CN103007857A - Industrial water-free oxygen-free production apparatus - Google Patents

Industrial water-free oxygen-free production apparatus Download PDF

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Publication number
CN103007857A
CN103007857A CN2012105201845A CN201210520184A CN103007857A CN 103007857 A CN103007857 A CN 103007857A CN 2012105201845 A CN2012105201845 A CN 2012105201845A CN 201210520184 A CN201210520184 A CN 201210520184A CN 103007857 A CN103007857 A CN 103007857A
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China
Prior art keywords
aqueous
reactor
cooling
oxygen
free
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CN2012105201845A
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Inventor
高建勋
丁雪
董洪荣
王碧波
孙磊
王总超
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New Shores Noah (beijing) Catalytic Technology Co Ltd
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New Shores Noah (beijing) Catalytic Technology Co Ltd
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Priority to CN2012105201845A priority Critical patent/CN103007857A/en
Publication of CN103007857A publication Critical patent/CN103007857A/en
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Abstract

The invention relates to a water-free oxygen-free production apparatus used in the chemical industry. The apparatus comprises a reaction vessel which is respectively connected with a feeding system, an inert gas pressure supplementing system and a condenser cooling system, and a non-aqueous medium cooling system and a non-aqueous medium heating system are arranged out of the reaction vessel. The invention further relates to a preparation method for a chemical product by using the production apparatus. According to the invention, the technical problem of requirements for no water and oxygen in a reaction with participation of an active alkali metal is overcome, effects of heating and cooling are realized through indirect heating and cooling of all the heat sources and cold sources in the whole reaction vessel reaction vessel without a water medium, the advantages of safety, reliability, easy operation and a low manufacturing cost are obtained, and the apparatus is applicable both to common reactions with participation of active alkali metals and strict requirements for no water and oxygen and to a majority of water-free oxygen-free production systems and has a high popularization value in industrial equipment.

Description

Industrialization anhydrous and oxygen-free process units
Technical field
The present invention relates to the anhydrous and oxygen-free process units that a kind of chemical industry is used, in particular under inert gas shielding, heating and the consersion unit system of cooling off by non-aqueous media, belong to technical field of chemical.
Background technology
In chemical experiment and Chemical Manufacture, often can run into some to steam and/or responsive compound or the system of air (wherein oxygenous and steam), in this case, need under the anhydrous and oxygen-free condition, operate.In anhydrous and oxygen-free is synthetic, generally need to carry out the anhydrous and oxygen-free processing to used reagent and solvent, for example with hydride reflow treatment under the atmosphere of inert gas such as nitrogen or argon gas of sodium metal or alkali metal or alkaline-earth metal, do to represent to meet the requirements when solvent that indicator processes is blueness with benzophenone.The reaction system that has even also will vacuumize and the filling inert gas with oil pump is to guarantee air and the aqueous vapor in the Ex-all system.Synthetic for requiring strict especially anhydrous and oxygen-free, also to burn roasting reaction system with fire when vacuumizing with oil pump, to remove the aqueous vapor of reaction system (being generally glass apparatus) adsorption.
Anhydrous and oxygen-free is generally realized by following approach in the laboratory: pass into protective gas in reaction system, for example common N 1. 2, or slightly expensive high-purity N 2Or Ar gas.Allow protective gas by dense H is housed 2SO 4Drexel bottle or the drying tower of drier is housed after result of use better.For not being very sensitive general chemical system for air and steam, this is the protected mode of common most convenient; 2. for the system that needs weighing, grinding, transfer, filtration etc. than complex operations; generally in being full of the glove box of protective gas, operate; put into therein drier and can carry out waterless operation, then can carry out oxygen free operation after passing into inert gas replacement air wherein.But, adopt the glove box of lucite not withstand voltage, can not by the displacement air wherein of bleeding, cause replacing not exclusively and a large amount of wastes of inert gas; 3. for operations such as the backflow under the anhydrous and oxygen-free condition, distillation and filtrations, can use the Schlenk technology, namely for ease of vacuumize, filling with inert gas and simple glass instrument or the device with the piston arm that design.
Also need in some cases inert gas is further processed with the dehydration deoxygenation.For example active copper is twined resistance wire or heating tape in order to deoxygenation; Sodium-potassium-sodium alloy can be further with O in the inert gas 2Be down to below the 1ppm, can remove moisture simultaneously; 4A molecular sieve, palladium-A molecular sieve also can be in order to dewater.
Also often need to adopt the operating condition of anhydrous and oxygen-free during extensive chemical industry is produced, for example need to design the anhydrous and oxygen-free reactor of batch (-type) or continued operation.Whether reach and satisfy this condition on anhydrous and oxygen-free condition and the much degree and often concern Chemical Manufacture and can carry out smoothly even can carry out.The synthetic higher organometallic reagent of activity that has of some anhydrous and oxygen-free participates in reaction, if the control of anhydrous and oxygen-free condition is bad, then can't effectively synthesize.For example relate in the reaction that active alkali metal such as lithium, sodium, potassium participates at some, must strictly prohibit water, otherwise, in case generation fault or seepage, break etc., have water to enter into reaction system after, will produce catastrophic consequence.
Some is difficult to laboratory scale anhydrous and oxygen-free condition realize in industrial production, even some feasiblely also will carry out the improvement that adapts with scale.Need at present a kind of industrialization anhydrous and oxygen-free equipment of safe and reliable, simple to operate and low cost of manufacture badly, this equipment not only will be applicable to general active alkali metal and participate in the strict anhydrous and oxygen-free requirement of reaction, but also will be applicable to the production system of most of anhydrous and oxygen-free.
Summary of the invention
Technical problem to be solved by this invention is to overcome the deficiencies in the prior art; satisfy the anhydrous and oxygen-free demand that extensive chemical industry is produced; the anhydrous and oxygen-free process units that provides a kind of chemical industry to use; this device can be under inert gas shielding; realize heating and cooling by non-aqueous media, can not only realize anhydrous and oxygen-free production with commercial scale, and equipment operating is simple, safety; even in device fails or when seepage occurring, can be not accidents caused yet.
The object of the present invention is to provide following aspect:
(1) the anhydrous and oxygen-free process units used of a kind of chemical industry, it comprises reactor, reactor links to each other with the condenser cooling system with feed system, inert gas ftercompction system respectively, is provided with non-aqueous media cooling system and non-aqueous media heating system in the reactor outside
Wherein, described condenser cooling system comprises condenser, heat exchanger III and cooling medium circulation pipe, they connect by pipeline in twos each other, wherein be filled with non-aqueous cooling medium, be provided with material evaporation mouth and condensation material refluxing opening on reactor top, the material evaporation mouth links to each other with condenser through condensation pipe, and condenser links to each other with road logistics refluxing opening through condenser pipe
Described non-aqueous media cooling system comprises kettle chuck, heat exchanger II and non-aqueous cooling medium circulation pipe, and they connect by pipeline in twos each other, wherein are filled with non-aqueous cooling medium,
Described non-aqueous media heating system comprises kettle chuck, heat exchanger I or heater and non-aqueous heat medium circulating tank, and they connect by pipeline in twos each other, wherein fill non-aqueous heat medium.
(2) according to the anhydrous and oxygen-free process units of above-mentioned (1), this device also is included in the non-aqueous media buffer system that the reactor outside is provided with, this system comprises kettle chuck and non-aqueous media surge tank, and they link to each other by pipeline each other, wherein fill non-aqueous media.
(3) according to the anhydrous and oxygen-free process units of above-mentioned (1) or (2), this device also comprises the pumped vacuum systems that links to each other with reactor.
(4) according to above-mentioned each described anhydrous and oxygen-free process units, this device also comprises the decompression discharge system that links to each other with reactor, this system comprises the decompression discharge bucket that links to each other with reactor by pipeline, wherein, pipeline one end inserts the reactor bottom, valve is set on the pipeline, and discharge bucket links to each other with decompressor.
(5) according to above-mentioned each described anhydrous and oxygen-free process units, wherein, described feed system comprises liquid charging subsystem and feeding-in solid body subsystem,
Liquid charging subsystem comprises the liquid feeder of being located at the reactor top, and the liquid feeder links to each other with reactor by the liquid charge pipe, and under liquid gravity or inert gas effect, liquid is fed to reactor from the liquid feeder through the liquid charge pipe,
The feeding-in solid body subsystem comprises the feeder for solid materials of being located at the reactor top, and feeder for solid materials links to each other with reactor by the solid charge pipe.
(6) according to the anhydrous and oxygen-free process units of upper magic arts (5), wherein, feeder for solid materials comprises stock chest and vibratory sieve, and solid material enters through the feeding-in solid body pipe from stock chest and to be fed to reactor under the effect of vibration of vibratory sieve.
(7) according to above-mentioned each described anhydrous and oxygen-free process units, wherein,
In described non-aqueous media cooling system, at pipeline pump and valve are set, to control circulating of non-aqueous cooling medium, in the heat exchanger II, non-aqueous cooling medium is used as the cooling medium cooling of outer circulation low-temperature receiver, is pumped in the kettle chuck, with the cooling reactor;
In described non-aqueous media heating system, at pipeline pump and valve are set, to control circulating of non-aqueous heat medium, in the situation of using the heat exchanger I, non-aqueous heat medium is used as the heat medium heating of outer circulation thermal source, be pumped in the kettle chuck, with the heating reactor, in the situation of using heater, non-aqueous heat medium is heated by heater, be pumped in the kettle chuck, with the heating reactor;
Described non-aqueous media cooling system and described non-aqueous media heating system are switched use, and described non-aqueous cooling medium is identical with non-aqueous heat medium.
(8) according to above-mentioned each described anhydrous and oxygen-free process units, wherein,
In described non-aqueous media buffer system, at pipeline pump and valve are set, with circulating of control non-aqueous media;
Described non-aqueous media cooling system, described non-aqueous media heating system and described non-aqueous media buffer system are switched and are used, and described non-aqueous cooling medium, non-aqueous heat medium are identical with non-aqueous media.
(9) according to above-mentioned each described anhydrous and oxygen-free process units, wherein,
In described condenser cooling system, at pipeline pump and valve are set, controlling circulating of non-aqueous cooling medium,
In the heat exchanger III, non-aqueous cooling medium is pumped the condenser of flowing through by as the cooling of the cooling medium of outer circulation low-temperature receiver, in condenser so that the volatile material condensing reflux that evaporates in the reactor to reactor.
(10) according to above-mentioned each described anhydrous and oxygen-free process units, wherein, described non-aqueous cooling medium, non-aqueous cooling medium, non-aqueous heat medium are identical with non-aqueous media, are conduction oil.
Adopt anhydrous and oxygen-free process units of the present invention, can beyond the mode of circulating cooling or heating, to cooling off with the contacted non-aqueous media of reaction system such as conduction oil or heating, then conduction oil is pumped into kettle chuck and/or condenser first, realize cooling or heating.Among the present invention, all thermals source of reactor (such as non-aqueous heat medium) and low-temperature receiver (such as non-aqueous cooling medium, non-aqueous cold energy medium etc.) all are the effects that reaches heating or cooling by the mode of indirect and cooling, these thermals source or low-temperature receiver medium are non-aqueous media, therefore, its heating and cooling are simple to operate, low cost of manufacture not only, and safe and reliable, thereby be applicable to the reaction that common active alkali metal participates in, also be applicable to the production system of other anhydrous and oxygen-frees.
The following specifically describes the present invention.
In this application, used term " non-aqueous media " refers to water-free conductivity of heat fluid media (medium), and preferred non-aqueous liquid medium is such as the heat conduction wet goods.Using under the heat conduction oil condition, its operating temperature interval is preferably-30 ~ 350 ℃, more preferably-10 ~ 200 ℃.
" the non-aqueous cooling medium " that relates to herein, " non-aqueous cooling medium " and " non-aqueous heat medium " all belong to " non-aqueous media ".
In anhydrous and oxygen-free process units according to the present invention, reactor refers to various still reaction containers commonly used in the Chemical Manufacture, for example, is applicable in the presence of sodium and the toluene as solvent the reactor that triphenylphosphine and 0-chloro-benzoic acid sodium react.Carry out under the anhydrous and oxygen-free condition in order to ensure reaction system, the preferred reaction still has good gas and liquid closed property, thereby avoids gas and moisture to enter in the reactor.
In order to ensure not introducing oxygen and moisture in the reaction system; realize non-water heating or cooling; in the present invention; reaction system is protected by inert gas; and; used heating, cooling, condensation and thermal insulation medium all use non-aqueous media, thereby avoid introducing oxygen and moisture in reaction system and the reaction.
Particularly, inert gas ftercompction system is set, inert gas ftercompction system is connected with reactor.When reaction system is carried out gas displacement or vacuum ftercompction, can replace or mend to pressure-fired with inert gas by inert gas, more to external world emptying, thus avoid air to enter in the reactor.
As inert gas, can use industrial inertia gas commonly used, such as in nitrogen, argon gas or the helium one or more.As the source of the gas of inert gas, can be the inert gas steel cylinder, as long as perhaps nitrogen, argon gas or helium generation systems are the water content of inert gas<0.1%.
Preferred embodiment a kind of according to the present invention, in the beginning production phase, the air in the reactor and/or aqueous vapor are removed.In the case; can reactor be vacuumized by pumped vacuum systems; then in reactor, be filled with inert gas by inert gas ftercompction system; preferred inert gas replacement repeatedly; until reach pressure-fired in the last still; and then to external world emptying, and keep in process of production inert gas shielding always.
Preferably, pumped vacuum systems is set, inert gas ftercompction system links to each other with reactor, can control by valve the connected state of pumped vacuum systems and reactor.When valve opening, pumped vacuum systems is communicated with reactor, and the gas in the reactor is evacuated system and extracts out; When valve closing, pumped vacuum systems is not communicated with reactor, and gas reactor is also discharged without pumped vacuum systems.By pumped vacuum systems, can easily with extractions such as reaction gas reactor such as air, be the anaerobic situation thereby keep in the reactor.
Preferably, the decompression discharge system is set, this system links to each other with reactor, comprises the decompression discharge bucket that links to each other with reactor by pipeline, and wherein, pipeline one end inserts the reactor bottom, and valve is set on the pipeline, and discharge bucket links to each other with decompressor.Valve can be controlled the connected state of decompression discharge system and reactor.When valve opening, reactor with the decompression discharge system be connected, this moment open pressure reducing device, under suction function, reaction mass enters the decompression discharge bucket through pipeline.When valve closing, reactor is not communicated with the decompression discharge system.By the decompression discharge system, can under reduced pressure collect reaction mass, namely simple and convenient, safe and reliable again.
In anhydrous and oxygen-free process units according to the present invention, at reactor outer setting kettle chuck, be used for holding non-aqueous heat medium or non-aqueous cooling medium etc.The kettle chuck can arrange one or more, links to each other with the pipeline of the pipeline of non-aqueous media cooling system, non-aqueous heating system and the pipeline of non-aqueous media buffer system respectively.Preferably, for the non-aqueous heat medium that heats, identical with the non-aqueous media that is used for cushioning for the non-aqueous cooling medium of cooling, like this, the kettle chuck can only arrange one, uses non-aqueous media cooling system, non-aqueous heating system and non-aqueous media buffer system by switching.
In described non-aqueous media cooling system, at pipeline pump and valve are set, to control circulating of non-aqueous cooling medium, in the heat exchanger II, non-aqueous cooling medium is used as the cooling medium cooling of outer circulation low-temperature receiver, is pumped in the kettle chuck, with the cooling reactor.In the situation of valve opening, non-aqueous cooling medium system starts, at this moment, non-aqueous cooling medium flows out from non-aqueous cooling medium circulating tank, is used as the cooling medium cooling of outer circulation low-temperature receiver in the heat exchanger II, at the effect of the pump kettle chuck of flowing through, in the kettle chuck, thereby carrying out heat exchange, the non-aqueous cooling medium of low temperature and reactor heat up, be back to non-aqueous cooling medium circulating tank, so circulate, finish the cooling to reactor.
As the cooling medium of outer circulation low-temperature receiver, can use recirculated water, chilled brine, liquefied ammonia or compression cold air etc.Like this, non-aqueous cooling medium can be cooled to by the cooling medium of outer circulation low-temperature receiver the temperature of expectation, thereby is used for lowering the temperature to reactor.
In described non-aqueous media heating system, at pipeline pump and valve are set, to control circulating of non-aqueous heat medium.In the situation of valve opening, non-aqueous heat medium system starts, at this moment, non-aqueous heat medium flows out from non-aqueous heat medium circulating tank, in the situation of using the heat exchanger I, non-aqueous heat medium is used as the heat medium heating of outer circulation thermal source in the heat exchanger I, in the situation of using heater, non-aqueous reaction medium is directly heated by heater, the non-aqueous heat medium of high temperature is pumped in the kettle chuck, the heating reactor, and the non-aqueous heat medium that temperature reduces flows back to non-aqueous heat medium circulating tank, so circulate, finish the heating to reactor.
As the heat medium of outer circulation thermal source, can use steam, hot water etc.
In preferred embodiment, in order to prevent quenching or shock heating reactor to be caused damage, the non-aqueous media buffer system is set, comprise with the kettle chuck by the non-aqueous property medium surge tank that pipeline links to each other pump and valve being set on the pipeline.When valve opening, the non-aqueous media buffer system is opened, and the suitable non-aqueous media of temperature flows back to non-aqueous property medium surge tank again from the non-aqueous property medium surge tank kettle chuck of flowing through.By the non-aqueous media buffer system is set, suitable non-aqueous media cushions suitably to utilize temperature between heating and cooling, can avoid temperature of reaction kettle sharply to raise or reduction, thereby improve production safety.
In the present invention, preferably, the non-aqueous media temperature that stores in the non-aqueous media surge tank is at the zone line of operation temperature, for example 30-80 ℃, because medium is identical, switch when using non-aqueous heating system, non-aqueous cooling system and the non-aqueous media circulatory system, can be owing to mixing of medium produces harmful effect, moderate moisture then can reduce quenching or the shock heating impact that reaction kettle body is caused relatively, avoids causing the kettle explosion.
In anhydrous and oxygen-free process units according to the present invention, at reactor the non-aqueous media condenser system is set, be used for the volatilization of cooling for reflux reaction system/evaporation material.Like this, can guarantee the volatile material in the reaction system or the evaporation material that is heated can not scatter and disappear, the material of backflow can continue to use after condensation.
In device according to the present invention, described condenser cooling system links to each other with reactor, comprise condenser, heat exchanger III and cooling medium circulating tank, they connect by pipeline in twos each other, wherein be filled with non-aqueous cooling medium, pipeline is provided with valve and pump, is used for controlling flowing of non-aqueous cooling medium; Be provided with material evaporation mouth and condensation material refluxing opening on reactor top, the material evaporation mouth links to each other with condenser through condensation pipe, and condenser links to each other with road logistics refluxing opening through condenser pipe.When valve opening, the condenser start-up of cooling system, non-aqueous cooling medium flows out from the cooling medium circulating tank, in the heat exchanger III, be used as the cooling medium cooling of outer circulation low-temperature receiver, be pumped in the condenser, in the case, volatile material or be subjected to thermal evaporation from the material evaporation mouth through the condensation pipe condenser of flowing through, in condenser, by the non-aqueous cooling medium condensation of low temperature, flow back in the reactor through condensation material refluxing opening by condensation pipe.
Wherein, as the cooling medium of outer circulation low-temperature receiver, can use recirculated water, chilled brine, liquefied ammonia or compression cold air etc.
In anhydrous and oxygen-free process units according to the present invention, as feed system, be used for adding the liquid or solid raw material to reaction kettle body, preferably include liquid charging subsystem and feeding-in solid body subsystem.
In preferred embodiment, as liquid charging subsystem, comprise the liquid feeder of being located at the reactor top, the liquid feeder links to each other with reactor by the liquid charge pipe, under liquid gravity or inert gas effect, liquid is fed to reactor from the liquid feeder through the liquid charge pipe.Like this, realize completely cutting off with air by the feed way that adopts the pushing of liquid self-flowing or inert gas, thereby realize the purpose that anhydrous and oxygen-free of the present invention is produced.
In liquid charging subsystem, reinforced its of described liquid can adopt elevated dosing vessel, by the adding speed of control measuring tank, for example controls with valve, can or add fast liquid material to dropping in the reactor.Described liquid material can be to be sent in the elevated dosing vessel in the mode of pump, hydraulic pressure or vacuum in batches or continuously.For example the toluene solution that is dissolved with triphenylphosphine can be pumped into elevated dosing vessel, then drop in the reactor.
In preferred embodiment, the feeding-in solid body subsystem comprises the feeder for solid materials of being located at the reactor top, feeder for solid materials links to each other with reactor by the solid charge pipe, wherein, feeder for solid materials comprises stock chest and vibratory sieve, solid material enters through the feeding-in solid body pipe from stock chest and to be fed to reactor under the effect of vibration of vibratory sieve.
In the feeding-in solid body subsystem, solid material is sent to stock chest, under inert gas shielding, can add solid material in reactor by the control vibratory sieve.For example the mode of the 0-chloro-benzoic acid sodium salt in the stock chest with vibratory sieve at the uniform velocity added in the reactor.
Preferred embodiment a kind of according to the present invention, can the similar liquids material such for the solid-liquid compound, be fed in the reactor by liquid charging subsystem.
The outstanding characteristics of anhydrous and oxygen-free process units of the present invention are, relate to the reaction that active alkali metal lithium, sodium, potassium participate in, various cooling/the cooling mediums or the heat medium that contact with reaction system are non-aqueous media, break down, break or damage or during exception parking, also be unlikely to have an accident owing to moisture content enters into reaction system at certain equipment or parts even can guarantee.
The invention still further relates to the application of above-mentioned anhydrous and oxygen-free process units.Particularly, the invention provides a kind of employing anhydrous and oxygen-free process units of the present invention and prepare the benzoic production technology of meta-diphenylphosphine, this process is take triphenylphosphine as initiation material, itself and alkali metal carry out cracking in solvent, generate the diphenylphosphine alkali metal salt, add again m-chlorobenzoic acid salt and generate the diphenylphosphine benzoate, generate meta-diphenylphosphine benzoic acid finally by basic hydrolysis.Described solvent adopts toluene, and described alkali metal can be to be lithium, sodium or potassium, and described 0-chloro-benzoic acid salt can be 0-chloro-benzoic acid lithium, 0-chloro-benzoic acid sodium, 0-chloro-benzoic acid potassium.
Particularly, production technology of the present invention may further comprise the steps:
1) starts pumped vacuum systems, reactor is vacuumized, by liquid charging subsystem charging organic solvent such as toluene, by feeding-in solid body subsystem charging alkali metal such as sodium, vacuumize by pumped vacuum systems, system carries out inert gas replacement by the inert gas ftercompction, until the still internal gas pressure is pressure-fired;
2) start the condenser cooling system, opening simultaneously the non-aqueous media heating system heats up reactor, preferably 95-105 to be warming up to ℃, after the sodium dissolving, preferably under stirring state, dropwise be fed in the reactor the complete rear insulation of charging by the toluene solution of liquid charging subsystem with triphenylphosphine;
3) close the non-aqueous media heating system, open the slow system of non-aqueous media heat, system temperature is reduced, preferably be down to 40-50 ℃ of interval, close the slow system of non-aqueous media heat and open the non-aqueous media cooling system, precooling choosing to-10-20 ℃ conduction oil is pumped into reacting kettle jacketing, system temperature is reduced, preferably be down to 0 when spending, with the mode of m-chlorobenzoic acid sodium salt with vibratory sieve, preferably at the uniform velocity add in the reaction system by the solid feeding device;
4) close the non-aqueous media cooling system, open the non-aqueous media buffer system, when treating that temperature is increased to preferred about 50 ℃ of left and right sides, close the non-aqueous media buffer system, start the decompression discharge system, decompression desolvation toluene, then drip absolute methanol by liquid charging subsystem, to destroy unreacted sodium metal, then drip alkaline aqueous solution, discharging.
Description of drawings
Fig. 1 is the structural representation of anhydrous and oxygen-free process units according to the preferred embodiment of the present invention.
The specific embodiment
Below in conjunction with accompanying drawing, further specify the present invention with reference to the preferred specific embodiment.Characteristics of the present invention and advantage will become more clear along with these explanations.But, these embodiments only are illustrative, and it is to protection scope of the present invention and do not constitute any limitation.It will be appreciated by those skilled in the art that in the situation that does not exceed or depart from protection domain of the present invention, technical solutions and their implementation methods of the present invention have multiple modification, improvement or equivalent, these all should fall within the scope of protection of the present invention.
As shown in Figure 1, anhydrous and oxygen-free process units of the present invention comprises reactor 1, condenser cooling system 2, feed system 3, inert gas ftercompction system 4, non-aqueous media cooling system 5, non-aqueous media heating system 6 and non-aqueous media buffer system 7.
Reactor 1 outer setting chuck 11 wherein can flow through non-aqueous heat medium or non-aqueous cooling medium.
In feed system 3, as the liquid feed pot 31 of liquid charging device be connected solid feeding device solid vibration material feeding 32 and be connected with reactor 1 respectively, each is controlling switch and flow by valve.Solid vibration material feeding 32 comprises stock chest (not shown) and vibratory sieve (not shown), and material wherein is in (not shown) under the nitrogen protection.
Inert gas ftercompction system 4 directly links to each other with reactor 1, when system gas displacement or vacuum ftercompction, is all replaced or mended just to external world emptying to the pressure-fired by inert gas.
Condenser cooling system 2 comprises condenser 21, wherein fills non-aqueous cooling medium such as conduction oil.The cooling mediums such as cold water, chilled brine, liquefied ammonia or compression cold air by outer circulation cool off the conduction oil that pumps from non-aqueous cooling medium circulating tank 23 in heat exchanger III 22 first, then with the pumping mode circular flow through condenser 21, realize non-aqueous condensation.
In non-aqueous media cooling system 5, use conduction oil as non-aqueous cooling medium.First cooling mediums such as the cold water by outer circulation, chilled brine, liquefied ammonia or compression cold air, the conduction oil that cooling is pumped from non-aqueous cooling medium circulating tank 52 in heat exchanger II 51, then Heat-transfer Oil Pump is delivered in the kettle chuck 11, realized non-aqueous cooling.
Non-aqueous media heating system 6 is to switch to use with non-aqueous media cooling system 5, and the non-aqueous heat medium of wherein filling is conduction oil.When needs heat for reactor 1, in heat exchanger I 61, heat the conduction oil that from non-aqueous heat medium circulating tank 62, pumps by heat mediums such as steam, hot water first, then Heat-transfer Oil Pump is delivered in the reaction kettle body chuck 11, realize non-aqueous heating.
In the non-aqueous media buffer system, reactor 1 also is connected with non-aqueous media surge tank 71, wherein contains the non-aqueous media conduction oil.
Reactor 1 also links to each other with pumped vacuum systems 8, inert gas ftercompction system 4 and decompression discharge system 9 respectively.
Below describe by using anhydrous and oxygen-free process units shown in Figure 1, produce the benzoic production technology of meta-diphenylphosphine.
Vacuum suction toluene is 1200 kilograms in the 3000L reactor 1, opens the still manhole cover, drops into sodium metal 69kg, covers manhole cover, vacuumize, nitrogen replacement three times rushes pressure-fired to the still for the last time, open drain, and keep always crack opening of nitrogen, with the maintenance system atmosphere of inert gases.
Open cold condenser refrigerating circulation system gives condenser 21 coolings.Then, open the non-aqueous media heating system, heat up to system, wait to be warming up to 95 ℃, sodium is opened and is stirred after slowly dissolving, and will be dissolved with the 393kg triphenylphosphine and drop to reactor to the 500L toluene solution, after dropwising, is incubated 30 minutes.
Close the non-aqueous media heating system, open the non-aqueous media buffer system, system temperature is down to 40-50 ℃ of interval after, close the non-aqueous media buffer system.Open the non-aqueous media cooling system, the conduction oil that is cooled in advance-10 ℃ is pumped into reacting kettle jacketing, treat that system temperature is down to 0 degree, at the uniform velocity join in reaction system by vibratory sieve 268kg m-chlorobenzoic acid sodium salt again, in the reinforced process, system has heat release, cold circulating pump one direct-open.
After temperature rises to maximum temperature, close the non-aqueous media cooling system, open the slow system of non-aqueous heat, when treating that temperature rises to 50 ℃ of left and right sides, close the non-aqueous media buffer system, open the non-aqueous media heating system, solvent toluene is deviate from decompression, then drip buck, blowing changes post processor over to.
Wash still, oven dry enters next batch and feeds intake.
More than switching can be manual operations, also can realize automaticallying switch by the mode of automation control, reduces the error that manually-operated may form.

Claims (10)

1. anhydrous and oxygen-free process units that chemical industry is used, it comprises reactor, reactor links to each other with the condenser cooling system with feed system, inert gas ftercompction system respectively, is provided with non-aqueous media cooling system and non-aqueous media heating system in the reactor outside
Wherein, described condenser cooling system comprises condenser, heat exchanger III and cooling medium circulation pipe, they connect by pipeline in twos each other, wherein be filled with non-aqueous cooling medium, be provided with material evaporation mouth and condensation material refluxing opening on reactor top, the material evaporation mouth links to each other with condenser through condensation pipe, and condenser links to each other with road logistics refluxing opening through condenser pipe
Described non-aqueous media cooling system comprises kettle chuck, heat exchanger II and non-aqueous cooling medium circulation pipe, and they connect by pipeline in twos each other, wherein are filled with non-aqueous cooling medium,
Described non-aqueous media heating system comprises kettle chuck, heat exchanger I or heater and non-aqueous heat medium circulating tank, and they connect by pipeline in twos each other, wherein fill non-aqueous heat medium.
2. according to claim 1 anhydrous and oxygen-free process units, this device also is included in the non-aqueous media buffer system that the reactor outside is provided with, this system comprises kettle chuck and non-aqueous media surge tank, and they link to each other by pipeline each other, wherein fill non-aqueous media.
3. according to claim 1 and 2 anhydrous and oxygen-free process units, this device also comprises the pumped vacuum systems that links to each other with reactor.
4. according to claim 1 to one of 3 anhydrous and oxygen-free process units, this device also comprises the decompression discharge system that links to each other with reactor, this system comprises the decompression discharge bucket that links to each other with reactor by pipeline, wherein, pipeline one end inserts the reactor bottom, valve is set on the pipeline, and discharge bucket links to each other with decompressor.
5. according to claim 1 to one of 4 anhydrous and oxygen-free process units, wherein, described feed system comprises liquid charging subsystem and feeding-in solid body subsystem,
Liquid charging subsystem comprises the liquid feeder of being located at the reactor top, and the liquid feeder links to each other with reactor by the liquid charge pipe, and under liquid gravity or inert gas effect, liquid is fed to reactor from the liquid feeder through the liquid charge pipe,
The feeding-in solid body subsystem comprises the feeder for solid materials of being located at the reactor top, and feeder for solid materials links to each other with reactor by the solid charge pipe.
6. according to claim 5 anhydrous and oxygen-free process units, wherein, feeder for solid materials comprises stock chest and vibratory sieve, solid material enters through the feeding-in solid body pipe from stock chest and to be fed to reactor under the effect of vibration of vibratory sieve.
7. according to claim 1 to one of 6 anhydrous and oxygen-free process units, wherein,
In described non-aqueous media cooling system, at pipeline pump and valve are set, to control circulating of non-aqueous cooling medium, in the heat exchanger II, non-aqueous cooling medium is used as the cooling medium cooling of outer circulation low-temperature receiver, is pumped in the kettle chuck, with the cooling reactor;
In described non-aqueous media heating system, at pipeline pump and valve are set, to control circulating of non-aqueous heat medium, in the situation of using the heat exchanger I, non-aqueous heat medium is used as the heat medium heating of outer circulation thermal source, be pumped in the kettle chuck, with the heating reactor, in the situation of using heater, non-aqueous heat medium is heated by heater, be pumped in the kettle chuck, with the heating reactor;
Described non-aqueous media cooling system and described non-aqueous media heating system are switched use, and described non-aqueous cooling medium is identical with non-aqueous heat medium.
8. according to claim 1 to one of 7 anhydrous and oxygen-free process units, wherein,
In described non-aqueous media buffer system, at pipeline pump and valve are set, with circulating of control non-aqueous media,
Described non-aqueous media cooling system, described non-aqueous media heating system and described non-aqueous media buffer system are switched and are used, and described non-aqueous cooling medium, non-aqueous heat medium are identical with non-aqueous media.
9. according to claim 1 to one of 8 anhydrous and oxygen-free process units, wherein,
In described condenser cooling system, at pipeline pump and valve are set, controlling circulating of non-aqueous cooling medium,
In the heat exchanger III, non-aqueous cooling medium is pumped the condenser of flowing through by as the cooling of the cooling medium of outer circulation low-temperature receiver, in condenser so that the volatile material condensing reflux that evaporates in the reactor to reactor.
The installation form of described heat exchanger can be vertical, also can be horizontal, wherein take vertical as preferred installation form.
10. according to claim 1 to one of 9 anhydrous and oxygen-free process units, wherein, described non-aqueous cooling medium, non-aqueous cooling medium, non-aqueous heat medium are identical with non-aqueous media, are conduction oil.
CN2012105201845A 2012-12-06 2012-12-06 Industrial water-free oxygen-free production apparatus Pending CN103007857A (en)

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