CN106540642A - Light-initiated controlled radical polymerization device and application - Google Patents
Light-initiated controlled radical polymerization device and application Download PDFInfo
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- CN106540642A CN106540642A CN201611058803.8A CN201611058803A CN106540642A CN 106540642 A CN106540642 A CN 106540642A CN 201611058803 A CN201611058803 A CN 201611058803A CN 106540642 A CN106540642 A CN 106540642A
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- 238000010526 radical polymerization reaction Methods 0.000 title claims abstract description 39
- 238000006243 chemical reaction Methods 0.000 claims abstract description 80
- 238000006116 polymerization reaction Methods 0.000 claims abstract description 34
- 230000001276 controlling effect Effects 0.000 claims abstract description 33
- 230000001105 regulatory effect Effects 0.000 claims abstract description 20
- 238000005286 illumination Methods 0.000 claims abstract description 15
- 230000008859 change Effects 0.000 claims abstract description 12
- 230000005855 radiation Effects 0.000 claims abstract description 11
- 238000005395 radioluminescence Methods 0.000 claims abstract description 10
- 239000003086 colorant Substances 0.000 claims abstract description 4
- 239000007788 liquid Substances 0.000 claims description 33
- 238000010512 small scale reaction Methods 0.000 claims description 12
- 238000004804 winding Methods 0.000 claims description 12
- 238000004020 luminiscence type Methods 0.000 claims description 11
- 239000000725 suspension Substances 0.000 claims description 10
- 239000011248 coating agent Substances 0.000 claims description 8
- 238000000576 coating method Methods 0.000 claims description 8
- 238000010667 large scale reaction Methods 0.000 claims description 8
- 238000010907 mechanical stirring Methods 0.000 claims description 8
- 239000012780 transparent material Substances 0.000 claims description 8
- 239000000463 material Substances 0.000 claims description 7
- 230000000379 polymerizing effect Effects 0.000 claims description 7
- 238000000034 method Methods 0.000 claims description 6
- 238000009434 installation Methods 0.000 claims description 5
- 230000017525 heat dissipation Effects 0.000 claims description 4
- 239000000376 reactant Substances 0.000 claims description 4
- 238000012546 transfer Methods 0.000 claims description 4
- 238000013019 agitation Methods 0.000 claims description 3
- 239000000110 cooling liquid Substances 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 3
- 238000013467 fragmentation Methods 0.000 claims description 2
- 238000006062 fragmentation reaction Methods 0.000 claims description 2
- 238000002789 length control Methods 0.000 claims description 2
- 238000007254 oxidation reaction Methods 0.000 claims description 2
- 230000027756 respiratory electron transport chain Effects 0.000 claims description 2
- 230000002441 reversible effect Effects 0.000 claims description 2
- 230000007704 transition Effects 0.000 claims description 2
- 238000002347 injection Methods 0.000 claims 1
- 239000007924 injection Substances 0.000 claims 1
- 230000000977 initiatory effect Effects 0.000 abstract description 4
- 238000004519 manufacturing process Methods 0.000 abstract description 4
- 230000003287 optical effect Effects 0.000 abstract description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 8
- 229910052757 nitrogen Inorganic materials 0.000 description 4
- 230000000694 effects Effects 0.000 description 3
- 239000000178 monomer Substances 0.000 description 3
- 229920000642 polymer Polymers 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 150000001253 acrylic acids Chemical class 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 150000002148 esters Chemical class 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- 238000011031 large-scale manufacturing process Methods 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
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- 238000002474 experimental method Methods 0.000 description 1
- 239000004744 fabric Substances 0.000 description 1
- 239000003999 initiator Substances 0.000 description 1
- 238000010550 living polymerization reaction Methods 0.000 description 1
- 229920002521 macromolecule Polymers 0.000 description 1
- 239000003863 metallic catalyst Substances 0.000 description 1
- 238000004377 microelectronic Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
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- 150000003254 radicals Chemical class 0.000 description 1
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Classifications
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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
- B01J19/08—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor
- B01J19/12—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor employing electromagnetic waves
-
- 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
- B01J19/0006—Controlling or regulating processes
- B01J19/0013—Controlling the temperature of the process
-
- 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
- B01J19/08—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor
- B01J19/12—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor employing electromagnetic waves
- B01J19/122—Incoherent waves
- B01J19/123—Ultra-violet light
-
- 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
- B01J19/08—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor
- B01J19/12—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor employing electromagnetic waves
- B01J19/122—Incoherent waves
- B01J19/127—Sunlight; Visible light
-
- 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
- B01J19/08—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor
- B01J19/12—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor employing electromagnetic waves
- B01J19/122—Incoherent waves
- B01J19/128—Infra-red light
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F2/00—Processes of polymerisation
- C08F2/01—Processes of polymerisation characterised by special features of the polymerisation apparatus used
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F2/00—Processes of polymerisation
- C08F2/46—Polymerisation initiated by wave energy or particle radiation
- C08F2/48—Polymerisation initiated by wave energy or particle radiation by ultraviolet or visible light
-
- 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
- B01J2219/08—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor
- B01J2219/0801—Controlling the process
Abstract
The invention discloses a kind of light-initiated controlled radical polymerization device and application, the light source part of photochemistry control device is constituted using series of LED lamp components, temperature regulating device carries out light radiation control to the reaction environment in polymerization container, radioluminescence is carried out by adjusting each LED device, the array light source distribution mode for thus being constituted can change polyreaction light radiation intensity.Apparatus of the present invention can be used for laboratory micro reaction, it can also be used to extensive reactor production.Apparatus of the present invention include dismountable LED lamp panel, temperature control tank, LED component, the controllable light initiation polymerization under different temperatures, intensity of illumination, light wave can be met, can be by changing the number of the canoe of LED, length, bulb regulating and controlling intensity of illumination, visible ray or ultraviolet light from different colours changes the optical wavelength required for causing, and by adjusting the temperature monitor in real time of temperature-controlled box and changing reaction temperature.
Description
Technical field
The present invention relates to a kind of polymerizing reactor and its application, more particularly to a kind of controlled radical polymerization dress
Put and apply, be applied to the synthesis technical field of polymer.
Background technology
Photoinitiated reactions it is with a long history, and which has in terms of the synthesis of chemosynthesis, particularly polymer extensively
Application.Using visible light polymerization be a kind of milder and be a kind of high-energy green condition.Relative to traditional heat
Cause radical polymerization, more win one by control aspect of the Light lnduced Free Radicals polyreaction in the conversion ratio and molecular weight of monomer
Raise.Traditional initiation reaction is typically necessary addition initiator, and reaction condition is harsher.Additionally, visible ray is biologically
It is less using the harm caused to cell or soft tissue.Controlled radical polymerization effectively can synthesize with controllable point
The polymer of son amount and narrow molecular weight distribution.At present, light-initiated controllable free-radical polymerisation be recent development a class it is controllable from
By base polymerization.Its reaction condition is gentle, can realize controllable living polymerization at ambient temperature, with poly- faster
Close efficiency, it is possible to achieve the "on" and "off" of polymerization system, while the consumption of metallic catalyst can also be reduced, therefore can also
Green Chemistry is realized preferably.Photochemistry is not only applied in traditional radical polymerization, particularly in adhesive, coating
And in the field such as microelectronics, also almost find application in each specific " activity "/controllable free radical polymerization process, and solve
Determined many problems, be also many new chances to be created using Macroscopic single crystal method for designing synthesising macromolecule copolymer, and
And also have good application prospect in commercial production.But only have simple and crude manual assembling currently used for photochemical experimental provision
Device, it is impossible to suitable for large-scale production, and exist radiating, light intensity and temperature be difficult to adjust, poor durability the shortcomings of.
The content of the invention
In order to solve prior art problem, it is an object of the invention to overcome the shortcomings of that prior art is present, there is provided a kind of
Light-initiated controlled radical polymerization device and application, preferably realize the control of reaction condition, and then to controllable free-radical
Polymerization process is regulated and controled.Apparatus of the present invention simple structure, part are installed and replace convenient, can be used for laboratory micro reaction,
Can be used for extensive reactor production.Apparatus of the present invention are mainly used in the reaction of LED visible light initiation, and can regulate and control reaction
Intensity of illumination and polymerization temperature.
Purpose is created to reach foregoing invention, the present invention adopts following technical proposals：
A kind of light-initiated controlled radical polymerization device, is made up of polymerizing reactor and photochemistry control device,
Polymerizing reactor is made up of polymerization container and temperature regulating device, and polymerization container is made using transparent material, temperature control dress
Put and the reaction temperature condition in polymerization container is controlled, the light source part of photochemistry control device is using a series of
LED device is constituted, and each LED device is all arranged at the outside of polymerization container, and temperature regulating device is in polymerization container
Reaction environment carry out light radiation control, carry out radioluminescence by adjusting each LED device, the array light source for thus being constituted
Distribution mode can change polyreaction light radiation intensity.
Used as currently preferred technical scheme, each LED device is freely releasably arranged on shape in strip flexible strap
Into LED lamp bar band, LED lamp bar band is made to be arranged at the outside of polymerization container, by the canoe energy for adjusting LED lamp bar band
Change polyreaction light radiation intensity.
As the first further preferred technical scheme of such scheme, as small-scale reaction unit, specially：
Using the detachable reaction tube replaced, reaction tube volume is 0.005-30L to polymerization container；Temperature regulating device is adopted
Temperature controlling groove, reaction tube is detachably fixed and is installed in temperature controlling groove, forms transparent sandwich device, and temperature controlling groove adopts transparent material system
Into, temperature control liquid is injected in the transparent sandwich between temperature controlling groove and reaction tube, temperature control liquid adopts transparency liquid, can control anti-
At -20～200 DEG C, transparent sandwich connects a temperature-controlled box to temperature that should be in pipe, can realize controlling the temperature of transparency liquid
System, controls the temperature of temperature control liquid in temperature controlling groove by control device, and then regulates and controls the temperature of liquid in reaction tube；Photochemistry control
LED that device processed is made up of LED, can freely load and unload and replace the LED lamp panel that uses and LED temperature control tank is constituted, LED
Lamp plate is arranged at the outside of temperature controlling groove, and is arranged between temperature controlling groove outer wall and LED temperature control tank inwall, and LED is removable
Wind with unloading and be arranged in LED lamp panel, forming array of source carries out radioluminescence to reaction tube, is driven and adjusted by control device
Each LED, at least controls the luminous intensity and radiant light wavelength of correspondence LED, and LED temperature control tank is to the LED in LED
The radiating of lamp carries out assist control；It is additionally provided with agitating device to be stirred the liquid inserted in reaction tube；Reaction unit is set
Support base is fixedly connected to temperature controlling groove, LED lamp panel and LED temperature control tank.
Above-mentioned agitating device preferably adopts mechanical stirring device, is preferably made up of magnetic suspension magneton and agitator, magnetic suspension
Magneton is arranged in reaction tube, and agitator is arranged at below temperature controlling groove, controls agitator by control device, drives magnetic suspension magneton
Mechanical agitation is carried out to the liquid in reaction tube.
As second further preferred technical scheme of such scheme, as large-scale reaction unit, specially：
Polymerization container adopts reactor, reactor to make using transparent material, reactor inner chamber as reactive tank,
Reactor top arranges closure, and socket, blow vent and the installation mechanical stirring device of installation thermometer are covered with sealing
Through hole；Temperature regulating device adopts calandria and thermometer, heats physical ability to the liquid input heat in reactor, and control device passes through
Temperature of liquid information in the reactor of thermometer collection, controls the output of calandria；Photochemistry control device is sent out by LED
The LED tape of optical assembly composition, can freely load and unload and replace the LED fixed plate that uses and LED tape temperature control tank composition,
LED fixed plate is arranged at the outside of reactor, and LED tape removably winds and is arranged in LED fixed plate, forms light
Source array carries out radioluminescence to reactor, is driven and adjusted by control device each LED luminescence component, at least controls correspondence
The luminous intensity and radiant light wavelength of LED luminescence component, LED tape temperature control tank is to the luminous group of LED on LED tape
The radiating of part carries out assist control；Mechanical stirring device is stirred to the material inserted in reactor；Reaction unit is set
Support body is fixedly connected to reactor, LED fixed plate and LED tape temperature control tank.
Used as the further preferred technical scheme of such scheme, the canoe of LED lamp bar band adopts equidistant ring ring
Winding, the ring ring winding of unequal-interval, the winding of triangle or back-shaped winding；The LED device arranged on LED lamp bar band
Density it is adjustable.
As the further preferred technical scheme of such scheme, the LED temperature control tank of small-scale reaction unit or
The housing of the LED tape temperature control tank of large-scale reaction unit has closed middle cavity, is provided with circulation in hollow intracavity cold
But liquid, carries out auxiliary heat dissipation to the LED device on LED lamp bar band, LED temperature control tank outside wall surface or LED
Tape temperature control tank outside wall surface coats lighttight coating.
Used as the further preferred technical scheme of such scheme, the LED lamp panel of small-scale reaction unit is arranged at LED
On the inwall of light bar temperature control tank, the radiator portion of LED is made to be radiated by LED lamp panel and LED temperature control tank；Or big rule
The LED fixed plate of the reaction unit of mould is arranged on the inwall of LED tape temperature control tank, makes the radiating of LED luminescence component
Radiated by LED fixed plate and LED tape temperature control tank part.
As the further preferred technical scheme of such scheme, the LED lamp panel of small-scale reaction unit or big rule
The LED fixed plate of the reaction unit of mould at least adopts two pieces, in small-scale reaction unit, arranges corresponding LED lamp panel and encloses
It is symmetrical around temperature controlling groove；Or in large-scale reaction unit, corresponding LED fixed plate is set and is symmetrically divided around reactor
Cloth.
Used as the further preferred technical scheme of such scheme, the illumination mode of the LED device in LED is adopted
Different glow color combinations, when the group for having multiple energy to cause by illumination on the reactant in polymerization container, energy
The glow color of free switching LED.
As the further preferred technical scheme of such scheme, the adjustable length control of LED, the length of LED
No more than 200m.
Used as the further preferred technical scheme of such scheme, the density of the LED device in LED is per meter
In LED, the number of bulb is 5-1000.
A kind of application of light-initiated controlled radical polymerization device of the invention, it is characterised in that：Be applied to it is controllable from
By base polyreaction, specially atom transition free radical polymerization reaction, reversible addion-fragmentation chain transfer Raolical polymerizable,
Single electron transfer living free radical polymerization, the Raolical polymerizable of nitrogen-oxidation stability cause chain tra nsfer terminator method anti-
Should.
The present invention compared with prior art, obviously projects substantive distinguishing features and remarkable advantage with following：
1. the present invention is reacted for laboratory micro, it can also be used to extensive reactor production；
2. apparatus of the present invention include the experiment packages such as dismountable LED lamp panel, temperature control tank, LED, can meet not equality of temperature
Degree, intensity of illumination, the controllable light initiation polymerization under light wave；
3. the present invention can pass through the canoe of change LED, length, and the number of bulb is regulating and controlling intensity of illumination；
4. the present invention is changed using the visible ray or ultraviolet light of different colours and causes required optical wavelength, and by adjusting
The temperature monitor in real time of temperature-controlled box simultaneously changes the temperature of reaction；
5. the spacing in every meter of LED of the present invention between the number of bulb, the length of LED and light bar can
As change intensity of illumination variable, at least can select LED bulb color be blue and green light, the various visible rays of HONGGUANG and
Ultraviolet light, it is ensured that light-initiated controlled radical polymerization is smoothed out.
Description of the drawings
Structural representations of the Fig. 1 for one light-initiated controlled radical polymerization device of the embodiment of the present invention.
Structural representations of the Fig. 2 for two light-initiated controlled radical polymerization device of the embodiment of the present invention.
Fig. 3 is equidistant ring ring winding side of the LED of the embodiment of the present invention one in the LED lamp panel that freely can be dismantled
Formula.
Fig. 4 is the winding side of triangle of the LED of the embodiment of the present invention two in the LED lamp panel that freely can be dismantled
Formula.
Fig. 5 is back-shaped canoe of the LED of the embodiment of the present invention three in the LED lamp panel that freely can be dismantled.
Fig. 6 is the LED device illumination mode in the LED of the embodiment of the present invention four using different glow color combinations
Diagram.
Specific embodiment
Details are as follows for the preferred embodiments of the present invention：
Embodiment one：
In the present embodiment, referring to Fig. 1 and Fig. 3, a kind of light-initiated controlled radical polymerization device, as small-scale
Reaction unit, specially：
Using the detachable reaction tube 1 replaced, 1 volume of reaction tube is 0.1L to polymerization container；
Temperature regulating device adopts temperature controlling groove 2, reaction tube 1 is detachably fixed and is installed in temperature controlling groove 2, forms transparent sandwich dress
Put, temperature controlling groove 2 is made using transparent material, in the transparent sandwich between temperature controlling groove 2 and reaction tube 1, inject temperature control liquid, control
Geothermal liquid adopts transparency liquid, can control temperature in reaction tube 1 at 50 DEG C, and temperature control tank material is high-quality high temperature resistant and thoroughly
The high glass of light rate, the temperature control liquid of selection is a kind of high liquid of transmitance, can provide temperature required for reaction, transparent folder
Layer one temperature-controlled box of connection, can realize being controlled the temperature of transparency liquid, control temperature control in temperature controlling groove 2 by control device
The temperature of liquid, and then regulate and control the temperature of liquid in reaction tube 1；The LED 3, energy that photochemistry control device is made up of LED
Freely load and unload and replace the LED lamp panel 5 that uses and LED temperature control tank 6 is constituted, the length of LED 3 is 20m, in LED
LED device density be bulb in every meter of LED number be 50, LED lamp panel 5 is arranged at the outside of temperature controlling groove 2,
And be arranged between 6 inwall of 2 outer wall of temperature controlling groove and LED temperature control tank, LED 3 is removably twined using equidistant ring ring
Wind around mode and be arranged in LED lamp panel 5, forming array of source carries out radioluminescence to reaction tube 1, is driven simultaneously by control device
Each LED is adjusted, the luminous intensity and radiant light wavelength of correspondence LED is controlled, LED temperature control tank 6 is in LED 3
The radiating of LED carries out assist control；It is additionally provided with agitating device and is stirred to inserting the liquid in reaction tube 1；Reaction is set
Device support base 7 is fixedly connected to temperature controlling groove 2, LED lamp panel 5 and LED temperature control tank 6.The present embodiment is by LED 3
Be wrapped in LED lamp panel 5, not only can adopt equidistant ring ring canoe, and can using different canoes come
Using a kind of lamp plate, LED lamp panel can be directly used instead according to the needs of reaction, it is convenient and swift, the trouble of winding is eliminated, and
And the radiant intensity of each lamp plate can also be tested using light intensity meter；LED temperature control tank 6 is primarily to control LED 3
Temperature because LED long-time illumination can release substantial amounts of heat, affect the temperature stability of reaction unit, while this also can
Greatly reduce the service life of LED, so arranging a temperature control tank, the temperature of temperature light bar is controlled at 20 DEG C, be conducive to
Extend the service life of LED.
Referring to Fig. 1, agitating device adopts mechanical stirring device, is made up of magnetic suspension magneton 4 and agitator 8, magnetic suspension magnetic
Son 4 is arranged in reaction tube 1, and agitator 8 is arranged at below temperature controlling groove 2, controls agitator 8 by control device, drives magnetic suspension
Magneton 4 carries out mechanical agitation to the liquid in reaction tube 1.Magnetic suspension magneton 4 adopts tetrafluoro magneton, makes solution in the condition of stirring
Under can rotate, the size of magneton select can according to input raw material amount be selected.
Referring to Fig. 1 and Fig. 3, the housing of LED temperature control tank 6 has closed middle cavity, is provided with circulation in hollow intracavity
Cooling liquid, carries out auxiliary heat dissipation to the LED device on LED lamp bar band, coats not in the outside wall surface of LED temperature control tank 6
The coating of printing opacity.The LED lamp panel 5 of reaction unit is arranged on the inwall of LED temperature control tank 6, leads to the radiator portion of LED
Cross LED lamp panel 5 and LED temperature control tank 6 is radiated, radiating effect is notable.
Two pieces are adopted referring to the LED lamp panel 5 of Fig. 1, LED lamp panel 5 or large-scale reaction unit, in small-scale reaction
In device, it is symmetrical around temperature controlling groove 2 that corresponding LED lamp panel 5 is set.
Referring to Fig. 1 and Fig. 3, the light-initiated controlled radical polymerization device of the present embodiment, by polymerizing reactor and light
Chemical Control device is constituted, and polymerizing reactor is made up of polymerization container and temperature regulating device, and polymerization container is using saturating
Bright material is made, and temperature regulating device is controlled to the reaction temperature condition in polymerization container, the light of photochemistry control device
Source part is constituted using series of LED lamp components, and each LED device is all arranged at the outside of polymerization container, temperature regulating device
Light radiation control is carried out to the reaction environment in polymerization container, radioluminescence is carried out by adjusting each LED device, thus
The array light source distribution mode for being constituted can change polyreaction light radiation intensity.Each LED device is freely releasably arranged on
LED lamp bar band is formed in strip flexible strap, makes LED lamp bar band be arranged at the outside of polymerization container, by adjusting LED
The canoe of band can change polyreaction light radiation intensity.
Referring to Fig. 1 and Fig. 3, the temperature control of the present embodiment reaction is realized by using a transparent sandwich, should
The material of transparent sandwich uses U-shaped glass guide channel as temperature controlling groove 2, and it has good heat conductivity and good light transmission；
Transparent sandwich connects a temperature-controlled box, can realize the control to temperature.The control of the light intensity of reaction is by changing LED 3
LED device luminous parameters realizing.The innovative point of the present embodiment device is that LED 3 is wrapped in one to tear open
In the LED lamp panel 5 of the draw-in groove shape for unloading, the intensity of illumination of different specifications can be selected to change light intensity, facilitated and overhauled and change.
It is for the degree that preferably can be reacted with monitor in real time, convenient to observe, it is light tight in the outside wall surface coating of LED temperature control tank 6
Coating, so can convenient use, do not cause light pollution.LED 3 used by the present embodiment can launch blue light, green glow, HONGGUANG
A series of visible rays and ultraviolet light.
Referring to Fig. 1 and Fig. 3, the present embodiment is used for the small-scale reaction unit of laboratory, applies in general to several milligrams and arrives several
Ten grams of reactant.The present embodiment takes the monomer of 0.5g esters of acrylic acids in reaction tube 1, and is added thereto to correspondence ratio
RAFT reagents and appropriate solvent, it is reaction tube is closed with rubber stopper, nitrogen is replaced, and nitrogen will be full of in reaction tube, by LED
The temperature setting of light bar 3 is 20 DEG C, and the temperature setting of reaction tube 1 is 50 DEG C, opens LED, after reaction a period of time, can
To close LED 3, two temperature regulating devices can stopped reaction.
Embodiment two：
The present embodiment is essentially identical with embodiment one, is particular in that：
In the present embodiment, referring to Fig. 2 and Fig. 4, a kind of light-initiated controlled radical polymerization device, as extensive
Reaction unit, specially：
Polymerization container adopts reactor, reactor to make using transparent material, reactor inner chamber as reactive tank 12,
Closure 11 is set on reactor top, and socket 9, blow vent 10 and the installation machinery for installation thermometer being provided with closure 11 is stirred
The through hole of device 13 is mixed, thermometer socket 9 conveniently can detect the temperature in reaction system at any time, to the real-time monitoring reacted, lead to
QI KOU 10 can be passed through protective gas in reaction system when reaction needs gas shield with vacuum condition；Temperature regulating device is adopted
Calandria and thermometer, heat physical ability to the liquid input heat in reactor, the reaction that control device is gathered by thermometer
Temperature of liquid information in kettle, controls the output of calandria；Photochemistry control device is made up of LED luminescence component 15
LED tape, can freely load and unload and replace the LED fixed plate 14 that uses and LED tape temperature control tank 16 is constituted, LED
Length is 200m, and it is 5 that the density of the LED device on LED tape is the number of bulb in every meter of LED, and LED is solid
Fixed board 14 is arranged at the outside of reactor, and LED tape is removably arranged at LED with the canoe winding of triangle
In fixed plate 14, forming array of source carries out radioluminescence to reactor, is driven and adjusted by control device the luminous group of each LED
Part 15, the luminous intensity and radiant light wavelength of control correspondence LED luminescence component 15, LED tape temperature control tank 16 is to LED
The radiating of the LED luminescence component 15 on bar carries out assist control；13 pairs of materials inserted in reactor of mechanical stirring device enter
Row stirring；Arrange reaction unit supporting frame to be fixed reactor, LED fixed plate 14 and LED tape temperature control tank 16
Connection.
In the present embodiment, referring to Fig. 2, the housing of LED tape temperature control tank 16 has closed middle cavity, in middle cavity
Circulating cooling liquid is inside provided with, auxiliary heat dissipation is carried out to the LED device on LED lamp bar band, outside LED tape temperature control tank 16
Wall coats lighttight coating.LED fixed plate 14 is arranged on the inwall of LED tape temperature control tank 16, makes LED light
The radiator portion of component 15 passes through LED fixed plate 14 and LED tape temperature control tank 16 is radiated, effect is significant.
In the present embodiment, referring to Fig. 2 and Fig. 4, LED fixed plate 14 adopts 3 pieces, in large-scale reaction unit,
It is symmetrical around reactor that corresponding LED fixed plate 14 is set.
In the present embodiment, referring to Fig. 2 and Fig. 4, the present embodiment is used for the reaction kettle device of large-scale production, can be suitably used for
Tens grams are arrived several hectograms or more substantial large-scale process units.The present embodiment takes the monomer of 200g esters of acrylic acids in reaction
In kettle, and it is added thereto to correspond to the RAFT reagents and appropriate solvent of ratio, is sealed with closure 11, replace nitrogen, and will
Nitrogen is full of in reactor, is 20 DEG C by the temperature setting of LED tape, the temperature setting of reactor is 50 DEG C, opens LED
Luminescence component 15, after reaction a period of time, closes LED tape, can stopped reaction after two temperature regulating devices.
Embodiment three：
The present embodiment is substantially the same as in the previous example, and is particular in that：
In the present embodiment, referring to Fig. 5, back-shaped canoe of the LED in the LED lamp panel that freely can be dismantled,
Effective light-initiated controlled radical polymerization can be realized.
Example IV：
The present embodiment is substantially the same as in the previous example, and is particular in that：
In the present embodiment, referring to Fig. 6, the illumination mode of the LED device in LED adopts different glow colors
Combination, when the group for having multiple energy to cause by illumination on the reactant in polymerization container, can free switching LED
Glow color.
The embodiment of the present invention is illustrated above in conjunction with accompanying drawing, but the invention is not restricted to above-described embodiment, can be with
The purpose of innovation and creation of the invention makes various changes, under all spirit and principle according to technical solution of the present invention
Change, modification, replacement, combination or the simplification made, should be equivalent substitute mode, as long as meeting the goal of the invention of the present invention,
Without departing from light-initiated controlled radical polymerization device of the invention and know-why and the inventive concept of application, belong to
Protection scope of the present invention.
Claims (13)
1. a kind of light-initiated controlled radical polymerization device, is made up of polymerizing reactor and photochemistry control device, its
It is characterised by：Polymerizing reactor is made up of polymerization container and temperature regulating device, and the polymerization container adopts transparent material
Material is made, and the temperature regulating device is controlled to the reaction temperature condition in polymerization container, the light of photochemistry control device
Source part is constituted using series of LED lamp components, and each LED device is all arranged at the outside of polymerization container, described
Temperature regulating device carries out light radiation control to the reaction environment in polymerization container, is carried out by adjusting each LED device
Radioluminescence, the array light source distribution mode for thus being constituted can change polyreaction light radiation intensity.
2. light-initiated controlled radical polymerization device according to claim 1, it is characterised in that：Each LED device
Part is freely releasably arranged in strip flexible strap and forms LED lamp bar band, makes LED lamp bar band be arranged at polymerization container
Outside, can change polyreaction light radiation intensity by adjusting the canoe of LED lamp bar band.
3. light-initiated controlled radical polymerization device according to claim 2, it is characterised in that as small-scale anti-
Device is answered, specially：
Using the detachable reaction tube (1) replaced, reaction tube (1) volume is 0.005-30L to the polymerization container；
The temperature regulating device adopts temperature controlling groove (2), reaction tube (1) is detachably fixed and is installed in temperature controlling groove (2), formed transparent
Sandwich device, the temperature controlling groove (2) are made using transparent material, in the transparent sandwich between temperature controlling groove (2) and reaction tube (1)
Injection temperature control liquid, temperature control liquid adopts transparency liquid, can control temperature in reaction tube (1) at -20～200 DEG C, transparent folder
Layer one temperature-controlled box of connection, can realize being controlled the temperature of transparency liquid, control control in temperature controlling groove (2) by control device
The temperature of geothermal liquid, and then regulate and control the temperature of liquid in reaction tube (1)；
LED (3) that the photochemistry control device is made up of LED, can freely load and unload and replace the LED lamp panel (5) for using
Constitute with LED temperature control tank (6), LED lamp panel (5) is arranged at the outside of temperature controlling groove (2), and is arranged at temperature controlling groove (2) outer wall
And LED temperature control tank (6) inwall between, the LED (3) removably winds and is arranged in LED lamp panel (5), is formed
Array of source carries out radioluminescence to reaction tube (1), is driven and adjusted by control device each LED, at least controls correspondence LED
Luminous intensity and radiant light wavelength, radiating of the LED temperature control tank (6) to the LED in LED (3) carry out auxiliary control
System；
It is additionally provided with agitating device and is stirred to inserting the liquid in reaction tube (1)；Reaction unit support base (7) is set to temperature control
Groove (2), LED lamp panel (5) and LED temperature control tank (6) are fixedly connected.
4. light-initiated controlled radical polymerization device according to claim 3, it is characterised in that：The agitating device is adopted
With mechanical stirring device, it is made up of magnetic suspension magneton (4) and agitator (8), the magnetic suspension magneton (4) is arranged at reaction tube
(1) in, the agitator (8) is arranged at below temperature controlling groove (2), controls agitator (8) by control device, drives magnetic suspension magneton
(4) mechanical agitation is carried out to the liquid in reaction tube (1).
5. light-initiated controlled radical polymerization device according to claim 2, it is characterised in that as large-scale anti-
Device is answered, specially：
The polymerization container adopts reactor, the reactor to make using transparent material, and reactor inner chamber is used as reaction
Groove (12), arranges closure (11) on the reactor top, is provided with closure (11) and installs the socket (9) of thermometer, leads to
QI KOU (10) and the through hole of installation mechanical stirring device (13)；
The temperature regulating device adopts calandria and thermometer, heats physical ability to the liquid input heat in reactor, control device
By temperature of liquid information in the reactor that thermometer is gathered, the output of calandria is controlled；
LED tape that the photochemistry control device is made up of LED luminescence component (15), can freely load and unload and replace what is used
LED fixed plate (14) and LED tape temperature control tank (16) composition,
LED fixed plate (14) is arranged at the outside of reactor, and the LED tape removably winds and is arranged at LED admittedly
In fixed board (14), forming array of source carries out radioluminescence to reactor, is driven and adjusted by control device the luminous group of each LED
Part (15), at least controls the luminous intensity and radiant light wavelength of correspondence LED luminescence component (15), LED tape temperature control tank
(16) radiating to the LED luminescence component (15) on LED tape carries out assist control；
Mechanical stirring device (13) is stirred to the material inserted in reactor；Reaction unit supporting frame is set to reaction
Kettle, LED fixed plate (14) and LED tape temperature control tank (16) are fixedly connected.
6. the light-initiated controlled radical polymerization device according to any one in claim 2～5, it is characterised in that：
The canoe of LED lamp bar band is using the winding of equidistant ring ring, the ring ring winding of unequal-interval, the winding of triangle or back-shaped
Winding；The density of the LED device arranged on LED lamp bar band is adjustable.
7. the light-initiated controlled radical polymerization device according to any one in claim 3～5, it is characterised in that：
LED tape temperature control tank (16) of the LED temperature control tank (6) of the small-scale reaction unit or large-scale reaction unit
Housing there is closed middle cavity, be provided with circulating cooling liquid in hollow intracavity, the LED device on LED lamp bar band entered
Row auxiliary heat dissipation, LED temperature control tank (6) outside wall surface or LED tape temperature control tank (16) outside wall surface coating it is light tight
Coating.
8. the light-initiated controlled radical polymerization device according to any one in claim 3～5, it is characterised in that：
The LED lamp panel (5) of small-scale reaction unit is arranged on the inwall of LED temperature control tank (6), makes the radiator portion of LED
Radiated by LED lamp panel (5) and LED temperature control tank (6)；Or the LED fixed plate (14) of large-scale reaction unit
It is arranged on the inwall of LED tape temperature control tank (16), the radiator portion of LED luminescence component (15) is fixed by LED
Plate (14) and LED tape temperature control tank (16) are radiated.
9. the light-initiated controlled radical polymerization device according to any one in claim 3～5, it is characterised in that：
The LED fixed plate (14) of the LED lamp panel (5) of small-scale reaction unit or large-scale reaction unit at least adopts two
Block, in small-scale reaction unit, arranges corresponding LED lamp panel (5) symmetrical around temperature controlling groove (2)；Or extensive
Reaction unit in, it is symmetrical around reactor that corresponding LED fixed plate (14) is set.
10. the light-initiated controlled radical polymerization device according to any one in claim 2～5, it is characterised in that：
The illumination mode of the LED device in LED is combined using different glow colors, when the reactant in polymerization container
On when having the group that multiple energy are caused by illumination, can free switching LED glow color.
11. according to any one in claim 2～5 light-initiated controlled radical polymerization device, it is characterised in that：
The adjustable length control of LED, the length of LED are not more than 200m.
12. according to any one in claim 2～5 light-initiated controlled radical polymerization device, it is characterised in that：
It is 5-1000 that the density of the LED device in LED is the number of bulb in every meter of LED.
The application of light-initiated controlled radical polymerization device described in a kind of 13. claim 1, it is characterised in that：It is applied to
Controlled radical polymerization, specially atom transition free radical polymerization reaction, reversible addion-fragmentation chain transfer radical polymerization
Reaction, single electron transfer living free radical polymerization, the Raolical polymerizable of nitrogen-oxidation stability cause chain tra nsfer terminator
Method is reacted.
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| CN110237795A (en) * | 2019-05-15 | 2019-09-17 | 铜仁学院 | A kind of photocatalytic reaction device |
| CN110876915A (en) * | 2018-09-05 | 2020-03-13 | 捷微科技股份有限公司 | Temperature control light source device for photochemical reaction tank and photochemical reaction tank |
| CN111889050A (en) * | 2020-08-19 | 2020-11-06 | 四川大学 | Photocatalysis reaction appearance |
| CN112175586A (en) * | 2020-09-28 | 2021-01-05 | 杭州应星新材料有限公司 | UV-cured acrylic acid heat-conducting composition, heat-conducting sheet and preparation method thereof |
| CN112452279A (en) * | 2020-12-04 | 2021-03-09 | 吴凡 | Drug synthesis device based on different reaction parameters |
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| CN112175586A (en) * | 2020-09-28 | 2021-01-05 | 杭州应星新材料有限公司 | UV-cured acrylic acid heat-conducting composition, heat-conducting sheet and preparation method thereof |
| CN112175586B (en) * | 2020-09-28 | 2021-12-07 | 杭州应星新材料有限公司 | UV-cured acrylic acid heat-conducting composition, heat-conducting sheet and preparation method thereof |
| CN112452279A (en) * | 2020-12-04 | 2021-03-09 | 吴凡 | Drug synthesis device based on different reaction parameters |
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