CN2762875Y

CN2762875Y - Equipment used for thermal decomposition

Info

Publication number: CN2762875Y
Application number: CN 200520100339
Authority: CN
Inventors: 解卫宇
Original assignee: Individual
Current assignee: Individual
Priority date: 2005-01-27
Filing date: 2005-01-27
Publication date: 2006-03-08
Anticipated expiration: 2015-01-27

Abstract

The utility model discloses a device used for thermal decomposition. The utility model is provided with a reaction kettle. The upper part of the reaction kettle is provided with a solid material feed opening and a gas exhaust opening, and the bottom of the reaction kettle is provided with a slag outlet. The utility model is characterized in that the feed opening is connected with a screw rod conveying machine. The utility model has the advantages of continuous thermal decomposition, stable and reliable reaction, high security, simple technology control, strong operability, high productive efficiency, good production quality and little pollution. The utility model is suitable for the thermal decomposition reaction of solid material with shock sensitivity performance, such as diazonium salt and is especially suitable for the thermal decomposition of diazo fluoroborate or diazo fluo phosphate to prepare aromatic fluorine compounds.

Description

Pyrolytical reactor

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

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.