sodium methylate
The present embodiment provides a kind of preparation method of low residue particulate state sodium methylate, the method comprises the following steps: be with microwave heating to 1000ml, reflux exchanger, thermometer, 600ml anhydrous methanol (14.85mol) is added in the four-hole boiling flask of agitator, add 46.0 grams of sodium Metal 99.5s (2mol) under nitrogen protection, methyl alcohol is not only as reaction raw materials but also as solvent, microwave heating, frequency is 2450 ± 50MHz, temperature of reaction controls at 60 DEG C, draw the hydrogen that reaction produces, to producing without gas, change back stream for distillation, slowly steam excessive methyl alcohol, steam residual methanol (vacuum tightness 100mmHg) more under vacuo, , obtain granular solid product, with infrared spectrometer, this product is characterized, its infrared signature absorption data is as follows: IR:2954, 2830, 1645, 1557, 1486, 1455, 1367, 890, 772, consistent with sodium methylate standard diagram.Measure the residual lower than 0.01% of alcohol by vapor-phase chromatography, particle diameter is greater than 20 objects and is greater than 95%.
Accompanying drawing 1 is the pattern comparison diagram of the sodium methylate adopting the method for embodiment 1 and adopt produced in conventional processes, as can be seen from the figure the sodium methylate that traditional preparation method prepares is amorphous powder, and is uniform granular product with the sodium methylate of this patent explained hereafter.
Embodiment 2: the preparation of low residue particulate state potassium methylate
The present embodiment provides a kind of preparation method of low residue particulate state potassium methylate, the method comprises the following steps: be with microwave heating to 1000ml, reflux exchanger, thermometer, 400ml anhydrous methanol (9.9mol) is added in the four-hole boiling flask of agitator, 200ml sherwood oil (80 ~ 100 DEG C), add 78.0 grams of potassium metals (2mol) under nitrogen protection, microwave heating, frequency is 2450 ± 50MHz, temperature of reaction controls at 60 DEG C, draw the hydrogen that reaction produces, to producing without gas, change back stream for distillation, slowly steam excessive methyl alcohol, steam sherwood oil again, steam Residual petroleum ether (vacuum tightness 100mmHg) more under vacuo, obtain granular solid product, with infrared spectrometer, this product is characterized, its infrared signature absorption data is as follows: IR:1672, 1606, 1444, 1375, 1313, 1001, 887, 831, 707, consistent with potassium methylate standard diagram.Measure the residual lower than 0.01% of alcohol and sherwood oil by vapor-phase chromatography, particle diameter is greater than 30 objects and is greater than 95%.
Embodiment 3: the preparation of low residue particulate state sodium ethylate
The present embodiment provides a kind of preparation method of low residue particulate state sodium ethylate, the method comprises the following steps: be with microwave heating to 1000ml, reflux exchanger, thermometer, 400ml dehydrated alcohol (6.85mol) is added in the four-hole boiling flask of agitator, 200ml anhydrous 1, 4-dioxane, add 46.0 grams of sodium Metal 99.5s (2mol) under nitrogen protection, microwave heating, frequency is 2450 ± 50MHz, temperature of reaction controls at 70 DEG C, draw the hydrogen that reaction produces, to producing without gas, change back stream for distillation, slowly steam excessive ethanol, steam 1 again, 4-dioxane, steam remaining 1 more under vacuo, 4-dioxane (vacuum tightness 50mmHg), obtain particulate solid sodium ethylate, remaining lower than 0.01% of alcohol and solvent, particle diameter is greater than 10 objects and is greater than 95%.
Embodiment 4: the preparation of low residue particulate state potassium ethylate
The present embodiment provides a kind of preparation method of low residue particulate state potassium ethylate, the method comprises the following steps: be with microwave heating to 1000ml, reflux exchanger, thermometer, 400ml dehydrated alcohol (6.85mol) is added in the four-hole boiling flask of agitator, 200ml dry toluene, 78.0 grams of potassium metals (2mol) are added under argon shield, microwave heating, frequency is 2450 ± 50MHz, temperature of reaction controls at 70 DEG C, draw the hydrogen that reaction produces, to producing without gas, change back stream for distillation, slowly steam excessive ethanol, steam toluene again, steam residual toluene (vacuum tightness 50mmHg) more under vacuo, obtain particulate solid potassium ethylate, alcohol and solvent is residual lower than 0.01%, particle diameter is greater than 20 objects and is greater than 95%.
Embodiment 5: the preparation of low residue particulate state sodium isopropylate
The present embodiment provides a kind of preparation method of low residue particulate state sodium isopropylate, the method comprises the following steps: be with microwave heating to 1000ml, reflux exchanger, thermometer, 400ml Virahol (5.23mol) is added in the four-hole boiling flask of agitator, 200ml dry toluene, add 46.0 grams of sodium Metal 99.5s (2mol) under nitrogen protection, microwave heating, frequency is 2450 ± 50MHz, temperature of reaction controls at 90 DEG C, draw the hydrogen that reaction produces, to producing without gas, change back stream for distillation, slowly steam excessive Virahol, steam toluene again, steam residual toluene (vacuum tightness 50mmHg) more under vacuo, obtain particulate solid sodium isopropylate, alcohol and solvent is residual lower than 0.01%, particle diameter is greater than 20 objects and is greater than 96%.
Embodiment 6: the preparation of low residue particulate state 2-sodium butylate
The present embodiment provides a kind of preparation method of low residue particulate state 2-sodium butylate, the method comprises the following steps: be with microwave heating to 1000ml, reflux exchanger, thermometer, the 2-butanols (6.56mol) of 600ml is added in the four-hole boiling flask of agitator, 200ml dry toluene, 46.0 grams of sodium Metal 99.5s (2mol) are added under argon shield, microwave heating, frequency is 2450 ± 50MHz, temperature of reaction controls at 70 DEG C, draw the hydrogen that reaction produces, to producing without gas, change back stream for distillation, slowly steam excessive 2-butanols, steam toluene again, steam residual toluene (vacuum tightness 50mmHg) more under vacuo, obtain particulate solid 2-sodium butylate, alcohol and solvent is residual lower than 0.01%, particle diameter is greater than 20 objects and is greater than 95%.
Embodiment 7: the preparation of low residue particulate state butanols potassium
The present embodiment provides a kind of preparation method of low residue particulate state butanols potassium, the method comprises the following steps: be with microwave heating to 1000ml, reflux exchanger, thermometer, 600ml butanols (6.56mol) is added in the four-hole boiling flask of agitator, 200ml anhydrous dimethyl benzene, add 78.0 grams of potassium metals (2mol) under nitrogen protection, microwave heating, frequency is 2450 ± 50MHz, temperature of reaction controls at 100 DEG C, draw the hydrogen that reaction produces, to producing without gas, change back stream for distillation, slowly steam excessive butanols, steam dimethylbenzene again, steam remaining dimethylbenzene (vacuum tightness 100mmHg) more under vacuo, obtain particulate solid butanols potassium, alcohol and solvent is residual lower than 0.01%, particle diameter is greater than 20 objects and is greater than 96%.
Embodiment 8: the preparation of low residue particulate state sodium tert-butoxide
The present embodiment provides a kind of preparation method of low residue particulate state sodium tert-butoxide, the method comprises the following steps: be with microwave heating to 1000ml, reflux exchanger, thermometer, 600ml anhydrous tertiary butanol (6.27mol) is added in the four-hole boiling flask of agitator, 200ml anhydrous 1, 4-dioxane, add 46.0 grams of sodium Metal 99.5s (2mol) under nitrogen protection, microwave heating, frequency is 2450 ± 50MHz, temperature of reaction controls at 90 DEG C, draw the hydrogen that reaction produces, to producing without gas, change back stream for distillation, slowly steam the excessive trimethyl carbinol, steam 1 again, 4-dioxane, steam remaining 1 more under vacuo, 4-dioxane (vacuum tightness 50mmgH), obtain particulate solid sodium tert-butoxide, alcohol and solvent is residual lower than 0.005%, particle diameter is greater than 20 objects and is greater than 96%.
Embodiment 9: the preparation of low residue particulate state potassium tert.-butoxide
The present embodiment provides a kind of preparation method of low residue particulate state potassium tert.-butoxide, the method comprises the following steps: be with microwave heating to 1000ml, reflux exchanger, thermometer, 600ml anhydrous tertiary butanol (6.27mol) is added in the four-hole boiling flask of agitator, 200ml anhydrous 1, 4-dioxane, 78.0 grams of potassium metals (2mol) are added under argon shield, microwave heating, frequency is 2450 ± 50MHz, temperature of reaction controls at 100 DEG C, draw the hydrogen that reaction produces, to producing without gas, change back stream for distillation, slowly steam the excessive trimethyl carbinol, steam anhydrous 1 again, 4-dioxane, steam remaining anhydrous 1 more under vacuo, 4-dioxane (vacuum tightness 100mmHg), obtain particulate solid potassium tert.-butoxide, alcohol and solvent is residual lower than 0.005%, particle diameter is greater than 10 objects and is greater than 96%.
Embodiment 10: the preparation of low residue particulate state n-propyl alcohol sodium
The present embodiment provides a kind of preparation method of low residue particulate state n-propyl alcohol sodium, the method comprises the following steps: be with microwave heating to 1000ml, reflux exchanger, thermometer, the anhydrous n-propyl alcohol of 600ml (7.84mol) is added in the four-hole boiling flask of agitator, 200ml anhydrous dimethyl benzene, add 46.0 grams of sodium Metal 99.5s (2mol) under nitrogen protection, the frequency of microwave heating is 2450 ± 50MHz, temperature of reaction controls at 90 DEG C, draw the hydrogen that reaction produces, to producing without gas, change back stream for distillation, slowly steam excessive n-propyl alcohol, steam dimethylbenzene again, steam remaining dimethylbenzene (vacuum tightness 50mmHg) more under vacuo, obtain particulate solid n-propyl alcohol sodium, alcohol and solvent is residual lower than 0.01%, particle diameter is greater than 20 objects and is greater than 96%.
Embodiment 11: the preparation of low residue granular sodium tert-pentoxide
The present embodiment provides a kind of preparation method of low residue granular sodium tert-pentoxide, the method comprises the following steps: be with microwave heating to 1000ml, reflux exchanger, thermometer, the anhydrous tertiary amyl alcohol of 224ml (about 2.1mol) is added in the four-hole boiling flask of agitator, the anhydrous trimethylbenzene of 200ml, add 46.0 grams of sodium Metal 99.5s (2mol) under nitrogen protection, microwave heating, frequency is 2450 ± 50MHz, temperature of reaction controls at 90 DEG C, draw the hydrogen that reaction produces, to producing without gas, change back stream for distillation, slowly steam excessive tertiary amyl alcohol, steam trimethylbenzene again, steam remaining trimethylbenzene (vacuum tightness 50mmHg) more under vacuo, obtain particulate solid sodium tert-amyl alcohol, alcohol and solvent is residual lower than 0.01%, particle diameter is greater than 20 objects and is greater than 96%.
Embodiment 12: the preparation of low residue particulate state hexamethylene sodium alkoxide
The present embodiment provides a kind of preparation method of low residue particulate state hexamethylene sodium alkoxide, the method comprises the following steps: be with microwave heating to 1000ml, reflux exchanger, thermometer, 600ml hexalin (5.77mol) is added in the four-hole boiling flask of agitator, 200ml anhydrous tetrahydro furan, add 4.37 grams of sodium Metal 99.5s (0.19mol) under nitrogen protection, microwave heating, frequency is 2450 ± 50MHz, electrically heated mode assisted microwave synthesis heating in reaction process, temperature of reaction controls at 60 DEG C, draw the hydrogen that reaction produces, to producing without gas, change back stream for distillation, slowly steam excessive tetrahydrofuran (THF), steam hexalin again, steam remaining hexalin at ambient pressure again, when removing under vacuum, only adopt microwave action, do not adopt electrically heated.Obtain particulate solid hexamethylene sodium alkoxide, dissolvent residual is lower than 0.01%, and particle diameter is greater than 20 objects and is greater than 96%.
The solvent of the application is not limited to the solvent in above-described embodiment, in view of length, simply show the example that some are concrete in embodiment, the solvent adopted in the application at least comprises the solvent with Types Below: reaction raw materials alcohol itself or the varsol higher than alcohol boiling point, aromatic hydrocarbon solvent, organic amino kind solvent or ether solvent.Described varsol is straight-chain paraffin, branched paraffin, cyclic alkane or unsaturated olefin; Described aromatic hydrocarbon solvent is benzene,toluene,xylene, trimethylbenzene, ethylbenzene, diethylbenzene or isopropyl benzene; Described organic amino kind solvent is primary amine, secondary amine, tertiary amine, ring-type secondary amine or cyclic tertiary amine; Described ether solvent is fatty alcohol-ether, the aromatic ether of fat, cyclic ethers or dioxy cyclic ethers.
Claims (10)
1. the preparation method of a low residue particulate state sodium alkoxide or potassium alcoholate; it is characterized in that: the method with sodium or potassium and alcohol for raw material; with solvent; under protection of inert gas, adopt the mode of microwave heating to react; under microwave action, remove the remaining alcohol and solvent of reaction after reaction terminates, obtain particulate state sodium alkoxide, potassium alcoholate.
2. the method for claim 1, is characterized in that: described alcohol is the alcohol of the alcohol of straight chain, the alcohol of side chain or ring-type.
3. method as claimed in claim 2, is characterized in that: the alcohol of described straight chain is methyl alcohol, ethanol, propyl alcohol or butanols; The alcohol of described side chain is Virahol, 2-butanols, the trimethyl carbinol or tertiary amyl alcohol; The alcohol of described ring-type is hexalin.
4. the method for claim 1, is characterized in that: the mol ratio of described sodium or potassium and alcohol is 1:(1.05 ~ 30).
5. the method for claim 1, is characterized in that: described solvent is reaction raw materials alcohol itself or the varsol higher than alcohol boiling point, aromatic hydrocarbon solvent, organic amino kind solvent or ether solvent.
6. method as claimed in claim 5, is characterized in that: described varsol is straight-chain paraffin, branched paraffin, cyclic alkane or unsaturated olefin; Described aromatic hydrocarbon solvent is benzene,toluene,xylene, trimethylbenzene, ethylbenzene, diethylbenzene or isopropyl benzene; Described organic amino kind solvent is primary amine, secondary amine, tertiary amine, ring-type secondary amine or cyclic tertiary amine; Described ether solvent is fatty alcohol-ether, fragrant alcohol ether, cyclic ethers or dioxy cyclic ethers.
7. the method for claim 1, is characterized in that: described rare gas element is nitrogen, argon gas.
8. the method for claim 1, is characterized in that: the mode of described employing microwave heating carries out adopting other type of heating to carry out boosting in the process of reacting.
9. the method for claim 1, is characterized in that: described temperature of reaction controls at 60 DEG C ~ 150 DEG C with the temperature removing alcohol and solvent; The described pressure-controlling removing alcohol and solvent is at-0.5mmHg ~ normal pressure.
10. the method for claim 1, is characterized in that: described microwave frequency is 2450 ± 50MHz.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510554885.4A CN105254472A (en) | 2015-09-02 | 2015-09-02 | Preparation method for low residual granular sodium alkoxide or potassium alcoholate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510554885.4A CN105254472A (en) | 2015-09-02 | 2015-09-02 | Preparation method for low residual granular sodium alkoxide or potassium alcoholate |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN105254472A true CN105254472A (en) | 2016-01-20 |
Family
ID=55094472
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201510554885.4A Pending CN105254472A (en) | 2015-09-02 | 2015-09-02 | Preparation method for low residual granular sodium alkoxide or potassium alcoholate |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN105254472A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112920019A (en) * | 2021-01-25 | 2021-06-08 | 安徽金邦医药化工有限公司 | Novel process for preparing high-purity sodium tert-butoxide |
| CN113121312A (en) * | 2020-01-13 | 2021-07-16 | 潘小秋 | Rice potassium ethoxide oxidant and preparation method thereof |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101962315A (en) * | 2010-10-19 | 2011-02-02 | 常州吉恩化工有限公司 | Method for preparing granular potassium tert-butoxide |
| CN101962316A (en) * | 2010-10-19 | 2011-02-02 | 常州吉恩化工有限公司 | Manufacturing method of granular potassium tert-pentylate |
| CN102001914A (en) * | 2010-10-19 | 2011-04-06 | 常州吉恩化工有限公司 | Method of preparing granular sodium tert-butoxide |
| CN102001915A (en) * | 2010-10-19 | 2011-04-06 | 常州吉恩化工有限公司 | Manufacturing method of granular sodium tert-pentoxide |
| CN102674442A (en) * | 2012-04-28 | 2012-09-19 | 无锡隆傲电子有限公司 | Method for preparing strontium titanate nano powder through microwave hydrothermal method |
-
2015
- 2015-09-02 CN CN201510554885.4A patent/CN105254472A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101962315A (en) * | 2010-10-19 | 2011-02-02 | 常州吉恩化工有限公司 | Method for preparing granular potassium tert-butoxide |
| CN101962316A (en) * | 2010-10-19 | 2011-02-02 | 常州吉恩化工有限公司 | Manufacturing method of granular potassium tert-pentylate |
| CN102001914A (en) * | 2010-10-19 | 2011-04-06 | 常州吉恩化工有限公司 | Method of preparing granular sodium tert-butoxide |
| CN102001915A (en) * | 2010-10-19 | 2011-04-06 | 常州吉恩化工有限公司 | Manufacturing method of granular sodium tert-pentoxide |
| CN102674442A (en) * | 2012-04-28 | 2012-09-19 | 无锡隆傲电子有限公司 | Method for preparing strontium titanate nano powder through microwave hydrothermal method |
Non-Patent Citations (1)
| Title |
|---|
| 杨伯伦等: "微波加热在化学反应中的应用进展", 《现代化工》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113121312A (en) * | 2020-01-13 | 2021-07-16 | 潘小秋 | Rice potassium ethoxide oxidant and preparation method thereof |
| CN112920019A (en) * | 2021-01-25 | 2021-06-08 | 安徽金邦医药化工有限公司 | Novel process for preparing high-purity sodium tert-butoxide |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Li et al. | Magnesium oxide nanosheets as effective catalysts for the synthesis of diethyl carbonate from ethyl carbamate and ethanol | |
| CN105175224A (en) | Preparation method of low-residue granular sodium alkoxide or potassium alcoholate | |
| CN105254472A (en) | Preparation method for low residual granular sodium alkoxide or potassium alcoholate | |
| Andoulsi et al. | Preparation of lanthanum ferrite powder at low temperature | |
| CN102452684B (en) | Method for one-step synthesis of mono-dispersed barium titanate nanocrystalline by self-regulating solvent thermal | |
| Ranjbar et al. | Sonochemical synthesis of a novel nano-rod two-dimensional zinc (II) coordination polymer; preparation of zinc (II) oxide nanoparticles by direct thermolyses | |
| Watanabe et al. | Formation mechanism of electrically conductive nanoparticles by induction thermal plasmas | |
| CN107382645B (en) | Synthetic process method and device of isoprene | |
| Tian et al. | Preparation of spherical nanoparticles of LaAlO3 via the reverse microemulsion process | |
| CN109369342B (en) | Preparation method of high-purity aluminum isopropoxide | |
| Lee et al. | Synthesis of cuprous oxide using sodium borohydride under microwave irradiation and catalytic effects | |
| CN102206136A (en) | Catalyst-free synthesis method for preparing 3-methyl-3-butylene-1-alcohol | |
| CN103333137A (en) | Method for synthesizing allyl glycidyl ether | |
| Anandakumar et al. | Combustion-derived CuO nanoparticles: An effective and environmentally benign catalyst in the synthesis of aromatic nitriles from aromatic aldehydes | |
| CN107936048A (en) | A kind of preparation method of 2 fluorine, 4 methyl, 3 pyridine boronic acid | |
| Yang et al. | Liquid–solid–solution synthesis of ultrafine Gd2Zr2O7 nanoparticles with yield enhancement | |
| CN108408791A (en) | A kind of MPCVD methods prepare graphene coated Co3O4The method of powder | |
| CN105218339B (en) | Method for preparing methyl heptenone by using 3-methylcrotonaldehyde | |
| CN104477869A (en) | Method for synthesizing bismuth phosphate nano particles by room-temperature solid-phase chemical method | |
| Valenzuela et al. | Solvent effect on the sol–gel synthesis of lithium aluminate | |
| Liu et al. | Direct methylation and carbonylation of in situ generated arynes via HDDA-Wittig coupling | |
| CN105198768A (en) | Synthesis method for 2-aminobutanamide | |
| CN102757086B (en) | Method and device for synthesizing zinc oxide nanoribbon by self-propagating high-temperature reaction | |
| CN107215852A (en) | The method that a kind of utilization graphene and boron nitride nanosheet prepare boron carbon nitrogen nanometer sheet | |
| CN103613115A (en) | Method for synthesizing ZnO/ZnSe (zinc oxide/zinc selenide) coaxial nano structure through gas-phase anion exchange |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20160120 |
|
| RJ01 | Rejection of invention patent application after publication |