CN109627145A - A kind of high-efficiency low energy consumption sodium methoxide equipment for purifying - Google Patents

A kind of high-efficiency low energy consumption sodium methoxide equipment for purifying Download PDF

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Publication number
CN109627145A
CN109627145A CN201910087708.8A CN201910087708A CN109627145A CN 109627145 A CN109627145 A CN 109627145A CN 201910087708 A CN201910087708 A CN 201910087708A CN 109627145 A CN109627145 A CN 109627145A
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China
Prior art keywords
tower
methanol
positive pressure
atmospheric
reaction
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CN201910087708.8A
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Chinese (zh)
Inventor
朱善龙
王国才
郑小兵
陈阿明
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ZHEJIANG XIANFENG SCIENCE TECHNOLOGY Co Ltd
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ZHEJIANG XIANFENG SCIENCE TECHNOLOGY Co Ltd
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Priority to CN201910087708.8A priority Critical patent/CN109627145A/en
Publication of CN109627145A publication Critical patent/CN109627145A/en
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    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C29/00Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
    • C07C29/68Preparation of metal alcoholates
    • C07C29/70Preparation of metal alcoholates by converting hydroxy groups to O-metal groups
    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C29/00Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
    • C07C29/74Separation; Purification; Use of additives, e.g. for stabilisation
    • C07C29/76Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment
    • C07C29/80Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment by distillation
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P20/00Technologies relating to chemical industry
    • Y02P20/10Process efficiency

Abstract

The invention belongs to sodium methoxide Preparation equipment technical fields, refer in particular to a kind of high-efficiency low energy consumption sodium methoxide equipment for purifying.Multiple rectifying columns for rectifying are set in the present invention, including methanol atmospheric tower, methanol positive pressure tower, methanol distillation column is separated the vapor in mixed gas that reaction tower generates by the rectifying of multiple towers, to obtain anhydrous methanol, the waste of methanol feedstock is avoided.Methanol atmospheric tower, methanol positive pressure tower tower pressure interior force are different, tower resistance power can be overcome to convey methanol steam naturally by pressure difference when conveying gas, reduce pressurization, condense the process of vaporization, it is compared to pervious mode, reduce first by gas-condensate liquid, then liquid is greatly reduced into the energy consumption in distillation process by the process of pump pressure-increasing unit.

Description

A kind of high-efficiency low energy consumption sodium methoxide equipment for purifying
Technical field
The invention belongs to sodium methoxide Preparation equipment technical fields, refer in particular to a kind of high-efficiency low energy consumption sodium methoxide equipment for purifying.
Background technique
Sodium methoxide is the most common sodium alkoxide, is mainly used for the synthetic intermediate raw material of medicine, pesticide, and it is edible can also to make production The catalyst and analytical reagent of oil and biodiesel, good market prospect.The production method of country's sodium methoxide is mainly at present There are alkaline process and metallic sodium method, has realized heavy industrialization.Metallic sodium method refers to metallic sodium directly and alcohol effect produces sodium alkoxide And hydrogen, this method simple process, product purity is high, and equipment investment is few.But production process is absolutely unsafe, and metallic sodium price is high It is expensive.Alkaline process refers to that sodium hydroxide reacts generation sodium methoxide with methanol and water, the method raw material are easy to get, and cost is relatively low, and operates peace Good perfection, but one strong reversible reaction needs the water for constantly removing generation that could continue to be reversed to product when the reaction, it is raw The method of anti-rectifying is used in production.Due to reacting not exclusively, sodium hydroxide impurity is often contained in product, sodium hydroxide is participating in Its side effect often of medical synthetic reaction, therefore the sodium hydroxide in sodium methoxide will be controlled in lower range, the production of two alkaline process Product be often difficult to reach this requirement, this is to restrict where alkaline process produces main bottleneck.In addition, moisture removes and methanol Recycling huge energy consumption, this be also alkaline process production shortcoming.
Summary of the invention
The object of the present invention is to provide a kind of structure is simple, the sodium methoxide equipment for purifying for consuming energy few.
The object of the present invention is achieved like this:
A kind of high-efficiency low energy consumption sodium methoxide equipment for purifying, including reaction tower, methanol atmospheric tower, methanol positive pressure tower and methanol Recovery tower;
The bottom of the reaction tower offers discharge port, and the discharge port is connect with finished pot by pipeline, the discharging Discharging pump is provided on pipeline between mouth and finished pot;
Exhaust outlet is offered at the top of the reaction tower, the exhaust outlet passes through the bottom of pipeline and the methanol atmospheric tower Connection, is delivered to methanol atmospheric tower for the gas in reaction tower by the pipeline;
The bottom of methanol atmospheric tower is also provided under atmospheric tower and exports, and exit is provided with atmospheric tower discharging under atmospheric tower Pump, is delivered to methanol positive pressure tower for liquid in methanol atmospheric tower by the atmospheric tower discharging pump;
Atmospheric tower upper outlet is offered at the top of methanol atmospheric tower, atmospheric tower upper outlet connects No.1 by pipeline and flows back Tank;
The outlet of the No.1 return tank is provided with No.1 reflux pump, outlet there are two settings on the No.1 reflux pump, No.1 reflux pot liquid is delivered to respectively in methanol atmospheric tower and methanol positive pressure tower by two discharge ports;
The bottom of methanol positive pressure tower is also provided under positive pressure tower and exports, and outlet connects methanol by pipeline under the positive pressure tower Recovery tower;
Positive pressure tower upper outlet is also provided at the top of methanol positive pressure tower, the positive pressure tower upper outlet is connected by pipeline to react Tower;
The bottom of methanol distillation column offers drainage system, will react waste water generated by the drainage system and arrange Out;
Recovery tower upper outlet is offered at the top of methanol distillation column, recovery tower upper outlet connects No. two reflux by pipeline Tank;
The outlet of No. two return tanks is provided with No. two reflux pumps, outlet there are two settings on No. two reflux pumps, No. two reflux pot liquids are delivered to respectively in methanol distillation column and methanol positive pressure tower by two discharge ports.
It further, further include alkali liquid tank described in the alkali liquid tank that is connect with the reaction tower, by pipeline and reaction tower company It connects, the outlet end of alkali liquid tank is provided with feed pump, and preheater, the bottom of reaction tower are provided with before the feed pump and reaction tower It is provided with the reaction tower heater heated to reaction tower, by the heater by the water vapor in reaction tower, generates reaction Water and sodium methoxide separation.
Further, the bottom of the methanol atmospheric tower is provided with the atmospheric tower heater heated to methanol atmospheric tower.
Further, the bottom of the methanol positive pressure tower is provided with the positive pressure tower heater heated to methanol positive pressure tower.
Further, the bottom of methanol distillation column is provided with the recovery tower heater heated to methanol distillation column.
Further, the pressure in the methanol positive pressure tower is greater than reaction tower, methanol atmospheric tower, methanol distillation column.
Further, it is provided with cooler between atmospheric tower upper outlet and No.1 return tank, will be managed by the cooler Gas in road is converted to liquid and flow to No.1 return tank.
Further, it is provided with cooler between recovery tower upper outlet and No. two return tanks, will be managed by the cooler Gas in road is converted to liquid and flow to No. two return tanks.
Further, the cooler includes that first latter linked condenser and tail condenser, tail condenser can be in pipelines Gas carries out secondary cooling.
The present invention is prominent and beneficial compared with prior art to be had the technical effect that
Multiple rectifying columns for rectifying, including methanol atmospheric tower, methanol positive pressure tower, Methanol Recovery are set in the present invention Tower is separated the vapor in mixed gas that reaction tower generates by the rectifying of multiple towers, so that anhydrous methanol is obtained, Avoid the waste of methanol feedstock.Methanol atmospheric tower, methanol positive pressure tower tower pressure interior force are different, can pass through when conveying gas Pressure difference overcomes tower resistance power to convey methanol steam naturally, reduces the process of pressurization, condensation vaporization, is compared to pervious mode, Reduce first by gas-condensate liquid, then liquid is greatly reduced in distillation process by the process of pump pressure-increasing unit Energy consumption.
Detailed description of the invention
Fig. 1 is structure diagram of the invention.
Fig. 2 is the structure diagram of reactive distillation of the invention.
Fig. 3 is reactive distillation schematic diagram of the invention.
Fig. 4 is the connection schematic diagram of methanol atmospheric tower in the present invention, reaction tower and methanol positive pressure tower.
Fig. 5 is the connection schematic diagram of reaction tower in the present invention, methanol positive pressure tower and methanol distillation column.
Fig. 6 is the connection schematic diagram of methanol atmospheric tower, methanol positive pressure tower and methanol distillation column in the present invention.
Fig. 7 is the enlarged drawing of cooler in the present invention.
Meaning represented by figure label:
1- reaction tower;2- methanol atmospheric tower;3- methanol positive pressure tower;4- methanol distillation column;5- methanol tank;6- alkali liquid tank;8- No.1 return tank;No. bis- return tanks of 9-;10- cooler;11- reaction tower heater;13- discharging pump;17- finished pot;21- is normal Press tower heater;22- atmospheric tower discharging pump;31- positive pressure tower heater;41- recovery tower heater;42- drainage system;51- first Alcohol pump;61- feed pump;62- preheater;81- No.1 reflux pump;No. bis- reflux pumps of 91-;101- condenser;102- bis- reflux Pump.
Specific embodiment
The invention will be further described combined with specific embodiments below:
As shown in the picture, including reaction tower 1, reaction tower 1 are all set by the exit that pipeline connects 6 alkali liquid tank 6 of alkali liquid tank It is equipped with booster pump, lye is transported in reaction tower 1 by booster pump and is reacted, is additionally provided between alkali liquid tank 6 and reaction tower 1 pre- Hot device 62 first does one to the lye being just transported in reaction tower 1 and preheats in advance, substantially 50 DEG C of the temperature of preheater 62, can To reduce the energy consumption in reaction tower 1.Reaction equation in reaction tower 1:
This reaction is reversible reaction, needs constantly water to be removed from reaction system obtained sodium methoxide.
A horizontal heater is arranged in 1 bottom of reaction tower, by heater to heating in reaction tower 1, accelerates methanol and lye Reaction speed, temperature requirement is maintained at 95-100 DEG C, this is determined by certain concentration product boiling point.When in reaction tower 1 When the temperature is excessively high, the intake of steam should be reduced, on the contrary, temperature should increase the additional amount of steam when too low.
Since methanol and lye will not completely attach to and react, by the raising of temperature, gaseous mixture can be generated in reaction tower 1 Body is discharged from 1 upper outlet of reaction tower, and sodium methoxide finished product is discharged from tower bottom, then is transported to sodium methoxide finished product by discharging pump 13 In finished pot 17.The water that mass fraction is about 2% is contained only in mixed gas, remaining is all methanol.
Mixed gas flows separately through methanol atmospheric tower 2, methanol positive pressure tower 3, methanol distillation column 4, and will mix mixed gas In methanol be separated from water out, water device for transferring makes, the anhydrous methanol separated be re-delivered in reaction tower 1 again into Capable and alkaline reaction, makes methanol reenter circulation.
Mixed gas is delivered to methanol atmospheric tower 2 at first, and 2 bottom of methanol atmospheric tower is provided with atmospheric tower heater 21, often Pressing 21 heating temperature of tower heater is 85 DEG C, and since the boiling point of methanol is about 65 degree, the boiling point of water is 100 degree, methanol atmospheric tower 2 Interior generation methanol gas and liquid alcohol water, methanol gas is discharged from atmospheric tower upper outlet, through subcooler 10 methanol steam Cooling generates liquid methanol and flow to the storage of No.1 return tank 8.Liquid water exports discharge under atmospheric tower, by exporting under atmospheric tower Liquid alcohol water is delivered to methanol positive pressure tower 3 by the atmospheric tower discharging pump 22 at place.
8 exit of No.1 return tank is provided with No.1 reflux pump 81, and there are two outlets for setting on No.1 reflux pump 81, respectively Methanol in No.1 return tank 8 is delivered to methanol atmospheric tower 2 and methanol positive pressure tower 3, the methanol for being delivered to methanol atmospheric tower 2 is used It is used in reflux, because the inlet and discharge rate of the raw material in methanol atmospheric tower are inconsistent, by the reflux of raw material, prevents first Lack reactant in alcohol atmospheric tower 2.
The first alcohol and water in methanol atmospheric tower 2 is being transported to methanol just by No.1 reflux pump 81 and atmospheric tower discharging pump 13 Tower 3 is pressed, the bottom of methanol positive pressure tower 3 is provided with positive pressure tower heater 31, and the heating temperature of positive pressure tower heater 31 is 90 DEG C, It being heated by heater and mixture in tower is divided into steam and liquid, the head tower of methanol positive pressure tower 3 offers positive pressure tower upper outlet, Bottom offers to be exported under positive pressure tower, and positive pressure tower upper outlet is directly connected to reaction tower 1 by pipeline, and steam methanol is directly passed through The pressure difference of positive pressure tower and reaction tower 1 is transported to reaction tower 1, without not having to be pressurized to steam, directly by the methanol cooling liquid of steam Connecing reduces two steps, very big to reduce energy consumption.It is exported under positive pressure tower and methanol distillation column is directly connected by pipeline 4, the mixing liquid in methanol positive pressure tower 3 is transported to by methanol by the pressure difference between methanol positive pressure tower 3 and methanol distillation column 4 and is returned It receives in tower 4.
The tower bottom of methanol distillation column 4 is provided with recovery tower heater 41, and the heating temperature of recovery tower heater 41 is 100 DEG C, tower bottom is additionally provided with drainage system 42, and the water that generation is reacted in reaction tower 1 is discharged.Methanol steam is discharged from tower top, then passes through The cooling of subcooler 10 is converted into liquid and flow to No. two return tanks 9.
The exit of No. two return tanks 9 is provided with No. two reflux pumps 91, and there are two outlets for setting on No. two reflux pumps 91, divides The methanol in No. two return tanks 9 methanol distillation column 4 and methanol positive pressure tower 3 are not delivered to.
Above-described embodiment is only presently preferred embodiments of the present invention, is not limited the scope of the invention according to this, therefore: it is all according to The equivalence changes that structure of the invention, shape, principle are done, should all be covered by within protection scope of the present invention.

Claims (7)

1. a kind of high-efficiency low energy consumption sodium methoxide equipment for purifying, it is characterised in that: including reaction tower (1), methanol atmospheric tower (2), first Alcohol positive pressure tower (3) and methanol distillation column (4);The alkali liquid tank (6) of reaction tower (1) connection, the methanol tank (5) pass through pipe Road is connect with reaction tower (1);
The bottom of the reaction tower (1) offers discharge port, and the discharge port is connect with finished pot (17) by pipeline, it is described go out Discharging pump (13) are provided on pipeline between material mouth and finished pot (17);
Exhaust outlet is offered at the top of the reaction tower (1), the exhaust outlet passes through the bottom of pipeline and the methanol atmospheric tower (2) Portion connection, by the pipeline by reaction tower (1) water and methanol steam be delivered to methanol atmospheric tower (2);
The bottom of methanol atmospheric tower (2) is also provided under atmospheric tower and exports, and exit is provided with atmospheric tower discharging pump under atmospheric tower (22), methanol atmospheric tower (2) interior liquid is delivered to by methanol positive pressure tower (3) by the atmospheric tower discharging pump (22);
Atmospheric tower upper outlet is offered at the top of methanol atmospheric tower (2), atmospheric tower upper outlet connects No.1 return tank by pipeline (8);
The outlet of the No.1 return tank (8) is provided with No.1 reflux pump (81), is provided with two on the No.1 reflux pump (81) No.1 return tank (8) interior liquid is delivered to methanol atmospheric tower (2) and methanol positive pressure by two discharge ports by a outlet respectively In tower (3);
The bottom of methanol positive pressure tower (3) is also provided under positive pressure tower and exports, and outlet connects methanol by pipeline under the positive pressure tower Recovery tower (4);
Positive pressure tower upper outlet is also provided at the top of methanol positive pressure tower (3), the positive pressure tower upper outlet is connected by pipeline to react Tower (1);
The bottom of methanol distillation column (4) offers drainage system (42), will react generated by the drainage system (42) Waste water discharge;
Recovery tower upper outlet is offered at the top of methanol distillation column (4), recovery tower upper outlet connects No. two return tanks by pipeline (9);
The outlet of No. two return tanks (9) is provided with No. two reflux pumps (91), is provided with two on No. two reflux pumps (91) No. two interior liquid of return tank (9) are delivered to methanol distillation column (4) and methanol positive pressure by two discharge ports by a outlet respectively In tower (3).
2. a kind of high-efficiency low energy consumption sodium methoxide equipment for purifying according to claim 1, it is characterised in that: the alkali liquid tank (6) outlet end is provided with feed pump (61), is provided with preheater (62), first between the feed pump (61) and reaction tower (1) The outlet end of alcohol tank (5) is provided with methanol pump (51);The bottom of reaction tower (1) is provided with the reaction tower heated to reaction tower (1) Heater (11), by the heater by the water vapor in reaction tower (1), the water for generating reaction and sodium methoxide separation.
3. a kind of high-efficiency low energy consumption sodium methoxide equipment for purifying according to claim 2, it is characterised in that: the methanol normal pressure The bottom of tower (2) is provided with the atmospheric tower heater (21) heated to methanol atmospheric tower (2);
The bottom of the methanol positive pressure tower (3) is provided with the positive pressure tower heater (31) heated to methanol positive pressure tower (3);
The bottom of methanol distillation column (4) is provided with the recovery tower heater (41) heated to methanol distillation column (4).
4. a kind of high-efficiency low energy consumption sodium methoxide equipment for purifying according to claim 3, it is characterised in that: the methanol positive pressure Pressure in tower (3) is greater than reaction tower (1), methanol atmospheric tower (2), methanol distillation column (4).
5. a kind of high-efficiency low energy consumption sodium methoxide equipment for purifying according to claim 4, it is characterised in that: atmospheric tower upper outlet It is provided with cooler (10) between No.1 return tank (8), the gas in pipeline is converted to by liquid by the cooler (10) Body flow to No.1 return tank (8).
6. a kind of high-efficiency low energy consumption sodium methoxide equipment for purifying according to claim 5, it is characterised in that: recovery tower upper outlet Cooler (10) are provided between No. two return tanks (9), the gas in pipeline is converted to by liquid by the cooler (10) Body flow to No. two return tanks (9).
7. a kind of high-efficiency low energy consumption sodium methoxide equipment for purifying according to claim 6, it is characterised in that: the cooler It (10) include that first latter linked condenser (101) and tail condenser (102), tail condenser (102) can carry out the gas in pipeline Secondary cooling.
CN201910087708.8A 2019-01-29 2019-01-29 A kind of high-efficiency low energy consumption sodium methoxide equipment for purifying Pending CN109627145A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP4074684A1 (en) * 2021-04-16 2022-10-19 Evonik Functional Solutions GmbH Method for the energy-efficient production of alkali metal ethanolates
EP4074685A1 (en) * 2021-04-16 2022-10-19 Evonik Functional Solutions GmbH Method for the energy-efficient production of alkali metal ethanolates

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Publication number Priority date Publication date Assignee Title
EP4074684A1 (en) * 2021-04-16 2022-10-19 Evonik Functional Solutions GmbH Method for the energy-efficient production of alkali metal ethanolates
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