CN106732288A - It is a kind of to be heated to reflux device for prepared by porous polymer - Google Patents
It is a kind of to be heated to reflux device for prepared by porous polymer Download PDFInfo
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- CN106732288A CN106732288A CN201710032761.9A CN201710032761A CN106732288A CN 106732288 A CN106732288 A CN 106732288A CN 201710032761 A CN201710032761 A CN 201710032761A CN 106732288 A CN106732288 A CN 106732288A
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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
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/0053—Details of the reactor
- B01J19/0066—Stirrers
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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
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/18—Stationary reactors having moving elements inside
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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
- B01J2219/00051—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
- B01J2219/00051—Controlling the temperature
- B01J2219/00132—Controlling the temperature using electric heating or cooling elements
- B01J2219/00135—Electric resistance heaters
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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
- B01J2219/18—Details relating to the spatial orientation of the reactor
- B01J2219/185—Details relating to the spatial orientation of the reactor vertical
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Abstract
Device is heated to reflux for prepared by porous polymer the invention discloses a kind of, porous polymer preparation facilities field is related generally to.Including support component, retort, connecting pipe, top cover, power set and reflux, agitating device is provided with inside the retort, the retort is provided with reactant storage bin, reaction-ure inlet and leakage fluid dram, the connecting pipe two ends are connected with top cover and retort respectively, the power set include micromachine, decelerator and rotary shaft, the reflux includes escaping pipe, the first condensing reflux tank, the second condensing reflux tank, and for connecting the connecting tube of the first condensing reflux tank and the second condensing reflux tank.The beneficial effects of the present invention are：It can realize that just a certain component in reaction system is removed or separated during the course of the reaction, improve the yield or performance of polymer, and can automatically control raw material needed for addition course of reaction, flexible and convenient to use.
Description
Technical field
It is specifically a kind of to be returned for heating prepared by porous polymer the present invention relates to porous polymer preparation facilities field
Stream device.
Background technology
Porous material in gas absorption, separation and catalytic field due to larger specific surface area, having important answering
With.The development experience of porous material from traditional inorganic porous material such as micro-pore zeolite and molecular sieve etc., to organic and inorganic
Hydridization Porous materials such as organosilicon mesoporous material (Periodic Mesoporous Organosilicas, PMOs) and metal-have
Machine frame frame material (Metal-Organic Frameworks, MOFs) etc., then the pure organic component risen to Recent study
Covalent organic porous material, from the first covalent organic frame material (the Covalent Organic of Yaghi groups report in 2005
Frameworks, COFs) since, this kind of material just causes the extensive attention of people, has triggered covalent organic porous polymer
Research boom.Compared to the unstability for being difficult to functionalization and hybrid inorganic-organic porous material of traditional inorganic porous material, have
The appearance of machine porous material compensate for these shortcomings well.
Organic porous polymer be a class connected by way of covalent bond by lightweight element (C, H, O, N, B etc.) completely and
Into organic porous material, porous polymer be using Polymer Synthesizing means prepare polymer.Organic porous polymer has
Have the advantage that：1. organic porous material is made up of some lighter chemical elements more, and density is low；2. connected by covalent bond
High polymer network is formed, with good heat endurance and chemical stability；3. organic porous material is with organic molecule as structure
Primitive is built, with structural controllability and the characteristics of function adjustability, some functionalization groups is just easily introduced when building, it is real
Now its application in a certain field.Because with these unique advantages, organic porous polymer is expected in hydrogen storage, absorption, divides
Play a significant role from fields such as, catalysis, the energy, chemical sensitisation and biological medicines, as a kind of new with development potentiality
Porous material.
Would generally be used to device is heated to reflux when organic porous polymer is prepared, the existing device that is heated to reflux makes
Used time has the following disadvantages：
1st, it is conventional to be heated to reflux device and realize the removal or separation of a certain component in the middle of reaction system, so that shadow
Ring the yield or performance of polymer；
2nd, it is existing to be heated to reflux device, the raw material according to needed for reaction needs artificial addition is needed during the course of the reaction, when
Between can not accurately control, in-convenience in use.
The content of the invention
To solve deficiency of the prior art, present invention offer is a kind of to be heated to reflux dress for prepared by porous polymer
Put, it can realize that just a certain component in reaction system is removed or separated during the course of the reaction, improve the yield of polymer
Or performance, and raw material needed for addition course of reaction can be automatically controlled, it is flexible and convenient to use.
The present invention to achieve the above object, is achieved through the following technical solutions：
It is a kind of to be heated to reflux device, including support component, retort, connecting pipe, top for prepared by porous polymer
Lid, power set and reflux, the support component include support frame, and support frame as described above top is provided with geometrical clamp, described anti-
Answer tank wall to be provided with reaction-ure inlet and leakage fluid dram, agitating device is provided with inside the retort, the retort top sets
There are first flange disk and support protrusion, the support protrusion is arranged at first flange disk lower section, and the support protrusion is provided with instead
Thing storage bin and time controller, the reactant storage bin is answered to be provided with the reactant conveying being connected with reaction-ure inlet
Pipe, the reactant gas delivery path is provided with control valve, the time controller and control valve with reactant storage bin junction
Connected by wire, the connecting pipe is respectively arranged at two ends with second flange disk and the 3rd ring flange, the second flange disk with
First flange disk is bolted, and the second flange disk is provided with the first sealing gasket, the top with first flange disk junction
Base portion is provided with the 4th ring flange, and the 4th ring flange is bolted with the 3rd ring flange, the 4th ring flange with
3rd ring flange junction is provided with the second sealing gasket, and the top cover sidewall is arcuate structure, and the top cover sidewall is provided with backflow
Device projection connector, the reflux projection connector includes outlet connecting tube and backflow connecting tube, the backflow connection
Check valve is provided with pipe, the power set include micromachine, decelerator and rotary shaft, and the micromachine passes through decelerator
It is connected with rotary shaft, the rotary shaft is connected with agitating device top, the reflux includes escaping pipe, the first condensing reflux
Tank, the second condensing reflux tank, the connecting tube for connecting the first condensing reflux tank and the second condensing reflux tank, the escaping pipe with
Outlet connecting tube is connected, and the first condensation chamber for holding condensate liquid, first condensation chamber are provided with the first condensing reflux tank
Outer wall is provided with the first constant temperature meter, and the first condensation chamber center is provided with the first condenser pipe, the first condensing reflux tank
Bottom is provided with collecting bag, and first switch valve, the first switch valve are set between the collecting bag and the first condensing reflux tank
Door is located at escaping pipe and the first condensing reflux tank junction lower section, and the second condensing reflux tank bottom end connects with backflow connecting tube
It is logical, second switch valve is set in the backflow connecting tube, it is provided with the second condensing reflux tank and holds the second of condensate liquid
Condensation chamber, the second condensation cavity outer wall is provided with the second constant temperature meter, and the second condensation chamber center sets the second condenser pipe.
Also include cleaning device, the cleaning device includes syringe and washing hose, and the washing hose is provided with clearly
Control valve is washed, the top cover sidewall is provided with cleaning device projection connector, and the cleaning device projection connector is soft with cleaning
Pipe is connected.
The support component also includes base plate, and the base plate is provided with heating mantle seat platform, away from heating mantle on the base plate
Seat platform one end is provided with ballast box.
The agitating device is double-deck anchor type agitator, and the double-deck anchor type agitator includes puddler and stirring anchor, institute
State puddler top to be connected with rotary shaft, the stirring anchor is provided with poke hole.
Also include pressure gauge and thermometer, the top cover sidewall is provided with meter projection connector, and the meter is convex
Play connector and be provided with measured hole, the induction contact of the pressure gauge and thermometer is arranged in measured hole.
The reaction pot bottom is circular arc.
The top cover top is provided with bearing block, and deep groove ball bearing is provided with the bearing block, and the bearing block top is provided with
End cap, the end cap is bolted with bearing block, and the end cap is provided with the 3rd sealing gasket with bearing block junction.
The top cover is provided with iron stand, and the iron stand includes the first iron stand and the second iron stand, first iron
Pallet is connected with the first condensing reflux tank and the second condensing reflux tank, and second iron stand is connected with syringe.
The retort is transparent tank body.
Contrast prior art, the beneficial effects of the present invention are：
1st, the first condensing reflux tank and the second condensing reflux tank that the present apparatus passes through setting, according to certain component in reaction system
With the difference of solvent liquefaction point, when being heated to reflux to reaction system, in reaction system certain component or solvent respectively through
Condensation temperature different the first condensing reflux tank and the second condensing reflux tank, wherein the temperature of the first condensing reflux tank is set in needing
, it is necessary to separate or both the component that remove and solvent between the liquefaction point of certain component and the liquefaction point of solvent of to be separated or removal
Middle liquefaction point is higher to be first liquefied, and the component or solvent not being liquefied are entered into the second condensing reflux tank, and second condenses back
The temperature of stream tank is set below the temperature of the liquefaction point of solvent, and the component or solvent not being liquefied now are condensed back by second
It is liquefied during stream tank, by adjusting first switch valve and/or second switch valve, certain component that selection will need backflow to use
Or solvent refluxing is in retort, it would be desirable to which removal or separate component are isolated to outside reaction system.On reactant storage bin
The reactant gas delivery path being connected with reaction-ure inlet is provided with, reactant storage bin has multilayer, its every layer is deposited different anti-
Thing, every layer of reactant storage bin is answered to be connected with reactant gas delivery path, and connectivity part is equipped with control reactant outflow
Control valve, raw material needed for addition can be automatically controlled by time controller, flexible and convenient to use.
2nd, support component also includes base plate, and base plate is provided with heating mantle seat platform, and heating mantle seat platform is used for putting in course of reaction
Automatic constant-temperature electric heating set is put, ballast box is provided with away from heating mantle seat platform one end on base plate, ballast box is used for balanced support frame both sides
Weight.
3rd, double-deck anchor type agitator is set to by by agitating device, poke hole is set on stirring anchor, can be to reactant
That stirs is more uniform, thorough.
The 4th, cleaning device is set, device inside is cleaned by cleaning device afterwards before the reaction, carrying out porous gathering
When prepared by compound, poromeric preparation quality is improved.
The 5th, pressure gauge and thermometer are set, temperature and pressure in reaction unit can be accurately controlled in course of reaction.
6th, reaction pot bottom is set to circular arc, can be heated evenly reaction pot bottom.
7th, top cover top is set and deep groove ball bearing is set in bearing block, bearing block, and rotary shaft can be made in whipping process
What is rotated more stablizes, and improves the service life of device.
8th, iron stand is set on top cover, effective fixation preferably can be carried out to condensing reflux tank and syringe.
9th, retort is set to transparent tank body, being capable of preferably observing response phenomenon and course of reaction.
Brief description of the drawings
Accompanying drawing 1 is concrete structure schematic diagram of the present invention；
Accompanying drawing 2 is retort stereogram in the present invention；
Accompanying drawing 3 is internal structure schematic diagram of the present invention.
Label shown in accompanying drawing：1st, retort；2nd, connecting pipe；3rd, top cover；4th, support frame；5th, geometrical clamp；6th, reactant
Import；7th, leakage fluid dram；8th, first flange disk；9th, support protrusion；10th, reactant storage bin；11st, time controller；12nd, valve is controlled
Door；13rd, second flange disk；14th, the 3rd ring flange；15th, the first sealing gasket；16th, the 4th ring flange；17th, the second sealing gasket；18、
Reflux projection connector；19th, outlet connecting tube；20th, flow back connecting tube；21st, check valve；22nd, micromachine；23rd, slow down
Device；24th, rotary shaft；25th, escaping pipe；26th, the first condensing reflux tank；27th, connecting tube；28th, the first condensation chamber；29th, the first constant temperature
Meter；30th, the first condenser pipe；31st, the second condensing reflux tank；32nd, heating mantle seat platform；33rd, ballast box；34th, puddler；35th, stir
Anchor；36th, poke hole；37th, syringe；38th, washing hose；39th, purge control valve；40th, cleaning device projection connector；41st, press
Power meter；42nd, thermometer；43rd, meter projection connector；44th, measured hole；45th, collecting bag；46th, bearing block；47th, deep-groove ball axle
Hold；48th, end cap；49th, the 3rd sealing gasket；50th, the first iron stand；51st, the second iron stand；52nd, the second condensation chamber；53rd, first open
Closing valve；54th, the second constant temperature meter；55th, first switch valve；56th, the second condenser pipe.
Specific embodiment
With reference to specific embodiment, the present invention is expanded on further.It should be understood that these embodiments are merely to illustrate the present invention
Rather than limitation the scope of the present invention.In addition, it is to be understood that after the content for having read instruction of the present invention, people in the art
Member can make various changes or modifications to the present invention, and these equivalent form of values equally fall within scope defined herein.
A kind of to be heated to reflux device for prepared by porous polymer, agent structure includes support component, retort 1, connects
Jointed tubular workpieces 2, top cover 3, power set and reflux, the support component include support frame 4, and support frame 4 is used for supporting whole
Device.The top of support frame as described above 4 is provided with geometrical clamp 5, and geometrical clamp 5 is U-shaped, and the diameter with the middle part of connecting pipe 2 is adapted.Institute
State the outer wall of retort 1 and be provided with reaction-ure inlet 6 and leakage fluid dram 7, during the course of the reaction, reaction-ure inlet 6 is used for according to reaction
Process timing to injecting reactant in retort 1.Agitating device is provided with inside the retort 1, facilitates reaction stirred.Institute
State the top of retort 1 and be provided with first flange disk 8 and support protrusion 9, the support protrusion 9 is arranged at the lower section of first flange disk 8, institute
State support protrusion 9 and be provided with reactant storage bin 10 and time controller 11, the reactant storage bin 10 is provided with and reaction
The reactant gas delivery path that thing import 6 is connected, the reactant gas delivery path is provided with control valve with the junction of reactant storage bin 10
Door 12, the time controller 11 is connected with control valve 12 by wire, and reactant storage bin 10 has multilayer, its every layer storage
Different reactants, every layer of reactant storage bin 10 is connected with reactant gas delivery path, and connectivity part is equipped with control
The control valve 12 of reactant outflow.The connecting pipe 2 is respectively arranged at two ends with the ring flange 14 of second flange disk 13 and the 3rd, institute
State second flange disk 13 to be bolted with first flange disk 8, the second flange disk 13 sets with the junction of first flange disk 8
There is the first sealing gasket 15, the first sealing gasket 15 is used to seal reaction unit.The bottom of the top cover 3 is provided with the 4th ring flange
16, the 4th ring flange 16 is bolted with the 3rd ring flange 14, the 4th ring flange 16 and the 3rd ring flange 14
Junction is provided with the second sealing gasket 17, and the second sealing gasket 17 is used to seal reaction unit.The side wall of the top cover 3 is arc
Structure, the side wall of the top cover 3 is provided with reflux projection connector 18, and reflux projection connector 18 is used for connecting backflow
Device.The reflux projection connector 18 includes outlet connecting tube 19 and backflow connecting tube 20.The backflow connecting tube 20
Inside it is provided with check valve 21.The power set include micromachine 22, decelerator 23 and rotary shaft 24, by the top of top cover 3
Power set are set, can be stirred using micromachine 22, in that context it may be convenient to control mixing speed, stir more uniform.
The micromachine 22 is connected by decelerator 23 with rotary shaft 24, and decelerator 23 is used for reducing the rotating speed of rotary shaft 24, and then
Reduce the rotating speed of agitating device.The rotary shaft 24 is connected with agitating device top.The reflux includes escaping pipe 25, the
One condensing reflux tank 26, the second condensing reflux tank 31, for connecting the first condensing reflux tank 26 and the second condensing reflux tank 31
Connecting tube 27, the escaping pipe 25 is connected with outlet connecting tube 19, is provided with the first condensing reflux tank 26 and holds condensate liquid
The first condensation chamber 28, the outer wall of the first condensation chamber 28 is provided with the first constant temperature meter 29, the centre bit of the first condensation chamber 28
The first condenser pipe 30 is installed, the bottom of the first condensing reflux tank 26 is provided with collecting bag 45, and the collecting bag 45 is cold with first
First switch valve 53 is set between solidifying return tank 26, and the first switch valve 53 is located at the condensing reflux of escaping pipe 25 and first
The junction of tank 26 lower section, the bottom of the second condensing reflux tank 31 connects with backflow connecting tube 20, in the backflow connecting tube 20
Set and the second condensation chamber 52 for holding condensate liquid is provided with second switch valve 55, the second condensing reflux tank 31, described the
The outer wall of two condensation chamber 52 is provided with the second constant temperature meter 54, and the center of second condensation chamber 52 sets the second condenser pipe 56.By setting
The the first condensing reflux tank and the second condensing reflux tank put, according to the difference of certain component in reaction system and solvent liquefaction point, when
When being heated to reflux to reaction system, certain component or solvent are respectively through the first different condensation of condensation temperature in reaction system
Return tank and the second condensing reflux tank, wherein the temperature of the first condensing reflux tank is set in certain component of needs separation or removal
, it is necessary to separate or the middle liquefaction point of both the component that removes and solvent is higher first by liquid between liquefaction point and the liquefaction point of solvent
Change, the component or solvent not being liquefied are entered into the second condensing reflux tank, and the temperature of the second condensing reflux tank is set below
It is liquefied when the temperature of the liquefaction point of solvent, the component not being liquefied now or solvent are by the second condensing reflux tank, by adjusting
Section first switch valve and/or second switch valve, selection will need certain component for using of backflow or solvent refluxing to retort
In, it would be desirable to removal or separate component are isolated to outside reaction system.
In order to easily be cleaned to device inside afterwards before the reaction, when porous polymer preparation is carried out, carry
Poromeric preparation quality high, also including cleaning device, the cleaning device includes syringe 37 and washing hose 38, note
Emitter 37 is used for depositing cleaning fluid, and syringe 37 is used for applying cleaning fluid pressure, and increase cleaning fluid is rushed with projection inside pipe wall
Brushing force, makes cleaning more thorough.The washing hose 38 is provided with purge control valve 39, and purge control valve 39 is used for preventing reaction
During retort 1 and cleaning device connection, prevent gaseous reactant from entering into cleaning device, it is ensured that reaction unit
Sealing.The side wall of the top cover 3 is provided with cleaning device projection connector 40, and cleaning device projection connector 40 ensure that cleaning
Connection inside flexible pipe 38 and retort 1, the cleaning device projection connector 40 is connected with washing hose 38.
In order to ensure the practicality and adaptability of device, the support component also includes base plate, and the base plate is provided with and adds
Hot jacket seat platform 32, heating mantle seat platform 32 is used for placing automatic constant-temperature electric heating set in course of reaction, away from heating mantle on the base plate
The one end of seat platform 32 is provided with ballast box 33, and ballast box 33 is used for the weight of the both sides of balanced support frame 4.
More uniform, thorough in order to what is stirred to reactant, the agitating device is double-deck anchor type agitator, double-deck
Anchor type agitator can sufficiently be stirred to the reactant of each layer.The double-deck anchor type agitator includes puddler 34 and stirs
Anchor 35 is mixed, the top of the puddler 34 is connected with rotary shaft 24, the stirring anchor 35 is provided with poke hole 36, poke hole 36 sets
Put and ensure that can mix between reactant more uniform.
In order to the temperature and pressure that are accurately controlled in reaction unit, also including pressure gauge 41 and thermometer 42, institute
State the side wall of top cover 3 and be provided with meter projection connector 43, the meter projection connector 43 is provided with measured hole 44, described
The induction contact of pressure gauge 41 and thermometer 42 is arranged in measured hole 44.The induction contact of pressure gauge 41 and thermometer 42 is equal
It is arranged in measured hole 44, the temperature and pressure in reaction unit can be learnt by the registration of observed pressure meter 41 and thermometer 42
By force, the reaction condition in course of reaction can rationally be controlled.
In order to be heated evenly the bottom of retort 1, the bottom of the retort 1 is circular arc.
More stablize in order to rotate rotary shaft 24, improve the service life of device, the top of the top cover 3 is provided with
Deep groove ball bearing 47 is provided with bearing block 46, the bearing block 46, the top of the bearing block 46 is provided with end cap 48, and bearing block 46 is used
To place deep groove ball bearing 47, end cap 48 is used for fixing deep groove ball bearing 47.The end cap 48 is connected with bearing block 46 by bolt
Connect, the end cap 48 is provided with the 3rd sealing gasket 49 with the junction of bearing block 46, and the 3rd sealing gasket 49 can be to deep groove ball bearing 47
Play a protective role.
In order to preferably carry out effective fixation to the first condensing reflux tank 26 and syringe 37, on the top cover 3
Iron stand is provided with, the iron stand includes the first iron stand 50 and the second iron stand 51, and first iron stand 50 is cold with first
The solidifying condensing reflux tank 31 of return tank 26 and second is connected, and second iron stand 51 is connected with syringe 37.
In order to more preferable observing response phenomenon and course of reaction, the retort 1 is transparent tank body.
Embodiment 1：
In the preparation method of organic porous polymer, it is the preparation method being in daily use to be reacted by schiff alkali, and this is anti-
Should be using the compound of aldehyde radical and amido, be heated to reflux occurring condensation reaction in organic solvent DMSO generate per se with
The organic porous polymer of micropore, while the reaction has water byproduct to produce, the reaction is a reversible reaction, due to water and DMSO
Dissolve each other, in the process reclaimed water of being heated to reflux can all the time be present in whole reaction system, can so influence the balance of chemical reaction, from
And reduce yield, for solve the above problems the present invention provides it is a kind of for porous polymer preparation be heated to reflux device, main body
Structure includes support component, retort 1, connecting pipe 2, top cover 3, power set and reflux, and the support component includes
Support frame 4, support frame 4 is used for supporting whole device.The top of support frame as described above 4 is provided with geometrical clamp 5, and geometrical clamp 5 is U-shaped, with company
The diameter at the middle part of jointed tubular workpieces 2 is adapted.The outer wall of the retort 1 is provided with reaction-ure inlet 6 and leakage fluid dram 7, is reacting
Cheng Zhong, reaction-ure inlet 6 is used for according to reaction process timing to injecting reactant in retort 1.Set inside the retort 1
There is agitating device, facilitate reaction stirred.The top of the retort 1 is provided with first flange disk 8 and support protrusion 9, the support
Raised 9 are arranged at the lower section of first flange disk 8, and the support protrusion 9 is provided with reactant storage bin 10 and time controller 11, institute
State reactant storage bin 10 and be provided with the reactant gas delivery path being connected with reaction-ure inlet 6, the reactant gas delivery path with it is anti-
The junction of thing storage bin 10 is answered to be provided with control valve 12, the time controller 11 is connected with control valve 12 by wire, instead
Answering thing storage bin 10 has multilayer, and its every layer is deposited different reactants, and every layer of reactant storage bin 10 is conveyed with reactant
Pipe is connected, and connectivity part is equipped with the control valve 12 of control reactant outflow.The connecting pipe 2 is respectively arranged at two ends with
The ring flange 14 of second flange disk 13 and the 3rd, the second flange disk 13 is bolted with first flange disk 8, and described second
Ring flange 13 is provided with the first sealing gasket 15 with the junction of first flange disk 8, and the first sealing gasket 15 is close for being carried out to reaction unit
Envelope.The bottom of the top cover 3 is provided with the 4th ring flange 16, and the 4th ring flange 16 is bolted with the 3rd ring flange 14,
4th ring flange 16 and the junction of the 3rd ring flange 14 are provided with the second sealing gasket 17, and the second sealing gasket 17 is used to fill reaction
Put and sealed.The side wall of the top cover 3 is arcuate structure, and the side wall of the top cover 3 is provided with reflux projection connector 18, returns
Stream device projection connector 18 is used for connecting reflux.The reflux projection connector 18 includes the He of outlet connecting tube 19
Backflow connecting tube 20.Check valve 21 is provided with the backflow connecting tube 20.The power set include micromachine 22, decelerator
23 and rotary shaft 24, by the top of top cover 3, power set are set, can be stirred using micromachine 22, can facilitate
Control mixing speed, stir it is more uniform.The micromachine 22 is connected by decelerator 23 with rotary shaft 24, decelerator 23
For reducing the rotating speed of rotary shaft 24, and then reduce the rotating speed of agitating device.The rotary shaft 24 is connected with agitating device top.
The reflux includes escaping pipe 25, the first condensing reflux tank 26, the second condensing reflux tank 31, first condenses back for connecting
The connecting tube 27 of the condensing reflux tank 31 of tank 26 and second is flowed, the escaping pipe 25 is connected with outlet connecting tube 19, and described first is cold
The first condensation chamber 28 for holding condensate liquid is provided with solidifying return tank 26, the outer wall of the first condensation chamber 28 is provided with the first constant temperature meter
29, the center of the first condensation chamber 28 is provided with the first condenser pipe 30, and the bottom of the first condensing reflux tank 26 is provided with collection
Bag 45, sets first switch valve 53, the first switch valve 53 between the condensing reflux tank 26 of the collecting bag 45 and first
Positioned at the junction of 25 and first condensing reflux tank of escaping pipe 26 lower section, the bottom of the second condensing reflux tank 31 with backflow connecting tube
20 connections, set in the backflow connecting tube 20 be provided with second switch valve 55, the second condensing reflux tank 31 hold it is cold
Second condensation chamber 52 of lime set, the outer wall of the second condensation chamber 52 is provided with the second constant temperature meter 54, in second condensation chamber 52
Centre sets the second condenser pipe 56.By the first condensing reflux tank and the second condensing reflux tank that set, during being heated to reflux,
The temperature of the first condensing reflux tank is set between the liquefaction point of DMSO and water liquefaction point, because the liquefaction point of water is less than DMSO
Liquefaction point, water vapour and DMSO steam simultaneously by the first condensing reflux tank when, DMSO is first liquefied, because DMSO is also needed to
Again it is back in retort, so needing to close the first valve switch, the vapor not being liquefied is entered by connecting tube
To in the second condensing reflux tank, wherein the second condensing reflux tank is using originally water condensation, vapor is in the second condensing reflux tank
It is liquefied, because water needs to be discharged to outside reaction system, closes second switch valve, liquefied water is stored in the second condensation and returns
In stream tank；One of product water in due to the reaction is discharged to outside reaction system, and the concentration of reaction system reclaimed water is big
It is big to reduce, promote the reaction forward to carry out, so as to improve poromeric yield.：
Embodiment 2：
In the preparation method of organic porous polymer, suspension polymerization prepare porous polymer microsphere be also it is a kind of very
Important method.Suspension polymerization prepares porous polymer microsphere, and its system typically has monomer, crosslinking agent, pore-foaming agent, initiator
With water composition, oil phase is dispersed into drop in the presence of mixing power, adds surfactant or dispersion stabilizer to improve drop
Suspension stability.In the presence of pore-foaming agent, the formation of suspension polymerisation central hole structure can be divided into three phases.First stage：
The formation of micro- glueballs and aggregation.Second stage：Micro- glueballs aggregation is interconnected to form loose structure.Phase III：In hole
The removing of pore-foaming agent.The removing method of pore-foaming agent is the cause that will be remained in copolymer duct using the method for heating distillation in hole
Hole agent is removed, and loose structure is formed.Because the liquefaction point bottom of nonaqueous solvents is in the liquefaction point of pore-foaming agent, distilled by heating
Method by pore-foaming agent liquefy discharge when, due to reaction unit of the prior art be difficult control pore-foaming agent liquefy when temperature,
Nonaqueous solvents follows pore-foaming agent to liquefy together after causing heating to be distilled, so as to influence porous polymer to prepare quality.For in solution
State the problem present invention provide it is a kind of be heated to reflux device for prepared by porous polymer, agent structure includes support component, anti-
Tank 1, connecting pipe 2, top cover 3, power set and reflux are answered, the support component includes support frame 4, and support frame 4 is used for
Support whole device.The top of support frame as described above 4 is provided with geometrical clamp 5, and geometrical clamp 5 is U-shaped, the diameter with the middle part of connecting pipe 2
It is adapted.The outer wall of the retort 1 is provided with reaction-ure inlet 6 and leakage fluid dram 7, and during the course of the reaction, reaction-ure inlet 6 is used for
According to reaction process timing to injecting reactant in retort 1.Agitating device, convenient stirring are provided with inside the retort 1
Reactant.The top of the retort 1 is provided with first flange disk 8 and support protrusion 9, and the support protrusion 9 is arranged at first flange
The lower section of disk 8, the support protrusion 9 is provided with reactant storage bin 10 and time controller 11, on the reactant storage bin 10
It is provided with the reactant gas delivery path being connected with reaction-ure inlet 6, the reactant gas delivery path and the junction of reactant storage bin 10
Control valve 12 is provided with, the time controller 11 is connected with control valve 12 by wire, and reactant storage bin 10 has multilayer,
Its every layer is deposited different reactants, and every layer of reactant storage bin 10 is connected with reactant gas delivery path, and connectivity part
It is equipped with the control valve 12 of control reactant outflow.The connecting pipe 2 is respectively arranged at two ends with second flange disk 13 and the 3rd
Ring flange 14, the second flange disk 13 is bolted with first flange disk 8, the second flange disk 13 and first flange
The junction of disk 8 is provided with the first sealing gasket 15, and the first sealing gasket 15 is used to seal reaction unit.The bottom of the top cover 3 sets
Have the 4th ring flange 16, the 4th ring flange 16 is bolted with the 3rd ring flange 14, the 4th ring flange 16 with
The junction of 3rd ring flange 14 is provided with the second sealing gasket 17, and the second sealing gasket 17 is used to seal reaction unit.The top
The side wall of lid 3 is arcuate structure, and the side wall of the top cover 3 is provided with reflux projection connector 18, reflux projection connector
18 are used for connecting reflux.The reflux projection connector 18 includes outlet connecting tube 19 and backflow connecting tube 20.Institute
State in backflow connecting tube 20 and be provided with check valve 21.The power set include micromachine 22, decelerator 23 and rotary shaft 24, lead to
Cross and power set be set at the top of top cover 3, can be stirred using micromachine 22, in that context it may be convenient to control mixing speed,
Stirring is more uniform.The micromachine 22 is connected by decelerator 23 with rotary shaft 24, and decelerator 23 is used for reducing rotary shaft
24 rotating speed, and then reduce the rotating speed of agitating device.The rotary shaft 24 is connected with agitating device top.The reflux bag
Include tracheae 25, the first condensing reflux tank 26, the second condensing reflux tank 31, for connect the first condensing reflux tank 26 and second it is cold
The connecting tube 27 of solidifying return tank 31, the escaping pipe 25 is connected with outlet connecting tube 19, is set in the first condensing reflux tank 26
There is the first condensation chamber 28 for holding condensate liquid, the outer wall of the first condensation chamber 28 is provided with the first constant temperature meter 29, and described first is cold
The solidifying center of chamber 28 is provided with the first condenser pipe 30, and the bottom of the first condensing reflux tank 26 is provided with collecting bag 45, the collection
Bag 45 and first sets first switch valve 53 between condensing reflux tank 26, the first switch valve 53 be located at escaping pipe 25 with
The junction of first condensing reflux tank 26 lower section, the bottom of the second condensing reflux tank 31 connects with backflow connecting tube 20, described time
Set in stream connecting tube 20 and the second condensation for holding condensate liquid is provided with second switch valve 55, the second condensing reflux tank 31
Chamber 52, the outer wall of the second condensation chamber 52 is provided with the second constant temperature meter 54, and the center of second condensation chamber 52 sets second and condenses
Pipe 56.By the first condensing reflux tank and the second condensing reflux tank that set, during being heated to reflux, by the first condensing reflux
The temperature of tank is set between the liquefaction point of nonaqueous solvents and the liquefaction point of pore-foaming agent, because the liquefaction point of pore-foaming agent is higher than non-aqueous
The liquefaction point of solvent, the steam of pore-foaming agent and the steam of nonaqueous solvents simultaneously by the first condensing reflux tank when, the steaming of pore-foaming agent
Vapour is first liquefied, and because pore-foaming agent needs to be separated, so needing to open the first valve switch, what is be not liquefied is non-aqueous
Solvent vapour is entered into the second condensing reflux tank by connecting tube, wherein the second condensing reflux tank is using less than nonaqueous solvents liquid
Change the ice water condensation of point, nonaqueous solvents is liquefied in the second condensing reflux tank, because nonaqueous solvents needs to be back to again instead
Answer among system, open second switch valve, liquefied nonaqueous solvents is back to again by second switch valve and check valve
In retort.Excluded by by liquefied pore-foaming agent, so as to ensure that porous polymer prepares quality.
Claims (9)
- It is 1. a kind of to be heated to reflux device for prepared by porous polymer, it is characterised in that：Including support component, retort (1), Connecting pipe (2), top cover (3), power set and reflux, the support component include support frame (4), support frame as described above (4) top is provided with geometrical clamp (5), and retort (1) outer wall is provided with reaction-ure inlet (6) and leakage fluid dram (7), the reaction Agitating device is provided with inside tank (1), retort (1) top is provided with first flange disk (8) and support protrusion (9), the branch Support raised (9) is arranged at first flange disk (8) lower section, and the support protrusion (9) is provided with reactant storage bin (10) and time Controller (11), the reactant storage bin (10) is provided with the reactant gas delivery path being connected with reaction-ure inlet (6), described Reactant gas delivery path is provided with control valve (12), the time controller (11) and control with reactant storage bin (10) junction Valve (12) is connected by wire, and the connecting pipe (2) is respectively arranged at two ends with second flange disk (13) and the 3rd ring flange (14), the second flange disk (13) is bolted with first flange disk (8), the second flange disk (13) and the first method Blue disk (8) junction is provided with the first sealing gasket (15), and top cover (3) bottom is provided with the 4th ring flange (16), the 4th method Blue disk (16) is bolted with the 3rd ring flange (14), the 4th ring flange (16) and the 3rd ring flange (14) junction The second sealing gasket (17) is provided with, top cover (3) side wall is arcuate structure, and it is convex that top cover (3) side wall is provided with reflux Connector (18) is played, reflux projection connector (18) includes outlet connecting tube (19) and backflow connecting tube (20), institute State and check valve (21) is provided with backflow connecting tube (20), the power set include micromachine (22), decelerator (23) and turn Moving axis (24), the micromachine (22) is connected by decelerator (23) with rotary shaft (24), the rotary shaft (24) with stirring Device top connects, and the reflux includes escaping pipe (25), the first condensing reflux tank (26), the second condensing reflux tank (31), for the first condensing reflux tank (26) of connection and the connecting tube (27) of the second condensing reflux tank (31), the escaping pipe (25) it is connected with outlet connecting tube (19), the first condensation chamber for holding condensate liquid is provided with the first condensing reflux tank (26) (28), the first condensation chamber (28) outer wall is provided with the first constant temperature meter (29), and the first condensation chamber (28) centre bit is installed There is the first condenser pipe (30), the first condensing reflux tank (26) bottom is provided with collecting bag (45), the collecting bag (45) and the Between one condensing reflux tank (26) set first switch valve (53), the first switch valve (53) positioned at escaping pipe (25) with First condensing reflux tank (26) junction lower section, the second condensing reflux tank (31) bottom connects with backflow connecting tube (20), Set to be provided with second switch valve (55), the second condensing reflux tank (31) on backflow connecting tube (20) and hold condensation Second condensation chamber (52) of liquid, the second condensation chamber (52) outer wall is provided with the second constant temperature meter (54), second condensation chamber (52) center sets the second condenser pipe (56).
- It is 2. a kind of according to claim 1 to be heated to reflux device for prepared by porous polymer, it is characterised in that：Also include Cleaning device, the cleaning device includes syringe (37) and washing hose (38), and the washing hose (38) is provided with cleaning Control valve (39), top cover (3) side wall is provided with cleaning device projection connector (40), the cleaning device projection connector (40) it is connected with washing hose (38).
- It is 3. a kind of according to claim 1 to be heated to reflux device for prepared by porous polymer, it is characterised in that：The branch Support component also includes base plate, and the base plate is provided with heating mantle seat platform (32), away from heating mantle seat platform (32) on the base plate End is provided with ballast box (33).
- It is 4. a kind of according to claim 1 to be heated to reflux device for prepared by porous polymer, it is characterised in that：It is described to stir It is double-deck anchor type agitator to mix device, and the double-deck anchor type agitator includes puddler (34) and stirring anchor (35), the stirring Bar (34) top is connected with rotary shaft (24), and stirring anchor (35) is provided with poke hole (36).
- It is 5. a kind of according to claim 1 to be heated to reflux device for prepared by porous polymer, it is characterised in that：Also include Pressure gauge (41) and thermometer (42), top cover (3) side wall are provided with meter projection connector (43), and the meter is convex Play connector (43) and be provided with measured hole (44), the induction contact of the pressure gauge (41) and thermometer (42) is arranged at measuring In hole (44).
- It is 6. a kind of according to claim 1 to be heated to reflux device for prepared by porous polymer, it is characterised in that：It is described anti- It is circular arc to answer tank (1) bottom.
- It is 7. a kind of according to claim 1 to be heated to reflux device for prepared by porous polymer, it is characterised in that：The top Lid (3) top is provided with and deep groove ball bearing (47) is provided with bearing block (46), the bearing block (46), bearing block (46) top End cap (48) is provided with, the end cap (48) is bolted with bearing block (46), the end cap (48) is with bearing block (46) even The place of connecing is provided with the 3rd sealing gasket (49).
- It is 8. a kind of according to claim 1 to be heated to reflux device for prepared by porous polymer, it is characterised in that：The top Lid (3) is provided with iron stand, and the iron stand includes the first iron stand (50) and the second iron stand (51), first iron stand (50) it is connected with the first condensing reflux tank (26) and the second condensing reflux tank (31), second iron stand (51) and syringe (37) connect.
- It is 9. a kind of according to claim 1 to be heated to reflux device for prepared by porous polymer, it is characterised in that：It is described anti- It is transparent tank body to answer tank (1).
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| CN201710032761.9A CN106732288B (en) | 2017-01-12 | 2017-01-12 | It is a kind of to be heated to reflux device for porous polymer preparation |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5885313A (en) * | 1996-09-12 | 1999-03-23 | Shionogi & Co., Ltd. | Temperature-gradient type multistage condenser |
| CN102085472A (en) * | 2010-12-16 | 2011-06-08 | 中国科学院高能物理研究所 | Reduced pressure distillation ultrasonic reactor |
| CN204952888U (en) * | 2015-08-23 | 2016-01-13 | 淮安洪阳化工有限公司 | Benzoyl chloride produces reaction unit |
| CN105732327A (en) * | 2016-04-27 | 2016-07-06 | 锡矿山闪星锑业有限责任公司 | Method and device for preparing ethylene glycol antimony through microwave reaction |
-
2017
- 2017-01-12 CN CN201710032761.9A patent/CN106732288B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5885313A (en) * | 1996-09-12 | 1999-03-23 | Shionogi & Co., Ltd. | Temperature-gradient type multistage condenser |
| CN102085472A (en) * | 2010-12-16 | 2011-06-08 | 中国科学院高能物理研究所 | Reduced pressure distillation ultrasonic reactor |
| CN204952888U (en) * | 2015-08-23 | 2016-01-13 | 淮安洪阳化工有限公司 | Benzoyl chloride produces reaction unit |
| CN105732327A (en) * | 2016-04-27 | 2016-07-06 | 锡矿山闪星锑业有限责任公司 | Method and device for preparing ethylene glycol antimony through microwave reaction |
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