CN112812039B - Chlorothalonil lattice transformation device and method - Google Patents
Chlorothalonil lattice transformation device and method Download PDFInfo
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- CN112812039B CN112812039B CN202110168917.2A CN202110168917A CN112812039B CN 112812039 B CN112812039 B CN 112812039B CN 202110168917 A CN202110168917 A CN 202110168917A CN 112812039 B CN112812039 B CN 112812039B
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- 230000009466 transformation Effects 0.000 title claims abstract description 200
- CRQQGFGUEAVUIL-UHFFFAOYSA-N chlorothalonil Chemical compound ClC1=C(Cl)C(C#N)=C(Cl)C(C#N)=C1Cl CRQQGFGUEAVUIL-UHFFFAOYSA-N 0.000 title claims abstract description 142
- 239000005747 Chlorothalonil Substances 0.000 title claims abstract description 141
- 238000000034 method Methods 0.000 title claims abstract description 37
- 239000007787 solid Substances 0.000 claims abstract description 35
- 238000000926 separation method Methods 0.000 claims abstract description 34
- 239000002994 raw material Substances 0.000 claims abstract description 24
- 238000010438 heat treatment Methods 0.000 claims abstract description 22
- 238000006243 chemical reaction Methods 0.000 claims abstract description 6
- 238000003756 stirring Methods 0.000 claims description 33
- 239000013078 crystal Substances 0.000 claims description 28
- 238000012546 transfer Methods 0.000 claims description 23
- 239000002245 particle Substances 0.000 claims description 14
- 230000008439 repair process Effects 0.000 claims description 12
- 230000005540 biological transmission Effects 0.000 claims description 6
- 230000009471 action Effects 0.000 claims description 5
- 230000014759 maintenance of location Effects 0.000 claims description 4
- 239000000463 material Substances 0.000 claims description 4
- 239000003638 chemical reducing agent Substances 0.000 claims description 3
- 238000007789 sealing Methods 0.000 claims description 2
- 238000010924 continuous production Methods 0.000 abstract description 7
- 238000004134 energy conservation Methods 0.000 abstract description 6
- 238000012545 processing Methods 0.000 abstract description 6
- 239000002912 waste gas Substances 0.000 abstract 1
- 230000008569 process Effects 0.000 description 12
- 230000001131 transforming effect Effects 0.000 description 10
- 239000011229 interlayer Substances 0.000 description 9
- 230000000052 comparative effect Effects 0.000 description 6
- 239000000428 dust Substances 0.000 description 6
- 239000004744 fabric Substances 0.000 description 5
- 238000004519 manufacturing process Methods 0.000 description 5
- 238000004140 cleaning Methods 0.000 description 4
- 238000013461 design Methods 0.000 description 4
- 238000005054 agglomeration Methods 0.000 description 3
- 238000005485 electric heating Methods 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 238000004806 packaging method and process Methods 0.000 description 3
- 239000000575 pesticide Substances 0.000 description 3
- 230000002776 aggregation Effects 0.000 description 2
- 238000005660 chlorination reaction Methods 0.000 description 2
- 238000005265 energy consumption Methods 0.000 description 2
- 230000002265 prevention Effects 0.000 description 2
- 238000004064 recycling Methods 0.000 description 2
- 239000010963 304 stainless steel Substances 0.000 description 1
- 229910000619 316 stainless steel Inorganic materials 0.000 description 1
- 229910000975 Carbon steel Inorganic materials 0.000 description 1
- 229910000792 Monel Inorganic materials 0.000 description 1
- 208000031888 Mycoses Diseases 0.000 description 1
- 229910000589 SAE 304 stainless steel Inorganic materials 0.000 description 1
- 230000000844 anti-bacterial effect Effects 0.000 description 1
- 239000003899 bactericide agent Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000004071 biological effect Effects 0.000 description 1
- 239000010962 carbon steel Substances 0.000 description 1
- 208000037516 chromosome inversion disease Diseases 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 235000013399 edible fruits Nutrition 0.000 description 1
- 229910000856 hastalloy Inorganic materials 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 231100000053 low toxicity Toxicity 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 238000007790 scraping Methods 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 230000001954 sterilising effect Effects 0.000 description 1
- 238000004659 sterilization and disinfection Methods 0.000 description 1
- 238000005728 strengthening Methods 0.000 description 1
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Classifications
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C253/00—Preparation of carboxylic acid nitriles
- C07C253/32—Separation; Purification; Stabilisation; Use of additives
- C07C253/34—Separation; Purification
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07B—GENERAL METHODS OF ORGANIC CHEMISTRY; APPARATUS THEREFOR
- C07B2200/00—Indexing scheme relating to specific properties of organic compounds
- C07B2200/13—Crystalline forms, e.g. polymorphs
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- Physical Or Chemical Processes And Apparatus (AREA)
- Processing Of Solid Wastes (AREA)
Abstract
The invention relates to a chlorothalonil lattice transformation device and a method, wherein the chlorothalonil lattice transformation device comprises a feeding device, a transformation device, a crushing device and a gas-solid separation device which are sequentially connected, the transformation device comprises at least 2 stages, the transformation device comprises a primary transformation device and a secondary transformation device which are connected in series, and the primary transformation device and the secondary transformation device respectively and independently comprise a jacket cylinder and a stirrer. The chlorothalonil lattice transformation device provided by the invention firstly realizes full and uniform preheating of the chlorothalonil raw material through the primary transformation device, achieves the purpose of partial transformation of the chlorothalonil raw material, and then realizes uniform heating and lattice transformation of the preheated chlorothalonil through the secondary transformation device, so that the chlorothalonil raw material can be fully and uninterruptedly turned over, heated and lattice transformed, and the device has the advantages of continuous production, high conversion rate, small equipment selection, small equipment investment, large processing capacity, energy conservation, no waste gas emission and the like.
Description
Technical Field
The invention relates to the technical field of pesticide production, in particular to a chlorothalonil lattice transformation device and method.
Background
Chlorothalonil, which is known as tetrachloro isophthalonitrile, is a high-efficiency, low-toxicity, broad-spectrum and low-residue protective bactericide, and is widely applied to the prevention and treatment of fungal diseases in agriculture and forestry, especially to the application of the chlorothalonil to economic crops such as vegetables, fruits and the like, and is also used for sterilization of golf courses, lawns, ornamental plants and the like; in addition, chlorothalonil has important application in the mildew-proof industry field, such as mildew-proof paint, mildew-proof wallpaper, mildew-proof of electrical appliances, timber and the like. The chlorothalonil is usually obtained by adopting a gas-phase chlorination process, the production scale is continuously expanded at home and abroad, and the chlorothalonil becomes one of large-tonnage good pesticide varieties in the world.
The crystal lattices of the chlorothalonil technical product are three types, namely I type, II type and III type, the stability and the efficacy of the chlorothalonil technical product are related to the crystal lattices, the II type and the III type chlorothalonil technical product has poor stability and biological activity, the product is easy to agglomerate, and the chlorothalonil technical product can only be used for industrial mildew prevention and has poor efficacy as a pesticide; the chlorothalonil type I has high stability, high bioactivity, large usage amount and wide application. However, in the process of producing chlorothalonil, the directly obtained products are basically of the type II and the type III, so that the type II and type III mainly products obtained in the process of producing chlorothalonil by gas-phase chlorination are required to be converted into the type I.
CN 201823519U discloses a novel alpha-lattice chlorothalonil production device, which comprises an airflow crusher, a sealed warehouse, a boiler and a heat exchanger, wherein the transformation of lattices is completed in the sealed warehouse by taking the chlorothalonil of mixed lattices as a raw material. CN102432504a discloses a preparation method of novel alpha-type lattice chlorothalonil, which is completed in the device, but the device and the method can only perform intermittent operation, and the time required for single batch transformation is long, so that the energy consumption is high. CN209259977U discloses a device for transforming chlorothalonil crystal lattice, which is characterized in that chlorothalonil is directly put into an electric heating furnace for heating, but the roller of the transforming furnace is longer, caking is easy to occur in the transforming process, the transforming is incomplete, the device cannot be directly used after the transforming, and cleaning holes cannot be arranged on the inner roller, so that the cleaning is very difficult. CN207576415U discloses a chlorothalonil crude drug changes crystal form device, including chlorothalonil product receiver, transformation blender and screw stirrer, transformation blender is equipped with the clamp cover outward, transformation blender internal transformation can divide into 3 sections: the front to the back is respectively an A section, a B section and a C section, wherein the A section is a transformation area, the B section is a transformation point, the section C is a transformed transition zone, and the screw stirrer of the materials in the transformed zone of the section C runs reversely. The transformation mixer is longer, is easy to agglomerate in the transformation process, is incomplete in transformation, and has the problem of larger occupied space.
In view of the foregoing, there is a need to develop a novel chlorothalonil lattice transformation device and method, which has the advantages of high processing capacity, low energy consumption, high transformation rate, anti-caking, convenient cleaning and the like.
Disclosure of Invention
In view of the problems existing in the prior art, the invention provides a chlorothalonil lattice transformation device and a chlorothalonil lattice transformation method, wherein the chlorothalonil lattice transformation device firstly realizes full and uniform preheating of chlorothalonil raw materials through a primary transformation device, achieves the aim of partial transformation of the chlorothalonil raw materials, and then realizes uniform heating of the preheated chlorothalonil and completes lattice transformation through a secondary transformation device, so that the chlorothalonil raw materials can be fully and uninterruptedly turned over, heated and lattice transformed, and the device has the advantages of continuous production, high transformation rate, small equipment selection, small equipment investment, high processing capacity, energy conservation, no exhaust emission and the like.
To achieve the purpose, the invention adopts the following technical scheme:
the invention aims to provide a chlorothalonil lattice transformation device, which comprises a feeding device, a transformation device, a crushing device and a gas-solid separation device which are sequentially connected, wherein the transformation device comprises at least 2 stages, the transformation device comprises a primary transformation device and a secondary transformation device which are connected in series, and the primary transformation device and the secondary transformation device respectively and independently comprise a jacket cylinder and a stirrer.
The chlorothalonil lattice transformation device comprises at least 2 stages of primary transformation devices and secondary transformation devices which are connected in series, wherein the primary transformation devices are used for fully and uniformly preheating the chlorothalonil raw material to achieve the aim of partial transformation of the chlorothalonil raw material, and the secondary transformation devices are used for uniformly heating the preheated chlorothalonil and completing lattice transformation, so that the chlorothalonil raw material can be fully and uninterruptedly turned over, heated and lattice transformed, and the device has the advantages of continuous production, high transformation rate, small equipment selection, small equipment investment, high processing capacity, energy conservation, no exhaust emission and the like.
As a preferable technical scheme of the invention, the jacket cylinder body is a straight cylinder, a heating medium inlet is arranged at the upper part of one side of the jacket cylinder body, and a heating medium outlet is arranged at the bottom of the other side of the jacket cylinder body.
Preferably, the length of the inner cylinder of the jacket cylinder is 2-15m, for example, 2m, 4m, 5m, 7m, 10m, 12m or 15m, etc., but is not limited to the recited values, and other non-recited values within the above-mentioned range are equally applicable.
Preferably, the diameter of the inner cylinder of the jacket cylinder is 400-1800mm, such as 400mm, 500mm, 800mm, 1000mm, 1200mm, 1500mm, 1600mm or 1800mm, etc., but is not limited to the recited values, and other non-recited values within the above-recited ranges are equally applicable.
Preferably, the interlayer thickness of the jacket cylinder is 50-150mm, such as 50mm, 70mm, 100mm, 120mm or 150mm, etc., but is not limited to the recited values, and other non-recited values within the above-recited ranges are equally applicable.
The interlayer of the jacket cylinder body refers to a hole between the inner cylinder and the outer cylinder.
Preferably, the heat exchange area of the jacket cylinder is 20-200m 2 For example 20m 2 、50m 2 、70m 2 、100m 2 、120m 2 、150m 2 、170m 2 Or 200m 2 And the like, but are not limited to the recited values, and other non-recited values within the above-recited ranges are equally applicable.
As a preferable technical scheme of the invention, a repair hole is arranged at the upper part of the jacket cylinder.
Preferably, the repair hole is rectangular, and has a length of 1000 x 600mm.
Preferably, a seal is provided on the repair hole.
The design of the repair hole is convenient for repairing when the device fails, can be used for cleaning during maintenance, and can even be used for observing the degree of internal lattice transformation.
As a preferable technical scheme of the invention, the number of the stirrers is 1-4, namely, 1-4 stirrers are arranged in the same jacket cylinder, and the rotation directions of the stirrers can be the same or opposite, for example, when 2 stirrers are arranged in the same jacket cylinder, one stirrer can rotate positively and the other stirrer rotates reversely, so that the maximum mixing is realized.
Preferably, the stirrer comprises a hollow stirring blade and a hollow shaft, wherein the hollow stirring blade is fixedly connected to the hollow shaft, so that the connection of the hollow part is realized, and the hollow stirring blade is used for passing through a heating medium.
The interlayer of the jacket cylinder, the hollow stirring blade and the hollow part of the hollow shaft are all provided with flowing heating mediums, so that an internal heat transfer system of the device is formed, and the chlorothalonil can be heated more uniformly and has higher heat transfer efficiency; in addition, the inner cylinder, the hollow stirring blade and the hollow shaft are made of any one of carbon steel, 304 stainless steel, 316L stainless steel, hastelloy or monel.
Preferably, the heating medium is steam or heat conducting oil, and compared with electric heating, the heating medium has the advantages of more stable control, energy saving, recycling and the like.
Preferably, the hollow stirring vane comprises any one of a paddle type, a screw type or a wedge type.
Preferably, one end of the hollow shaft extends out of the inner cylinder and is fixedly connected to the outer cylinder, and the other end of the hollow shaft sequentially extends out of the inner cylinder and the outer cylinder and is connected with the driving device.
Preferably, the driving device comprises a driving motor, a transmission speed reducer and a transmission gear.
Preferably, the driving motor is a variable frequency control motor.
As a preferable technical scheme of the invention, the chlorothalonil lattice transformation device also comprises an anti-caking device.
Preferably, the anti-caking device is a scraper and/or a hinge which are uniformly distributed on the hollow stirring blade, so that caking materials in the jacket cylinder can be cleaned conveniently.
Preferably, the included angle between the scraper and the hollow stirring blade is 30-90 degrees, for example, 30-40 degrees, 50 degrees, 60 degrees, 70 degrees, 80 degrees or 90 degrees, etc., but the included angle is not limited to the listed values, and other non-listed values in the above-mentioned range are equally applicable.
As a preferable technical scheme of the invention, the feeding device comprises a feeding pipe and a feeding screw conveyor, and an outlet of the feeding screw conveyor is connected with an inlet of the primary transformation device.
Preferably, the feed screw conveyor comprises a feed screw motor.
Preferably, the feeding spiral motor is a variable frequency controllable motor.
Preferably, the outlet of the secondary transformation device is connected to the inlet of the comminution device, which comprises a jet mill.
As a preferable technical scheme of the invention, the chlorothalonil lattice transformation device further comprises an induced draft fan, an inlet of the gas-solid separation device is connected with an outlet of the crushing device, a gas outlet of the gas-solid separation device is connected with the induced draft fan, and a solid outlet of the gas-solid separation device is connected with a product packaging machine.
Preferably, the tail gas collecting ports of the primary transformation device and the secondary transformation device are arranged at the upper part of the jacket cylinder body, and the tail gas collecting ports are connected with the inlet of the gas-solid separation device.
Another object of the present invention is to provide a method for lattice transformation of chlorothalonil using the device of the object, the method comprising:
the chlorothalonil raw material enters a heated primary transformation device through a feeding device, then enters a heated secondary transformation device, and then sequentially enters a crushing device and a gas-solid separation device to obtain a chlorothalonil product of a target crystal form.
In a preferred embodiment of the present invention, the particle size of the chlorothalonil material is 20 to 200 mesh, for example, 20 mesh, 50 mesh, 80 mesh, 100 mesh, 120 mesh, 150 mesh, 170 mesh or 200 mesh, but the present invention is not limited to the listed values, and other non-listed values within the above-mentioned range are equally applicable.
Preferably, the temperature of the inner cylinder of the primary transformation device is 50-130 ℃, such as 50 ℃, 60 ℃, 70 ℃, 80 ℃, 90 ℃, 100 ℃, 110 ℃, 120 ℃, 130 ℃, etc., the rotation speed of the stirrer is 10-40rpm, such as 10rpm, 15rpm, 20rpm, 25rpm, 30rpm, 35rpm, 40rpm, etc., and the residence time is 1-10 hours, such as 1 hour, 3 hours, 5 hours, 6 hours, 7 hours, 8 hours, 9 hours, 10 hours, etc., but not limited to the recited values, and other non-recited values within the above-recited values are equally applicable.
Preferably, the temperature of the inner cylinder of the secondary transformation device is 100-200 ℃, such as 100 ℃, 120 ℃, 150 ℃, 180 ℃, 200 ℃, etc., the rotation speed of the stirrer is 20-60rpm, such as 20rpm, 25rpm, 30rpm, 35rpm, 40rpm, 45rpm, 50rpm, 55rpm, 60rpm, etc., the residence time is 2-8 hours, such as 2 hours, 2.5 hours, 3 hours, 3.5 hours, 4 hours, 4.5 hours, 5 hours, 6 hours, 8 hours, etc., but not limited to the recited values, and other non-recited values within the above-recited values are equally applicable.
It is worth to say that the condition settings of the primary transformation device and the secondary transformation device are different, wherein the residence time and the stirring mode are controlled by the types of hollow stirring blades, for example, the primary transformation device adopts blade type hollow stirring blades, although the propelling speed is smaller, the stirring is sufficient, and the secondary transformation device adopts spiral type hollow stirring blades, although the stirring degree is lower, the heating requirement can be completely met, the lattice transformation is realized, the propelling speed is higher, and the productivity is convenient to improve.
Preferably, the crushing device crushes the chlorothalonil after lattice transformation to a particle size of 200-400 meshes, for example, 200-250 meshes, 300 meshes, 350 meshes or 400 meshes, etc., but the crushing device is not limited to the listed values, and other non-listed values in the above-mentioned value range are equally applicable.
As a preferred technical solution of the present invention, the method includes:
(1) Feeding the chlorothalonil raw material with the particle size of 20-200 meshes into a primary transformation device through a feeding device, controlling the temperature of an inner cylinder to be 50-130 ℃, the rotating speed of a stirrer to be 10-40rpm, the retention time to be 1-10h, feeding the processed chlorothalonil into a secondary transformation device, controlling the temperature of the inner cylinder to be 100-200 ℃, the rotating speed of the stirrer to be 20-60rpm, and the retention time to be 2-8h, and completing the crystal transformation;
(2) Crushing the chlorothalonil subjected to the crystal form conversion in the step (1) to a particle size of 200-400 meshes by a crushing device, and then carrying out gas-solid separation by a gas-solid separation device under the action of a draught fan to obtain a chlorothalonil product of a target crystal form; and (2) carrying out gas-solid separation on the tail gas generated by the primary transformation device and the secondary transformation device in the step (1) through a gas-solid separation device.
Compared with the prior art, the invention has at least the following beneficial effects:
(1) The transformation device of the chlorothalonil lattice transformation device comprises at least 2 stages of primary transformation devices and secondary transformation devices which are connected in series, wherein the primary transformation devices are used for fully and uniformly preheating the chlorothalonil raw materials to achieve the aim of partial transformation of the chlorothalonil raw materials, and then the secondary transformation devices are used for uniformly heating the preheated chlorothalonil and completing lattice transformation, so that the chlorothalonil raw materials can be fully and uninterruptedly turned over, heated and lattice transformed, and the device has the advantages of continuous production, high transformation rate, small equipment selection, small equipment investment, high processing capacity, energy conservation, no exhaust emission and the like, and can realize large-scale production;
(2) The anti-caking device can effectively avoid the thermal caking of the chlorothalonil in the lattice transformation process, avoid the influence of caking on the heat transfer efficiency, effectively ensure the sufficiency of the lattice transformation of the chlorothalonil and avoid the problem of low conversion rate;
(3) Compared with electric heating, the chlorothalonil lattice transformation device provided by the invention uses steam or heat conduction oil as a heating medium, so that the control is more stable, the chlorothalonil lattice transformation device has the advantages of energy conservation, recycling and the like, and the production cost is greatly reduced.
Drawings
FIG. 1 is a schematic diagram of a chlorothalonil lattice transformation device according to example 1 of the invention;
FIG. 2 is a top view of the anti-caking apparatus and hollow stirring blade in the primary inversion apparatus according to example 1 of the present invention;
FIG. 3 is a schematic view in the direction A-A of FIG. 2;
FIG. 4 is a side view of the anti-caking apparatus and hollow stirring blade according to the second-stage transformation apparatus according to the embodiment 1 according to the present invention, corresponding to FIG. 3;
in the figure: 1. a feed screw conveyor; 2. a primary transformation device; 3. a secondary transformation device; 4. an air flow pulverizer; 5. a cyclone separator; 6. a bag-type dust collector; 7. an induced draft fan; 8. a product packaging machine;
i-scraping knife; an I' -hinge; II-hollow stirring blade.
Detailed Description
The technical scheme of the invention is further described below by the specific embodiments with reference to the accompanying drawings.
For a better illustration of the present invention, which is convenient for understanding the technical solution of the present invention, exemplary but non-limiting examples of the present invention are as follows:
example 1
The embodiment provides a chlorothalonil lattice transformation device, as shown in fig. 1, wherein the chlorothalonil lattice transformation device comprises a feeding device, a transformation device, a crushing device and a gas-solid separation device which are sequentially connected, the transformation device is of a 2-stage design of a primary transformation device 2 and a secondary transformation device 3 which are connected in series, and the primary transformation device 2 and the secondary transformation device 3 respectively and independently comprise a jacket cylinder and a stirrer;
wherein the primary transformation device 2 and the secondary transformation device 3 are arranged as follows: the corresponding jacket cylinder body is a straight cylinder, a heating medium inlet is arranged at the upper part of one side of the jacket cylinder body, and a heating medium outlet is arranged at the bottom of the other side of the jacket cylinder body; the number of the corresponding stirrers is 2, the stirrers comprise hollow stirring blades and a hollow shaft, the hollow stirring blades are fixedly connected to the hollow shaft, so that the connection of hollow parts is realized, and the stirrer is used for passing through a heating medium; one end of the hollow shaft extends out of the inner cylinder and is fixedly connected to the outer cylinder, and the other end of the hollow shaft sequentially extends out of the inner cylinder and the outer cylinder and is connected with a driving device, wherein the driving device comprises a driving motor, a transmission speed reducer and a transmission gear, and the driving motor is a variable frequency control motor; 3 repair holes are uniformly arranged at the upper part of the jacket cylinder body at equal intervals, the repair holes are rectangular, the length of each repair hole is 1000mm, the width of each repair hole is 600mm, and sealing elements are arranged on the repair holes; the heating medium is steam;
the primary transformation device 2 is different from the secondary transformation device 3 in the following arrangement: the length of the inner cylinder of the jacket cylinder body corresponding to the primary transformation device 2 is 8m, the diameter of the inner cylinder is 1000mm, the thickness of the interlayer is 100mm, and the heat exchange area is 60m 2 The hollow stirring blade is a blade type; the length of the inner cylinder of the jacket cylinder body corresponding to the secondary transformation device 3 is 12m, the diameter of the inner cylinder is 1500mm, the thickness of the interlayer is 120mm, and the heat exchange area is 80m 2 The hollow stirring blade is spiral;
as shown in fig. 2 and fig. 3, the primary transformation device 2 further comprises an anti-caking device, wherein the anti-caking device is a scraper I uniformly distributed on the blade type hollow stirring blade II, and the plane included angle between the scraper I and the hollow stirring blade II is 45 degrees; as shown in fig. 3, the secondary transformation device 3 further comprises an anti-caking device, wherein the anti-caking device is hinges I' uniformly distributed on the spiral hollow stirring blade II;
the feeding device comprises a feeding pipe and a feeding screw conveyer 1, an outlet of the feeding screw conveyer 1 is connected with an inlet of a primary transformation device 2, the feeding screw conveyer 1 comprises a feeding screw motor, the feeding screw motor is a variable frequency controllable motor, an outlet of a secondary transformation device 3 is connected with an inlet of a crushing device, the crushing device comprises a jet mill 4, the gas-solid separation device comprises a cyclone separator 5 and a cloth bag dust remover 6, an outlet of the jet mill 4 is connected with the inlet of the cyclone separator 5, a gas outlet of the cyclone separator 5 is connected with an inlet of the cloth bag dust remover 6, the chlorothalonil lattice transformation device further comprises a draught fan 7, a gas outlet of the cloth bag dust remover 6 is connected with the draught fan 7, the tail gas collecting ports of the primary transformation device 2 and the secondary transformation device 3 are all arranged on the upper part of a jacket cylinder, the tail gas collecting ports are all connected with the inlet of the cloth bag dust remover 6, and the cyclone separator 5 and the cloth bag dust remover 6 are packaged to obtain products by a packaging machine 8.
Example 2
The present embodiment provides a chlorothalonil lattice transformation device, and other conditions are identical to those of embodiment 1 except that the hollow stirring blades corresponding to the primary transformation device are replaced by spiral stirring blades, that is, the hollow stirring blades of the primary transformation device and the secondary transformation device are spiral stirring blades.
Example 3
This example provides a chlorothalonil lattice transformation device, and the conditions are exactly the same as in example 1, except that the anti-caking device is omitted entirely.
Example 4
The present embodiment provides a chlorothalonil lattice transformation device, the connection relationship and the structure arrangement are the same as those of embodiment 1, and the difference is that:
the length of the inner cylinder of the jacket cylinder body corresponding to the primary transformation device is 2m, the diameter of the inner cylinder is 400mm, the thickness of the interlayer is 50mm, and the heat exchange area is 20m 2 The method comprises the steps of carrying out a first treatment on the surface of the The length of the inner cylinder of the jacket cylinder body corresponding to the secondary transformation device is 4m, the diameter of the inner cylinder is 800mm, the thickness of the interlayer is 100mm, and the heat exchange area is 40m 2 。
Example 5
The present embodiment provides a chlorothalonil lattice transformation device, the connection relationship and the structure arrangement are the same as those of embodiment 1, and the difference is that:
the length of the inner cylinder of the jacket cylinder body corresponding to the primary transformation device is 12m, the diameter of the inner cylinder is 1500mm, the thickness of the interlayer is 120mm, and the heat exchange area is 180m 2 The method comprises the steps of carrying out a first treatment on the surface of the The length of the inner cylinder of the jacket cylinder body corresponding to the secondary transformation device is 15m, the diameter of the inner cylinder is 1800mm, the thickness of the interlayer is 150mm, and the heat exchange area is 200m 2 。
Comparative example 1
This comparative example provides a chlorothalonil lattice strengthening device, and the conditions are exactly the same as in example 1, except that the primary transformation device is omitted entirely, i.e., the 2-stage design of the transformation device is modified to a 1-stage design.
Application example 1
The application example provides a method for transforming the crystal lattice of chlorothalonil, which is carried out by adopting the device described in the embodiment 1 and comprises the following steps:
(1) Feeding a chlorothalonil raw material with the particle size of 150 meshes into a primary transformation device through a feeding device, controlling the temperature of an inner cylinder to be 80 ℃, controlling the rotating speed of a stirrer to be 15rpm, keeping the time to be 5 hours, feeding the processed chlorothalonil into a secondary transformation device, controlling the temperature of the inner cylinder to be 150 ℃, controlling the rotating speed of the stirrer to be 30rpm, keeping the time to be 3 hours, and finishing the crystal transformation;
(2) Crushing the chlorothalonil subjected to the crystal form conversion in the step (1) to 300 meshes of particle size by a crushing device, and then carrying out gas-solid separation by a gas-solid separation device under the action of a draught fan to obtain a chlorothalonil product of a target crystal form; and (2) carrying out gas-solid separation on the tail gas generated by the primary transformation device and the secondary transformation device in the step (1) through a gas-solid separation device.
The application example can realize continuous crystal lattice transformation of the chlorothalonil, caking is not easy to occur in the transformation process, the content of the chlorothalonil of type I after transformation can reach 97%, and the treatment capacity can reach 2.5t/h.
Application example 2
The application example provides a method for transforming the crystal lattice of chlorothalonil, which is carried out by adopting the device described in the embodiment 1 and comprises the following steps:
(1) Feeding a chlorothalonil raw material with the particle size of 20 meshes into a primary transformation device through a feeding device, controlling the temperature of an inner cylinder to be 100 ℃, controlling the rotating speed of a stirrer to be 40rpm, keeping the time for 10 hours, feeding the processed chlorothalonil into a secondary transformation device, controlling the temperature of the inner cylinder to be 200 ℃, controlling the rotating speed of the stirrer to be 60rpm, keeping the time for 5 hours, and finishing the crystal form transformation;
(2) Crushing the chlorothalonil converted in the step (1) to 200 meshes of particle size by a crushing device, and then carrying out gas-solid separation by a gas-solid separation device under the action of a draught fan to obtain a chlorothalonil product of a target crystal form; and (2) carrying out gas-solid separation on the tail gas generated by the primary transformation device and the secondary transformation device in the step (1) through a gas-solid separation device.
The application example can realize continuous crystal lattice transformation of the chlorothalonil, caking is not easy to occur in the transformation process, the content of the chlorothalonil of type I after transformation can reach 95%, and the treatment capacity can reach 2.5t/h.
Application example 3
The application example provides a method for transforming the crystal lattice of chlorothalonil, which is carried out by adopting the device described in the embodiment 1 and comprises the following steps:
(1) Feeding a chlorothalonil raw material with the particle size of 200 meshes into a primary transformation device through a feeding device, controlling the temperature of an inner cylinder to be 50 ℃, controlling the rotating speed of a stirrer to be 10rpm, keeping the time to be 5 hours, feeding the processed chlorothalonil into a secondary transformation device, controlling the temperature of the inner cylinder to be 150 ℃, controlling the rotating speed of the stirrer to be 20rpm, keeping the time to be 2 hours, and finishing the crystal transformation;
(2) Crushing the chlorothalonil subjected to the crystal form conversion in the step (1) to 400 meshes of particle size by a crushing device, and then carrying out gas-solid separation by a gas-solid separation device under the action of a draught fan to obtain a chlorothalonil product of a target crystal form; and (2) carrying out gas-solid separation on the tail gas generated by the primary transformation device and the secondary transformation device in the step (1) through a gas-solid separation device.
The application example can realize continuous crystal lattice transformation of the chlorothalonil, caking is not easy to occur in the transformation process, the content of the chlorothalonil of type I after transformation can reach 96%, and the treatment capacity can reach 2.5t/h.
Application example 4
The application example provides a method for transforming the crystal lattice of chlorothalonil, which is carried out by adopting the device described in the embodiment 2, so that the residence time of the primary transformation device in the step (1) is changed from 7h to 3h, and other conditions are identical to those in the application example 1.
The application example can realize continuous process of the chlorothalonil lattice transformation, agglomeration is not easy to occur in the transformation process, but the raw material of the chlorothalonil is preheated unevenly due to the shortened residence time of the primary transformation device, so that the content of the I-type chlorothalonil after transformation is 91%, and the treatment capacity can reach 2.5t/h.
Application example 5
The application example provides a method for transforming the crystal lattice of chlorothalonil, which is carried out by adopting the device described in the embodiment 3, and other conditions are identical to those of the application example 1.
The application example can realize continuous process of the chlorothalonil lattice transformation, but the agglomeration phenomenon is very easy to occur in the transformation process due to the fact that an anti-agglomeration device is not used, so that the transformation rate is uneven, the content of the I-type chlorothalonil after transformation is only 66%, and the treatment capacity can reach 2.5t/h.
Comparative example 1 was used
The comparative application example provides a method for lattice transformation of chlorothalonil, which is carried out by using the device described in the comparative example 1, and other conditions are exactly the same as those in the application example 1.
In the application comparative example, the preheating treatment of the primary transformation device is not carried out, so that the content of the type I chlorothalonil after transformation is 65%, and the transformation rate is greatly reduced.
In summary, the transformation device of the chlorothalonil lattice transformation device comprises at least 2 stages of primary transformation devices and secondary transformation devices which are connected in series, wherein the primary transformation devices are used for fully and uniformly preheating the chlorothalonil raw materials to achieve the aim of partial transformation of the chlorothalonil raw materials, and then the secondary transformation devices are used for uniformly heating the preheated chlorothalonil and completing lattice transformation, so that the chlorothalonil raw materials can be fully and uninterruptedly turned over, heated and lattice transformed, and the device has the advantages of continuous production, high transformation rate, small equipment selection, small equipment investment, high processing capacity, energy conservation, no exhaust emission and the like, and can realize mass production; in addition, the anti-caking device can effectively avoid the thermal caking of the chlorothalonil in the lattice transformation process, avoid the caking from influencing the heat transfer efficiency, effectively ensure the sufficiency of the lattice transformation of the chlorothalonil and avoid the problem of low transformation rate.
The applicant states that the detailed structural features of the present invention are described by the above embodiments, but the present invention is not limited to the above detailed structural features, i.e. it does not mean that the present invention must be implemented depending on the above detailed structural features. It should be apparent to those skilled in the art that any modifications of the present invention, equivalent substitutions of selected components of the present invention, addition of auxiliary components, selection of specific modes, etc., are within the scope of the present invention and the scope of the disclosure.
The preferred embodiments of the present invention have been described in detail above, but the present invention is not limited to the specific details of the above embodiments, and various simple modifications can be made to the technical solution of the present invention within the scope of the technical concept of the present invention, and all the simple modifications belong to the protection scope of the present invention.
In addition, the specific features described in the above embodiments may be combined in any suitable manner, and in order to avoid unnecessary repetition, various possible combinations are not described further.
Moreover, any combination of the various embodiments of the invention can be made without departing from the spirit of the invention, which should also be considered as disclosed herein.
Claims (27)
1. The chlorothalonil lattice transformation device is characterized by comprising a feeding device, a transformation device, a crushing device and a gas-solid separation device which are sequentially connected, wherein the transformation device comprises at least 2 stages, the transformation device comprises a primary transformation device and a secondary transformation device which are connected in series, and the primary transformation device and the secondary transformation device respectively and independently comprise a jacket cylinder and a stirrer;
the stirrer comprises a hollow stirring blade and a hollow shaft, wherein the hollow stirring blade is fixedly connected to the hollow shaft to realize connection of hollow parts and is used for heating a medium;
the chlorothalonil lattice transformation device also comprises an anti-caking device;
the anti-caking device is a scraper and/or a hinge which are uniformly distributed on the hollow stirring blade;
the plane included angle between the scraper and the hollow stirring blade is 30-90 degrees.
2. The chlorothalonil lattice transfer type device according to claim 1, wherein the jacket cylinder is a straight cylinder, a heating medium inlet is formed in the upper portion of one side of the jacket cylinder, and a heating medium outlet is formed in the bottom of the other side of the jacket cylinder.
3. The chlorothalonil lattice transfer device according to claim 1, wherein the inner cylinder of the jacket cylinder has a length of 2-15m.
4. The chlorothalonil lattice transfer device according to claim 1, wherein the diameter of the inner cylinder of the jacket cylinder is 400-1800mm.
5. The chlorothalonil lattice transfer device according to claim 1, wherein the jacketed cylinder has a sandwich thickness of 50-150mm.
6. The chlorothalonil lattice transformation device according to claim 1, wherein the heat exchange area of the jacket cylinder is 20-200m 2 。
7. The chlorothalonil lattice transformation device according to claim 1 or 2, wherein a repair hole is provided at an upper portion of the jacket cylinder.
8. The chlorothalonil lattice transfer device according to claim 7, wherein the repair hole is rectangular.
9. The chlorothalonil lattice transfer device according to claim 7, wherein a sealing member is provided on the repair hole.
10. The chlorothalonil lattice transfer device according to claim 1, wherein the number of agitators is 1-4.
11. The chlorothalonil lattice transfer device according to claim 1, wherein the heating medium is steam or heat conducting oil.
12. The chlorothalonil lattice transfer device according to claim 1, wherein the hollow stirring blade comprises any one of a paddle type, a screw type or a wedge type.
13. The chlorothalonil lattice transfer device according to claim 1, wherein one end of the hollow shaft extends out of the inner cylinder and is fixedly connected to the outer cylinder, and the other end sequentially extends out of the inner cylinder and the outer cylinder and is connected with the driving device.
14. The chlorothalonil lattice transfer device according to claim 13, wherein the driving means comprises a driving motor, a transmission reducer and a transmission gear.
15. The chlorothalonil lattice transfer device according to claim 14, wherein the drive motor is a variable frequency control motor.
16. The chlorothalonil lattice transfer device according to claim 1, wherein the feeding device comprises a feed pipe and a feed screw conveyor, an outlet of the feed screw conveyor being connected to an inlet of the primary transfer device.
17. The chlorothalonil lattice transfer device according to claim 16, wherein the feed screw conveyor comprises a feed screw motor.
18. The chlorothalonil lattice transfer device according to claim 17, wherein the feed screw motor is a variable frequency controllable motor.
19. The chlorothalonil lattice transfer device according to claim 1, wherein the outlet of the secondary transfer device is connected to the inlet of the comminution device, the comminution device comprising a jet mill.
20. The chlorothalonil lattice transformation device according to claim 1, further comprising an induced draft fan, wherein an inlet of the gas-solid separation device is connected with an outlet of the crushing device, and a gas outlet of the gas-solid separation device is connected with the induced draft fan.
21. The chlorothalonil lattice transformation device according to claim 1, wherein the tail gas collecting ports of the primary transformation device and the secondary transformation device are arranged at the upper part of the jacket cylinder, and the tail gas collecting ports are connected with the inlet of the gas-solid separation device.
22. A method of performing a chlorothalonil lattice transformation using the device of any one of claims 1-21, the method comprising:
the chlorothalonil raw material enters a heated primary transformation device through a feeding device, then enters a heated secondary transformation device, and then sequentially enters a crushing device and a gas-solid separation device to obtain a chlorothalonil product of a target crystal form.
23. The method of claim 22, wherein the chlorothalonil material has a particle size of 20-200 mesh.
24. The method of claim 22, wherein the primary transfer apparatus has an inner barrel temperature of 50-130 ℃, a stirrer rotation speed of 10-40rpm, and a residence time of 1-10 hours.
25. The method of claim 22, wherein the secondary transformation device has an inner barrel temperature of 100-200 ℃, a stirrer rotation speed of 20-60rpm, and a residence time of 2-8h.
26. The method of claim 22, wherein the comminuting device comminuting the lattice-transformed chlorothalonil to a particle size of 200-400 mesh.
27. The method according to claim 22, characterized in that the method comprises:
(1) Feeding the chlorothalonil raw material with the particle size of 20-200 meshes into a primary transformation device through a feeding device, controlling the temperature of an inner cylinder to be 50-130 ℃, the rotating speed of a stirrer to be 10-40rpm, the retention time to be 1-10h, feeding the processed chlorothalonil into a secondary transformation device, controlling the temperature of the inner cylinder to be 100-200 ℃, the rotating speed of the stirrer to be 20-60rpm, and the retention time to be 2-8h, and completing the crystal transformation;
(2) Crushing the chlorothalonil subjected to the crystal form conversion in the step (1) to a particle size of 200-400 meshes by a crushing device, and then carrying out gas-solid separation by a gas-solid separation device under the action of a draught fan to obtain a chlorothalonil product of a target crystal form; and (2) carrying out gas-solid separation on the tail gas generated by the primary transformation device and the secondary transformation device in the step (1) through a gas-solid separation device.
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