CN112226782A - Refining process of solid sodium methoxide - Google Patents
Refining process of solid sodium methoxide Download PDFInfo
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- CN112226782A CN112226782A CN202010969196.0A CN202010969196A CN112226782A CN 112226782 A CN112226782 A CN 112226782A CN 202010969196 A CN202010969196 A CN 202010969196A CN 112226782 A CN112226782 A CN 112226782A
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Abstract
The invention belongs to the technical field of preparation processes of sodium methoxide, and particularly relates to a refining process of solid sodium methoxide, which comprises the following steps: s1, dissolving sodium acetate in methanol to form a sodium acetate methanol solution, and dropwise adding sodium hydroxide to form electrolyte; s2, taking graphite and metal oxide electrode materials as working electrodes and copper sheet electrodes as auxiliary electrodes, adding additives, and stirring for electrolytic reaction; s3, heating after the reaction is finished, dropwise adding phosphoric acid, and filtering to obtain pure electrolyte; s4, evaporating and concentrating the pure electrolyte, and drying in vacuum to obtain solid sodium methoxide. The purity of the sodium methoxide obtained by the invention is as high as 98.5%, and the content of free alkali is only 0.45% at least, so that the problems of high production cost, high operation risk, reversible production process, poor product quality, high energy consumption and the like of the existing sodium methoxide production process are solved.
Description
Technical Field
The invention relates to the technical field of a preparation process of sodium methoxide, in particular to a refining process of solid sodium methoxide.
Background
Sodium methoxide is an important chemical product, has strong basicity and high activity, and can be used for producing vitamin A1Vitamin B1And sulfadiazine, etc. Sodium methoxide is also a common catalyst for producing biodiesel, has the advantages of high activity, easy separation and recovery, little corrosion to equipment and the like, and has wide market prospect.
The sodium methoxide product mainly has two forms of solid and liquid, and the solid sodium methoxide can be prepared from liquid sodium methoxide. The sodium methoxide production method mainly comprises a metallic sodium method and an alkaline method. The sodium metal method is characterized in that metal sodium directly reacts with methanol to obtain liquid sodium methoxide, the purity of the sodium methoxide product obtained by the method is high, but the metal sodium is used as a raw material, so that the price is high, the production cost is high, hydrogen is generated in the reaction process, and the danger in the operation process is increased; the alkaline method is to dissolve sodium hydroxide in methanol to react with methanol to generate sodium methoxide, the method has the advantages of cheap raw materials, relatively safe operation, reversible reaction, stronger alkalinity of the sodium methoxide than the sodium hydroxide, and easy reverse reaction of the sodium methoxide when meeting water to regenerate the sodium hydroxide and the methanol. Based on the statement, the invention provides a refining process of solid sodium methoxide aiming at the defects of the existing sodium methoxide production process.
Disclosure of Invention
The invention aims to solve the problems of high production cost, high operation risk, reversible production process, poor product quality, high energy consumption and the like of the conventional sodium methoxide production process.
A refining process of solid sodium methoxide comprises the following steps:
s1, dissolving sodium acetate in methanol to form a sodium acetate methanol solution, and dropwise adding sodium hydroxide into the sodium acetate methanol solution until the pH value reaches 7.8-12 to form electrolyte;
s2, adding the electrolyte into an electrolytic cell, taking graphite and metal oxide electrode materials as working electrodes and copper sheet electrodes as auxiliary electrodes, adding additives, and stirring by using a magnetic stirrer to perform an electrolytic reaction;
s3, heating the electrolyte after the reaction to 20-50 ℃, keeping the temperature, dropwise adding phosphoric acid until the pH value reaches 1.8-5, and filtering to remove impurities to obtain pure electrolyte;
s4, evaporating and concentrating the pure electrolyte, and drying in vacuum at 140-160 ℃ to obtain solid sodium methoxide.
Preferably, in the step S1, the mass ratio of the methanol to the sodium acetate is 7-10: 1, and the dropping rate of the sodium hydroxide is 2-10 ml/min.
Preferably, the metal oxide electrode material in step S2 is PbO2Electrode, SnO2Electrode, MnO2Either the electrode or the DSA anode.
Preferably, the addition amount of the additive in the step S2 is 0.08-0.12% of the total amount of the electrolyte; the additive is prepared by compounding N' N-dimethylformamide, zinc dialkyl dithiophosphate and furan formaldehyde in a mass ratio of 4-7: 1: 1-2.5.
Preferably, the electrolysis current density in the step S2 is 25 to 50mA/cm2The electrolytic reaction time is 3-6 h.
Preferably, the dropping rate of the phosphoric acid in the step S3 is 8-15 ml/min.
Preferably, the pressure of the evaporation concentration in the step S4 is 5-10 kPa, and the temperature is 60-80 ℃.
The refining process of solid sodium methoxide provided by the invention has the following beneficial effects:
1. the refining process of the solid sodium methoxide provided by the invention adopts sodium acetate and methanol as raw materials, sodium methoxide is prepared by electrolyzing sodium acetate methanol solution, the purity of the obtained sodium methoxide is up to 98.5%, and the content of free alkali is only 0.45% at the lowest.
2. According to the invention, through setting a reasonable proportion, the additive for electrolysis is prepared by compounding N' N-dimethylformamide, zinc dialkyl dithiophosphate and furfural, the obtained additive can greatly increase the utilization efficiency of current, and when the current density is 40mA/cm2When the electrolysis reaction time is 4.5h, the sodium methoxide concentration is measured to be as high as 5.83 g/L.
Detailed Description
The present invention will be further illustrated with reference to the following specific examples.
Example one
The invention provides a refining process of solid sodium methoxide, which comprises the following steps:
s1, dissolving sodium acetate in methanol to form a sodium acetate methanol solution according to the mass ratio of 7:1, keeping the dropping rate at 2ml/min, and dropping sodium hydroxide into the sodium acetate methanol solution until the pH value reaches 7.8 to form electrolyte;
s2, adding the electrolyte into the electrolytic bath, and adding graphite and PbO2The electrode is used as a working electrode, the copper sheet electrode is used as an auxiliary electrode, after the additive is added, a magnetic stirrer is used for stirring, and the electrolytic current density is set to be 25mA/cm2Carrying out electrolytic reaction for 3h, wherein the addition of the additive is 0.082% of the total amount of the electrolyte; the additive is prepared by compounding N' N-dimethylformamide, zinc dialkyl dithiophosphate and furan formaldehyde in a mass ratio of 4:1: 1;
s3, heating the electrolyte after the reaction is finished to 20 ℃, keeping the dropping rate at 8-15 ml/min, keeping the temperature, dropping phosphoric acid until the pH value reaches 1.8, and filtering to remove impurities to obtain pure electrolyte;
s4, evaporating and concentrating the pure electrolyte in an environment with the pressure of 5kPa and the temperature of 60 ℃, and finally, drying in vacuum at the temperature of 140 ℃ to obtain the solid sodium methoxide.
Example two
The invention provides a refining process of solid sodium methoxide, which comprises the following steps:
s1, dissolving sodium acetate in methanol to form a sodium acetate methanol solution according to the mass ratio of 8:1, keeping the dropping speed at 4ml/min, and dropping sodium hydroxide into the sodium acetate methanol solution until the pH value reaches 9 to form electrolyte;
s2, adding the electrolyte into the electrolytic cell, and adding graphite and SnO2The electrode is used as a working electrode, the copper sheet electrode is used as an auxiliary electrode, after the additive is added, a magnetic stirrer is used for stirring, and the electrolytic current density is set to be 35mA/cm2Carrying out electrolytic reaction for 4h, wherein the addition of the additive accounts for 0.09% of the total amount of the electrolyte; the additive is prepared by compounding N' N-dimethylformamide, zinc dialkyl dithiophosphate and furan formaldehyde in a mass ratio of 5:1: 1.5;
s3, heating the electrolyte after the reaction is finished to 30 ℃, keeping the dropping speed at 10ml/min, keeping the temperature, dropping phosphoric acid until the pH value reaches 2.5, and filtering to remove impurities to obtain pure electrolyte;
s4, evaporating and concentrating the pure electrolyte in an environment with the pressure of 6kPa and the temperature of 65 ℃, and finally drying in vacuum at the temperature of 145 ℃ to obtain the solid sodium methoxide.
EXAMPLE III
The invention provides a refining process of solid sodium methoxide, which comprises the following steps:
s1, dissolving sodium acetate in methanol to form a sodium acetate methanol solution according to the mass ratio of 8.5:1, keeping the dropping speed at 6ml/min, and dropping sodium hydroxide into the sodium acetate methanol solution until the pH value reaches 9.5 to form electrolyte;
s2, adding the electrolyte into the electrolytic cell, adding graphite and MnO2The electrode is used as a working electrode, the copper sheet electrode is used as an auxiliary electrode, after the additive is added, a magnetic stirrer is used for stirring, and the electrolytic current density is set to be 40mA/cm2Carrying out electrolytic reaction for 4.5h, wherein the addition of the additive accounts for 0.1% of the total amount of the electrolyte; the additive is prepared by compounding N' -N-dimethylformamide, zinc dialkyl dithiophosphate and furan formaldehyde in a mass ratio of 5.5:1: 1.5;
s3, heating the electrolyte after the reaction to 35 ℃, keeping the dropping rate at 12ml/min, keeping the temperature, dropping phosphoric acid until the pH value reaches 3.2, and filtering to remove impurities to obtain pure electrolyte;
s4, evaporating and concentrating the pure electrolyte in an environment with the pressure of 7.5kPa and the temperature of 70 ℃, and finally drying in vacuum at the temperature of 150 ℃ to obtain the solid sodium methoxide.
Example four
The invention provides a refining process of solid sodium methoxide, which comprises the following steps:
s1, dissolving sodium acetate in methanol to form a sodium acetate methanol solution according to the mass ratio of 10:1, keeping the dropping speed at 10ml/min, and dropping sodium hydroxide into the sodium acetate methanol solution until the pH value reaches 12 to form electrolyte;
s2, adding the electrolyte into an electrolytic cell, taking the graphite and DSA electrodes as working electrodes, taking the copper sheet electrode as an auxiliary electrode, and addingAfter the addition, the mixture was stirred with a magnetic stirrer, and the electrolytic current density was set to 50mA/cm2Carrying out electrolytic reaction for 6h, wherein the addition of the additive accounts for 0.12% of the total amount of the electrolyte; the additive is prepared by compounding N' N-dimethylformamide, zinc dialkyl dithiophosphate and furan formaldehyde in a mass ratio of 7:1: 2.5;
s3, heating the electrolyte after the reaction to 50 ℃, keeping the dropping rate at 15ml/min, keeping the temperature, dropping phosphoric acid until the pH value reaches 5, and filtering to remove impurities to obtain pure electrolyte;
s4, evaporating and concentrating the pure electrolyte in an environment with the pressure of 10kPa and the temperature of 80 ℃, and finally drying in vacuum at the temperature of 160 ℃ to obtain the solid sodium methoxide.
Comparative example 1
The invention provides a refining process of solid sodium methoxide, which comprises the following steps:
s1, dissolving sodium acetate in methanol to form a sodium acetate methanol solution according to the mass ratio of 8.5:1, keeping the dropping speed at 6ml/min, and dropping sodium hydroxide into the sodium acetate methanol solution until the pH value reaches 9.5 to form electrolyte;
s2, adding the electrolyte into the electrolytic cell, adding graphite and MnO2The electrode is used as a working electrode, the copper sheet electrode is used as an auxiliary electrode, a magnetic stirrer is used for stirring, and the electrolytic current density is set to be 40mA/cm2Carrying out electrolytic reaction for 4.5 h;
s3, heating the electrolyte after the reaction to 35 ℃, keeping the dropping rate at 12ml/min, keeping the temperature, dropping phosphoric acid until the pH value reaches 3.2, and filtering to remove impurities to obtain pure electrolyte;
s4, evaporating and concentrating the pure electrolyte in an environment with the pressure of 7.5kPa and the temperature of 70 ℃, and finally drying in vacuum at the temperature of 150 ℃ to obtain the solid sodium methoxide.
The second comparative example is sodium methoxide prepared by the traditional metallic sodium method.
Comparative example three is sodium methoxide prepared by a conventional alkaline process.
The properties of the solid sodium methoxide prepared in the first to third examples and the first comparative example are respectively tested, and the following results are obtained:
table 1:
as can be seen from Table 1: the solid sodium methoxide prepared in the first to third embodiments of the invention has high purity, low free alkali content and excellent comprehensive performance.
Comparative example one differs from example three only in that no additives are added in step S2, and the purity of the prepared sodium methoxide comparative example one is much lower than example three, and the free base content is higher than example three; in addition, the sodium methoxide concentrations in the first comparative example and the third example were measured, respectively, and it was found that when the current density was 40mA/cm2When the electrolysis reaction time is 4.5h, the concentration of sodium methoxide in the comparative example is only 3.73g/L, while the concentration of sodium methoxide in the example III is as high as 5.83 g/L.
Comparing the third embodiment of the invention with the second embodiment of the invention, it can be known that the comprehensive performance of the sodium methoxide prepared by the invention is similar to that of the sodium methoxide prepared by the traditional metal sodium method, but the traditional metal sodium method has high preparation cost and large operational risk in the production process.
Comparing the third embodiment of the present invention with the third comparative example, it can be seen that the third embodiment of the present invention has similar advantages to the conventional alkaline process, and both have the advantages of simple raw materials, simple operation, low production cost, etc., but the comprehensive performance of the sodium methoxide prepared by the third embodiment of the present invention is far better than that of the sodium methoxide prepared by the conventional alkaline process.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered to be within the technical scope of the present invention, and the technical solutions and the inventive concepts thereof according to the present invention should be equivalent or changed within the scope of the present invention.
Claims (7)
1. A refining process of solid sodium methoxide is characterized by comprising the following steps:
s1, dissolving sodium acetate in methanol to form a sodium acetate methanol solution, and dropwise adding sodium hydroxide into the sodium acetate methanol solution until the pH value reaches 7.8-12 to form electrolyte;
s2, adding the electrolyte into an electrolytic cell, taking graphite and metal oxide electrode materials as working electrodes and copper sheet electrodes as auxiliary electrodes, adding additives, and stirring by using a magnetic stirrer to perform an electrolytic reaction;
s3, heating the electrolyte after the reaction to 20-50 ℃, keeping the temperature, dropwise adding phosphoric acid until the pH value reaches 1.8-5, and filtering to remove impurities to obtain pure electrolyte;
s4, evaporating and concentrating the pure electrolyte, and drying in vacuum at 140-160 ℃ to obtain solid sodium methoxide.
2. The refining process of solid sodium methoxide according to claim 1, wherein the mass ratio of methanol to sodium acetate in step S1 is 7-10: 1, and the dropping rate of sodium hydroxide is 2-10 ml/min.
3. The refining process of solid sodium methoxide according to claim 1, wherein the metal oxide electrode material in step S2 is PbO2Electrode, SnO2Electrode, MnO2Either an electrode or a DSA electrode.
4. The refining process of solid sodium methoxide according to claim 1, wherein the additive is added in an amount of 0.08-0.12% of the total amount of the electrolyte in step S2; the additive is prepared by compounding N' N-dimethylformamide, zinc dialkyl dithiophosphate and furan formaldehyde in a mass ratio of 4-7: 1: 1-2.5.
5. The refining process of solid sodium methoxide of claim 1, wherein the electrolytic current density in step S2 is 25E to E50mA/cm2The electrolytic reaction time is 3-6 h.
6. The refining process of solid sodium methoxide according to claim 1, wherein the dropping rate of phosphoric acid in step S3 is 8-15 ml/min.
7. The refining process of solid sodium methoxide according to claim 1, wherein the pressure of evaporation concentration in step S4 is 5-10 kPa, and the temperature is 60-80 ℃.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116120151A (en) * | 2023-02-17 | 2023-05-16 | 东营富华达远新材料有限公司 | Sodium methoxide production process |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0146771A2 (en) * | 1983-12-21 | 1985-07-03 | Hüls Aktiengesellschaft | Process for manufacturing alcali alcoholates |
| CN1086550A (en) * | 1992-11-05 | 1994-05-11 | 萨尔斯吉建筑公司 | The regeneration of methyl-formiate synthetic catalyst and alkali metal alcoholates synthetic electrochemical method |
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2020
- 2020-09-15 CN CN202010969196.0A patent/CN112226782B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0146771A2 (en) * | 1983-12-21 | 1985-07-03 | Hüls Aktiengesellschaft | Process for manufacturing alcali alcoholates |
| CN1086550A (en) * | 1992-11-05 | 1994-05-11 | 萨尔斯吉建筑公司 | The regeneration of methyl-formiate synthetic catalyst and alkali metal alcoholates synthetic electrochemical method |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116120151A (en) * | 2023-02-17 | 2023-05-16 | 东营富华达远新材料有限公司 | Sodium methoxide production process |
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