CN209393167U - Optical chlorinating reaction pipe and optical chlorinating reaction device - Google Patents
Optical chlorinating reaction pipe and optical chlorinating reaction device Download PDFInfo
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- CN209393167U CN209393167U CN201821974713.8U CN201821974713U CN209393167U CN 209393167 U CN209393167 U CN 209393167U CN 201821974713 U CN201821974713 U CN 201821974713U CN 209393167 U CN209393167 U CN 209393167U
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Abstract
Disclose optical chlorinating reaction pipe and optical chlorinating reaction device.The reactor includes multiple optical chlorinating reaction pipes, and the reaction tube includes inner and outer tubes and upper plate and lower plate annular in shape；Said inner tube is hollow tube, its tube wall includes the internal layer towards hollow space and the outer layer towards outer tube side, there are many LED lamp beads for arrangement at least partly surface between internal layer and outer layer, the LED lamp bead is sealed in the tube wall of said inner tube by internal layer together with outer layer, and the outer layer is that can transmit made of the material of LED peak value spectrum；The outer pipe encapsulation said inner tube, and the spacing between the outer surface of said inner tube and the inner surface of outer tube forms reaction channel；The cricoid upper plate and lower plate respectively have material outlet or entrance；The material outlet or entrance and the reaction channel are in fluid communication, and outer surface, outer tube lateral surface and the inner tube medial surface of the upper plate and lower plate constitute the surface of the optical chlorinating reaction device.
Description
Technical field
The utility model relates to a kind of optical chlorinating reaction devices, especially a kind of to prepare one chloroethene of difluoro for highly selective
The optical chlorinating reaction device of alkane.Byproduct of reaction can be advantageously reduced with the utility model reactor, reduce energy consumption.
Background technique
Difluoromono-chloroethane (abbreviation HCFC-142b) is a kind of very important organic intermediate, be commonly used for refrigerant,
Foaming agent or raw material as vinylidene fluoride monomers.
Document " technological design of chlorodifluoroethane process units " (" chemical engineering and equipment ", the 10th phase in 2015) is right
The production method of chlorodifluoroethane is summarized, and manufacturing method generally comprises the manufacture using methyl chloroform as raw material
Method, using vinylidene chloride as the manufacturing method of raw material, using vinyl chloride as the manufacturing method of raw material and using acetylene as the manufacture of raw material
Method.
Acetylene method is the commercial run of a relative maturity, it includes occurring that acetylene and HF in the presence of a catalyst
Addition reaction generates Difluoroethane (F152a), and then it is anti-to carry out Light chlorimation with chlorine under conditions of 50-90 DEG C for Difluoroethane
It answers, obtains HCFC-142b:
CH≡CH+2HF→CH3CHF2
CH3CHF2+Cl2→CH3CF2Cl+HCl
Optical chlorinating reaction therein includes making to be fluorinated the Difluoroethane (F152a) generated and chlorine according to a certain percentage
In blending tank mix after enter optical chlorinating reaction device reacted, generate difluoromono-chloroethane (HCFC-142b) and on a small quantity
More chloro by-products:
Main reaction:
C2H4F2+Cl2→C2H3F2Cl(F142b)+HCl
Fluorochemical test result in 1 reaction product of table
The utility model is illustrated above by embodiment, it should be understood that the scope of the utility model with
Subject to claim.
C2H4F2+4Cl2→C2F2Cl4+4HCl
Common optical chlorinating reaction device is helix tube type reactor, and material is transmitance of the quartz glass to guarantee light.Light
Source is high-pressure sodium lamp or ultraviolet lamp, is the most suitable light source of optical chlorinating reaction.
Optical chlorinating reaction is exothermic reaction, and the heat released is taken out of through cold wind, makes reaction temperature control at 100 DEG C
Below.
Chinese patent CN101781164A discloses a kind of preparation method of difluoromono-chloroethane, it includes with liquid phase two
Fluoroethane and chlorine are raw material, carry out reaction by dry method optical chlorinating reaction device after gasifying, mixing in proportion and generate difluoro
Monochlorethane crude product.The dry method optical chlorinating reaction device that the patent uses includes spaced reaction tower section and outer circulation temperature-reducing tower
Two kinds of tower sections are saved, the reaction tower section includes the section of reaction tower up and down equipped with Lighting Interface and the intermediate reaction equipped with fluorescent tube interface
Tower section, the structure of the outer circulation temperature-reducing tower section to walk material in its pipe, shell walks the arrangement of temperature lowering water.
Chinese patent CN103012053A discloses a kind of preparation method of difluoromono-chloroethane, including raw material is pressed 1.15
: optical chlorinating reaction device is passed through after 1 molar ratio mixing.The optical chlorinating reaction device is connected in series by more piece conversion zone, each to react
Section includes the reactor and shell-and-tube heat exchanger that middle and lower part is equipped with light-source system, and light-source system is ultraviolet lamp tube.
" the photochemical selection for generating HCFC-142b device of HFC-152a " (" Zhejiang chemistry " the 1st phase of volume 30) of Wang Min is right
The reaction that Difluoroethane Light chlorimation generates difluoromono-chloroethane is summarized, it is believed that and the optical chlorinating reaction belongs to exothermic reaction,
Since the selectivity of c h bond chloros various in Difluoroethane molecule is poor, and binary replaces speed to replace speed with unitary again
It is equal, be difficult to control, light there are selective, but light is too strong, and temperature height generates high-boiling components.The photochemical dissociation of chlorine molecule can be
59.7Kcal/mol can make chlorine molecule that the longest wavelength of photochemical dissociation occur no more than 478.5-479.5nm.The wavelength of light is got over
Short, the luminous energy of absorption is bigger.The wavelength that Difluoroethane Light chlorimation needs is 400- in 300-500nm, the wavelength of general fluorescent lamp
The wavelength of 700nm, mercury lamp are 20-750nm, therefore are mercury lamps as the most suitable light source of Difluoroethane Light chlorimation, especially high
Pressure mercury lamp, because its light wave is continuous light wave, optical power is ok from 40W to 300W.
In conclusion existing optical chlorinating reaction device multiselect ultraviolet lamp, high-pressure sodium lamp, sodium vapor lamp, fluorescent lamp etc. are as light chlorine
Change reactor light source.It was found that this reactor is easy to produce side reaction, proportion of by-product is higher.Such as Difluoroethane be raw material
During Light chlorimation produces chlorodifluoroethane, discovery can generate a chlorine difluoro of 5%-10% when using fluorescent lamp etc. as light source
Ethane isomer and depth chlorination higher boiling contain fluoride mixture.Further, since high wavelength components be not used to it is really necessary anti-
It answers, energy consumption is caused to waste.
Therefore, it is still necessary to provide a kind of optical chlorinating reaction device, it can overcome in the prior art, and proportion of by-product is higher, energy consumption
Big defect reduces manufacturing cost to improve product quality.
Summary of the invention
One goal of the invention of the utility model is to provide a kind of optical chlorinating reaction device, it can overcome by-product in the prior art
The higher defect of object ratio, the defect that energy consumption is high reduce manufacturing cost to improve product quality.
Therefore, the one aspect of the utility model provides a kind of optical chlorinating reaction pipe, it includes inner and outer tubes and is in
Cricoid upper plate and lower plate, inner edge shape and the said inner tube section shape of the annular base plate match, the ring-type
The outer edge shape of bottom plate matches with the outer tube section shape；
Said inner tube is hollow tube, and tube wall includes the internal layer towards hollow space and the outer layer towards outer tube side, internal layer and
LED lamp bead is disposed at least partly internal layer surface between outer layer, the LED lamp bead is sealed in institute together with outer layer by internal layer
It states in the tube wall of inner tube, the outer layer is that can transmit made of the material of LED peak value spectrum；
The outer pipe encapsulation said inner tube, and the spacing between the outer surface of said inner tube and the inner surface of outer tube is formed
Reaction channel；
The cricoid upper plate and lower plate respectively have material outlet or entrance；The material outlet or entrance
It is in fluid communication with the reaction channel, outer surface, outer tube lateral surface and the inner tube medial surface of the upper plate and lower plate are constituted
The surface of the optical chlorinating reaction pipe.
The another aspect of the utility model is related to a kind of optical chlorinating reaction device, it includes shell and upper and lower bottom plate, Yi Ji
Multiple optical chlorinating reaction pipes in shell, the upper and lower bottom plate of the shell has to be gone out with the raw material of each optical chlorinating reaction pipe
The feed outlet port or entrance and cooling medium input port and cooling medium delivery outlet that mouth or entrance fluidly connect, the cooling
Medium input port and cooling medium delivery outlet respectively with the inner tube hollow space of the optical chlorinating reaction pipe and multiple smooth chlorine
The gap changed between reaction tube is in fluid communication.
Detailed description of the invention
The utility model is illustrated below with reference to example, in attached drawing:
Fig. 1 is the structural schematic diagram of the optical chlorinating reaction pipe of one example of the utility model；
Fig. 2 is the optical chlorinating reaction device cross-sectional view of one example of the utility model, it includes 7 optical chlorinating reaction pipes.
Specific embodiment
The utility model relates to a kind of optical chlorinating reaction pipe, the utility model optical chlorinating reaction pipe include inner and outer tubes with
And upper plate and lower plate annular in shape.
In the utility model one preferable example, the inner tube of the optical chlorinating reaction pipe is hollow circular tube, during outer tube is
Empty round tube, upper plate and lower plate are annular in shape.
In a preferable example of the utility model, the optical chlorinating reaction pipe include concentric inner and outer tubes and
Upper plate and lower plate annular in shape.
Fig. 1 is the schematic diagram of the optical chlorinating reaction pipe of one example of the utility model.As shown in Figure 1, the utility model light
Chlorination reaction pipe includes concentric inner tube 1 and outer tube 2 and upper plate 6 and lower plate 7 annular in shape.
Said inner tube 1 is the hollow tube with annulus section, at least partly surface of the tube wall internal layer 3 towards 2 side of outer tube
On be disposed with LED lamp bead 4, the LED lamp bead 4 is sealed in the tube wall of said inner tube 1 by tube wall outer layer 5 together with internal layer 3.
In an example of the utility model, the tube wall outer layer 5 of said inner tube 1 is with internal layer 3 together by the LED lamp bead
4 are sealed in the tube wall of said inner tube 1, and are sealed with the evacuated processing in tube wall space of LED lamp bead.
Material for manufacturing 1 outer layer 5 of said inner tube is without particular limitation, if to LED issue light it is unobstructed or
Person absorbs.In an example of the utility model, the outer layer 5 of said inner tube is the material by that can transmit LED peak value spectrum
Made of material, such as quartz glass, transparent Teflon etc..
In an example of the utility model, the optical chlorinating reaction pipe is used to arrange the internal layer 3 of LED light by thermally conductive
Material is made.In an example of the utility model, the Heat Conduction Material is selected from the metal materials such as aluminium alloy, stainless steel, copper.
The inner tube 1 and outer tube 2 of the utility model optical chlorinating reaction pipe can have identical or different shape, preferably have phase
Same shape, such as round, polygon.In an example of the utility model, the inner tube 1 of the optical chlorinating reaction pipe and outer
Pipe 2 is concentric round tube.
In an example of the utility model, the outer tube 2 of the optical chlorinating reaction pipe using quartz glass, glass or
The materials such as steel lining enamel are made.In an example of the utility model, the inner wall and/or outer wall of the outer tube are coated with anti-
Light coating.
In the present invention, term " circle " not only includes circle itself, but also polygon including polygon, such as just
Shape.Therefore, term " annulus section " includes not only annulus itself, but also including being formed by concentric inner circle and outer regular polygon
Ring, the ring formed by concentric internal regular polygon and outer circle and the ring formed by concentric regular polygon.
LED light is one piece of electroluminescent chip of semiconductor material, on elargol or latex solidified to bracket, then uses silver
Line or gold thread connection chip and circuit board, surrounding are sealed with epoxy resin, play the role of protecting internal core.It is most of at present
Commercially available LED light is the white light for exciting one or more fluorescent powders to be formed by blue chip, therefore its spectrum is a kind of Line of light
Spectrum, and it is different from the continuous spectrum of fluorescent lamp or mercury lamp.
The utility model uses light source of the LED light as Light chlorimation, and advantage is to can choose fixed wave length, Wavelength distribution model
It encloses narrow, can effectively inhibit side reaction, reduce by-products content.But reaction is higher with LED light power, and fuel factor is brighter
It is aobvious.LED is a kind of cold light source, this refers to the principle of luminosity of LED.LED bulb can generate heat, the reason is that the electric energy being added
It is not completely converted into luminous energy, but a part transforms into thermal energy, electro-optical efficiency is 20-30% or so.Namely
Say that about 70% electric energy all becomes thermal energy.Specifically, the generation of LED junction temperature is due to caused by two factors: interior
Portion's quantum efficiency is not high, that is, in electrons and holes compound tense, 100% photon can not be all generated, commonly referred to as by " electric current
The recombination rate of the leakage " area Er Shi PN carrier reduces.Leakage current multiplied by voltage is exactly the power of this part, that is, is converted into
Thermal energy, but this part does not account for main component, because internal photon efficiency is already close to 90% now.Inside generate photon without
Method all injects to chip exterior and is finally translated into heat, this part is main, because this at present be known as internal quantum
Efficiency only has 30% or so, be largely converted to heat (although the light efficiency of incandescent lamp is very low, only 151m/W or so,
It is that all electric energy are almost converted to luminous energy and radiate by it, because most radiation energy is infrared ray, light
Imitate it is very low, but the problem of eliminate heat dissipation).If the heat generated that shines is removed not in time, will in the fluorescent tube short time
High temperature is generated, fluorescent tube will be burned out, so important considerations when heat dissipation is such tube design.Meanwhile such as general
In optical chlorinating reaction, optical chlorinating reaction temperature between 60 DEG C -110 DEG C, this be to the use of LED light it is unfavorable, LED can be shortened
The service life of lamp；Therefore, use requirement of the LED light as the light source of optical chlorinating reaction device to heat dissipation very high.
In an example of the utility model, the wave-length coverage of the single light emitting diode of LED light used is 360-
490nm, preferably 370-480nm, more preferably 380-470nm, preferably 390-460nm, preferably 400-450nm.It is practical new at this
In one example of type, the LED light is single optical wavelength LED light.
In an example of the utility model, the LED lamp bead is evenly distributed on the surface of 1 internal layer 3 of inner tube.At this
In one example of utility model, the LED lamp bead distribution area accounts for the 50% to 100% of internal layer surface, and is uniformly distributed
On the surface of 1 internal layer of inner tube.
The utility model optical chlorinating reaction pipe includes outer tube 2, the encapsulating of outer tube 2 said inner tube 1, and said inner tube
Radial spacing between outer surface and the inner surface of outer tube is 1mm to 25cm, and reaction channel is consequently formed.In the utility model
In one example, the reaction channel is spiral shape reaction channel.
In an example of the utility model, the outer tube 2 and inner tube 1 of the optical chlorinating reaction pipe are circle, described
Outer tube 2 encapsulates said inner tube 1, and the two is concentric, and the radial spacing between the outer surface of said inner tube and the inner surface of outer tube
For 1mm to 25cm, spiral shape reaction channel is consequently formed.
The outer shape (being then outer diameter when circle) of the utility model optical chlorinating reaction pipe and hollow inside dimension (when
Then it is inner hollow diameter when for circle) it is without particular limitation, actual needs are depended on, as long as the outer surface of said inner tube and outer
Radial spacing between the inner surface of pipe is 1mm to 25cm.
In an example of the utility model, the inner and outer pipes of the optical chlorinating reaction pipe are circle, and outer diameter is
0.5-40cm, preferably 1-35cm, more preferably 2-30cm, preferably 3-25cm, preferably 4-20cm, preferably 5-15cm.
The length (i.e. with the length of radial vertical direction) of the utility model optical chlorinating reaction pipe is without particular limitation, depends on
In actual needs.In an example of the utility model, the length of the optical chlorinating reaction pipe is 20-200cm, preferably
25-180cm, more preferably 30-150cm, preferably 35-120cm, preferably 40-100cm.
The utility model optical chlorinating reaction pipe further includes the upper plate 6 and lower plate 7 annular in shape, the upper and lower bottom plate
The outer wall of the utility model optical chlorinating reaction pipe is constituted together with inner and outer tubes.The upper plate 6 and lower plate 7 respectively have
There are an inner edge and outside, the shape of inner edge and inner tube matches, and the shape of outside and outer tube matches.The upper plate is under
Bottom plate respectively has material outlet or entrance (not showing in Fig. 1), one end and the spiral of the material outlet or entrance
Shaped reaction channel fluid is connected.Described in the outer surface of the upper plate and lower plate, outer tube lateral surface and inner tube medial surface are constituted
The surface of optical chlorinating reaction pipe.
In an example of the utility model, said inner tube and outer tube all have circular section, and the two is concentric, it is described on
Bottom plate and lower plate are in matching annular shape.
In use, reaction raw materials enter the reaction channel (in an example of the utility model by one end of bottom plate
For spiral shape reaction channel), optical chlorinating reaction is occurred by the irradiation of LED light during flowing through the reaction channel, shape
At product by other end bottom plate flow out reaction tube.Meanwhile cooling medium flows through the hollow inside and the outer surface of outer tube of inner tube,
Reaction system to be cooled to required reaction temperature.
It is anti-that the another aspect of the utility model is related to a kind of Light chlorimation comprising the above-mentioned optical chlorinating reaction pipe of the utility model
Answer device.
Fig. 2 is the schematic diagram of the optical chlorinating reaction device of one example of the utility model, and the optical chlorinating reaction device includes 7
Optical chlorinating reaction pipe.As shown in Fig. 2, the optical chlorinating reaction device of the utility model example include shell 10 and with the shell 10
The upper and lower bottom plate (not shown) that shape matches, and multiple optical chlorinating reaction pipes in shell 10, it is described outer
The upper and lower bottom plate of shell has the feed outlet port or entrance fluidly connected with the material outlet or entrance of each optical chlorinating reaction pipe, with
And cooling medium input port and cooling medium delivery outlet, the optical chlorinating reaction device further include each optical chlorinating reaction pipe inner tube 1
The cooling medium channel that gap is formed between the hollow central cooling medium channel 11 and each optical chlorinating reaction pipe that inner wall surrounds
11。
In the present invention, term " on the upper and lower bottom plate of shell with the material outlet or entrance of each optical chlorinating reaction pipe
The feed outlet port or entrance fluidly connected ", which refers to, to be connected with the material outlet of each optical chlorinating reaction pipe in parallel or entrance fluid
Feed outlet port or entrance, the connected method of fluid make reaction raw materials or reaction product not to leak to surrounding enviroment, wrap
Including will not leak in cooling water.
In the present invention, term " cooling medium input port and cooling medium output on the upper and lower bottom plate of shell
Mouthful " referring to such cooling medium input port and cooling medium delivery outlet, it makes cooling medium along each optical chlorinating reaction pipe
Gap 11 between the space 11 and optical chlorinating reaction pipe in pipe center is flowed from cooling medium input port to cooling medium delivery outlet,
To take away reaction heat.
In an example of the utility model, the cooling medium includes cooling water.
In an example of the utility model, the optical chlorinating reaction device shell 10 is rounded, and trans D is
0.5m-4m, preferably 0.5m-3.5m, more preferably 0.5m-3m, preferably 0.5m-2m.
In a preferable example of the utility model, the utility model optical chlorinating reaction device includes multiple optical chlorinating reactions
Pipe, each pipe chlorination reaction pipe includes inner tube, spiral shape reaction channel and outer tube；Said inner tube include limited by internal layer it is hollow
Cooling medium channel, the sealing cavity limited by outer layer and internal layer and in the sealing cavity on internal layer at least partly surface
LED light.Cooling medium inlet or outlet is respectively set in optical chlorinating reaction pipe both ends, and cooling medium is under optical chlorinating reaction pipe
It holds import to enter, is flowed out from upper end outlet；Multiple LED lamp beads form light bar, and LED light strip is connected by collection spool and external circuit
It connects, (i.e. inside tube outer layer) is saturating ultraviolet-visible protection pipe, the sealing space vacuum-pumping between internal layer and outer layer outside light bar
It is thermally shielded, the wavelength of each light emitting diode is consistent in LED light strip used, and range is between 350-500nm；The reaction
Channel is made of the inner tube with clear outer layers with outer tube, between the outer surface of the inner surface and inner tube (i.e. the outer layer of inner tube) of outer tube
Distance be 1mm-25cm, the two composition reaction channel use helical structure.
In use, reaction raw materials by one end of bottom plate enter reactor and along the optical chlorinating reaction tube bottom plates of each parallel connection
Feed(raw material)inlet enters the spiral shape reaction channel of each reaction tube, by LED light during flowing through the reaction channel
Irradiation and optical chlorinating reaction occurs, the product of formation flows out each reaction by the material outlet of each reaction tube other end bottom plate
Pipe, and the outlet outflow reactor of reacted device other end bottom plate.Meanwhile cooling medium is defeated through the cooling medium input port of shell
Enter, the gap between the hollow inside and reaction tube of reacted pipe inner tube flows to the cooling medium delivery outlet of shell, will react
System is cooled to required reaction temperature.
Known Light chlorimation needs a length of 300-500nm of light wave used.It is usually used in the light wave of the fluorescent lamp of Light chlorimation at present
A length of 400-700nm, a length of 20-750nm of the light wave of mercury lamp, although optical wavelength needed for the optical wavelength of these light sources and Light chlorimation
Range overlapping, but they have part wavelength beyond wave-length coverage needed for Light chlorimation, as a result cause some unnecessary pairs
Reaction, to reduce reaction efficiency, increases cost.
Existing Difluoroethane Light chlorimation prepares the method for difluoromono-chloroethane although product selectivity is very high, also
It is a large amount of thermal energy removal difficulty for thering is the higher boiling fluorine-containing accessory substance of 4%-10% to occur and being generated in chlorination process.To solve
The above problem, the utility model select the LED light of single wavelength, specified between 400nm-490nm by wavelength control is reacted
Wavelength makes only chlorine molecule during optical chlorinating reaction that photodissociation formation chlorine atom occur, and C-H is not broken then, from
And inhibit side reaction, effectively reduce the higher boiling fluorine-containing accessory substance amount generated in chlorination process；
The utility model method uses specially designed optical chlorinating reaction device, and tap water can be used as refrigerant to LED in it
Lamp is cooled down, and compared with air refrigerant, because of more than 20 times that the thermal coefficient of water is air conduction coefficient, the specific heat capacity of water is sky
3 times or so of gas specific heat capacity, therefore LED light only needs fraction of cooling water that can reach highly stable cooling effect, reacts
The heat that LED light work generates in journey can be taken away in time by interior substrate round tube cooling water, stablize lamp bead in assigned temperature, make
Fluorescent tube reaches longest service life.The utility model uses similar shell and tube reactor, if W-response is distinguished into dry reaction
Unit, the heat that optical chlorinating reaction generates can be taken away in time by the cooling water to circulate between reaction outer tube, improve shifting thermal effect
Rate keeps optical chlorinating reaction more stable, and reactor length is greatly shortened compared to currently used reaction tower length.
The difluoromono-chloroethane crude product produced using the optical chlorinating reaction device of the utility model, can be adopted after compression
With the de- light separation of multistage, the hydrogen chloride of unreacted raw material chlorine and Difluoroethane and high-purity is separately recovered, hydrogen chloride can
It is compressed and liquefied and hydrogen chloride liquid product is made, to reduce raw materials consumption, improve economic benefit, while reducing land occupation.
Remaining crude product difluoromono-chloroethane is again successively by liquid phase water, the difluoromono-chloroethane of neutralization, rectifying, dry obtained high-purity.
The utility model is by improving reactor light source type, light source arrangement, apparatus-form, connection type, the type of cooling
Etc. reaching control reaction temperature, selectivity of product is improved, realizes the purpose of steady production.The utility model uses LED Single wavelength
Light source is reaction light source, and dry method light chlorination process prepares difluoromono-chloroethane, moves heat, vacuum heat-insulation and outer tube by substrate and moves heat etc.
Means efficiently solve the problems such as by-product higher boiling fluorochemical is more, and heat of reaction shifts hardly possible in time, realize stable life
It produces.
Embodiment
The utility model is further elaborated below by embodiment, but is not limited only to the present embodiment.
Comparative example 1
Using optical chlorinating reaction device described in CN101781164A, using incandescent lamp as light source, reaction condition: by raw material difluoro
After ethane and liquid chlorine vaporizing, 1.15:1, into optical chlorinating reaction device, carries out Light chlorimation after static mixer mixing in molar ratio
Reaction, 80 DEG C of reaction temperature, reaction pressure 0.05MPa, reaction time 90s, Difluoroethane inventory is 120Kg/h.It produces
Object sampling and testing
Comparative example 2
Using optical chlorinating reaction device described in CN101781164A, using incandescent lamp as light source, reaction condition: by raw material difluoro
After ethane and liquid chlorine vaporizing, 1.15:1, into optical chlorinating reaction device, carries out Light chlorimation after static mixer mixing in molar ratio
Reaction, 100 DEG C of reaction temperature, reaction pressure 0.1MPa, reaction time 90s, Difluoroethane inventory is 120Kg/h.It produces
Object sampling and testing.
Embodiment 1
Using optical chlorinating reaction device shown in Fig. 2, reaction channel uses helical structure, and the LED light with wavelength 450nm is
Light source, reaction condition: after raw material Difluoroethane and liquid chlorine vaporizing, in molar ratio 1.15:1 static mixer mixing after, into
Enter optical chlorinating reaction device, carries out optical chlorinating reaction, 100 DEG C of reaction temperature, reaction pressure 15kPa, reaction time 90s, two
Fluoroethane inventory is 120Kg/h.It is cold to LED light and reaction system progress as refrigerant using subzero 15 DEG C of -20 DEG C of recirculated waters
But, for the cooling flow of inlet water of LED light between 0.5-2L/min, cooling water stable in outlet water temperature is warm in 0-35 DEG C or so, lamp body
It spends consistent with cooling water leaving water temperature.Product sampling and testing.
It was run through 10000 hours, does not find that LED light damages phenomenon, product index is basicly stable, surface this reality under this condition
It is not less than 10000 hours with the service life of the LED light of novel offer.
Embodiment 2
Referring to embodiment 1, other conditions are constant, and reaction temperature is adjusted to 80 DEG C.
Embodiment 3
Referring to embodiment 1, other conditions are constant, and reaction optical source wavelength is adjusted to 400nm.
Embodiment 4
Referring to embodiment 1, other conditions are constant, and reaction optical source wavelength is adjusted to 360nm.
Comparative example and embodiment product test result show and (see the table below): it is anti-to carry out Light chlorimation using the utility model device
In the product that should be obtained, more chlorine high-boiling components contents are substantially reduced, and reaction effect is significant.Fluorochemical is surveyed in 1 reaction product of table
Test result
Claims (10)
1. a kind of optical chlorinating reaction pipe, it is characterised in that it includes inner and outer tubes and upper plate and lower plate annular in shape,
The inner edge shape of the annular base plate matches with said inner tube section shape, the outer edge shape of the annular base plate and institute
Outer tube section shape is stated to match；
Said inner tube is hollow tube, and tube wall includes the internal layer towards hollow space and the outer layer towards outer tube side, internal layer and outer layer
Between at least partly surface on arrangement there are many LED lamp bead, the LED lamp bead is sealed in described by internal layer together with outer layer
In the tube wall of pipe, the outer layer is that can transmit made of the material of LED peak value spectrum；
The outer pipe encapsulation said inner tube, and the spacing formation between the outer surface of said inner tube and the inner surface of outer tube is reacted
Channel；
The cricoid upper plate and lower plate respectively have material outlet or entrance；The material outlet or entrance and institute
Reaction channel fluid communication is stated, described in outer surface, outer tube lateral surface and the inner tube medial surface of the upper plate and lower plate are constituted
The surface of optical chlorinating reaction device.
2. optical chlorinating reaction pipe as described in claim 1, it is characterised in that said inner tube and outer tube include the circle placed with one heart
Shape inner tube and circular outer pipe, the upper plate and lower plate are annular in shape.
3. optical chlorinating reaction pipe as claimed in claim 1 or 2, it is characterised in that the radial width of the reaction channel is 1mm-
25cm。
4. optical chlorinating reaction pipe as claimed in claim 3, it is characterised in that the inner and outer pipes of the optical chlorinating reaction pipe are circle
Shape, outer diameter 0.5-40cm.
5. optical chlorinating reaction pipe as claimed in claim 3, it is characterised in that the inner and outer pipes of the optical chlorinating reaction pipe are circle
Shape, outer diameter 1-35cm.
6. optical chlorinating reaction pipe as claimed in claim 3, it is characterised in that the length of the optical chlorinating reaction pipe is 20-
200cm。
7. optical chlorinating reaction pipe as claimed in claim 3, it is characterised in that the length of the optical chlorinating reaction pipe is 35-
120cm。
8. optical chlorinating reaction pipe as claimed in claim 1 or 2, it is characterised in that the inner wall and/or outer wall of the outer tube coat
There is reflecting coating.
9. optical chlorinating reaction pipe as claimed in claim 1 or 2, it is characterised in that the reaction channel is that spiral shaped reaction is logical
Road.
10. a kind of optical chlorinating reaction device, it is characterised in that it includes shell and upper and lower bottom plate, and inside the shell it is multiple such as
The upper and lower bottom plate of optical chlorinating reaction pipe of any of claims 1-9, the shell has and each optical chlorinating reaction pipe
Material outlet or inlet seal connection feed outlet port or entrance and cooling medium input port and cooling medium delivery outlet,
The cooling medium input port and cooling medium delivery outlet respectively with the inner tube hollow space of the optical chlorinating reaction pipe and described
Gap between optical chlorinating reaction pipe is in fluid communication.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201821974713.8U CN209393167U (en) | 2018-11-28 | 2018-11-28 | Optical chlorinating reaction pipe and optical chlorinating reaction device |
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| CN201821974713.8U CN209393167U (en) | 2018-11-28 | 2018-11-28 | Optical chlorinating reaction pipe and optical chlorinating reaction device |
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| CN201821974713.8U Active CN209393167U (en) | 2018-11-28 | 2018-11-28 | Optical chlorinating reaction pipe and optical chlorinating reaction device |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2023011951A1 (en) | 2021-08-02 | 2023-02-09 | Basf Se | Apparatus for carrying out photochemical reactions |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2023011951A1 (en) | 2021-08-02 | 2023-02-09 | Basf Se | Apparatus for carrying out photochemical reactions |
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