CN209210671U - Steam infiltration-alkaline process coupling prepares the device of sodium methoxide - Google Patents
Steam infiltration-alkaline process coupling prepares the device of sodium methoxide Download PDFInfo
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- CN209210671U CN209210671U CN201821197717.XU CN201821197717U CN209210671U CN 209210671 U CN209210671 U CN 209210671U CN 201821197717 U CN201821197717 U CN 201821197717U CN 209210671 U CN209210671 U CN 209210671U
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Abstract
The utility model provides the device that steam infiltration-alkaline process coupling prepares sodium methoxide, and described device includes sodium methoxide reactor, pressurizing device and vapor permeable film separator.The device of the utility model is with vapor permeable film separative unit instead of traditional rectifying methanol distillation column, compared with the existing technology, not only realize recycling and recycling completely for anhydrous methanol, it ensure that the steady and continuous operation of reaction process, and increase operating flexibility, energy consumption is reduced, operating cost, occupied area and cost of investment are saved.Package unit is simple to operate, runs smoothly.
Description
Technical field
The utility model belongs to the energy-saving production field of sodium methoxide, and in particular to a kind of coupling vapor permeable film separates back
Receive the device that anhydrous methanol prepares sodium methoxide.
Background technique
Sodium methoxide is a kind of strong basicity organic salt, as condensing agent, catalyst etc., can be used to produce methyl formate, carbonic acid
The ester-based organic compounds such as dimethyl ester also can be used as the intermediate of vitamin and pyridine substance, be of wide application, and market prospects are wide
It is wealthy.Also have in recent years and sodium methoxide is used for catalytically synthesizing biological diesel oil, receives significant attention.
Metallic sodium method and alkaline process are two kinds of main methods of industrial volume production sodium methoxide at present.Metallic sodium method is prepared
Sodium methoxide free alkali content is low, and impurity is few, but due to that can generate hydrogen in production process, and exothermic heat of reaction is significant, to operation
Safety and stability proposes very high requirement, therefore alkaline process is the synthetic route more generallyd use.Alkaline process uses hydrogen-oxygen
Change sodium water solution as reaction liquid phase, reaction condition is more mild, and water is generated in reaction process, meets water electrode due to sodium methoxide and easily sends out
Raw hydrolysis, back reaction generates methanol and sodium hydroxide again, therefore needs in time to remove the water of generation in reaction process,
To promote the progress of positive reaction, reaction efficiency is improved.
Traditional Methanol Recovery mode uses rectifying and dewatering, and a methanol rectifying tower is arranged after reaction tower, needs to cool down
Medium and heat medium, energy consumption are larger.Have other techniques at present to be used to improve or substitute traditional methanol rectification mode.
Patent CN103288593B discloses a kind of mechanical vapor recompression sodium methoxide process units and method, using steam
The method of compression, the anhydrous methanol steam that methanol rectifying tower is ejected carry out pressurization heating, are mentioned using its steam phase-change thermal energy
Enter tower methanol vapor for reaction tower, while heating is vaporized to methanol rectification tower bottom feed liquid.The benefit of the program is section
Rectifying tower section energy consumption is saved, energy consumption mainly on Pistonless compressor, has good energy-saving effect, is disadvantageous in that generation
Part dilute methanol solution, needs subsequent processing.In addition, the operational reliability and on-site noise of organic steam compressor and shake
The unfavorable factors such as dynamic also cause the technology to never have plant-scale implementation.
Patent CN1626488A discloses the method for another recycling methanol, using simultaneous with adsorption tower and Analytic Tower
Two molecular sieve towers, the suction-operated using molecular sieve to moisture, by the moisture removal in methanol-water mixed vapour, after dehydration
Methanol vapor return in the reaction tower of leading portion.Absorption, parsing can continuous, automatic operating, easy to operate, production efficiency
It is high.But disadvantage is it is also obvious that most importantly resolving produces dilute methanol solution, it is subsequent also to need to increase rectifying device
The higher methanol of purity can be just obtained, equipment investment, operating cost are increased.It also has the following deficiencies simultaneously: 1, resolving
It is required that high, energy consumption is larger；2, resolution temperature is high, as misoperation will increase molecular sieve deterioration and loss；3, molecular sieve price is high
Expensive, replacement cost is high；4, it needs frequent progress to adsorb to operate with parsing, it is more demanding to automating, to automatic switchover valve
Reliability requirement is very high；7, molecular sieve leads to the molecular sieve work under violent alternating temperature operating condition repeatedly because of absorption parsing frequent operation
Make, therefore molecular sieve loss is more serious.
Steam infiltration is the membrane technology novel for one kind of gas (liquid) body mixture separation, the group partial pressure difference in film two sides
Under promotion, component penetrates film layer by diffusion, is vaporizated into steam in per-meate side.Vapor permeable film it is high-efficient, single-stage is able to achieve
Very high separating degree, and low energy consumption is compared to distillation process and can consume energy and saves 1/2-2/3.Process is simple simultaneously, is not necessarily to
More mating processing, system is reliable, stability is high, does not introduce other components during the separation process, belongs to environmentally-friendly technique.
Summary of the invention
It is an object of the invention to solve, Methanol Recovery rate present in existing methanol process for producing sodium is low, energy consumption is high, sets
The standby high problem of cost of investment, provides a kind of methanol of Methanol Recovery recycle utilization module for having coupled high efficiency, low cost
Sodium device.
Steam infiltration-alkaline process coupling of the invention prepare sodium methoxide device include sodium methoxide reactor, pressurizing device and
Vapor permeable film separator, in which:
Sodium methoxide reactor is equipped with top liquid material entrance, the outlet of top gas material, bottom gas material entrance and the outlet of bottom liquid material；
Vapor permeable film separator is equipped with feed(raw material)inlet, the outlet of retentate material and infiltration material outlet；
Feed preheater is equipped with before the top liquid material entrance of the sodium methoxide reactor；The top gas of sodium methoxide reactor
Material exports pressurized device and is connected with the feed(raw material)inlet of vapor permeable film separator；
The retentate material outlet of the vapor permeable film separator is connected with the bottom gas material entrance of sodium methoxide reactor.
It includes as follows for preparing the method that sodium methoxide device is produced using steam infiltration-alkaline process coupling of aforementioned present invention
Step:
(1) methanol aqueous solution containing sodium hydroxide enters from the liquid material entrance of sodium methoxide reactor head, top-down
Flowing；High-purity methanol vapor enters from the gas material entrance of sodium methoxide reactor bottom, with the methanol aqueous solution containing sodium hydroxide
It counter current contacting and reacts in sodium methoxide reactor, generates sodium methoxide；
(2) solution of the extraction containing sodium methoxide is exported from the liquid material of sodium methoxide reactor bottom, obtains sodium methoxide after cooling
Product；
(3) from the gas material outlet extraction gas material of sodium methoxide reactor head, steam is entered after pressurized heating and is permeated
Membrane separation device is separated；High-purity methanol vapor that retentate side obtains enters first from the gas material entrance of sodium methoxide reactor bottom
Sodium alkoxide reactor continues to participate in reaction；Per-meate side material acquires after condensing.
Sodium methoxide production is carried out using the device and method of aforementioned present invention, vapor permeable film separation is used for sodium methoxide first
Alcohol vapor recycling, instead of traditional rectifying methanol distillation column, compared with the existing technology, not only realizes the complete of anhydrous methanol
It recycles and recycles, ensure that the steady and continuous operation of reaction process, and increase operating flexibility, reduce energy consumption, save
Operating cost, occupied area and cost of investment are saved.Package unit is simple to operate, runs smoothly.
Detailed description of the invention
Fig. 1 is the structure drawing of device that steam infiltration-alkaline process coupling prepares sodium methoxide, in figure:
1, feed preheater, 2, sodium methoxide reactor, 3, sodium methoxide reactor product cooler, 4, pressurizing device, 5, steam infiltration
Membrane separation device, 6, infiltration material processing unit.
Specific embodiment
The present invention provides the device that steam infiltration-alkaline process coupling prepares sodium methoxide, and described device is mainly reacted by sodium methoxide
Module and methanol dehydration module are coupled to form, and structural schematic diagram is as shown in Fig. 1.The device includes sodium methoxide reactor 2, adds
Pressure device 4 and vapor permeable film separator 5, in which: sodium methoxide reactor 2 is equipped with top liquid material entrance, top gas material exports,
Bottom gas material entrance and the outlet of bottom liquid material；Vapor permeable film separator 5 is equipped with feed(raw material)inlet, the outlet of retentate material and infiltration
Material outlet；Feed preheater 1 is equipped with before the top liquid material entrance of the sodium methoxide reactor 2；Bottom liquid material outlet connection
Sodium methoxide reactor product cooler 3, top gas material outlet pass through the feed(raw material)inlet of pressurizing device 4 and vapor permeable film separator 5
It is connected；The retentate material outlet of vapor permeable film separator 5 is connected with the bottom gas material entrance of sodium methoxide reactor 2,
Permeate material outlet connection infiltration material processing unit 6.
In the structure description of above-mentioned apparatus, the pressurizing device 4 is used to be into vapor permeable film separator 5
Gas material carries out pressurization heating.The portion gas material is exported from the top gas material of sodium methoxide reactor 2, is methanol and water
Mixed vapour.The pressurized pressurization of device 4 heating, effectively improves the taste of steam, and provide the motive force of steam infiltration, is steaming
The anhydrous methanol steam that dehydration is completed in impervious membrane separation device 5, which is also able to satisfy into the stripping reaction of sodium methoxide reaction tower, to be wanted
It asks.Specifically, the preferred organic vapor compression device of pressurizing device 4 can be mechanical vapor recompression equipment, can also
To be steam jet heat pump equipment, preferably mechanical vapor recompresses equipment.
In the structure of above-mentioned apparatus, zero of state of the art determination can be passed through for those skilled in the art
Part is not described by, these components can illustrate but be not limited to: water-soluble for storing and/or supplying the methanol containing sodium hydroxide
The raw material storage tank of liquid, product storage tank for receiving/handling sodium methoxide product etc..
Further, the present invention provides the method that steam infiltration-alkaline process coupling prepares sodium methoxide, this method combination above-mentioned apparatus
Implement, includes the following steps:
(1) methanol aqueous solution containing sodium hydroxide is after feed preheater 1 from the liquid material at 2 top of sodium methoxide reactor
Entrance enters, top-down flowing；High-purity methanol vapor enters from the gas material entrance of 2 bottom of sodium methoxide reactor, and contains hydrogen
The methanol aqueous solution of sodium oxide molybdena counter current contacting and reacts in sodium methoxide reactor 2, generates sodium methoxide；As containing for raw material
55~65 DEG C of the methanol aqueous solution preheating temperature of sodium hydroxide, is preferably preheated to 60 ± 2 DEG C；Operation temperature in sodium methoxide reactor
Degree is 100 ± 2 DEG C.
(2) solution of the extraction containing sodium methoxide being exported from the liquid material of 2 bottom of sodium methoxide reactor, the solution water content is extremely low,
Sodium methoxide product is obtained after sodium methoxide reactor product cooler 3 is cooling；
It (3) is the mixed vapour of first alcohol and water, warp from the gas material outlet extraction gas material at 2 top of sodium methoxide reactor
Enter vapor permeable film separator 5 after the pressurization heating of pressurizing device 4 to be separated.In specific embodiment, with mechanical vapor
Recompression equipment carries out pressurization heating to mixed vapour, and pressurizing device pressure ratio is 1.1-3；In more specifical embodiment, mix
It closes steam and is pressurized to 0.2-0.6MPa, be warming up to 50-180 DEG C, preferably 80-110 DEG C.Whereby, it is ensured that enter steam and permeate
The material of membrane separation device 5 is effectively dehydrated, and dewatered methanol vapor keeps temperature and pressure appropriate, and satisfaction returns to first
The power and thermal requirement of sodium alkoxide reaction tower 2.
On the other hand, anti-from sodium methoxide to make since mixed vapour rising can carry residual lye secretly in sodium methoxide reactor 2
The gas material produced at the top of device 2 removal residual lye is answered, can be arranged in sodium methoxide reactor head and remove alkali mist device.Described
Except alkali mist device can be the wire mesh demister being built in sodium methoxide reactor, it is also possible to the external gas-liquid with demister
Separator.
Gas material from the gas material outlet extraction at 2 top of sodium methoxide reactor is the mixed vapour of first alcohol and water, steam
The purpose of infiltration membrane separation device 5 is to realize efficiently separating for first alcohol and water.To realize the purpose, the vapor permeable film
The preferred organic zeolite membrane separator of separator 5.Described device includes n (n is positive integer) a molecular screen membrane component, film group
Part can be single tube journey or multitube distance, and single membrane module area is controllably in 5 square meters to 300 square meters.It is every to be set with the film centered
Number of components n is determined according to separation purpose；When n is greater than 1, according to material situation, separation target etc., membrane module can be connected or
It is in parallel.On the other hand, from modular construction, the present invention can use but be not limited to constant temperature diaphragm component or baffle plate type membrane module etc.
Concrete form.
In a specific embodiment of the invention, molecular screen membrane component concrete example but can be not limited to board-like, tubular type, hollow
Fiber type or spiral plate type molecular screen membrane component, preferably tubular type molecular screen membrane component.Applicable molecular sieve type includes LTA,
SOD, FAU, MOR, FER, MFI, PHI, BEA, CHA, ERI and its co-crystalline zeolite film.
Per-meate side material acquires after condensing, which is completed by infiltration material processing unit 6.At the infiltration material
Specific structure is designed according to demand in reason unit 6, and in a specific embodiment of the invention, penetrant processing unit 6 includes
With the sequentially connected permeate condenser of infiltration material outlet, penetrating fluid surge tank and the infiltration of vapor permeable film separator 5
Liquid delivery pump is finally coupled to infiltration liquid storage tank；Since the condensation of penetrating fluid preferably uses vacuum condensation, infiltration condensation
Device connects vacuum plant.
Overall technical architecture of the present invention preferably removes the application for considering above-mentioned preferred feature, and technology spy should also be considered
Influence of the combination of sign for overall plan.The present invention provides the method that above-mentioned steam infiltration-alkaline process coupling prepares sodium methoxide
One of specific embodiment is illustrated.In the embodiment, the method includes the following steps:
(1) it is anti-from sodium methoxide to be preheated to the mass flowrate after 60 DEG C with 1000kg/h for the methanol aqueous solution containing sodium hydroxide
The liquid material entrance at the top of device is answered to enter, top-down flowing；The methanol vapor of purity 99.98% is with the quality stream of 3000kg/h
Rate enters from the gas material entrance of sodium methoxide reactor bottom, with the methanol aqueous solution containing sodium hydroxide in sodium methoxide reactor
Interior counter current contacting simultaneously reacts, and generates sodium methoxide, 100 ± 2 DEG C of the operation temperature of sodium methoxide reactor；Meanwhile to keep anti-
The operation temperature of device is answered, while guaranteeing that methanol does not vaporize, thus material inlet is provided with feed preheater, is preheating to 60 DEG C；
(2) solution of the extraction containing sodium methoxide is exported from the liquid material of sodium methoxide reactor bottom, wherein methanol sodium content is 21-
30%, methanol solution, water content is extremely low, obtains sodium methoxide product after cooling；
(3) gas material that residual lye is eliminated from the gas material of sodium methoxide reactor head outlet acquisition is methanol with
The mixed vapour of water is forced into 0.2-0.3MPa by pressurizing device, is warming up to 80-110 DEG C, subsequently into vapor permeable film point
It is separated from device；The separator includes the constant temperature diaphragm component (CN101396640A) of 2 series connections, using tubular type point
Son sieve inoranic membrane, loads loaded LTA molecular screen membrane, and the area of single membrane module is 10m2；The operating pressure of per-meate side is
0.1-30kPa.High-purity methanol vapor that retentate side obtains, water content is less than 0.02%, pressure 0.28MPa；It is pressurizeing
Under pressure provided by device 4 pushes, which enters sodium methoxide from the gas material entrance of sodium methoxide reactor bottom
Reactor continues to participate in reaction；Per-meate side material obtains penetrating fluid using vacuum condensation mode, produces after collection, matched true
Empty device uses roots pump systems with water ring, and membrane module vacuum lateral pressure is 1kPa.
By methanol quality concentration in treated penetrating fluid less than 1%, entire process methanol rate of recovery >
99.9%.
Claims (4)
1. steam infiltration-alkaline process coupling prepares the device of sodium methoxide, including sodium methoxide reactor (2), pressurizing device (4) and steam
It permeates membrane separation device (5), in which:
Sodium methoxide reactor (2) is equipped with top liquid material entrance, the outlet of top gas material, bottom gas material entrance and the outlet of bottom liquid material；
Vapor permeable film separator (5) is equipped with feed(raw material)inlet, the outlet of retentate material and infiltration material outlet；
Feed preheater (1) is equipped with before the top liquid material entrance of the sodium methoxide reactor (2)；Sodium methoxide reactor (2)
Top gas material exports pressurized device (4) and is connected with the feed(raw material)inlet of vapor permeable film separator (5)；
The bottom gas material entrance of retentate the material outlet and sodium methoxide reactor (2) of the vapor permeable film separator (5)
It is connected.
2. the apparatus according to claim 1, which is characterized in that the top liquid material entrance of the sodium methoxide reactor (2)
It is preceding to be equipped with feed preheater (1)；Bottom liquid material outlet connection sodium methoxide reactor product cooler (3).
3. the apparatus according to claim 1, which is characterized in that the penetrant of the vapor permeable film separator (5)
Material outlet connection infiltration material processing unit (6).
4. the apparatus according to claim 1, which is characterized in that the vapor permeable film separator (5) is inorganic molecule
Sieve membrane separator；Including n molecular screen membrane component, n is positive integer；When n is greater than 1, membrane module serial or parallel connection.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201821197717.XU CN209210671U (en) | 2018-07-27 | 2018-07-27 | Steam infiltration-alkaline process coupling prepares the device of sodium methoxide |
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| CN201821197717.XU CN209210671U (en) | 2018-07-27 | 2018-07-27 | Steam infiltration-alkaline process coupling prepares the device of sodium methoxide |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112209808A (en) * | 2020-09-15 | 2021-01-12 | 安徽金邦医药化工有限公司 | Novel process for producing sodium methoxide |
| CN113087596A (en) * | 2021-04-07 | 2021-07-09 | 宁波浙铁江宁化工有限公司 | Process for preparing low free alkali sodium methoxide methanol solution based on alkaline method |
-
2018
- 2018-07-27 CN CN201821197717.XU patent/CN209210671U/en active Active
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112209808A (en) * | 2020-09-15 | 2021-01-12 | 安徽金邦医药化工有限公司 | Novel process for producing sodium methoxide |
| CN113087596A (en) * | 2021-04-07 | 2021-07-09 | 宁波浙铁江宁化工有限公司 | Process for preparing low free alkali sodium methoxide methanol solution based on alkaline method |
| CN113087596B (en) * | 2021-04-07 | 2022-08-26 | 宁波浙铁江宁化工有限公司 | Process for preparing low free alkali sodium methoxide methanol solution based on alkaline method |
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