CN112844253A - Fluidized bed chlorine gas distributor for chlorothalonil production and use method thereof - Google Patents
Fluidized bed chlorine gas distributor for chlorothalonil production and use method thereof Download PDFInfo
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- CN112844253A CN112844253A CN202110208904.3A CN202110208904A CN112844253A CN 112844253 A CN112844253 A CN 112844253A CN 202110208904 A CN202110208904 A CN 202110208904A CN 112844253 A CN112844253 A CN 112844253A
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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
- B01J8/00—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
- B01J8/18—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with fluidised particles
- B01J8/24—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with fluidised particles according to "fluidised-bed" technique
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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
- B01J8/00—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
- B01J8/18—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with fluidised particles
- B01J8/1818—Feeding of the fluidising gas
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C253/00—Preparation of carboxylic acid nitriles
- C07C253/30—Preparation of carboxylic acid nitriles by reactions not involving the formation of cyano groups
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C255/00—Carboxylic acid nitriles
- C07C255/49—Carboxylic acid nitriles having cyano groups bound to carbon atoms of six-membered aromatic rings of a carbon skeleton
- C07C255/50—Carboxylic acid nitriles having cyano groups bound to carbon atoms of six-membered aromatic rings of a carbon skeleton to carbon atoms of non-condensed six-membered aromatic rings
- C07C255/51—Carboxylic acid nitriles having cyano groups bound to carbon atoms of six-membered aromatic rings of a carbon skeleton to carbon atoms of non-condensed six-membered aromatic rings containing at least two cyano groups bound to the carbon skeleton
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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
- B01J2208/00—Processes carried out in the presence of solid particles; Reactors therefor
- B01J2208/00796—Details of the reactor or of the particulate material
- B01J2208/00893—Feeding means for the reactants
- B01J2208/00911—Sparger-type feeding elements
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Abstract
The invention relates to a fluidized bed chlorine distributor for chlorothalonil production and a use method thereof, wherein the fluidized bed chlorine distributor comprises a main pipe, a wing pipe and an annular pipe which are communicated with each other, a plurality of air holes are formed in the main pipe, the wing pipe and the annular pipe, a spray pipe with at least 2 spray holes is fixedly connected to each air hole, the side surface of the spray pipe is surrounded by the spray pipe, and one end of the spray pipe, which is far away from the air holes, is sealed. The fluidized bed chlorine distributor can obviously improve the distribution condition of chlorine and the spraying rate of the chlorine, effectively ensure that the mixed gas of isophthalonitrile and nitrogen and the chlorine can be uniformly and fully mixed, improve the conversion rate, synthesize chlorothalonil with the hexachlorobenzene content less than or equal to 10ppm, reduce reaction hot spots, avoid the problem of damage of a heat conduction oil pipe caused by the fact that reaction gas directly blows the heat conduction oil pipe, and avoid the problem of blockage of the chlorine distributor.
Description
Technical Field
The invention relates to the technical field of fluidization equipment, in particular to a fluidized bed chlorine distributor for chlorothalonil production and a using method thereof.
Background
Chlorothalonil, chemically named tetrachloroisophthalonitrile, is a high-efficiency, low-toxicity, broad-spectrum and low-residue protective bactericide, is widely applied to the control of fungal diseases in agriculture and forestry, and is particularly applied to economic crops such as vegetables and fruits; in addition, chlorothalonil has important application in the mildew-proof industrial field, such as the mildew prevention of manufacturing mildew-proof coating, mildew-proof wallpaper, electrical appliance mildew resistance, wood and the like, the production scale is continuously expanded at home and abroad, and the chlorothalonil becomes one of large-tonnage excellent pesticide varieties in the world.
Chlorothalonil is usually prepared by a gas phase chlorination method, and the production process of the chlorothalonil is mainly divided into three processes, namely a fluidized bed, a fixed bed and a composite bed. The chlorothalonil production is a strong exothermic reaction, so that the heat exchange effect of a fixed bed is poor, a prominent hot spot is easily generated, the catalyst is sintered, the service life of the catalyst is shortened, even the reaction is out of control, and the amplification effect of the catalyst is difficult to overcome; the fluidized bed has high process thermal efficiency, uniform temperature distribution in the bed layer, convenient loading and unloading of the catalyst, easy back mixing in the reaction process and reduced conversion rate; in recent years, a composite bed process combining the above two processes has been studied more and more.
Adopt the fluidized bed to carry out the gaseous phase chlorination method of chlorothalonil, if the mist of isophthalonitrile and nitrogen gas earlier, after the chlorine mixes, the rethread fluidized bed distributing plate lets in the fluidized bed, on the one hand, because this reaction is the strong exothermic reaction, very easily cause and produce a large amount of heats in fluidized bed distributing plate department, in case the improper will cause the distributing plate gas pocket to block up in cooling, on the other hand, because the chemical property of chlorine is unusual lively, and mixing process is in higher temperature, make a series of side reactions can take place in the mixing process, generate complicated solid-state or liquid accessory substance, can adhere to on the orifice plate that distributes the catalyst after getting into the fluidized bed, and then cause the orifice plate to block up, influence chlorination's conversion, lead to the cycle of shutdown maintenance. Therefore, researchers have focused on introducing a mixed gas of isophthalonitrile and nitrogen into the fluidized bed from the distribution plate of the fluidized bed by a separate feeding method, and introducing chlorine into the fluidized bed at the same time, so that the two gases are mixed in the fluidized bed and then subjected to chlorination reaction. Because the chlorine pipeline is directly inserted into the fluidized bed, the chlorine is distributed unevenly, the yield is low, the energy consumption is high, a large amount of tail chlorine is generated, and a chlorine distributor is required to improve the chlorine distribution effect.
CN201482467U discloses a fluidized bed distribution plate for tetrachloroisophthalonitrile production, which is circular, the middle area of the distribution plate is provided with air holes, the diameter of the distribution plate is 1100-1300mm, and the diameter of the air holes is 15-30 mm. Although the distribution plate has a simple structure, the production pressure of chlorothalonil is stable, and the content of hexachlorobenzene is lower than 40ppm, the raw material gas for mixing the isophthalonitrile, the nitrogen and the chlorine is introduced into the fluidized bed, and the distribution plate is not a chlorine distributor and does not meet the requirement that the content of hexachlorobenzene is lower than 10 ppm. CN109317060A discloses a fluidized bed distributor for chlorothalonil production, the distributor comprises a distribution plate and an air cap, a plurality of air holes are arranged on the distribution plate, the air cap is correspondingly arranged above each air hole, the air cap is fixedly connected to the distribution plate, and a gap is reserved between the edge of the air cap and the distribution plate; the aperture ratio of the distribution plate is 0.5-5%. The fluidized bed distributor can promote the uniform distribution of reaction gas through the arrangement of the air holes and the air caps and the adjustment of the opening rate, but is not a chlorine distributor for introducing the raw material gas mixed by the m-phthalonitrile, the nitrogen and the chlorine into the fluidized bed.
In summary, there is a need to develop a novel fluidized bed chlorine distributor for chlorothalonil production and a method for using the same, which can not only effectively solve the problem of uneven chlorine distribution, improve the fluidized state of the fluidized bed, reduce reaction hot spots, but also avoid the problem of damage to the heat conducting oil pipe caused by the direct blowing of the reaction gas through the heat conducting oil pipe, and avoid the problem of blockage of the chlorine distributor.
Disclosure of Invention
In view of the problems in the prior art, the invention provides a fluidized bed chlorine gas distributor for chlorothalonil production and a use method thereof, wherein the fluidized bed chlorine gas distributor comprises a main pipe, a wing pipe and an annular pipe which are communicated with each other, a plurality of air holes are formed in the main pipe, the wing pipe and the annular pipe, a spray pipe with at least 2 spray holes circumferentially formed in the side surface is fixedly connected to each air hole, and one end, far away from the air holes, of the spray pipe is closed. The fluidized bed chlorine distributor can obviously improve the distribution condition of chlorine and the spraying rate of the chlorine, effectively ensure that the mixed gas of isophthalonitrile and nitrogen and the chlorine can be uniformly and fully mixed, improve the conversion rate, synthesize chlorothalonil with the hexachlorobenzene content less than or equal to 10ppm, reduce reaction hot spots, avoid the problem of damage of a heat conduction oil pipe caused by the fact that reaction gas directly blows the heat conduction oil pipe, and avoid the problem of blockage of the chlorine distributor.
In order to achieve the purpose, the invention adopts the following technical scheme:
one of the purposes of the invention is to provide a fluidized bed chlorine distributor for chlorothalonil production, which comprises a main pipe, a wing pipe, an annular pipe and a spray pipe; one end of the main pipe is closed, and the other end of the main pipe is used as a chlorine inlet; the main pipe is vertical to the wing pipe, and the annular pipes are radially distributed by taking the intersection point of the main pipe and the wing pipe as the center of a circle; the main pipe, the wing pipes and the annular pipe are provided with a plurality of air holes, and each air hole is fixedly connected with one spray pipe; the main pipe, the wing pipes and the annular pipe are communicated with each other; one end of the spray pipe, which is far away from the air hole, is closed, and at least 2 spray holes are formed in the side face of the spray pipe in a surrounding mode.
The fluidized bed chlorine distributor of the invention controls the direction and the diameter size of each pipeline through reasonable distribution of the main pipe, the wing pipe and the annular pipe, and the side surface of the air hole is fixedly connected with the spray pipe which is provided with at least 2 spray holes in a surrounding way, so that the distribution condition of chlorine can be obviously improved, the spraying speed of the chlorine can be effectively controlled, the mixed gas of isophthalonitrile and nitrogen and the chlorine can be effectively and fully mixed, the conversion rate is improved, the service cycle of the catalyst is prolonged, the chlorination reaction can be stably operated, the vulcanization state of a fluidized bed is improved, the stability of the reaction is ensured, and the product quality of chlorothalonil is improved, chlorothalonil with hexachlorobenzene of less than or equal to 10ppm can be synthesized in one step, reaction hot spots are reduced, the problem of damage of a heat-conducting oil pipe caused by direct blowing of reaction gas to the heat-conducting oil pipe can be avoided, and the problem of blockage of a chlorine distributor is avoided.
It is worth to say that one end of the main pipe is closed, and the other end of the main pipe is used as a chlorine inlet, namely, chlorine enters in a direction parallel to the whole plane of the fluidized bed chlorine distributor, and compared with the prior art that chlorine enters vertically in the same direction as the mixed gas of phthalonitrile and nitrogen, the equipment can be simplified, and the influence on the mixing uniformity is avoided.
In a preferred embodiment of the present invention, the side surface of the nozzle is surrounded by 2 to 50 orifices, for example, 2, 5, 10, 15, 20, 25, 30, 35, 40, 45 or 50, preferably 4 to 16 orifices, but the present invention is not limited to the recited values, and other values not recited in the above range of values are also applicable. It should be noted that the spray holes may be distributed in a manner of encircling in multiple circles, for example, 5 spray holes are encircled to form one circle along the side surface of the spray pipe, and then 4 circles of spray holes are evenly distributed along the axial direction of the spray pipe, that is, the spray pipe is encircled with 20 spray holes on the corresponding side surface.
As a preferred embodiment of the present invention, a nozzle is fixedly connected to each of the nozzle holes, and an angle between a central axis of the nozzle and a central axis of the nozzle tube is 10 to 90 degrees, for example, 10 degrees, 20 degrees, 30 degrees, 45 degrees, 50 degrees, 55 degrees, 60 degrees, 70 degrees, 80 degrees, or 90 degrees, preferably 45 to 70 degrees, but the present invention is not limited to the above-mentioned values, and other values not listed in the above-mentioned range of values are also applicable.
Through the experimental verification of this application inventor many times, the restriction the central axis of nozzle with the contained angle between the central axis of spray tube is 10-90 degrees, especially 45-70 degrees, can make chlorine spray away evenly slantwise, and then make chlorine can mix with the form that the mist of isophthalonitrile and nitrogen gas is reverse and have certain inclination, can further accelerate the misce bene degree, improve the conversion.
In a preferred embodiment of the invention, the nozzle has a diameter of 5 to 30mm, for example 5mm, 10mm, 15mm, 20mm, 25mm or 30mm, but the nozzle is not limited to the values listed above, and other values not listed above within the above range of values are also applicable.
Preferably, the length of the nozzle is 10-100mm, such as 10mm, 30mm, 50mm, 70mm or 100mm, but is not limited to the recited values, and other values not recited within the above numerical range are equally applicable.
In a preferred embodiment of the invention, the fluidized bed chlorine distributor is circular, and the fluidized bed chlorine distributor has a diameter of 300-4000mm, for example 300mm, 500mm, 1000mm, 1200mm, 1500mm, 2000mm, 2400mm, 3000mm or 4000mm, preferably 1000-2400mm, but is not limited to the values listed above, and other values not listed above are equally applicable.
It is worth mentioning that the diameter of the fluidized bed chlorine distributor refers to the corresponding annular overall diameter of the outermost annular tube.
In a preferred embodiment of the invention, the diameter of the main tube is 50 to 300mm, for example 50mm, 80mm, 100mm, 120mm, 150mm, 200mm, 250mm or 300mm, preferably 80 to 150mm, but is not limited to the values listed, and other values not listed within the above range of values are also applicable.
In a preferred embodiment of the invention, the diameter of the wing tube is 20 to 150mm, for example 20mm, 50mm, 70mm, 100mm, 120mm or 150mm, preferably 50 to 100mm, but is not limited to the values listed above, and other values not listed above within the above range of values are equally applicable.
In a preferred embodiment of the present invention, the number of the ring-shaped pipes is 1 to 10, for example, 1, 2, 3, 5, 7, 8 or 10, preferably 2 to 5, turns, but is not limited to the above-mentioned values, and other values not listed in the above-mentioned range of values are also applicable.
It is worth mentioning that when the number of the annular pipes is more than or equal to 2 circles, the annular pipes are concentrically distributed, and the distance between two adjacent annular pipes is equal.
Preferably, the diameter of the annular tube is 20 to 150mm, for example 20mm, 40mm, 50mm, 70mm, 100mm, 120mm or 150mm, etc., preferably 50 to 100mm, but is not limited to the recited values, and other values not recited within the above range of values are equally applicable.
In a preferred embodiment of the present invention, the number of the nozzles is 4 to 200, for example, 4, 20, 40, 50, 70, 100, 150 or 200, preferably 40 to 100, but is not limited to the above-mentioned values, and other values not listed in the above-mentioned range of values are also applicable.
Preferably, the nozzle has a diameter of 20 to 50mm, for example 20mm, 25mm, 30mm, 35mm, 40mm, 45mm or 50mm, but is not limited to the values listed, and other values not listed within the above range of values are equally applicable.
Preferably, the length of the nozzle is 100-200mm, such as 100mm, 120mm, 150mm, 180mm or 200mm, but is not limited to the recited values, and other values within the above range are equally applicable.
Each part of the fluidized bed chlorine distributor comprises a main pipe, a wing pipe, an annular pipe and a spray pipe, and the material of each part is any one of carbon steel, 304 stainless steel, 316L stainless steel, Monel alloy or Hastelloy, preferably Monel alloy or Hastelloy.
A second object of the present invention is to provide a method for using the fluidized bed chlorine gas distributor according to the first object, wherein the spraying rate of the chlorine gas is controlled to be 5 to 40m/s, for example, 5m/s, 10m/s, 15m/s, 20m/s, 25m/s, 30m/s or 40m/s, preferably 10 to 30m/s, but not limited to the above-mentioned values, and other values not listed in the above-mentioned range of values are also applicable.
Compared with the prior art, the invention at least has the following beneficial effects:
the fluidized bed chlorine distributor of the invention controls the direction and the diameter size of each pipeline through reasonable distribution of the main pipe, the wing pipe and the annular pipe, and the side surface of the air hole is fixedly connected with the spray pipe which is provided with at least 2 spray holes in a surrounding way, so that the distribution condition of chlorine can be obviously improved, the spraying speed of the chlorine can be effectively controlled, the mixed gas of isophthalonitrile and nitrogen and the chlorine can be effectively and fully mixed, the conversion rate is improved, the service cycle of the catalyst is prolonged, the chlorination reaction can be stably operated, the vulcanization state of a fluidized bed is improved, the stability of the reaction is ensured, and the product quality of chlorothalonil is improved, chlorothalonil with hexachlorobenzene of less than or equal to 10ppm can be synthesized in one step, reaction hot spots are reduced, the problem of damage of a heat-conducting oil pipe caused by direct blowing of reaction gas to the heat-conducting oil pipe can be avoided, and the problem of blockage of a chlorine distributor is avoided.
Drawings
FIG. 1 is a top view of a fluidized bed chlorine sparger (without lances and nozzles) for chlorothalonil production as set forth in example 1 of the present invention;
FIG. 2 is a partial side view of a fluidized bed chlorine gas distributor for chlorothalonil production according to example 1 of the present invention;
FIG. 3 is a schematic view of a nozzle-equipped nozzle according to example 2 of the present invention;
in the figure: 1-main tube; 11-a chlorine inlet; 2-a wing tube; 3-a ring-shaped pipe; 4-pores; 5-spraying a pipe; 6-nozzle.
Detailed Description
The technical scheme of the invention is further explained by the specific implementation mode in combination with the attached drawings.
To better illustrate the invention and to facilitate the understanding of the technical solutions thereof, typical but non-limiting examples of the invention are as follows:
example 1
The embodiment provides a fluidized bed chlorine gas distributor for chlorothalonil production, which is shown in a top view and a partial side view in a figure 2 as shown in figure 1 (without a spray pipe 5 and a spray nozzle 6), and comprises a main pipe 1, a wing pipe 2, an annular pipe 3 and the spray pipe 5; one end of the main pipe 1 is closed, and the other end of the main pipe is used as a chlorine inlet 11; the main pipe 1 is perpendicular to the wing pipe 2, and the annular pipes 3 are radially distributed by taking the intersection point of the main pipe 1 and the wing pipe 2 as a circle center; a plurality of air holes 4 are formed in the main pipe 1, the wing pipes 2 and the annular pipe 3, and each air hole 4 is fixedly connected with one spray pipe 5; the main pipe 1, the wing pipes 2 and the annular pipe 3 are communicated with each other; one end of the spray pipe 5, which is far away from the air hole 4, is closed, 4 spray holes are formed in the side face of the spray pipe 5 in a surrounding mode, a spray nozzle 6 is fixedly connected to each spray hole, and an included angle between the central axis of each spray nozzle 6 and the central axis of the spray pipe 5 is 45 degrees;
wherein the diameter of the nozzle 6 is 10mm, and the length is 20 mm; the number of the annular pipes 3 is 2, the diameter of the annular whole of the annular pipe positioned on the outer side is 1000mm, the diameter of the annular whole of the annular pipe positioned on the inner side is 500mm, and the diameters of the annular pipes 3 are 32 mm; the diameter of the main pipe 1 is 50mm, and the diameter of the wing pipe 2 is 32 mm; the number of the spray pipes 5 is 49, namely the number of the air holes 4 is 49, the diameter of each spray pipe 5 is 30mm, and the length of each spray pipe 5 is 100 mm; all parts of the fluidized bed chlorine distributor are made of 316L stainless steel.
This embodiment fluidized bed chlorine distributor can obviously improve the chlorine distribution condition, the blowout rate that can control chlorine is 30m/s, it is even to have guaranteed chlorine and gaseous state isophthalonitrile intensive mixing, the conversion rate is improved, the life cycle of catalyst has been lengthened, can make chlorination reaction go on steadily, the fluidized state has been improved, the stability of reaction has been guaranteed, the product quality of chlorothalonil is improved, can synthesize the chlorothalonil that hexachlorobenzene is less than or equal to 10ppm by one step, reduce the reaction hotspot, can also avoid the problem that the heat conduction oil pipe that the reaction gas directly blows heat conduction oil pipe and lead to damages, and avoid the problem that the chlorine distributor blocks up.
Example 2
This example provides a fluidized bed chlorine distributor for chlorothalonil production, except that the number of spray holes formed around the side of each spray pipe 5 is changed from 4 (one circle) to 12 (3 circles), and each spray hole is fixedly connected with a nozzle 6, as shown in fig. 3, and the other conditions are identical to those of example 1.
This embodiment fluidized bed chlorine distributor can obviously improve the chlorine distribution condition, the blowout rate that can control chlorine is 35m/s, it is even to have guaranteed chlorine and gaseous state isophthalonitrile intensive mixing, the conversion rate is improved, the life cycle of catalyst has been lengthened, can make chlorination reaction go on steadily, the fluidized state has been improved, the stability of reaction has been guaranteed, the product quality of chlorothalonil is improved, can synthesize the chlorothalonil that hexachlorobenzene is less than or equal to 10ppm by one step, reduce the reaction hotspot, can also avoid the problem that the heat conduction oil pipe that the reaction gas directly blows heat conduction oil pipe and lead to damages, and avoid the problem that the chlorine distributor blocks up.
Example 3
The embodiment provides a fluidized bed chlorine distributor for chlorothalonil production, which has a structure similar to that of the embodiment 1, and comprises a main pipe 1, a wing pipe 2, an annular pipe 3 and a spray pipe 5; one end of the main pipe 1 is closed, and the other end of the main pipe is used as a chlorine inlet 11; the main pipe 1 is perpendicular to the wing pipe 2, and the annular pipes 3 are radially distributed by taking the intersection point of the main pipe 1 and the wing pipe 2 as a circle center; a plurality of air holes 4 are formed in the main pipe 1, the wing pipes 2 and the annular pipe 3, and each air hole 4 is fixedly connected with one spray pipe 5; the main pipe 1, the wing pipes 2 and the annular pipe 3 are communicated with each other; one end of the spray pipe 5, which is far away from the air hole 4, is closed, 2 spray holes are formed in the side face of the spray pipe 5 in a surrounding mode, a spray nozzle 6 is fixedly connected to each spray hole, and an included angle between the central axis of each spray nozzle 6 and the central axis of the spray pipe 5 is 60 degrees;
wherein the diameter of the nozzle 6 is 30mm, and the length is 100 mm; the number of the annular pipes 3 is 3, the diameter of the whole annular pipe positioned at the outer side is 2000mm, the diameter of the whole annular pipe positioned at the middle is 1400mm, the diameter of the whole annular pipe positioned at the inner side is 800mm, and the diameters of the annular pipes 3 are all 40 mm; the diameter of the main pipe 1 is 80mm, and the diameter of the wing pipe 2 is 40 mm; the number of the spray pipes 5 is 63, namely the number of the air holes 4 is 63, the diameter of each spray pipe 5 is 50mm, and the length of each spray pipe 5 is 200 mm; all parts of the fluidized bed chlorine distributor are made of hastelloy.
This embodiment fluidized bed chlorine distributor can obviously improve the chlorine distribution condition, the blowout rate that can control chlorine is 20m/s, it is even to have guaranteed chlorine and gaseous state isophthalonitrile intensive mixing, the conversion rate is improved, the life cycle of catalyst has been lengthened, can make chlorination reaction go on steadily, the fluidized state has been improved, the stability of reaction has been guaranteed, the product quality of chlorothalonil is improved, can synthesize the chlorothalonil that hexachlorobenzene is less than or equal to 10ppm by one step, reduce the reaction hotspot, can also avoid the problem that the heat conduction oil pipe that the reaction gas directly blows heat conduction oil pipe and lead to damages, and avoid the problem that the chlorine distributor blocks up.
Example 4
The embodiment provides a fluidized bed chlorine distributor for chlorothalonil production, which has a structure similar to that of the embodiment 1, and comprises a main pipe 1, a wing pipe 2, an annular pipe 3 and a spray pipe 5; one end of the main pipe 1 is closed, and the other end of the main pipe is used as a chlorine inlet 11; the main pipe 1 is perpendicular to the wing pipe 2, and the annular pipes 3 are radially distributed by taking the intersection point of the main pipe 1 and the wing pipe 2 as a circle center; a plurality of air holes 4 are formed in the main pipe 1, the wing pipes 2 and the annular pipe 3, and each air hole 4 is fixedly connected with one spray pipe 5; the main pipe 1, the wing pipes 2 and the annular pipe 3 are communicated with each other; one end of the spray pipe 5, which is far away from the air hole 4, is closed, 8 spray holes (4 spray holes per circle and 2 spray holes per circle) are formed in the side surface of the spray pipe 5 in a surrounding manner, a spray nozzle 6 is fixedly connected to each spray hole, and an included angle between the central axis of the spray nozzle 6 and the central axis of the spray pipe 5 is 70 degrees;
wherein the nozzle 6 has a diameter of 5mm and a length of 10 mm; the number of the annular pipes 3 is 4, the diameter of the annular whole of the annular pipe positioned on the outer side is 3000mm, the diameters of the annular whole of the annular pipes from outside to inside are 2200mm, 1400mm and 600mm in sequence, and the diameters of the annular pipes 3 are 65 mm; the diameter of the main pipe 1 is 150mm, and the diameter of the wing pipe 2 is 65 mm; the number of the spray pipes 5 is 89, namely the number of the air holes 4 is 89, the diameter of each spray pipe 5 is 20mm, and the length of each spray pipe 5 is 100 mm; all parts of the fluidized bed chlorine distributor are made of Monel alloy.
This embodiment fluidized bed chlorine distributor can obviously improve the chlorine distribution condition, the blowout rate that can control chlorine is 25m/s, it is even to have guaranteed chlorine and gaseous state isophthalonitrile intensive mixing, the conversion rate is improved, the life cycle of catalyst has been lengthened, can make chlorination reaction go on steadily, the fluidized state has been improved, the stability of reaction has been guaranteed, the product quality of chlorothalonil is improved, can synthesize the chlorothalonil that hexachlorobenzene is less than or equal to 10ppm by one step, reduce the reaction hotspot, can also avoid the problem that the heat conduction oil pipe that the reaction gas directly blows heat conduction oil pipe and lead to damages, and avoid the problem that the chlorine distributor blocks up.
Comparative example 1
This comparative example provides a fluidized bed chlorine sparger for chlorothalonil production, the conditions being exactly the same as in example 1, except that the lance 5 and lance 6 are omitted.
As the chlorine is sprayed perpendicular to the whole plane of the fluidized bed chlorine distributor, the comparative example not only easily causes uneven mixing, more reaction hot spots and reduced conversion rate, but also does not meet the requirement that the content of hexachlorobenzene is lower than 10ppm, and also has the problem of damage to a heat conduction oil pipe caused by directly blowing the heat conduction oil pipe and the problem of blockage of the chlorine distributor.
In conclusion, the fluidized bed chlorine distributor of the invention controls the direction and the diameter size of each pipeline through reasonable distribution of the main pipe, the wing pipe and the annular pipe, and the side surface of the air hole is fixedly connected with the spray pipe which is provided with at least 2 spray holes in a surrounding way, so that the distribution condition of chlorine can be obviously improved, the spraying speed of the chlorine can be effectively controlled, the mixed gas of isophthalonitrile and nitrogen and the chlorine can be effectively and fully mixed, the conversion rate is improved, the service cycle of the catalyst is prolonged, the chlorination reaction can be stably operated, the vulcanization state of a fluidized bed is improved, the stability of the reaction is ensured, and the product quality of chlorothalonil is improved, chlorothalonil with hexachlorobenzene of less than or equal to 10ppm can be synthesized in one step, reaction hot spots are reduced, the problem of damage of a heat-conducting oil pipe caused by direct blowing of reaction gas to the heat-conducting oil pipe can be avoided, and the problem of blockage of a chlorine distributor is avoided.
The applicant declares that the present invention illustrates the detailed structural features of the present invention through the above embodiments, but the present invention is not limited to the above detailed structural features, that is, it does not mean that the present invention must be implemented depending on the above detailed structural features. It should be understood by those skilled in the art that any modifications of the present invention, equivalent substitutions of selected components of the present invention, additions of auxiliary components, selection of specific modes, etc., are within the scope and disclosure of the present invention.
The preferred embodiments of the present invention have been described in detail, however, the present invention is not limited to the specific details of the above embodiments, and various simple modifications may be made to the technical solution of the present invention within the technical idea of the present invention, and these simple modifications are within the protective scope of the present invention.
It should be noted that the various technical features described in the above embodiments can be combined in any suitable manner without contradiction, and the invention is not described in any way for the possible combinations in order to avoid unnecessary repetition.
In addition, any combination of the various embodiments of the present invention is also possible, and the same should be considered as the disclosure of the present invention as long as it does not depart from the spirit of the present invention.
Claims (10)
1. A fluidized bed chlorine distributor for chlorothalonil production is characterized by comprising a main pipe, a wing pipe, an annular pipe and a spray pipe; one end of the main pipe is closed, and the other end of the main pipe is used as a chlorine inlet; the main pipe is vertical to the wing pipe, and the annular pipes are radially distributed by taking the intersection point of the main pipe and the wing pipe as the center of a circle; the main pipe, the wing pipes and the annular pipe are provided with a plurality of air holes, and each air hole is fixedly connected with one spray pipe; the main pipe, the wing pipes and the annular pipe are communicated with each other; one end of the spray pipe, which is far away from the air hole, is closed, and at least 2 spray holes are formed in the side face of the spray pipe in a surrounding mode.
2. The fluidized bed chlorine distributor as claimed in claim 1, wherein 2 to 50 spray holes, preferably 4 to 16 spray holes, are arranged around the side of the spray pipe.
3. The fluidized bed chlorine distributor as claimed in claim 1 or 2, wherein a nozzle is fixedly connected to each of the spray holes, and the angle between the central axis of the nozzle and the central axis of the spray pipe is 10 to 90 degrees, preferably 45 to 70 degrees.
4. The fluidized bed chlorine distributor of any of claims 1-3, wherein the nozzles have a diameter of 5-30 mm;
preferably, the length of the nozzle is 10-100 mm.
5. The fluidized bed chlorine distributor as claimed in any one of claims 1 to 4, wherein the fluidized bed chlorine distributor is circular and has a diameter of 300-4000mm, preferably 1000-2400 mm.
6. Fluidized bed chlorine distributor according to any one of claims 1 to 5, wherein the main pipe has a diameter of 50 to 300mm, preferably 80 to 150 mm.
7. Fluidized bed chlorine sparger as claimed in any one of claims 1 to 6, wherein the finned tubes have a diameter of 20 to 150mm, preferably 50 to 100 mm.
8. Fluidized bed chlorine sparger as claimed in any one of claims 1 to 7, wherein the number of said annular pipes is 1 to 10, preferably 2 to 5;
preferably, the diameter of the annular tube is 20-150mm, preferably 50-100 mm.
9. The fluidized bed chlorine distributor as claimed in any one of claims 1 to 8, wherein the number of lances is 4 to 200, preferably 40 to 100;
preferably, the diameter of the spray pipe is 20-50 mm;
preferably, the length of the nozzle is 100-200 mm.
10. Use of a fluidized bed chlorine sparger as claimed in any one of claims 1 to 9 wherein the rate of chlorine emission is controlled to be in the range of 5 to 40m/s, preferably 10 to 30 m/s.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115193347A (en) * | 2022-07-28 | 2022-10-18 | 常熟理工学院 | Chlorine distributor used in chlorination reaction kettle and chlorine distribution method |
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2021
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115193347A (en) * | 2022-07-28 | 2022-10-18 | 常熟理工学院 | Chlorine distributor used in chlorination reaction kettle and chlorine distribution method |
| CN115193347B (en) * | 2022-07-28 | 2024-04-02 | 常熟理工学院 | Chlorine distributor and chlorine distribution method for chlorination reaction kettle |
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