CN106378060B - High temperature and pressure full-automatic chemical reaction system - Google Patents
High temperature and pressure full-automatic chemical reaction system Download PDFInfo
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- CN106378060B CN106378060B CN201611089430.0A CN201611089430A CN106378060B CN 106378060 B CN106378060 B CN 106378060B CN 201611089430 A CN201611089430 A CN 201611089430A CN 106378060 B CN106378060 B CN 106378060B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J3/00—Processes of utilising sub-atmospheric or super-atmospheric pressure to effect chemical or physical change of matter; Apparatus therefor
- B01J3/04—Pressure vessels, e.g. autoclaves
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F25/00—Flow mixers; Mixers for falling materials, e.g. solid particles
- B01F25/50—Circulation mixers, e.g. wherein at least part of the mixture is discharged from and reintroduced into a receptacle
- B01F25/51—Circulation mixers, e.g. wherein at least part of the mixture is discharged from and reintroduced into a receptacle in which the mixture is circulated through a set of tubes, e.g. with gradual introduction of a component into the circulating flow
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F33/00—Other mixers; Mixing plants; Combinations of mixers
- B01F33/70—Mixers specially adapted for working at sub- or super-atmospheric pressure, e.g. combined with de-foaming
- B01F33/71—Mixers specially adapted for working at sub- or super-atmospheric pressure, e.g. combined with de-foaming working at super-atmospheric pressure, e.g. in pressurised vessels
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F35/00—Accessories for mixers; Auxiliary operations or auxiliary devices; Parts or details of general application
- B01F35/71—Feed mechanisms
- B01F35/716—Feed mechanisms characterised by the relative arrangement of the containers for feeding or mixing the components
- B01F35/7164—Feed mechanisms characterised by the relative arrangement of the containers for feeding or mixing the components the containers being placed in parallel before contacting the contents
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F35/00—Accessories for mixers; Auxiliary operations or auxiliary devices; Parts or details of general application
- B01F35/71—Feed mechanisms
- B01F35/717—Feed mechanisms characterised by the means for feeding the components to the mixer
- B01F35/71805—Feed mechanisms characterised by the means for feeding the components to the mixer using valves, gates, orifices or openings
- B01F35/718051—Feed mechanisms characterised by the means for feeding the components to the mixer using valves, gates, orifices or openings being adjustable
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F35/00—Accessories for mixers; Auxiliary operations or auxiliary devices; Parts or details of general application
- B01F35/90—Heating or cooling systems
- B01F35/93—Heating or cooling systems arranged inside the receptacle
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J3/00—Processes of utilising sub-atmospheric or super-atmospheric pressure to effect chemical or physical change of matter; Apparatus therefor
- B01J3/06—Processes using ultra-high pressure, e.g. for the formation of diamonds; Apparatus therefor, e.g. moulds or dies
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J4/00—Feed or outlet devices; Feed or outlet control devices
- B01J4/008—Feed or outlet control devices
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F35/00—Accessories for mixers; Auxiliary operations or auxiliary devices; Parts or details of general application
- B01F35/90—Heating or cooling systems
- B01F2035/99—Heating
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2204/00—Aspects relating to feed or outlet devices; Regulating devices for feed or outlet devices
- B01J2204/002—Aspects relating to feed or outlet devices; Regulating devices for feed or outlet devices the feeding side being of particular interest
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J2219/00049—Controlling or regulating processes
- B01J2219/00051—Controlling the temperature
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J2219/00049—Controlling or regulating processes
- B01J2219/00162—Controlling or regulating processes controlling the pressure
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J2219/00049—Controlling or regulating processes
- B01J2219/00245—Avoiding undesirable reactions or side-effects
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Abstract
A kind of high temperature and pressure full-automatic chemical reaction system, the circulation major loop including closure, circulation major loop are equipped with: high pressure liquid phase circulating pump, for driving the reaction mixture in circulation major loop to circulate；Detector, for monitoring the chemical reaction course in circulation major loop；Pressure regulator, for adjusting the pressure in circulation major loop；Switching valve is connected in circulation major loop, and for the input and output of material, switching valve includes the first switching valve and the second switching valve；Exhaust valve is connected on circulation major loop, discharges for gas；Reagent introduction device, for providing reaction reagent, reagent introduction device includes reaction mixed organization, and reaction mixed organization is connected in circulation major loop by the first switching valve；Product collecting device is connected in circulation major loop by the second switching valve, and is located between the input port and the delivery outlet for reacting mixed organization of high pressure liquid phase circulating pump.Reaction system controllability of the present invention is high；It can directly amplify.
Description
Technical field
The present invention relates to chemical reactor technical fields, and in particular to a kind of high temperature and pressure full-automatic chemical reaction system.
Background technique
Chemical reaction is that mutually collision generates the process of structural rearrangement between reactant molecule, therefore needs during the reaction
Temperature-pressure and stirring are wanted, so that molecular motion acutely furthers with distance, reaction could be accelerated in this way, it is flat to reach chemistry as early as possible
Weighing apparatus.It is exactly to reach terminal that reaction, which reaches chemical balance,.
Chemical reaction is carried out in opening, reflux or closed reaction vessel at present.Open and reflow type reaction unit
Reaction condition generally can only be normal pressure, temperature is at maximum up to 100 ~ 200oC, and generally required professional and waited for pass
Note.Under conditions of temperature, pressure is not high, reaction usually needs even time a couple of days a few hours that could complete, and has not only consumed artificial but also has deposited
In safety and endanger the problems such as healthy.Even with micro-wave oven reactor, reaction carries out in closed container, temperature and pressure
All relatively milder, maximum pressure also can only be within 10 atmospheric pressure, and temperature about can achieve 300 ~ 400oC.This reactant
It is that speed is accelerated, but closed system is not suitable for generating the reaction of gas, if because product gas cannot be from reactant
It is discharged in system, reaction cannot be complete, and yield when reaching chemical balance is accordingly relatively low.
Moreover overwhelming majority chemical reaction must be the homogeneous reaction under liquid-phase condition, otherwise reaction is difficult to carry out, and needs
It is lot more time to obtain product, cannot be used to do chemical synthesis.In order to allow chemical reaction to react under liquid phase homogeneous phase condition, instead
Answer object that must dissolve, but many reactants must use the dissolution that toxicity is big or price is high that could dissolve, cause it is safe and environment-friendly,
The various problems such as cost.
In addition, in the synthesis process of medicament research and development, the compound amount very little that initial drug screening needs, milligram quantities
Reaction is just able to satisfy requirement, and after screening determining drug effect and bioavilability, selected compounds can enter preclinical laboratory,
At this moment synthetic quantity must just reach feather weight, moreover, preclinical laboratory must have determining synthesis technology before carrying out, it is otherwise real
Testing data cannot act as the application of clinical certification.Therefore, a small amount of synthesis originally have to pass through enlarged experiment research, this process
Very time-consuming, expense also usually million or millions of, not only delays drug discovery process but also increases development cost.In addition to drug is opened
Hair, the research and development of all specific function compounds also all there is a problem of similar.
Therefore, ideal reaction unit should be totally-enclosed, full-automatic, can apply high temperature, high pressure, be suitable for generating gas
The reaction of body, and directly can be with enlarged experiment.High-temperature and high-pressure conditions can not only accelerate to react, and can also improve solubility,
So that the reactant that could be dissolved with toxic solvents is needed to be possible to be completely dissolved in low-toxic solvent and reacted.Obturator
The problems such as system can also topple over to avoid volatilization sputtering, unlikely generation environmental pollution or safety accident.
Summary of the invention
Based on this, the present invention provides a kind of chemical reaction system of high temperature and pressure Full automatic closed, and reaction system is controllable
Property it is high, it is applied widely；It can directly amplify, Speeding up development process simultaneously saves research and development cost.
In order to achieve the object of the present invention, the invention adopts the following technical scheme:
A kind of high temperature and pressure full-automatic chemical reaction unit, the circulation major loop including closure, the circulation major loop are
Closed system, the circulation major loop are equipped with:
High pressure liquid phase circulating pump, for driving the reaction mixture in the circulation major loop to circulate；
Detector, for monitoring the chemical reaction course in the circulation major loop；
Pressure regulator, for adjusting the pressure in the circulation major loop；
Switching valve is connected in the circulation major loop, and for the input and output of material, the switching valve includes first
Switching valve and the second switching valve；
Exhaust valve is connected on the circulation major loop, is discharged for gas；
Reagent introduction device, for providing reaction reagent, the reagent introduction device includes reaction mixed organization, described anti-
Mixed organization is answered to be connected in the circulation major loop by first switching valve；
Product collecting device is connected in the circulation major loop by second switching valve, and is located at the high pressure
Between the input port and the delivery outlet for reacting mixed organization of liquid phase circulation pump, for collecting the product of end of reaction.
In one embodiment, the reaction mixed organization includes several agent reservoirs, each agent reservoirs
It is equipped with import and outlet, the import and outlet of the agent reservoirs are separately connected two interfaces of first switching valve,
The interface that first switching valve connects the agent reservoirs is disposed adjacent with the interface for connecting the circulation major loop.
In one embodiment, the agent reservoirs are high-pressure-resistant vessel, and the exit of the agent reservoirs is set
There is high pressure resistant microporous filter element, for stopping the solid matter in the agent reservoirs to squeeze out from the delivery outlet.
In one embodiment, the reagent introduction device further includes liquid introducing member, the liquid introducing member
Include:
Triple valve connects the input terminal of the circulation major loop mesohigh liquid phase circulation pump；
The output end of liquid phase delivery pump is connect by a check valve with the triple valve, and the check valve makes liquid by institute
It states liquid phase delivery pump and flows to the triple valve；
Several liquid reagent storage bottles for being used to hold liquid reagent；
To channel selector valve, the common interface of the multi-center selection valve is connected to the input terminal of the liquid phase delivery pump；
Each selector channel interface of the multi-center selection valve is correspondingly connected with the liquid reagent storage bottle.
In one embodiment, the reagent introducing member may also include a waste liquid bottle, waste liquid bottle and multi-center selection
A wherein selector channel orifice for valve.
In one embodiment, the product collecting device includes:
Product collection vessel is connect with second switching valve, for collecting the product prepared in the circulation major loop；
Pressure slow release valve is mounted on the top of the product collection vessel, is collected into the product for slow release and receives
Collect the pressure of the product in container；
Air intake filter is connect with second switching valve, is entered in the product collection vessel or is entered for filtering
To the gas in circulation major loop.
In one embodiment, the product collecting device further includes the totally-enclosed pressure casing for processing gas,
The totally-enclosed pressure casing is between pressure slow release valve and product collection vessel, the air inlet of the totally-enclosed pressure casing
The gas outlet at the top of the product collection vessel and the air inlet of pressure slow release valve, the full envelope are respectively communicated with gas outlet
It closes in pressure casing filled with filter material.
It in one embodiment, further include a hybrid heating device, the body for solution in the circulation major loop
Product buffering, mixing and heating；The hybrid heating device include a mixing pit, the inert material being filled in the mixing pit and
Heated for controlling temperature mechanism in the mixing pit；The inert material is in pearl or cellular, for increasing wherein liquid object
The mixing efficiency of matter.
In one embodiment, the switching valve is at least there are four interface and two channels, institute under one of state
Circulation major loop is stated by one of channel by the switching valve, the circulation major loop passes through two under another state
A channel forms the state disconnected or forms the circulation major loop extended with the channel of periphery.
In one embodiment, multiple switching valves are connected to the circulation major loop in series or in parallel
In.
High temperature and pressure full-automatic chemical reaction system of the present invention, chemical reaction carry out in a closed loop,
Play circulation, periphery heating, pressure regulation, reagent and the column introducing of catalyst dress, the methods such as reaction process on-line checking by pump, it can be
Chemical reaction condition extremely extends, and reaction dissolvent almost can also be selected arbitrarily, many extreme toxicities or corrosive substance
Can safety and rapid synthesis comes out.New reaction system controllable precise, it is fully automated, can continuous output, can also directly put
Greatly, pilot scale is almost not necessarily to develop, and can not only accelerate the process of Preclinical Drug exploitation, but also can largely reduce expenses.
Detailed description of the invention
Fig. 1 is the first working condition of high temperature and pressure full-automatic chemical reaction system described in a preferred embodiment of the present invention
Structural schematic diagram.
Fig. 2 is the structural schematic diagram of second of working condition of high temperature and pressure full-automatic chemical reaction system shown in FIG. 1.
Fig. 3 is the structural schematic diagram of the third working condition of high temperature and pressure full-automatic chemical reaction system shown in FIG. 1.
In figure:
10, major loop is recycled；20, high pressure liquid phase circulating pump；30, pressure regulator；40, detector；51, the first switching
Valve；52, the second switching valve；60, exhaust valve；70, mixed organization is reacted；71, agent reservoirs；80, liquid introducing member；81,
Triple valve；82, liquid phase delivery pump；83, multi-center selection valve；84, selection switch；85, selector channel interface；86, liquid reagent
Storage bottle；87, check valve；90, product collecting device；91, product collection vessel；92, pressure slow release valve；93, air intake filter；
94, totally-enclosed pressure casing；100, hybrid heating device.
Specific embodiment
To facilitate the understanding of the present invention, below in conjunction with attached drawing to invention is more fully described.But it is of the invention
It can be realized using many different forms, however it is not limited to embodiment described herein.The purpose of these embodiments is provided
It is intended merely to help the understanding to the disclosure.
Unless otherwise defined, all technical and scientific terms used herein and belong to technical field of the invention
The normally understood meaning of technical staff is identical.Term as used herein in the specification of the present invention is intended merely to description tool
The purpose of the embodiment of body should not constitute any limitation of the invention.
Fig. 1 to Fig. 3 is please referred to, a kind of high temperature and pressure full-automatic chemical reaction system is a preferred embodiment of the present invention,
The high temperature and pressure full-automatic chemical reaction system includes the circulation major loop 10 of closure, and the height on circulation major loop 10
Hydraulic fluid phase circulating pump 20, detector 40, pressure regulator 30, switching valve, exhaust valve 60, reagent introduction device and product collect dress
Set 90.High pressure liquid phase circulating pump 20 is used to that the reaction mixture in circulation major loop 10 to be driven to circulate；Detector 40 is used
Chemical reaction course in monitoring circulation major loop 10；Pressure regulator 30 is used to adjust the pressure in circulation major loop 10；
Switching valve is connected in circulation major loop 10, and for the input and output of material, switching valve includes the first switching valve 51 and second
Switching valve 52；Exhaust valve 60 is connected on circulation major loop 10, is discharged for gas, the gas generated in reaction can thus from
It is excluded in system, so that reaction can faster more completely；For providing reaction reagent, reagent introduction device includes reagent introduction device
Mixed organization 70 is reacted, reaction mixed organization 70 is connected in circulation major loop 10 by the first switching valve 51；Product collects dress
Set 90 by the second switching valve 52 be connected to circulation major loop 10 in, and be located at high pressure liquid phase circulating pump 20 input port with react
Between the delivery outlet of mixed organization 70, for collecting the product of end of reaction.
Switching valve is at least there are four interface and two channels, and circulation major loop 10 passes through one of them under one of state
Channel is by switching valve, for example, it is this kind that product collecting device 90, which is accessed with the second switching valve 52 on circulation major loop 10,
State, circulation major loop 10 forms the state disconnected by two channels or is formed with peripheral channel under another state
The circulation major loop 10 extended, for example, being linked into the first switching valve 51 recycled in major loop 10 for mixed organization 70 is reacted
For this kind of state.In the present embodiment, the first switching valve 51 and the second switching valve 52 all have four interfaces and two channels.
Reacting mixed organization 70 includes several agent reservoirs 71, there is two interfaces of disengaging on each agent reservoirs 71,
The import and outlet of agent reservoirs 71 are separately connected two adjacent interfaces of the first switching valve 51, the connection examination of the first switching valve 51
The interface of agent reservoir 71 is adjacent with the interface difference for connecting circulation major loop 10.It, can in agent reservoirs 71 in the present embodiment
To place liquid reagent, solid reagent and/or catalyst.Reaction carry out in, the first switching valve 51 by agent reservoirs 71 with follow
Ring major loop 10 is isolated；When need to introduce reaction reagent, agent reservoirs 71 are connected to by the first switching valve 51 with circulation major loop 10.
Reagent introduction device further includes liquid introducing member 80, and liquid introducing member 80 includes triple valve 81, liquid phase conveying
Pump 82, multi-center selection valve 83 and several liquid reagent storage bottles 86；The connection circulation 10 mesohigh liquid phase of major loop of triple valve 81
The input terminal of circulating pump 20；The output end of liquid phase delivery pump 82 is connect by a check valve 87 with triple valve 81, and check valve 87 makes
It obtains liquid and triple valve 81 is flowed to by liquid phase delivery pump 82, it is reversely then obstructed；The common interface of multi-center selection valve 83 is connected to liquid
The input terminal of phase delivery pump 82；The selector channel interface 85 of each multi-center selection valve 83 is correspondingly connected with a liquid reagent storage
Bottle 86.When needing one of multiple liquid reagent storage bottles 86 reagent, liquid phase conveying can be connected to by liquid switching valve
The outflow interface for the liquid reagent storage bottle 86 that the input terminal and required reagent of pump 82 are held, so that the reaction raw materials in reagent bottle
Liquid can be pumped into circulation major loop 10 by liquid phase delivery pump 82, this makes the feed liquor controllable precise entirely reacted, can be with
Adapt to the reaction system of a variety of reaction reagents.
Multi-center selection valve 83 be flowing valve, with one connection liquid phase delivery pump 82 input terminal selection switch 84 with
And at least two selector channel interfaces 85, in the present embodiment, the tool of multi-center selection valve 83 is there are six selector channel interface 85, and six
A selector channel interface 85 six liquid reagent storage bottles 86 of corresponding connection.As needed, the channel number of multi-center selection valve
And the number of corresponding reagent storage bottle can arbitrarily increase and decrease, number does not have any restrictions.
In other embodiments, reagent introducing member may also include a waste liquid bottle, waste liquid bottle and multi-center selection valve 83
Wherein a selector channel interface 85 is connected to, and after cleaning the first liquid phase pump, selects 84 dozens, switch to lead in the selection of corresponding waste liquid bottle
At pipeline joint 85, the waste liquid for cleaning generation can be flowed into waste liquid bottle by multi-center selection valve 83.
Agent reservoirs 71 are high-pressure-resistant vessel, and agent reservoirs 71 have input port and delivery outlet, and delivery outlet is set
There is high pressure resistant microporous filter element, for stopping the solid matter in agent reservoirs 71 to squeeze out from delivery outlet.
Product collecting device 90 includes product collection vessel 91, pressure slow release valve 92 and air intake filter 93；Product is received
Collection container 91 is connect with the second switching valve 52, for collecting the product prepared in circulation major loop 10；Pressure slow release valve 92 is installed
At the top of product collection vessel 91, the pressure of the product in product collection vessel 91 is collected into for slow release, to avoid
Product collection vessel 91 needs to remove that do subsequent processes occurred to spray or splash phenomenon because pressure is excessive after collecting product.
Air intake filter 83 is connect with the second switching valve 52, is followed for filtering to enter in product collection vessel 91 or enter when collecting
Gas in ring major loop 10.During reaction carries out, major loop 10 channels passed through in the second switching valve 52 of circulation,
Product collecting device 90 is then connected directly by another channel in the second switching valve 52 with air intake filter 93, and circulation is led back
Road 10 and product collector 90 are now in mutually isolated state, as shown in Figure 2；When 40 Indicator Reaction of detector is completed
When, the second switching valve 52 is switched to state as shown in Figure 3, i.e. circulation major loop 10 disconnects, and one end passes through the second switching valve 52
In a channel be connected with air intake filter 93, the other end is connected to product by another channel of the second switching valve 52 and collects
The entrance of container 91, at this moment high pressure liquid phase circulating pump 20 continues to run, and major loop will be recycled by sucking air from air intake filter 93
Reaction mixture push in 10 enters in product collection vessel 91.
Product collecting device 90 further includes the discharge filter 94 for processing gas, is connected to pressure slow release valve 92 and produces
Between product collection vessel 91, the air inlet and air outlet of discharge filter 94 are respectively communicated with set on 91 top of product collection vessel
The air inlet of gas outlet and pressure slow release valve 92, discharge filter 91 is interior to be filled with filter material, because of product collection vessel 91
The gas of domestic demand discharge has certain pollution, if being immediately discharged to atmosphere, can generate shadow to the health of environment and people
It rings, by the discharge filter 94 of setting connection product collection vessel 91, and fills filter material in discharge filter 94, make
It obtains after the gas in product collection vessel 91 is filtered by discharge filter 94 and discharges again, avoid environmental pollution.
High temperature and pressure full-automatic chemical reaction system of the invention, further includes a hybrid heating device 100, for recycling
Volume buffering, mixing and the heating of solution, hybrid heating device 100 include a mixing pit, are filled in mixing pit in major loop 10
Interior inert material and the heated for controlling temperature mechanism in mixing pit.Inert material is in pearl or cellular, for increasing wherein
The mixing efficiency of liquid.Heated for controlling temperature mechanism is for heating up to reaction mixture, being cooled down and thermostatic control, so that instead
Each substance in mixture is answered rapidly can sufficiently to be reacted in mixing pit.
In the present embodiment, multiple switching valves are connected in a series arrangement in circulation major loop 10.Certainly, in the present invention
In, the arrangement of switching valve is not limited only to this, and in other embodiments, multiple switching valves can in series or in parallel with each other or string
The connection mode in parallel combined is connected in circulation major loop 10, and the several agent reservoirs 71 of example as shown in figure 1 are exactly by mutual
Concatenated mode is linked into circulation major loop 10.
Above-mentioned high temperature and pressure full-automatic chemical reaction system is controlled by computer, high temperature and pressure full-automatic chemical reaction
System, as shown in Figure 1, the channel of the first switching valve 51 and the second switching valve 52 is to disconnect, works as high temperature during not working
When high-voltage full-automatic chemical reaction system works, the course of work is as follows: at the beginning, as shown in Fig. 2, computer first by setting in advance
The first switching valve 51 equipped with liquid reagent or the reagent storing device 71 of solvent is switched to circulation and led back by the response procedures set
In road 10, flow liquid reactions reagent in circulation major loop 10 under the promotion of high pressure liquid phase circulating pump 20.Liquid reagent
Or the input of solvent can also be introduced into circulation major loop 10 by liquid reagent input unit, also that is, by computer control
Multi-center selection valve 83 processed connects the storage bottle 88 of required liquid reagent or solvent, restarts liquid phase delivery pump 82, passes through liquid phase
Required liquid is sent in circulation major loop 10 by delivery pump 82 from suction in liquid reagent storage bottle 86, once needed for reaching
Conveying capacity, liquid phase delivery pump 82 are just out of service.Then one by one the first switching of the reagent storing device 71 equipped with solid reagent
Valve 51 is switched in circulation major loop 10.When liquid reagent passes through the fixating reagent in agent reservoirs 71, liquid reagent
Dissolved solid reagent simultaneously reacts with solid reagent, recycles in major loop 11 if there is being filled with the agent reservoirs of catalyst
71, chemical reaction is accelerated；When mixed reactant enters hybrid heating device 100, by heating, reaction speed is added again
Speed, meanwhile, the pressure of liquid in circulation major loop 10 is adjusted by pressure regulator 30, but also reaction is further speeded up；When
When mixed reactant passes through detector 40, product and reactant all can generate signal on detector 40, as reaction carries out most
Reach chemical balance eventually, at this point, detector 40 generate various signals also reach stablize it is constant, show reaction complete, computer
After the completion signal for receiving the transmission of detector 40, with can be linked into product collecting device 90 on circulation major loop 10 the
Two switching valves 52 switch over, as shown in figure 3, at this moment circulation major loop 10 disconnects, high pressure liquid phase circulating pump 20 is continued to run, pushed away
Fluid in dynamic circulation major loop 11 fully enters in product collection vessel 91.Gas in product collection vessel 91 can be with guide
It other filters 94 and is purified out by it, goes in the air then discharged again and do not lie in pollution environment.
The reaction system has the advantage that the 1, reaction system is completely enclosed state, and the gas in disjunctor system is also all
It can be introduced into absorption by circulation loop or reforming unit purifies to be unlikely to be discharged into and goes to pollute in atmosphere, realize that zero is dirty
Dye, had not only guaranteed safe operation but also had protected environment.2, due to that can apply super-pressure to reaction, many solvents, especially water can be with
As reaction dissolvent, the reagent for being insoluble in water can dissolve to guarantee homogeneous reaction in water, due to pressure after product discharge
Reduction can also be precipitated out automatically；Water makees solvent and can also reduce cost and reduce toxicity.3, system is easy to apply high temperature
High pressure, many conventional methods are difficult to the reaction carried out can carry out quickly in the apparatus of the present.4, system is fully automated
Reaction, is accurately controlled, automatic test reaction terminal by software, and if installing automatic sampling apparatus additional, even nothing is may be implemented in system
People operates continuous production.5, enlarged experiment is such as needed, it is only necessary to the liquid phase pump in the present apparatus is scaled up flow, thus can
To save the R&D process of conventional pilot amplification, research and development of products time and expense are greatlyd save.
High temperature and pressure full-automatic chemical reaction system of the invention, chemical reaction carry out in a closed loop, pass through
Pump plays circulation, peripheral heating, pressure regulation, reagent and catalyst and fills the methods such as column introducing, reaction process on-line checking, can be chemistry
Reaction condition extremely extends, and reaction dissolvent almost can also select arbitrarily, and many extreme toxicities or corrosive substance can also be with
Safety and rapid synthesis comes out.New reaction system controllable precise, it is fully automated, can continuous output, can also directly amplify, in
Examination almost without exploitation, can not only accelerate the process of Preclinical Drug exploitation, but also can largely reduce expenses.
The embodiments described above only express several embodiments of the present invention, and the description thereof is more specific and detailed, but simultaneously
Limitations on the scope of the patent of the present invention therefore cannot be interpreted as.It should be pointed out that for those of ordinary skill in the art
For, without departing from the inventive concept of the premise, various modifications and improvements can be made, these belong to guarantor of the invention
Protect range.Therefore, the scope of protection of the patent of the invention shall be subject to the appended claims.
Claims (7)
1. a kind of high temperature and pressure full-automatic chemical reaction unit, which is characterized in that the circulation major loop including closure, the circulation
Major loop is closed system, includes: in the circulation major loop
High pressure liquid phase circulating pump, for driving the reaction mixture in the circulation major loop to circulate；
Detector, for monitoring the chemical reaction course in the circulation major loop；
Pressure regulator, for adjusting the pressure in the circulation major loop；
Switching valve is connected in the circulation major loop, and for the input and output of material, the switching valve includes the first switching
Valve and the second switching valve；
Exhaust valve is connected on the circulation major loop, is discharged for gas；
Reagent introduction device, for providing reaction reagent, the reagent introduction device includes reaction mixed organization, and the reaction is mixed
Mechanism is closed to be connected in the circulation major loop by first switching valve；
Product collecting device is connected in the circulation major loop by second switching valve, and is located at the high pressure liquid phase
Between the input port of circulating pump and the delivery outlet for reacting mixed organization, for collecting the product of end of reaction；
The reaction mixed organization includes several agent reservoirs, and each agent reservoirs are equipped with import and outlet, described
The imports of agent reservoirs and outlet are separately connected two interfaces of first switching valve, described in the first switching valve connection
The interface of agent reservoirs is disposed adjacent with the interface for connecting the circulation major loop；
The agent reservoirs are high-pressure-resistant vessel, and the exit of the agent reservoirs is equipped with high pressure resistant microporous filter element,
For stopping the solid matter in the agent reservoirs to squeeze out from the delivery outlet；
At least there are four interface and two channels for the switching valve, and under a kind of switching state, the circulation major loop only passes through
One of channel, under another switching state, the circulation major loop pass through two channels, formed disconnection state or
The channel of person and periphery forms the circulation major loop extended.
2. high temperature and pressure full-automatic chemical reaction unit according to claim 1, which is characterized in that the reagent introduces dress
Setting further includes liquid introducing member, and the liquid introducing member includes:
Triple valve connects the input terminal of the circulation major loop mesohigh liquid phase circulation pump；
The output end of liquid phase delivery pump is connect by a check valve with the triple valve, and the check valve makes liquid by the liquid
Phase delivery pump flows to the triple valve；
Several liquid reagent storage bottles for being used to hold liquid reagent；
Multi-center selection valve, the common interface of the multi-center selection valve are connected to the input terminal of the liquid phase delivery pump；It is described
Each selector channel interface of multi-center selection valve is correspondingly connected with the liquid reagent storage bottle.
3. high temperature and pressure full-automatic chemical reaction unit according to claim 2, which is characterized in that the reagent introducing portion
Part further includes a waste liquid bottle, one of selector channel orifice of waste liquid bottle and multi-center selection valve.
4. high temperature and pressure full-automatic chemical reaction unit according to claim 1, which is characterized in that the product collects dress
It sets and includes:
Product collection vessel is connect with second switching valve, for collecting the product prepared in the circulation major loop；
Pressure slow release valve is mounted on the top of the product collection vessel, is collected into the product for slow release and collects and holds
The pressure of product in device；
Air intake filter is connect with second switching valve, is followed for filtering to enter in the product collection vessel or enter
Gas in ring major loop.
5. high temperature and pressure full-automatic chemical reaction unit according to claim 4, which is characterized in that the product collects dress
Setting further includes totally-enclosed pressure casing for processing gas, and the totally-enclosed pressure casing is located at pressure slow release valve and product is received
Collect between container, the air inlet and air outlet of the totally-enclosed pressure casing are respectively communicated at the top of the product collection vessel
Gas outlet and pressure slow release valve air inlet, filter material is filled in the totally-enclosed pressure casing.
6. high temperature and pressure full-automatic chemical reaction unit according to claim 1, which is characterized in that further include a mixing
Heating device, volume buffering, mixing and heating for solution in the circulation major loop；The hybrid heating device includes one
Mixing pit, the inert material being filled in the mixing pit and the heated for controlling temperature mechanism in the mixing pit；The inertia
Material, for increasing the mixing efficiency of wherein liquid.
7. high temperature and pressure full-automatic chemical reaction unit according to claim 1, which is characterized in that multiple switching valves
It is connected in the circulation major loop in series or in parallel.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201611089430.0A CN106378060B (en) | 2016-11-30 | 2016-11-30 | High temperature and pressure full-automatic chemical reaction system |
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| CN201611089430.0A CN106378060B (en) | 2016-11-30 | 2016-11-30 | High temperature and pressure full-automatic chemical reaction system |
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| CN106378060B true CN106378060B (en) | 2019-06-04 |
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| US2776284A (en) * | 1957-01-01 | Apparatus and method for producing melamine | ||
| FR2536676B1 (en) * | 1982-11-26 | 1993-01-22 | Inst Francais Du Petrole | PLATE REACTORS FOR CHEMICAL SYNTHESIS CARRIED OUT UNDER HIGH PRESSURE IN THE GAS PHASE AND IN HETEROGENEOUS CATALYSIS |
| CA2530750A1 (en) * | 2003-06-30 | 2005-01-06 | Academisch Ziekenhuis Groningen | Method for histoprocessing |
| CN201431882Y (en) * | 2009-03-27 | 2010-03-31 | 杭州白浪助剂有限公司 | Spray polymerization kettle with regulating valve |
| CN203853071U (en) * | 2014-05-15 | 2014-10-01 | 上海沣勃新材料科技有限公司 | Reaction kettle for synthesizing carbamates compound by urea method |
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