CN107602346A - A kind of metallic sodium Division A League Matches of French Football sodium alkoxide continuous production processes - Google Patents

A kind of metallic sodium Division A League Matches of French Football sodium alkoxide continuous production processes Download PDF

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Publication number
CN107602346A
CN107602346A CN201710798869.9A CN201710798869A CN107602346A CN 107602346 A CN107602346 A CN 107602346A CN 201710798869 A CN201710798869 A CN 201710798869A CN 107602346 A CN107602346 A CN 107602346A
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Prior art keywords
sodium
metallic sodium
metallic
nitrogen
reactor
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CN201710798869.9A
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Chinese (zh)
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王奎
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ANHUI PROVINCE CHEMICAL INDUSTRY DESIGN INSTITUTE
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ANHUI PROVINCE CHEMICAL INDUSTRY DESIGN INSTITUTE
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Abstract

The invention discloses a kind of metallic sodium Division A League Matches of French Football sodium alkoxide continuous production processes, process innovation:Realize that the production of metallic sodium method production sodium methoxide is changed to continuous production processes by batch production process.The characteristics of this technique:Realize by the production technology of solid metal sodium method production sodium methoxide serialization;The heating of solid metal sodium is molten into liquid metals sodium by technique using electrically heated method, has just exempted from the possibility that metallic sodium touches water, this process is employed nitrogen as to protect gas, has just been exempted from the possibility that metallic sodium touches air, greatly ensure that safety;Solid metal sodium melts realizes liquid flowing automatically continuously charging for liquid metals sodium;Technique is simple, product is stable, it is easy to operate, large-scale production can be realized;Small investment, floor space are small.

Description

A kind of metallic sodium Division A League Matches of French Football sodium alkoxide continuous production processes
Technical field
The invention belongs to chemical field, specially a kind of metallic sodium Division A League Matches of French Football sodium alkoxide continuous production processes.
Background technology
Sodium methoxide solution application field is very extensive, and the demand in the field such as medicine, agricultural chemicals, dyestuff, bioenergy is all very Greatly.Medical aspect is the raw material of vitamin B1, A and sulphadiazine, is a kind of catalyst of organic synthesis for pesticide producing.Oil Sodium methoxide also also serves as processing edible fat and edible oil catalyst in terms of fat processing industry, to change lipid structure.Also serve as Analytical reagent is widely used in the industry such as spices, pesticide producing, dyestuff.
Production technology:
Methanol and liquid metals sodium reaction production sodium methoxide.
Chemical equation:2CH3OH+2Na=2CH3ONa+H2
The defects of existing synthesis technique is present:
1) intermittent production technology is belonged to;
2) the solid metal sodium operation sequence that feeds intake is complicated, easily contact taboo thing water, and potential safety hazard is more, and security risk is big;
3) the big production of scale can not be realized;
4) labour-intensive production technology is belonged to, recruitment cost is very big;
5) floor space is big, and investment is big.
This production technology is the continuous production processes by methanol and liquid metals sodium reaction production sodium methoxide, and it is significantly special Point:The characteristics of this technique:
(1) heating of solid metal sodium is molten into liquid metals sodium, realizes automatically continuously charging;
(2) metallic sodium uses power supply to ensure that safety as heat source.
The content of the invention
The technical problems to be solved by the invention are to be directed to the above-mentioned state of the art, and provide a kind of metallic sodium Division A League Matches of French Football sodium alkoxide and connect Continuous production technology.
Technical scheme is used by the present invention solves above-mentioned technical problem:
A kind of metallic sodium Division A League Matches of French Football sodium alkoxide continuous production processes, are divided into three steps:Preparatory stage, metallic sodium melt stage, The continuous production operation phase;
Step 1) the preparatory stage, nitrogen displacement is carried out to reaction member system, close metallic sodium charging regulating valve, methanol enters Expect regulating valve, sodium methoxide discharging regulating valve and atmospheric valve, then condensed to reactor, circulating pump, circulation fluid cooler, one-level Device, secondary condenser and its pipeline are passed through nitrogen, when pressure reaches 0.1MPa on reactor, open atmospheric valve pressure release, repeat 3 Atmospheric valve is opened after secondary procedure above to continue to be passed through nitrogen;
Step 2) metallic sodium melt stage, solid metal sodium is put into the first metallic sodium melting tank and the second metal sodium fusion Melt in tank, metallic sodium melting tank, which is heated to 110 DEG C, with electrical heating makes solid metal sodium fusion turn to liquid metals sodium, the first metal Sodium fusion melts tank and the second metallic sodium melting tank is standby each other;
Step 3) the continuous production operation phase, reacting kettle jacketing, first-stage condenser, recirculation cooler are passed through circulating cooling Water, secondary condenser are passed through circulated refrigerated water;Methanol is inputted to reactor, stops logical nitrogen, liquid level reaches in question response kettle When 50%, start circulating pump, metallic sodium inlet valve enters liquid metallic sodium to reactor, controls rate of charge methanol:Metallic sodium= 6.85:1,90-95 DEG C of temperature of reaction kettle, 65-68 DEG C of gas phase pipe temperature, continuously run when operating balance, sampled by sampling valve Analyze it is qualified after, sodium methoxide product solution by pipeline through sodium methoxide discharge regulating valve flow regulation extraction enter products pot it is temporary Deposit.
Beneficial effects of the present invention:
1st, realize by the production technology of solid metal sodium method production sodium methoxide serialization;
2nd, the heating of solid metal sodium is molten into liquid metals sodium by technique using electrically heated method, has just been exempted from metallic sodium and has been connect The possibility of water is contacted, this process is employed nitrogen as to protect gas, has just exempted from the possibility that metallic sodium touches air, greatly It ensure that safety;
3rd, solid metal sodium melts realizes liquid flowing automatically continuously charging for liquid metals sodium;
4th, technique is simple, product is stable, it is easy to operate, large-scale production can be realized;
5th, small investment, floor space are small.
Brief description of the drawings
The present invention is further described below in conjunction with the accompanying drawings.
Fig. 1 is technological process of production schematic diagram of the present invention.
In figure:The metallic sodiums of 1- first melt tank, the metallic sodiums of 2- second melting tank, 3- reactors, 4- circulating pumps, 5- filterings Device, 6- circulation fluid coolers, 7- first-stage condensers, 8- secondary condensers, 9- nitrogen air inlet direct-operated regulators, 10- chargings are adjusted Save valve, 11- methanol charging regulating valve, 12- sodium methoxides discharging regulating valve, 13- atmospheric valves, 14- sampling valves.
Embodiment
The present invention is described in further detail with specific embodiment below in conjunction with the accompanying drawings.
As shown in figure 1, a kind of metallic sodium Division A League Matches of French Football sodium alkoxide continuous production processes, are divided into three steps:Preparatory stage, metallic sodium Melt stage, continuous production operation phase;
Step 1) the preparatory stage, nitrogen displacement is carried out to reaction member system, close metallic sodium charging regulating valve 10, methanol Regulating valve 11, sodium methoxide discharging regulating valve 12 and atmospheric valve 13 are fed, then to reactor 3, circulating pump 4, filter 5, circulation Liquid cooler 6, first-stage condenser 7, secondary condenser 8 and its pipeline are passed through nitrogen, and pressure reaches 0.1MPa on reactor 3 When, the pressure release of atmospheric valve 3 is opened, opening atmospheric valve 3 continues to be passed through nitrogen after being repeated 3 times procedure above;
Step 2) metallic sodium melt stage, the equipment batching hole that solid metal sodium is melted to tank 1 by metallic sodium are put into In metallic sodium melting tank 1, first provision for sealing batching hole before heating, then by being connected to the nitrogen tube on metallic sodium melting tank 1 top Nitrogen is passed through to metallic sodium melting tank 1, pressure is adjusted with nitrogen air inlet direct-operated regulator 9, operating pressure 100Pa, opens It is standby that heating power supply makes solid metal sodium fusion turn to liquid metals sodium when metallic sodium melting tank temperature is heated to 110 DEG C.Equally Method operation metallic sodium melting tank 2, metallic sodium melting tank 1 and metallic sodium melting tank 2 are standby each other;
Step 3) the continuous production operation phase, the chuck of reactor 3, first-stage condenser 7, recirculation cooler 6 are passed through circulation Cooling water, secondary condenser 8 are passed through circulated refrigerated water;Methanol is inputted to reactor 3, stops logical nitrogen, liquid level in question response kettle 3 When reaching 50%, start circulating pump 4, make in kettle material by being returned after entering circulation fluid cooler 6 after the impurity screening of filter 5 Reactor 3 realizes Matter Transfer, while opens metallic sodium inlet valve 10 and enter liquid metallic sodium to reactor, controls rate of charge first Alcohol:Metallic sodium=6.85:1,90-95 DEG C of temperature of reaction kettle, 65-68 DEG C of gas phase pipe temperature, continuously run, pass through when operating balance After the sampling analysis of sampling valve 14 is qualified, sodium methoxide product solution is produced by pipeline through sodium methoxide discharging regulating valve 12 Flow-rate adjustment Kept in into products pot.
Workflow principle:Feed intake nitrogen displacement before running, and carries out nitrogen displacement to reaction member system, first closes metal Sodium charging regulating valve 10, methanol charging regulating valve 11, sodium methoxide discharging regulating valve 12 and atmospheric valve 13, then by pipeline to anti- Answer kettle 3 to be passed through nitrogen, when pressure reaches 0.1MPa on reactor 3, open the pressure release of atmospheric valve 3, be repeated 3 times after procedure above Atmospheric valve 3 is opened to continue to be passed through nitrogen;
Then metallic sodium melts, and solid metal sodium is put into the first metallic sodium by batching hole melts in tank 1, and heating is molten First provision for sealing batching hole before melting, is passed through nitrogen and carries out nitrogen envelope, adjusts pressure using direct-operated regulator 9, operating pressure is 100Pa;Temperature in first metallic sodium melting tank 1 is heated to 110 DEG C by opening heating power supply makes solid metal sodium fusion turn to liquid It is standby.Same method operates the second metallic sodium melting tank 2, and the second metallic sodium melting tank 2 is standby;
When continuous production is run, the chuck of reactor 3, first-stage condenser 7, the recirculated cooling water of recirculation cooler 6 are opened, is beaten Open the circulated refrigerated water of secondary condenser 8;Regulating valve 11 is fed by methanol and inputs methanol to reactor 3, stops logical nitrogen, is treated anti- When answering that liquid level reaches 50% in kettle 3, start circulating pump 4, material is entered circulation fluid after the impurity screening of filter 5 and cool down Device 6, then return again to reactor 3 and realize Matter Transfer, while open metallic sodium inlet valve 10 and enter liquid metallic sodium to reactor, Control rate of charge methanol:Metallic sodium=6.85:1, open atmospheric valve 13,90-95 DEG C of temperature of reaction kettle, gas phase pipe temperature 65-68 DEG C, operation balance when continuously run, by the sampling analysis of sampling valve 14 it is qualified after, sodium methoxide product solution is by pipeline through methanol Sodium discharging regulating valve 12 Flow-rate adjustment extraction is kept in into products pot.
Above content is only citing made for the present invention and explanation, and affiliated those skilled in the art are to being retouched The specific embodiment stated is made various modifications or supplement or substituted using similar mode, without departing from the design of invention Or surmount scope defined in the claims, protection scope of the present invention all should be belonged to.

Claims (1)

1. a kind of metallic sodium Division A League Matches of French Football sodium alkoxide continuous production processes, it is characterised in that be divided into three steps:Preparatory stage, metallic sodium Melt stage, continuous production operation phase;
Step 1) the preparatory stage, nitrogen displacement is carried out to reaction member system, close metallic sodium charging regulating valve (10), methanol enters Regulating valve (11), sodium methoxide discharging regulating valve (12) and atmospheric valve (13) are expected, then to reactor (3), circulating pump (4), filtering Device (5), circulation fluid cooler (6), first-stage condenser (7), secondary condenser (8) and its pipeline are passed through nitrogen, in reactor (3) When upper pressure reaches 0.1MPa, atmospheric valve (3) pressure release is opened, is repeated 3 times after procedure above and is opened atmospheric valve (3) and continue to be passed through Nitrogen;
Step 2) metallic sodium melt stage, the equipment batching hole that solid metal sodium is melted to tank (1) by metallic sodium put into gold Category sodium fusion melts in tank (1), first provision for sealing batching hole before heating, then the nitrogen on tank (1) top is melted by being connected to metallic sodium Pipe melts tank (1) to metallic sodium and is passed through nitrogen, adjusts pressure with nitrogen air inlet direct-operated regulator, operating pressure 100Pa, beats Open that solid metal sodium fusion is turned to liquid metals sodium when metallic sodium melting tank temperature is heated to 110 DEG C by heating power supply standby, together Quadrat method operation metallic sodium melting tank (2), metallic sodium melting tank (1) and metallic sodium melting tank (2) are standby each other;
Step 3) the continuous production operation phase, reactor (3) chuck, first-stage condenser (7), recirculation cooler (6) are passed through and followed Ring cooling water, secondary condenser (8) are passed through circulated refrigerated water;Methanol is inputted to reactor (3), stops logical nitrogen, question response kettle (3) when liquid level reaches 50% in, start circulating pump (4), make in kettle material by entering circulation fluid after filter (5) impurity screening Cooler (6) returns to reactor (3) and realizes Matter Transfer afterwards, while opens metallic sodium inlet valve (10) and enter liquid gold to reactor Belong to sodium, control rate of charge methanol:Metallic sodium=6.85:1,90-95 DEG C of temperature of reaction kettle, 65-68 DEG C of gas phase pipe temperature, operate flat Continuously run during weighing apparatus, by sampling valve (14) sampling analysis it is qualified after, sodium methoxide product solution is discharged by pipeline through sodium methoxide The extraction of regulating valve (12) Flow-rate adjustment is kept in into products pot.
CN201710798869.9A 2017-09-07 2017-09-07 A kind of metallic sodium Division A League Matches of French Football sodium alkoxide continuous production processes Pending CN107602346A (en)

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Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108950208A (en) * 2018-06-04 2018-12-07 山东习尚喜新材料科技股份有限公司 A kind of continuous production device and technique of metallic potassium
CN110203873A (en) * 2019-04-30 2019-09-06 中国神华煤制油化工有限公司 Metallic sodium conveying method and metallic sodium storing and transporting system
CN112159307A (en) * 2020-09-18 2021-01-01 安徽金邦医药化工有限公司 Novel process for preparing sodium methoxide by using metal sodium
CN112250543A (en) * 2020-09-18 2021-01-22 安徽金邦医药化工有限公司 Production process of medicinal raw material sodium methoxide
CN113372192A (en) * 2021-06-10 2021-09-10 江苏诺盟氢能技术有限公司 Synthetic method of low-carbon sodium alkoxide
CN113372194A (en) * 2021-06-10 2021-09-10 江苏诺盟氢能技术有限公司 Continuous production method of sodium methoxide
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 (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB629184A (en) * 1947-02-26 1949-09-14 Robert Arthur Rosser Improvements in or relating to a process for the production of alkali metal alkoxides
JPH05170680A (en) * 1991-12-25 1993-07-09 Nippon Soda Co Ltd Production of sodium t-butoxide
USH1697H (en) * 1996-03-20 1997-11-04 E. I. Du Pont De Nemours And Company Continuous process for sodium methylate
CN105693469A (en) * 2014-11-24 2016-06-22 雷印平 Technology for producing sodium methoxide from metallic sodium

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB629184A (en) * 1947-02-26 1949-09-14 Robert Arthur Rosser Improvements in or relating to a process for the production of alkali metal alkoxides
JPH05170680A (en) * 1991-12-25 1993-07-09 Nippon Soda Co Ltd Production of sodium t-butoxide
USH1697H (en) * 1996-03-20 1997-11-04 E. I. Du Pont De Nemours And Company Continuous process for sodium methylate
CN105693469A (en) * 2014-11-24 2016-06-22 雷印平 Technology for producing sodium methoxide from metallic sodium

Cited By (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108950208A (en) * 2018-06-04 2018-12-07 山东习尚喜新材料科技股份有限公司 A kind of continuous production device and technique of metallic potassium
CN108950208B (en) * 2018-06-04 2023-09-29 山东习尚喜新材料科技股份有限公司 Continuous production device and process of metal potassium
CN110203873A (en) * 2019-04-30 2019-09-06 中国神华煤制油化工有限公司 Metallic sodium conveying method and metallic sodium storing and transporting system
CN110203873B (en) * 2019-04-30 2021-08-24 中国神华煤制油化工有限公司 Metal sodium storage and transportation method and metal sodium storage and transportation system
CN112159307A (en) * 2020-09-18 2021-01-01 安徽金邦医药化工有限公司 Novel process for preparing sodium methoxide by using metal sodium
CN112250543A (en) * 2020-09-18 2021-01-22 安徽金邦医药化工有限公司 Production process of medicinal raw material sodium methoxide
CN113372192A (en) * 2021-06-10 2021-09-10 江苏诺盟氢能技术有限公司 Synthetic method of low-carbon sodium alkoxide
CN113372194A (en) * 2021-06-10 2021-09-10 江苏诺盟氢能技术有限公司 Continuous production method of sodium methoxide
CN113372194B (en) * 2021-06-10 2023-09-01 江苏诺盟氢能技术有限公司 Continuous production method of sodium methoxide
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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