CN112159307A - Novel process for preparing sodium methoxide by using metal sodium - Google Patents
Novel process for preparing sodium methoxide by using metal sodium Download PDFInfo
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- CN112159307A CN112159307A CN202010984297.5A CN202010984297A CN112159307A CN 112159307 A CN112159307 A CN 112159307A CN 202010984297 A CN202010984297 A CN 202010984297A CN 112159307 A CN112159307 A CN 112159307A
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- sodium methoxide
- methanol
- sodium
- novel process
- cooling
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- WQDUMFSSJAZKTM-UHFFFAOYSA-N Sodium methoxide Chemical compound [Na+].[O-]C WQDUMFSSJAZKTM-UHFFFAOYSA-N 0.000 title claims abstract description 192
- 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 title claims abstract description 58
- 239000011734 sodium Substances 0.000 title claims abstract description 58
- 229910052708 sodium Inorganic materials 0.000 title claims abstract description 57
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 30
- 229910052751 metal Inorganic materials 0.000 title abstract description 23
- 239000002184 metal Substances 0.000 title abstract description 23
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims abstract description 339
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 76
- 238000006243 chemical reaction Methods 0.000 claims abstract description 68
- 238000001816 cooling Methods 0.000 claims abstract description 41
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 38
- 239000007789 gas Substances 0.000 claims abstract description 30
- 239000001257 hydrogen Substances 0.000 claims abstract description 29
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 29
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 27
- 238000004064 recycling Methods 0.000 claims abstract description 24
- 239000002994 raw material Substances 0.000 claims abstract description 21
- 239000012043 crude product Substances 0.000 claims abstract description 20
- 238000007599 discharging Methods 0.000 claims abstract description 19
- 238000003756 stirring Methods 0.000 claims abstract description 19
- KEAYESYHFKHZAL-UHFFFAOYSA-N Sodium Chemical compound [Na] KEAYESYHFKHZAL-UHFFFAOYSA-N 0.000 claims abstract description 17
- 239000000047 product Substances 0.000 claims abstract description 15
- 239000002893 slag Substances 0.000 claims description 20
- 239000012267 brine Substances 0.000 claims description 17
- 238000010438 heat treatment Methods 0.000 claims description 17
- HPALAKNZSZLMCH-UHFFFAOYSA-M sodium;chloride;hydrate Chemical group O.[Na+].[Cl-] HPALAKNZSZLMCH-UHFFFAOYSA-M 0.000 claims description 17
- 238000001291 vacuum drying Methods 0.000 claims description 11
- 238000004806 packaging method and process Methods 0.000 claims description 9
- 230000001681 protective effect Effects 0.000 claims description 9
- 238000004821 distillation Methods 0.000 claims description 6
- 150000002431 hydrogen Chemical class 0.000 claims description 2
- 238000000034 method Methods 0.000 abstract description 17
- 239000003513 alkali Substances 0.000 abstract description 7
- 208000012839 conversion disease Diseases 0.000 abstract description 2
- 238000005265 energy consumption Methods 0.000 abstract description 2
- 239000000463 material Substances 0.000 abstract description 2
- 238000002360 preparation method Methods 0.000 abstract description 2
- 230000002441 reversible effect Effects 0.000 abstract description 2
- 239000002699 waste material Substances 0.000 abstract description 2
- 238000001035 drying Methods 0.000 abstract 1
- 238000007670 refining Methods 0.000 abstract 1
- 239000007787 solid Substances 0.000 abstract 1
- 230000000052 comparative effect Effects 0.000 description 8
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 239000003960 organic solvent Substances 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 238000010923 batch production Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000010924 continuous production Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 239000012442 inert solvent Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 229910001948 sodium oxide Inorganic materials 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
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
Abstract
The invention belongs to the technical field of sodium methoxide preparation processes, in particular to a novel process for preparing sodium methoxide by using metal sodium, which solves 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, and the refining process of the solid sodium methoxide comprises the following steps: adding raw materials of sodium metal and methanol into a reaction kettle, and stirring for reaction to obtain a sodium methoxide crude product and hydrogen; cooling and recycling the gas phase of the methanol, and discharging nitrogen and hydrogen from the high altitude; distilling the sodium methoxide crude product at normal pressure, and drying in vacuum to obtain the high-purity sodium methoxide. The method has the advantages of high utilization rate of raw materials, high reaction conversion rate, high yield, reduced material waste, effectively reduced reaction cost, high purity of the prepared sodium methoxide and low content of free alkali.
Description
Technical Field
The invention relates to the technical field of sodium methoxide preparation processes, in particular to a novel process for preparing sodium methoxide by using metal sodium.
Background
The traditional production method of sodium methoxide comprises a metal sodium method and an alkali method, wherein the metal sodium and sodium hydroxide react with methanol to prepare sodium methoxide respectively, and the industrial production is realized. The metallic sodium method adopts metallic sodium to react with methanol to produce sodium methoxide, and the reaction equation is as follows:
2Na+2CH3OH→2CH3ONa+H2↑
the sodium methoxide produced by the metal sodium method can adopt a continuous or intermittent production mode, the process flow is relatively simple, and the content of free alkali in the obtained liquid sodium methoxide is low. The intermittent process of the metallic sodium method is to carry out reaction in a nitrogen environment, firstly, metallic sodium is added into a reaction kettle, and then methanol is dripped; the dripping speed of the methanol is not too high in the initial stage of the reaction, the reaction temperature is prevented from rising due to excessive heat release, the methanol is evaporated in large quantity, and the dripping speed can be increased in the later stage of the reaction to increase the reaction temperature; the intermittent production process flow can lead the yield of the prepared sodium methoxide solution to be more than 98 percent, the content of free alkali to be less than 0.5 percent, and the intermittent process is only suitable for small-batch production. The continuous production process of the metal sodium method comprises the steps of dispersing metal sodium in an inert organic solvent which is not mutually soluble with alcohol, continuously adding the metal sodium into a reaction kettle, and mixing and reacting the metal sodium with methanol at the temperature of 20-75 ℃ to prepare sodium methoxide; the method needs to use an inert organic solvent to disperse the metal sodium, and needs to remove the inert solvent in the product after the reaction is finished, so that the process is complex. Based on the statement, the invention provides a novel process for preparing sodium methoxide by using metal sodium, aiming at the defects in the process for producing sodium methoxide by using the existing metal sodium method.
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 existing sodium methoxide production process, and provides a novel process for preparing sodium methoxide by using metal sodium.
A new process for preparing sodium methoxide by using metallic sodium comprises the following steps:
s1, adding raw material methanol into a methanol metering tank, adding raw material sodium metal into a reaction kettle, introducing nitrogen into the reaction kettle, adding the methanol in the metering tank into the reaction kettle under the protection of the nitrogen and ice bath conditions, stirring for reaction until no bubbles are generated, and slowly heating to 72-85 ℃ to obtain a sodium methoxide crude product and hydrogen;
s2, cooling the hydrogen, the gas phase of the methanol and the protective gas nitrogen generated in the step S1 through a condenser, reusing the methanol in a methanol metering tank, and discharging the nitrogen and the hydrogen from the high altitude;
s3, clarifying the sodium methoxide crude product in the step S1 by a clarifying tank, discharging unreacted sodium slag, recycling the sodium slag into the reaction kettle, sending the clarified sodium methoxide into a vacuum rake dryer, and cooling the gas phase of the methanol after atmospheric distillation by a condenser to recycle the gas phase into a methanol metering tank;
and S4, vacuum drying the sodium methoxide distilled in the step S3, and packaging the dried sodium methoxide to obtain the high-purity sodium methoxide product.
Preferably, the mass ratio of the sodium metal to the methanol in the step S1 is 1: 8-12, and the adding rate of the methanol is 0.3-3 ml/min.
Preferably, the temperature rise rate in the step S1 is 8-15 ℃/h.
Preferably, the condenser in the steps S2 and S3 comprises a primary water-cooled condenser and a secondary brine condenser, wherein the cooling temperature of the primary water-cooled condenser is 38-45 ℃, and the cooling temperature of the secondary brine condenser is 20-30 ℃.
Preferably, the distillation temperature in the step S3 is 70 to 90 ℃.
Preferably, the temperature of the vacuum drying in the step S4 is 140-160 ℃, and the stirring speed is 800-1000 r/min.
The novel process for preparing sodium methoxide by using metallic sodium provided by the invention has the following beneficial effects:
1. the method effectively controls the stable reaction by reasonably controlling the reaction temperature and the dropping rate of the methanol, the prepared sodium methoxide has high purity and low free alkali content, the whole reaction is carried out in a nitrogen-protected closed environment, the safety is good, and the problems of violent reaction and dangerous operation of the traditional methanol and the metal sodium are solved.
2. According to the invention, the first-stage water-cooled condenser and the second-stage brine condenser are arranged, so that unreacted methanol can be effectively recovered and reused for reaction, and the clarifying tank is arranged to recover unreacted sodium slag and reuse the sodium slag for reaction, so that the raw material utilization rate is high, the reaction conversion rate is high, the high yield can be realized, the material waste is reduced, and the reaction cost is effectively reduced.
Detailed Description
The present invention will be further illustrated with reference to the following specific examples.
Example one
The invention provides a novel process for preparing sodium methoxide by using metallic sodium, which comprises the following steps:
s1, adding raw material methanol into a methanol metering tank, adding raw material sodium metal into a reaction kettle, introducing nitrogen into the reaction kettle, adding the methanol in the metering tank into the reaction kettle under the conditions of nitrogen protection and ice bath, stirring for reaction until no bubbles are generated, and slowly heating to 72 ℃ to obtain a sodium methoxide crude product and hydrogen; wherein the mass ratio of the metal sodium to the methanol is 1:8, the adding rate of the methanol is 0.3ml/min, and the heating rate is 8 ℃/h;
s2, cooling the gas phase of hydrogen and methanol generated in the step S1 and the protective gas nitrogen to 38 ℃ through a primary water-cooled condenser, cooling to 20 ℃ through a secondary brine condenser, recycling the cooled methanol to a methanol metering tank, and discharging the nitrogen and the hydrogen from the high altitude;
s3, clarifying the sodium methoxide crude product in the step S1 by a clarifying tank, discharging unreacted sodium slag, recycling the sodium slag into a reaction kettle, sending the clarified sodium methoxide into a vacuum rake dryer, cooling the gas phase of methanol to 38 ℃ by a primary water-cooled condenser at the temperature of 70 ℃, cooling to 20 ℃ by a secondary brine condenser, and recycling the methanol into a methanol metering tank after cooling;
and S4, carrying out vacuum drying on the sodium methoxide distilled in the step S3 at the temperature of 140 ℃ and the stirring speed of 800r/min, and carrying out packaging on the dried sodium methoxide to obtain the high-purity sodium methoxide product.
Example two
The invention provides a novel process for preparing sodium methoxide by using metallic sodium, which comprises the following steps:
s1, adding raw material methanol into a methanol metering tank, adding raw material sodium metal into a reaction kettle, introducing nitrogen into the reaction kettle, adding the methanol in the metering tank into the reaction kettle under the conditions of nitrogen protection and ice bath, stirring for reaction until no bubbles are generated, and slowly heating to 78 ℃ to obtain a sodium methoxide crude product and hydrogen; wherein the mass ratio of the metal sodium to the methanol is 1:10, the adding rate of the methanol is 1.8ml/min, and the heating rate is 12 ℃/h;
s2, cooling the gas phase of hydrogen and methanol generated in the step S1 and the protective gas nitrogen to 42 ℃ through a primary water-cooled condenser, cooling to 25 ℃ through a secondary brine condenser, recycling the cooled methanol to a methanol metering tank, and discharging the nitrogen and the hydrogen from the high altitude;
s3, clarifying the sodium methoxide crude product in the step S1 by a clarifying tank, discharging unreacted sodium slag, recycling the sodium slag into a reaction kettle, sending the clarified sodium methoxide into a vacuum rake dryer, cooling the gas phase of methanol to 42 ℃ by a primary water-cooled condenser at the temperature of 80 ℃ after atmospheric distillation, cooling to 25 ℃ by a secondary brine condenser, and recycling the methanol into a methanol metering tank after cooling;
and S4, carrying out vacuum drying on the sodium methoxide distilled in the step S3 at the temperature of 150 ℃ and the stirring speed of 900r/min, and carrying out packaging on the dried sodium methoxide to obtain the high-purity sodium methoxide product.
EXAMPLE III
The invention provides a novel process for preparing sodium methoxide by using metallic sodium, which comprises the following steps:
s1, adding raw material methanol into a methanol metering tank, adding raw material sodium metal into a reaction kettle, introducing nitrogen into the reaction kettle, adding the methanol in the metering tank into the reaction kettle under the conditions of nitrogen protection and ice bath, stirring for reaction until no bubbles are generated, and slowly heating to 85 ℃ to obtain a sodium methoxide crude product and hydrogen; wherein the mass ratio of the metal sodium to the methanol is 1:12, the adding speed of the methanol is 3ml/min, and the heating rate is 15 ℃/h;
s2, cooling the gas phase of hydrogen and methanol generated in the step S1 and the protective gas nitrogen to 45 ℃ through a primary water-cooled condenser, cooling to 30 ℃ through a secondary brine condenser, recycling the cooled methanol to a methanol metering tank, and discharging the nitrogen and the hydrogen from the high altitude;
s3, clarifying the sodium methoxide crude product in the step S1 by a clarifying tank, discharging unreacted sodium slag, recycling the sodium slag into a reaction kettle, sending the clarified sodium methoxide into a vacuum rake dryer, cooling the gas phase of methanol to 45 ℃ by a primary water-cooled condenser at the temperature of 90 ℃, cooling to 30 ℃ by a secondary brine condenser, and recycling the methanol into a methanol metering tank after cooling;
and S4, carrying out vacuum drying on the sodium methoxide distilled in the step S3 at the temperature of 160 ℃ and the stirring speed of 1000r/min, and carrying out packaging on the dried sodium methoxide to obtain the high-purity sodium methoxide product.
Comparative example 1
The invention provides a novel process for preparing sodium methoxide by using metallic sodium, which comprises the following steps:
s1, adding raw material methanol into a methanol metering tank, adding raw material sodium metal into a reaction kettle, introducing nitrogen into the reaction kettle, adding the methanol in the metering tank into the reaction kettle under the conditions of nitrogen protection and ice bath, stirring for reaction until no bubbles are generated, and slowly heating to 72 ℃ to obtain a sodium methoxide crude product and hydrogen; wherein the mass ratio of the metal sodium to the methanol is 1:8, the adding rate of the methanol is 0.3ml/mi, and the heating rate is 8 ℃/hn;
s2, cooling the gas phase of hydrogen and methanol generated in the step S1 and the protective gas nitrogen to 38 ℃ through a water-cooled condenser, recycling the cooled methanol to a methanol metering tank, and discharging the nitrogen and the hydrogen from the high altitude;
s3, clarifying the sodium methoxide crude product in the step S1 by a clarifying tank, discharging unreacted sodium slag, recycling the sodium slag into the reaction kettle, sending the clarified sodium methoxide into a vacuum rake dryer, cooling the gas phase of the methanol to 38 ℃ by a water-cooled condenser at the temperature of 70 ℃, and recycling the methanol into a methanol metering tank after cooling;
and S4, carrying out vacuum drying on the sodium methoxide distilled in the step S3 at the temperature of 140 ℃ and the stirring speed of 800r/min, and carrying out packaging on the dried sodium methoxide to obtain the high-purity sodium methoxide product.
Comparative example No. two
The invention provides a novel process for preparing sodium methoxide by using metallic sodium, which comprises the following steps:
s1, adding raw material methanol into a methanol metering tank, adding raw material sodium metal into a reaction kettle, introducing nitrogen into the reaction kettle, adding the methanol in the metering tank into the reaction kettle under the conditions of nitrogen protection and ice bath, stirring for reaction until no bubbles are generated, and slowly heating to 72 ℃ to obtain a sodium methoxide crude product and hydrogen; wherein the mass ratio of the metal sodium to the methanol is 1:8, the adding rate of the methanol is 0.3ml/min, and the heating rate is 8 ℃/h;
s2, cooling the gas phase of hydrogen and methanol generated in the step S1 and the protective gas nitrogen to 20 ℃ through a brine condenser, recycling the cooled methanol to a methanol metering tank, and discharging the nitrogen and the hydrogen from the high altitude;
s3, clarifying the sodium methoxide crude product in the step S1 by a clarifying tank, discharging unreacted sodium slag, recycling the sodium slag into the reaction kettle, sending the clarified sodium methoxide into a vacuum rake dryer, cooling the gas phase of the methanol after atmospheric distillation to 20 ℃ by a brine condenser at the temperature of 70 ℃, and recycling the methanol into a methanol metering tank after cooling;
and S4, carrying out vacuum drying on the sodium methoxide distilled in the step S3 at the temperature of 140 ℃ and the stirring speed of 800r/min, and carrying out packaging on the dried sodium methoxide to obtain the high-purity sodium methoxide product.
Comparative example No. three
The invention provides a novel process for preparing sodium methoxide by using metallic sodium, which comprises the following steps:
s1, adding raw material methanol into a methanol metering tank, adding raw material sodium metal into a reaction kettle, introducing nitrogen into the reaction kettle, adding the methanol in the metering tank into the reaction kettle under the conditions of nitrogen protection and ice bath, stirring for reaction until no bubbles are generated, and slowly heating to 72 ℃ to obtain a sodium methoxide crude product and hydrogen; wherein the mass ratio of the metal sodium to the methanol is 1:8, the adding rate of the methanol is 0.1ml/min, and the heating rate is 8 ℃/h;
s2, cooling the gas phase of hydrogen and methanol generated in the step S1 and the protective gas nitrogen to 38 ℃ through a primary water-cooled condenser, cooling to 20 ℃ through a secondary brine condenser, recycling the cooled methanol to a methanol metering tank, and discharging the nitrogen and the hydrogen from the high altitude;
s3, clarifying the sodium methoxide crude product in the step S1 by a clarifying tank, discharging unreacted sodium slag, recycling the sodium slag into a reaction kettle, sending the clarified sodium methoxide into a vacuum rake dryer, cooling the gas phase of methanol to 38 ℃ by a primary water-cooled condenser at the temperature of 70 ℃, cooling to 20 ℃ by a secondary brine condenser, and recycling the methanol into a methanol metering tank after cooling;
and S4, carrying out vacuum drying on the sodium methoxide distilled in the step S3 at the temperature of 140 ℃ and the stirring speed of 800r/min, and carrying out packaging on the dried sodium methoxide to obtain the high-purity sodium methoxide product.
Comparative example No. four
The invention provides a novel process for preparing sodium methoxide by using metallic sodium, which comprises the following steps:
s1, adding raw material methanol into a methanol metering tank, adding raw material sodium metal into a reaction kettle, introducing nitrogen into the reaction kettle, adding the methanol in the metering tank into the reaction kettle under the conditions of nitrogen protection and ice bath, stirring for reaction until no bubbles are generated, and slowly heating to 72 ℃ to obtain a sodium methoxide crude product and hydrogen; wherein the mass ratio of the metal sodium to the methanol is 1:12, the adding speed of the methanol is 3.5ml/min, and the heating rate is 8 ℃/h;
s2, cooling the gas phase of hydrogen and methanol generated in the step S1 and the protective gas nitrogen to 45 ℃ through a primary water-cooled condenser, cooling to 30 ℃ through a secondary brine condenser, recycling the cooled methanol to a methanol metering tank, and discharging the nitrogen and the hydrogen from the high altitude;
s3, clarifying the sodium methoxide crude product in the step S1 by a clarifying tank, discharging unreacted sodium slag, recycling the sodium slag into a reaction kettle, sending the clarified sodium methoxide into a vacuum rake dryer, cooling the gas phase of methanol to 45 ℃ by a primary water-cooled condenser at the temperature of 90 ℃, cooling to 30 ℃ by a secondary brine condenser, and recycling the methanol into a methanol metering tank after cooling;
and S4, carrying out vacuum drying on the sodium methoxide distilled in the step S3 at the temperature of 160 ℃ and the stirring speed of 1000r/min, and carrying out packaging on the dried sodium methoxide to obtain the high-purity sodium methoxide product.
The purity and performance of the sodium methoxide products prepared in examples one to three and comparative examples one to four were respectively tested, and the following results were obtained:
table 1:
as can be seen from Table 1: the sodium methoxide prepared in the first to third embodiments of the invention has high yield and purity, the lowest content of free alkali is only 0.38, the product quality is high, and the sodium methoxide can be widely applied to drug synthesis;
according to the embodiment I and the comparative examples I and II, the two-stage condenser is arranged, the reasonable cooling temperature is set, the methanol can be efficiently recovered and reused in the reaction, the utilization rate of the methanol can be effectively improved, and the reaction cost is reduced;
as can be seen from the first embodiment and the third comparative example, and the third embodiment and the fourth comparative example, the invention can effectively ensure the stable reaction by setting the reasonable methanol adding rate, and the prepared methanol has high purity and low free alkali content.
In addition, in the invention, the methanol and the metallic sodium react under the ice bath condition, so that the operation safety is effectively ensured, and then the slow heating treatment is carried out, so that the reaction yield and the product purity are effectively ensured.
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 (6)
1. A novel process for preparing sodium methoxide by using metallic sodium is characterized by comprising the following steps:
s1, adding raw material methanol into a methanol metering tank, adding raw material sodium metal into a reaction kettle, introducing nitrogen into the reaction kettle, adding the methanol in the metering tank into the reaction kettle under the protection of the nitrogen and ice bath conditions, stirring for reaction until no bubbles are generated, and slowly heating to 72-85 ℃ to obtain a sodium methoxide crude product and hydrogen;
s2, cooling the hydrogen, the gas phase of the methanol and the protective gas nitrogen generated in the step S1 through a condenser, reusing the methanol in a methanol metering tank, and discharging the nitrogen and the hydrogen from the high altitude;
s3, clarifying the sodium methoxide crude product in the step S1 by a clarifying tank, discharging unreacted sodium slag, recycling the sodium slag into the reaction kettle, sending the clarified sodium methoxide into a vacuum rake dryer, and cooling the gas phase of the methanol after atmospheric distillation by a condenser to recycle the gas phase into a methanol metering tank;
and S4, vacuum drying the sodium methoxide distilled in the step S3, and packaging the dried sodium methoxide to obtain the high-purity sodium methoxide product.
2. The novel process for preparing sodium methoxide with sodium metal according to claim 1, wherein the mass ratio of sodium metal to methanol in step S1 is 1: 8-12, and the addition rate of methanol is 0.3-3 ml/min.
3. The novel process for preparing sodium methoxide with sodium metal according to claim 1, wherein the temperature rise rate in step S1 is 8-15 ℃/h.
4. The novel process for preparing sodium methoxide from sodium metal according to claim 1, wherein the condensers in steps S2 and S3 comprise a primary water-cooled condenser and a secondary brine condenser, wherein the cooling temperature of the primary water-cooled condenser is 38-45 ℃, and the cooling temperature of the secondary brine condenser is 20-30 ℃.
5. The novel process for preparing sodium methoxide with sodium metal according to claim 1, wherein the distillation temperature in step S3 is 70-90 ℃.
6. The novel process for preparing sodium methoxide with sodium metal according to claim 1, wherein the temperature of vacuum drying in step S4 is 140-160 ℃, and the stirring speed is 800-1000 r/min.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112851472A (en) * | 2021-01-25 | 2021-05-28 | 安徽金邦医药化工有限公司 | Novel process for preparing sodium tert-butoxide by using xylene as solvent |
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|---|---|---|---|---|
| CN101412659A (en) * | 2008-11-28 | 2009-04-22 | 曹衍军 | Production process of lithium alcoholate |
| CN107602346A (en) * | 2017-09-07 | 2018-01-19 | 安徽省化工设计院 | A kind of metallic sodium Division A League Matches of French Football sodium alkoxide continuous production processes |
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- 2020-09-18 CN CN202010984297.5A patent/CN112159307A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101412659A (en) * | 2008-11-28 | 2009-04-22 | 曹衍军 | Production process of lithium alcoholate |
| CN107602346A (en) * | 2017-09-07 | 2018-01-19 | 安徽省化工设计院 | A kind of metallic sodium Division A League Matches of French Football sodium alkoxide continuous production processes |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112851472A (en) * | 2021-01-25 | 2021-05-28 | 安徽金邦医药化工有限公司 | Novel process for preparing sodium tert-butoxide by using xylene as solvent |
| CN112851472B (en) * | 2021-01-25 | 2023-09-22 | 安徽金邦医药化工有限公司 | Novel process for preparing sodium tert-butoxide by using dimethylbenzene as solvent |
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