CN2762875Y - thermal decomposition reaction device - Google Patents
thermal decomposition reaction device Download PDFInfo
- Publication number
- CN2762875Y CN2762875Y CN 200520100339 CN200520100339U CN2762875Y CN 2762875 Y CN2762875 Y CN 2762875Y CN 200520100339 CN200520100339 CN 200520100339 CN 200520100339 U CN200520100339 U CN 200520100339U CN 2762875 Y CN2762875 Y CN 2762875Y
- Authority
- CN
- China
- Prior art keywords
- reactor
- thermal decomposition
- screw rod
- pyrolytical
- charge door
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Lifetime
Links
- 238000005979 thermal decomposition reaction Methods 0.000 title abstract description 21
- 239000002893 slag Substances 0.000 claims abstract description 8
- 239000011343 solid material Substances 0.000 claims abstract description 5
- 238000010438 heat treatment Methods 0.000 claims description 5
- 238000005485 electric heating Methods 0.000 claims description 3
- 239000012954 diazonium Substances 0.000 abstract description 18
- 238000006243 chemical reaction Methods 0.000 abstract description 14
- IJGRMHOSHXDMSA-UHFFFAOYSA-O diazynium Chemical group [NH+]#N IJGRMHOSHXDMSA-UHFFFAOYSA-O 0.000 abstract description 13
- 238000004519 manufacturing process Methods 0.000 abstract description 6
- 238000000034 method Methods 0.000 abstract description 5
- -1 aromatic fluorine compounds Chemical class 0.000 abstract description 4
- 150000001989 diazonium salts Chemical class 0.000 abstract description 2
- 238000004880 explosion Methods 0.000 abstract 1
- DWYMPOCYEZONEA-UHFFFAOYSA-L fluoridophosphate Chemical compound [O-]P([O-])(F)=O DWYMPOCYEZONEA-UHFFFAOYSA-L 0.000 abstract 1
- 238000004886 process control Methods 0.000 abstract 1
- 230000035945 sensitivity Effects 0.000 abstract 1
- 239000000463 material Substances 0.000 description 15
- 239000007789 gas Substances 0.000 description 14
- FBMGKRKUOZTARV-UHFFFAOYSA-N F.OB(O)O Chemical compound F.OB(O)O FBMGKRKUOZTARV-UHFFFAOYSA-N 0.000 description 5
- 235000021050 feed intake Nutrition 0.000 description 5
- 229910052731 fluorine Inorganic materials 0.000 description 5
- 239000000047 product Substances 0.000 description 5
- WZCQRUWWHSTZEM-UHFFFAOYSA-N 1,3-phenylenediamine Chemical compound NC1=CC=CC(N)=C1 WZCQRUWWHSTZEM-UHFFFAOYSA-N 0.000 description 4
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 4
- 239000007859 condensation product Substances 0.000 description 4
- FHIVAFMUCKRCQO-UHFFFAOYSA-N diazinon Chemical compound CCOP(=S)(OCC)OC1=CC(C)=NC(C(C)C)=N1 FHIVAFMUCKRCQO-UHFFFAOYSA-N 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 239000011737 fluorine Substances 0.000 description 4
- 229940018564 m-phenylenediamine Drugs 0.000 description 4
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 239000002360 explosive Substances 0.000 description 3
- 125000001153 fluoro group Chemical group F* 0.000 description 3
- 238000002360 preparation method Methods 0.000 description 3
- 238000000197 pyrolysis Methods 0.000 description 3
- 238000007670 refining Methods 0.000 description 3
- GOYDNIKZWGIXJT-UHFFFAOYSA-N 1,2-difluorobenzene Chemical compound FC1=CC=CC=C1F GOYDNIKZWGIXJT-UHFFFAOYSA-N 0.000 description 2
- XJCVRTZCHMZPBD-UHFFFAOYSA-N 3-nitroaniline Chemical compound NC1=CC=CC([N+]([O-])=O)=C1 XJCVRTZCHMZPBD-UHFFFAOYSA-N 0.000 description 2
- KRZCOLNOCZKSDF-UHFFFAOYSA-N 4-fluoroaniline Chemical compound NC1=CC=C(F)C=C1 KRZCOLNOCZKSDF-UHFFFAOYSA-N 0.000 description 2
- FQKMRXHEIPOETF-UHFFFAOYSA-N F.OP(O)(O)=O Chemical compound F.OP(O)(O)=O FQKMRXHEIPOETF-UHFFFAOYSA-N 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 230000009977 dual effect Effects 0.000 description 2
- MGNPLIACIXIYJE-UHFFFAOYSA-N n-fluoroaniline Chemical group FNC1=CC=CC=C1 MGNPLIACIXIYJE-UHFFFAOYSA-N 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- UEMGWPRHOOEKTA-UHFFFAOYSA-N 1,3-difluorobenzene Chemical compound FC1=CC=CC(F)=C1 UEMGWPRHOOEKTA-UHFFFAOYSA-N 0.000 description 1
- PWKNBLFSJAVFAB-UHFFFAOYSA-N 1-fluoro-2-nitrobenzene Chemical compound [O-][N+](=O)C1=CC=CC=C1F PWKNBLFSJAVFAB-UHFFFAOYSA-N 0.000 description 1
- 238000006350 Schiemann fluorination reaction Methods 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 238000010923 batch production Methods 0.000 description 1
- MFLAROGHONQVRM-UHFFFAOYSA-L calcium;dihydrogen phosphate;fluoride Chemical compound [F-].[Ca+2].OP(O)([O-])=O MFLAROGHONQVRM-UHFFFAOYSA-L 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 150000002222 fluorine compounds Chemical class 0.000 description 1
- RHFUXPCCELGMFC-UHFFFAOYSA-N n-(6-cyano-3-hydroxy-2,2-dimethyl-3,4-dihydrochromen-4-yl)-n-phenylmethoxyacetamide Chemical compound OC1C(C)(C)OC2=CC=C(C#N)C=C2C1N(C(=O)C)OCC1=CC=CC=C1 RHFUXPCCELGMFC-UHFFFAOYSA-N 0.000 description 1
- 239000000575 pesticide Substances 0.000 description 1
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Landscapes
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Physical Or Chemical Processes And Apparatus (AREA)
Abstract
The utility model discloses a thermal decomposition reaction device, it has reation kettle, and open on reation kettle's upper portion has solid material charge door and gas discharge port, and open the bottom has the slag notch, its characterized in that the charge door be connected with screw conveyer. The method has the advantages of continuous thermal decomposition, stable and reliable reaction, high safety, simple process control, strong operability, high production efficiency, good product quality and less pollution. Is suitable for the thermal decomposition reaction of solid materials with explosion sensitivity such as diazonium salt, in particular suitable for the thermal decomposition of diazonium fluoborate or diazonium fluorophosphate to prepare aromatic fluorine compounds.
Description
Technical field
The utility model relates to a kind of Pyrolytical reactor that is applicable to the material that has quick-fried quick property when adding thermal decomposition, especially is applicable to the Pyrolytical reactor of diazol thermal decomposition.
Background technology
The fluorochemical especially purposes of aromatic fluorine compounds is increasingly extensive, relates to fluoro-containing intermediate, fluorine-containing medicines, fluoro-containing pesticide, fluorine-containing surfactant and various fluorine-containing inorganic agents etc.Schiemann reaction is a common method of fluorine atom being introduced phenyl ring, its preparation process comprises fluoboric acid or fluorophosphoric acid is added in the diazonium salt solution, make it to generate diazonium fluoride borate or diazonium fluoride calcium phosphate precipitation, through separate and drying after carefully heating again, make it to decompose gradually and make corresponding aroma family fluorine compounds.Therefore, in the preparation technology of aromatic fluorine compounds, the phosphatic pyrolysis of diazonium fluoride borate or diazonium fluoride is one of organic important step of preparation fluorine chemistry.But diazonium fluoride borate or diazonium fluoride phosphate have certain quick-fried quick property and easy decomposability, and it is heated to a certain degree and promptly can decomposes, and decompose the back owing to produce N
2And BF
3Gas, volume will be expanded to 300~600 times of original volume, so its pyrolysis is wayward.
At present, tank reactor is all adopted in the thermal decomposition of above-mentioned diazol, and reactor top is provided with dog-house and gas vent, and the bottom has slag notch, in addition, also is provided with heating jacket.During production, normally earlier material is added in the reactor, build dog-house, heat up then and decompose, decompose the gas that produces and draw from gas vent, carry out product and separate and vent gas treatment, after reaction finished, cooling earlier is disposable slagging tap at the bottom of the still then.Owing to be subjected to the restriction of structure of reactor, many aborning employings once feed intake or repeatedly intermittently feed intake disposable slagging tap.But because diazol has quick-fried quick property and easy decomposability, if adopt a feeding mode, there is the difficult problem of reaction control aspect in it, in case control badly, its consequence is hardly imaginable.Adopt repeatedly intermittently to feed intake, act on to some extent reducing explosive problem, but effect is not very good, and before secondary charging, need lower the temperature and wait operation, behind reinforced the finishing, need row intensification more again, operate loaded down with trivial detailsly, efficient is not high; Moreover the gas of emerging from charge door also can not be underestimated to the danger of operator and environment.In addition, no matter be disposablely to feed intake or repeatedly intermittently feed intake, all belong to intermittent reaction, thereby need aborning constantly to adjust that product separates and the technological parameter of vent gas treatment, to having relatively high expectations of operator, workload is bigger, and the quality relative difficult of product has stable guarantee.Also have,, also often adopt following way at present: 1, reduce the secondary batching amount for solving explosive problem, reaction is controlled in the allowed band as far as possible, but therefore the result who brings be its reactor can only do especially little, generally only be about 50~200L, efficient is extremely low.2, be ready to cold oil,, pour avoiding blast with cold oil immediately, but material reclaimed to return basically, therefore will cause great waste, and be unfavorable for environmental protection if temperature in the kettle reaches a certain limit.3, with diazol with add thermal decomposition after inert substance mixes, to avoid the directly contact and reach and end quick-fried datonation-inhibition effect of pure material.But it often can not reach fully and end quick-fried effect, and uses too many filler can cause the severe contamination of environment.
Summary of the invention
Technical problem to be solved in the utility model be provide a kind of at above-mentioned prior art present situation and can effectively solve the explosive problem of the quick-fried quick property solid matter of tool when thermal decomposition, security is good, efficient is high and can realize the Pyrolytical reactor that serialization is produced.
The utility model solves the problems of the technologies described above the technical scheme that is adopted: this kind Pyrolytical reactor, it has reactor, the top of reactor has solid material charge door and gas discharge outlet, and the bottom has slag notch, it is characterized in that described charge door is connected with screw rod conveyor.Screw rod conveyor can be by Motor Drive, even also can adopt other machinery on-mechanical type of drive to drive.
The back segment of the barrel of described screw rod conveyor, promptly the barrel part near described charge door is provided with heater and corresponding attemperating unit.
Described screw rod conveyor is single screw rod conveyor or double-screw conveyor.
Described heater is electric heating watt or heating jacket.
The top of described reactor is cylindrical shape, and it is conical that the bottom is.
Be provided with agitating device in the described reactor.
Described reactor is provided with chuck.
The utility model Pyrolytical reactor has the thermal decomposition of the material of quick-fried quick property when being suitable for adding thermal decomposition.Such as: diazonium fluoride phosphate, perhaps, diazonium fluoride borates such as the dual nitrogen borofluoride of m-phenylene diamine (MPD), meta nitro aniline diazonium fluoride borate, adjacent fluoroaniline diazonium fluoride borate or para-fluoroaniline diazonium fluoride borate.
When using this Pyrolytical reactor, can be according to the characteristics of reaction mass, select the temperature of control screw rod conveyor barrel and the temperature in the reactor, not only can utilize the preheating of the bringing-up section realization of screw rod conveyor to material, also can make material promptly carry out thermal decomposition, even finish thermal decomposition process substantially by temperature control at the rear portion of bringing-up section.
Compared with prior art, advantage of the present utility model is: 1, realized continuous charging; 2, owing to the reaction mass negligible amounts that adds in the unit interval and controlled, the reactor space is enough to make its smooth reaction and has eliminated the possibility of exploding, and security can be fully protected; 3, because of can realizing serialization production, and serialization production has the stable characteristics of technological parameter, thereby operation is simple relatively, to operating personnel require relatively low; 4, compared to batch production, saved a lot of non-reaction time, production efficiency greatly improves; 5, steady because of technological parameter control, product quality is more secure; 6, can realize the closed operation of whole thermal decomposition process, reduce gas emissions, especially stop the direct discharging of the gas of thermal decomposition generation, alleviate pollution environment.
The specific embodiment
Fig. 1 is the structural representation of the utility model embodiment Pyrolytical reactor.
The specific embodiment
Embodiment describes in further detail the utility model below in conjunction with accompanying drawing.
Embodiment
As shown in Figure 1, be a preferred embodiment of the utility model Pyrolytical reactor.As shown in Figure 1, the present embodiment Pyrolytical reactor, it has reactor 1, and the top of reactor 1 has solid material charge door 2 and gas discharge outlet 3, the bottom has slag notch 4, and charge door 2 is connected with the single screw rod conveyor 6 by motor 5 drivings that is used for convey materials.The top of reactor 1 is cylindrical shape, and it is conical that the bottom is; Be provided with shaft in the reactor 1, shaft vertically is provided with and is positioned on the central axis of reactor, is fixed with the stirring blade (not shown) on the shaft; Also be provided with the chuck (not shown) that can play heating or cooling effect on the reactor 1.Single screw rod conveyor 6 has barrel 7, screw rod 8 is arranged in the barrel 7, the front end of screw rod 8 stretches out outside the barrel 7, barrel 7 front end ends and screw rod 8 cooperation places are provided with black box 9, screw rod 8 front ends are equipped with sprocket wheel 10, and sprocket wheel 10 is connected with motor 5 by driving chain 11 and reducing gear, and barrel 7 front ends are provided with hopper 12, the back segment of barrel 7 promptly is provided with electric heating watts 13 and corresponding attemperating unit (not shown) near the barrel part of the charge door 2 of reactor 1.Using in the production has the technological process brief introduction of the utility model device as follows: reaction mass is added in the hopper 12 of single screw rod conveyor 6, material is sent into reactor 1 continuously and is carried out thermal decomposition in a small amount through charge door 2 by single screw rod conveyor 6 under the driving of motor 5, simultaneously, single screw rod conveyor 6 at the back segment of barrel 7 to the material preheating, certainly, also can be by the temperature in the control barrel 7, make material promptly carry out pyrolysis at the end of barrel 7, the gas that reaction produces enters the condensation separation tower through gas discharge outlet 3 to be separated, product flows out through the knockout tower bottom, tail gas then enters absorption system by the knockout tower top and absorbs processing, the residual air emptying.When reactor 1 inner accumulated has enough slag charges, can open slag notch 4 and slag tap.
The application example of the utility model embodiment
Example 1
The thermal decomposition of the dual nitrogen borofluoride of m-phenylene diamine (MPD): with the delivery rate of 10~200Kg per hour, by the screw rod conveyor feed, the control reaction temperature is 150~200 ℃, material is divided uniformly take off, collect the condensation products therefrom, the purified yield that gets is 70% m-difluorobenzene.
Example 2
The boratory thermal decomposition of meta nitro aniline diazonium fluoride: with the delivery rate of 60~160Kg per hour, by the screw rod conveyor feed, the control reaction temperature is below 400 ℃, material is divided uniformly to be taken off, collect the condensation products therefrom, through refining, can get yield and be more than 50% between the nitro fluorobenzene.
Example 3
The boratory thermal decomposition of adjacent fluoroaniline diazonium fluoride: with the delivery rate of 20~200Kg per hour, by the screw rod conveyor feed, the control reaction temperature is below 300 ℃, material is divided uniformly to be taken off, constantly collect the condensation products therefrom,, can get yield and be the o-difluoro-benzene more than 70% through refining.
Example 4
The boratory thermal decomposition of para-fluoroaniline diazonium fluoride: with the delivery rate of 70~210Kg per hour, by the screw rod conveyor feed, the control reaction temperature is below 300 ℃, material is divided uniformly to be taken off, constantly collect the condensation products therefrom,, can get yield and be 50~70% o-difluoro-benzene through refining.
Claims (7)
1, a kind of Pyrolytical reactor, it has reactor, and the top of reactor has solid material charge door and gas discharge outlet, and the bottom has slag notch, it is characterized in that described charge door is connected with screw rod conveyor.
2, Pyrolytical reactor according to claim 1 is characterized in that the back segment of the barrel of described screw rod conveyor, and promptly the barrel part near described charge door is provided with heater and corresponding attemperating unit.
3, Pyrolytical reactor according to claim 1 is characterized in that described screw rod conveyor is single screw rod conveyor or double-screw conveyor.
4, Pyrolytical reactor according to claim 2 is characterized in that described heater is electric heating watt or heating jacket.
5, according to the described Pyrolytical reactor of arbitrary claim in the claim 1 to 4, the top that it is characterized in that described reactor is cylindrical shape, and it is conical that the bottom is.
6, according to the described Pyrolytical reactor of arbitrary claim in the claim 1 to 4, it is characterized in that being provided with agitating device in the described reactor.
7,, it is characterized in that described reactor is provided with chuck according to the described Pyrolytical reactor of arbitrary claim in the claim 1 to 4.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN 200520100339 CN2762875Y (en) | 2005-01-27 | 2005-01-27 | thermal decomposition reaction device |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN 200520100339 CN2762875Y (en) | 2005-01-27 | 2005-01-27 | thermal decomposition reaction device |
Publications (1)
Publication Number | Publication Date |
---|---|
CN2762875Y true CN2762875Y (en) | 2006-03-08 |
Family
ID=36140427
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
CN 200520100339 Expired - Lifetime CN2762875Y (en) | 2005-01-27 | 2005-01-27 | thermal decomposition reaction device |
Country Status (1)
Country | Link |
---|---|
CN (1) | CN2762875Y (en) |
-
2005
- 2005-01-27 CN CN 200520100339 patent/CN2762875Y/en not_active Expired - Lifetime
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Legal Events
Date | Code | Title | Description |
---|---|---|---|
C14 | Grant of patent or utility model | ||
GR01 | Patent grant | ||
C17 | Cessation of patent right | ||
CX01 | Expiry of patent term |
Expiration termination date: 20150127 Granted publication date: 20060308 |