Chlorothalonil lattice transformation device and process in chlorination reaction gas receiving process

Abstract

The invention relates to the technical field of pesticide production, in particular to a chlorothalonil lattice transformation device in a chlorination reaction gas collecting process, which is characterized in that a first-stage gas phase inlet and first-stage atomization equipment are arranged at the upper end of a first-stage thin-wall type collector, and a first-stage gas phase outlet is arranged at the lower end of the first-stage thin-wall type collector and is connected with a second-stage thin-wall type collector; a primary solid discharge hole is formed in the lower end of the primary screw conveyor and is connected with the primary screw conveyor; a second-stage gas phase inlet and a second-stage solid discharging port are formed in the lower end of the second-stage thin-wall type material collector, the second-stage solid discharging port is connected with the second-stage screw conveyor, and second-stage atomization equipment and a second-stage gas phase outlet are formed in the upper end of the second-stage thin-wall type material collector; the first-stage screw conveyor and the second-stage screw conveyor are both connected with the transformation stock bin, a discharge port of the transformation stock bin is connected with a rotary valve, an outlet of the rotary valve is divided into two branches, one branch is sequentially connected with the superfine pulverizer and the pipe chain conveyor, and the pipe chain conveyor is connected with the first-stage thin-wall type material collector and the second-stage thin-wall type material collector; and the other branch is connected with the transformed material storage system through a third rotary air blocking valve.

Description

Technical Field

[0001] The invention relates to the technical field of pesticide production, and in particular to a chlorothalonil lattice transformation device and process in a chlorination reaction gas collection process. Background Art

[0002] As a high-efficiency, low-toxic, broad-spectrum fungicide, chlorothalonil is mainly used to prevent crops from being infected by fungi. It is often used to prevent and control rust, anthracnose, powdery mildew, and downy mildew on fruit trees and vegetables. Chlorothalonil has no systemic conduction effect, but after being sprayed on the plant body, it has good adhesion on the body surface and is not easily washed away by rain, so the efficacy period is relatively long.

[0003] There are two main types of crystal lattices of chlorothalonil technical, namely type I and type II. Type II lattice chlorothalonil has poor stability, is easy to agglomerate, has poor biological activity, and has poor efficacy when used as a pesticide; while type I lattice chlorothalonil is the most stable at room temperature and has good bactericidal activity after processing. However, in the production of chlorothalonil, due to the production process, the directly obtained product is usually mainly type II, with less or almost no type I, and the spontaneous conversion of type II chlorothalonil to type I lattice chlorothalonil in a dry state is very slow. There are industrial transformation methods for converting type II chlorothalonil into type I lattice, but they all require that type II chlorothalonil be transported to the transformation equipment after collection, which brings the following problems: (1) Type II chlorothalonil is very easy to agglomerate at high temperature and has strong viscosity, and is easy to adhere to the wall of the equipment. (2) The high-temperature gas of the chlorination reaction is type I lattice during the condensation and precipitation of chlorothalonil. If the cooling is incomplete, it will form a liquid and then solidify, directly forming a solid agglomerate with a hardness as hard as stone. Therefore, an effective cooling and thiophanate-methyl collection method is urgently needed to ensure that Type I lattice thiophanate-methyl can be smoothly transported to subsequent equipment.

[0004] A Chinese patent (publication number CN207576415U) discloses a novel chlorothalonil technical drug crystal transformation device, including a chlorothalonil product receiver, a transformation mixer and a screw-type agitator; the chlorothalonil product receiver is arranged in series with the transformation mixer, a jacket is arranged outside the transformation mixer, and two screw-type agitators are arranged inside, one is forward and the other is reverse, and the screw is hollow inside for passing heat exchange medium. However, the production device of the patent cannot control the transformation rate and effect when the chlorothalonil receiver is blocked during operation. A Chinese patent (publication number CN109265366 A) discloses a chlorothalonil crystal lattice transformation device and method, the transformation device includes a transformation device, the transformation device includes a rotating drum in a furnace, and a spiral flap is arranged on the inner wall of the rotating drum; a heating element is arranged in the transformation device; the transformation device is inclined downward from the inlet to the outlet, and the inclination angle is 2 to 10 degrees. The rotary drum of the conversion device heats and turns the chlorothalonil to prevent the raw materials from agglomerating due to heating, and converts Type II and Type III chlorothalonil technical materials into Type I, thereby achieving continuous conversion of chlorothalonil. However, the conversion rate of Type I chlorothalonil in the resulting product reaches 90%, which cannot be completely converted. If the batch conversion effect is poor, manual re-feeding is required. A Chinese patent (publication number CN113019269A) discloses a chlorothalonil lattice transformation device and a preparation method, wherein the transformation device comprises a feeding tank, which is connected to the feed port of a transformation mixer via a screw feeder, and a discharge port and an air inlet are arranged at the bottom of the transformation mixer, and the air inlet is connected to a preheater, a flow meter, and a fluidizing gas storage tank in sequence; Type I lattice chlorothalonil and Type II lattice chlorothalonil are fluidized and mixed in a transformation mixer according to a certain mass ratio, and at the same time, the fluidizing gas in the fluidizing gas storage tank is preheated by a preheater and enters the transformation mixer at a certain flow rate, and Type II lattice chlorothalonil is transformed in the transformation mixer, and the transformation device does not require mechanical stirring, so that continuous and rapid transformation of chlorothalonil technical can be achieved, but the problem of block material in the process of collecting, storing and conveying Type II lattice chlorothalonil cannot be solved. Summary of the invention

[0005] In order to solve the above problems, the present invention provides a device for transforming the chlorothalonil crystal lattice during the collection process of chlorination reaction gas. The collection and transformation device is continuous and stable, and type I lattice chlorothalonil is directly formed during the condensation process of the chlorination reaction gas, thereby eliminating the phenomenon of chlorothalonil agglomerating at high temperature and the phenomenon of motor current exceeding high and screw jamming occurring during the process of conveying agglomerated chlorothalonil by the screw conveyor. The obtained chlorothalonil raw materials are all type I lattice chlorothalonil, which are basically completely converted.

[0006] The present invention provides a chlorothalonil lattice transformation device in a chlorination reaction gas collection process, which at least comprises a primary thin-walled material receiver, a secondary thin-walled material receiver, a primary screw conveyor, a secondary screw conveyor, a transformation silo, a rotary valve, an ultrafine grinder, and a pipe chain conveyor. The primary thin-walled material receiver is provided with a primary gas phase inlet and a primary atomizing device at the upper end, a primary gas phase outlet is provided at the lower end to be connected with the secondary thin-walled material receiver, and a primary solid discharge port is provided at the lower end to be connected with the primary screw conveyor; the secondary thin-walled material receiver is provided with a primary gas phase inlet and a primary atomizing device at the lower end, A secondary gas phase inlet and a secondary solid discharge port, the secondary solid discharge port is connected to a secondary screw conveyor, and a secondary atomization device and a secondary gas phase outlet are provided at the upper end; the primary screw conveyor and the secondary screw conveyor are both connected to the transformation silo, the discharge port of the transformation silo is connected to a rotary valve, the rotary valve outlet is divided into two streams, one stream is connected to an ultrafine grinder and a tube chain conveyor in sequence, the tube chain conveyor is respectively connected to a primary thin-walled receiver and a secondary thin-walled receiver; the other stream is connected to a transformation material storage system through a third rotary air lock valve.

[0007] As a preferred technical solution, a cyclone separator is arranged between the ultrafine grinder and the tube chain conveyor, the top outlet of the cyclone separator is connected to the bag dust collector, the top outlet of the bag dust collector is connected to the induced draft fan, the bottom discharge port of the cyclone separator and the bottom discharge port of the bag dust collector are connected to the tube chain conveyor through the first rotary air lock valve and the second rotary air lock valve respectively.

[0008] As a preferred technical solution, the first-level thin-walled material receiver, the second-level thin-walled material receiver, the first-level screw conveyor and the second-level screw conveyor are all provided with cooling elements on the outside. The cooling elements are preferably cooling jackets, and the circulating cooling fluid inside the cooling jackets can realize the cooling of the materials inside the first-level thin-walled material receiver and the second-level thin-walled material receiver as well as the first-level screw conveyor, the second-level screw conveyor and their conveyed materials.

[0009] As a preferred technical solution, the primary atomization equipment and the secondary atomization equipment both include an atomization tube and an atomization nozzle; the atomization tube and the atomization nozzle control the atomization pressure through high-pressure gas to spray and atomize the transformed ultrafine powder.

[0010] As a preferred technical solution, the secondary gas phase outlet is connected to a pulse dust collector.

[0011] As a preferred technical solution, the ultrafine pulverizer is equipped with a classifier. After the ultrafine pulverizer pulverizes the transformation material, the particle size after pulverization is adjusted by the classifier through frequency conversion to obtain the transformation ultrafine powder.

[0012] The device for transforming the chlorothalonil lattice during the chlorination reaction gas collection process provided by the present invention does not need to perform collection, transportation, storage and then prepare with type I crystal lattice chlorothalonil through mixing mechanical stirring, thereby realizing continuous and rapid collection and transformation, shortening the transformation time, and solving the problems of material agglomeration and transportation and storage difficulties during the collection process. The chlorothalonil technical obtained by collection is completely transformed into type I crystal lattice.

[0013] Specifically, the present invention obtains transformation ultrafine powder with a particle size of 300-400 mesh by designing an ultrafine pulverizer equipped with a classifier, and then atomizes the pulverized 300-400 mesh transformation ultrafine powder into a primary thin-walled receiver and a secondary thin-walled receiver through an atomization device using high-pressure nitrogen to prevent clogging of the atomization nozzle and ensure the atomization effect. At the same time, the cold nitrogen and the atomized type I crystal lattice thiophanate-methyl are more fully mixed with the reaction gas, and the cooling effect is better, which is more conducive to the transformation when the thiophanate-methyl crystals are precipitated.

[0014] In addition, the present invention provides cooling water jackets on the outside of the first-level thin-walled material receiver, the second-level thin-walled material receiver, the first-level screw conveyor, and the second-level screw conveyor, thereby ensuring the stability of the mechanical equipment while controlling the temperature of the Type I lattice thiophanate-methyl product obtained by collecting the material to 100-110°C.

[0015] Another aspect of the present invention provides a chlorothalonil lattice transformation process in a chlorination reaction gas collection process, which at least comprises the following steps:

[0016] S1: Manually put the transformation material into the transformation silo for the first time, control the frequency of the rotary valve to transport the transformation material to the ultrafine grinder through the discharge port of the transformation silo, and after the ultrafine grinder grinds the transformation material, the particle size after grinding is adjusted by the frequency conversion of the classifier to obtain the transformation ultrafine powder;

[0017] S2: The transformation ultrafine powder is transported to the cyclone separator and the bag dust collector by the negative pressure of the induced draft fan, and the frequencies of the first rotary air lock valve and the second rotary air lock valve are controlled to transport the transformation ultrafine powder to the tube chain conveyor through the bottom discharge port of the cyclone separator and the bottom discharge port of the bag dust collector, and the transformation ultrafine powder is transported to the primary atomization equipment and the secondary atomization equipment by the tube chain conveyor, and the transformation ultrafine powder is sprayed and atomized by controlling the atomization pressure by high-pressure gas to obtain atomized type I lattice thiophanate-methyl;

[0018] S3: The atomized Type I crystal lattice thiophanate-methyl enters the primary thin-walled receiver and the secondary thin-walled receiver, and the chlorination reaction gas is introduced into the primary thin-walled receiver. The chlorination reaction gas passes through the primary thin-walled receiver and then the secondary thin-walled receiver, and contacts with the atomized Type I crystal lattice thiophanate-methyl to undergo lattice transformation and precipitate Type I crystal lattice thiophanate-methyl product;

[0019] S4: Start the first-stage screw conveyor and the second-stage screw conveyor to transport the Type I lattice thiophanate-methyl product obtained in the first-stage thin-walled receiver and the second-stage thin-walled receiver to the transformation silo for recycling, thus establishing a material collection and transformation cycle.

[0020] As a preferred technical solution, the particle size of the transformation material is 20-100 μm, and the bulk density is 900-1050 kg / m 3 .

[0021] As a preferred technical solution, the feeding amount of the transformation material accounts for 40-60% of the volume of the transformation silo, preferably 50%.

[0022] As a preferred technical solution, the frequency of the rotary valve is 5-40HZ.

[0023] As a preferred technical solution, the frequency of the ultrafine grinder is 20-40HZ, preferably 30HZ.

[0024] As a preferred technical solution, the frequency of the classifier is 15-25HZ, and the particle size of the transformation ultrafine powder is 300-400 mesh. Preferably, the frequency of the classifier is 20HZ, and the particle size of the transformation ultrafine powder is 325 mesh.

[0025] As a preferred technical solution, the frequency of the first rotary air lock valve and the second rotary air lock valve is 30-50HZ, and the flow rate of the transformed ultrafine powder is 300-800kg / h.

[0026] As a preferred technical solution, the high-pressure gas is high-pressure nitrogen, and the atomization pressure is 1.0-1.5 MPa.

[0027] As a preferred technical solution, the temperature of the chlorination reaction gas is 240-280°C, and the theoretical content of chlorothalonil gas is 200 kg.

[0028] As a preferred technical solution, the mass ratio of the chlorination reaction gas to the atomized type I lattice thiophanate-methyl is (1-2): (2-5).

[0029] As a preferred technical solution, the temperature of the lattice transformation is 90-120°C, preferably 100-110°C.

[0030] As a preferred technical solution, the temperature of the Type I lattice thiophanate-methyl product is 90-120°C, preferably 100-110°C.

[0031] As a preferred technical solution, the temperature of the Type I lattice thiophanate-methyl product conveyed to the transformation silo by a primary screw conveyor and a secondary screw conveyor is 50-60°C.

[0032] As a preferred technical solution, the transition material silo is transported to the transition material storage system when the material level reaches 70% (v / v), and the transportation is stopped when the material level reaches 50% (v / v).

[0033] The present invention optimizes the process conditions based on the chlorothalonil lattice transformation device in the chlorination reaction gas collection process to ensure the cooling effect of the chlorination reaction gas collection process, and at the same time, no agglomerates are formed in the collection device. In particular, the frequency of the rotary valve, the frequency of the first rotary air lock valve and the second rotary air lock valve, and the atomization pressure are comprehensively controlled to ensure that the chlorination reaction gas and the atomized type I lattice chlorothalonil are mixed in a mass ratio of (1-2): (2-5) and the lattice transformation is carried out at 90-120°C, so that the greening reaction gas collection process is synchronously transformed and a type I chlorothalonil product with a transformation rate of more than 99% is obtained.

[0034] The material collection and transformation device provided in the present invention cooperates with the process to avoid the production of Type II lattice thiophanate-methyl from the source, avoids the agglomeration of Type II lattice thiophanate-methyl during the material collection process, reduces the investment in dynamic equipment (such as mixers and crushers), and greatly reduces the shutdown caused by the failure of a certain dynamic equipment. This is of great economic benefit to the production process of thiophanate-methyl and has a high market promotion value.

[0035] Beneficial Effects

[0036] 1. The present invention provides a device for transforming the chlorothalonil crystal lattice during the process of collecting chlorination reaction gas. The device is continuous and stable. Type I chlorothalonil crystal lattice is directly formed during the condensation process of the chlorination reaction gas, thereby eliminating the phenomenon of chlorothalonil agglomeration at high temperature and the phenomenon of motor current over-high stop and screw jamming during the process of conveying agglomerated chlorothalonil by the screw conveyor. The obtained chlorothalonil raw materials are all Type I chlorothalonil crystal lattice, which is basically completely converted.

[0037] 2. The device for transforming the chlorothalonil lattice during the chlorination reaction gas collection process provided by the present invention does not need to be collected, transported, stored, and then prepared with type I lattice chlorothalonil through mixing mechanical stirring, thereby realizing continuous and rapid collection and transformation, shortening the transformation time, and solving the problems of material agglomeration and transportation and storage difficulties during the collection process. The chlorothalonil technical obtained by collection is completely transformed into type I lattice.

[0038] 3. The present invention obtains the transformation ultrafine powder with a particle size of 300-400 mesh by designing an ultrafine pulverizer equipped with a classifier, and then atomizes the pulverized 300-400 mesh transformation ultrafine powder into a primary thin-walled receiver and a secondary thin-walled receiver through an atomization device using high-pressure nitrogen to prevent the atomization nozzle from being blocked and ensure the atomization effect. At the same time, the cold nitrogen and the atomized type I crystal lattice thiophanate-methyl are more fully mixed with the reaction gas, the cooling effect is better, and it is more conducive to the transformation when the thiophanate-methyl crystals are precipitated.

[0039] 4. The present invention optimizes the process conditions based on the chlorothalonil lattice transformation device in the chlorination reaction gas collection process to ensure the cooling effect of the chlorination reaction gas collection process and prevent the formation of agglomerates in the collection device. In particular, the frequency of the rotary valve, the frequency of the first rotary air lock valve and the second rotary air lock valve, and the atomization pressure are comprehensively controlled to ensure that the chlorination reaction gas and the atomized type I lattice chlorothalonil are mixed in a mass ratio of (1-2): (2-5) and the lattice transformation is carried out at 90-120°C, so as to achieve the synchronous transformation of the greening reaction gas collection process and obtain a type I chlorothalonil product with a transformation rate of more than 99%.

[0040] 5. The material collection and transformation device provided by the present invention cooperates with the process to avoid the production of Type II lattice thiophanate-methyl from the source, avoids the agglomeration of Type II lattice thiophanate-methyl during the material collection process, reduces the investment in dynamic equipment (such as mixers and crushers), and greatly reduces the shutdown caused by the failure of a certain dynamic equipment. This is of great economic benefit to the production process of thiophanate-methyl and has a high market promotion value. BRIEF DESCRIPTION OF THE DRAWINGS

[0041] Figure 1 It is a structural schematic diagram of the chlorination reaction gas receiving and transformation device in an embodiment of the present invention,

[0042] In the figure: 1 is a primary thin-walled material receiver, 1.1 is a primary atomizing device, 1.2 is a cooling water jacket, 1.3 is a pressure transmitter, 2 is a secondary thin-walled material receiver, 2.1 is a secondary atomizing device, 2.2 is a cooling jacket, 2.3 is a pressure transmitter, 3 is a primary screw conveyor, 4 is a secondary screw conveyor, 5 is a transformation silo, 5.1 is a material level meter, 6 is a rotary valve, 7 is an ultrafine grinder, 7.1 is a cyclone separator, 7.2 is a bag dust collector, 7.3 is an induced draft fan, 7.4 is a first rotary air lock valve, 7.5 is a second rotary air lock valve, 8 is a third rotary air lock valve, 8.1 is a pressure transmitter, and 9 is a pipe chain conveyor.

[0043] Figure 2 This is the XRD spectrum of the Type I lattice thiophanate-methyl product of the present invention.

[0044] Figure 3 This is the XRD pattern of type II lattice thiophanate-methyl. DETAILED DESCRIPTION

[0045] Example 1

[0046] Embodiment 1 of the present invention provides a chlorothalonil lattice transformation device in a chlorination reaction gas collection process, comprising a primary thin-walled material receiver 1, a secondary thin-walled material receiver 2, a primary screw conveyor 3, a secondary screw conveyor 4, a transformation silo 5, a rotary valve 6, an ultrafine grinder 7, and a tube chain conveyor 9, wherein the primary thin-walled material receiver 1 is provided with a primary gas phase inlet and a primary atomization device 1.1 at the upper end, a primary gas phase outlet connected to the secondary thin-walled material receiver 2 at the lower end, and a primary solid discharge port connected to the primary screw conveyor 3 at the lower end; the secondary thin-walled material receiver 2 is provided with a primary gas phase inlet and a primary atomization device 1.1 at the lower end, and a primary gas phase outlet connected to the secondary thin-walled material receiver 2 at the lower end. A secondary gas phase inlet and a secondary solid discharge port are provided, the secondary solid discharge port is connected to a secondary screw conveyor 4, and a secondary atomization device 2.1 and a secondary gas phase outlet are provided at the upper end; the primary screw conveyor 3 and the secondary screw conveyor 4 are both connected to a transformation silo 5, the discharge port of the transformation silo 5 is connected to a rotary valve 6, and the rotary valve outlet is divided into two streams, one stream is connected to an ultrafine grinder 7 and a tube chain conveyor 9 in sequence, and the tube chain conveyor 9 is respectively connected to a primary thin-walled receiver 1 and a secondary thin-walled receiver 2; the other stream is connected to a transformation material storage system through a third rotary air lock valve 8.

[0047] A cyclone separator 7.1 is arranged between the ultrafine pulverizer 7 and the tube chain conveyor 9, the top outlet of the cyclone separator 7.1 is connected to the bag dust collector 7.2, the top outlet of the bag dust collector 7.2 is connected to the induced draft fan 7.3, the bottom discharge port of the cyclone separator 7.1 and the bottom discharge port of the bag dust collector 7.2 are connected to the tube chain conveyor 9 through the first rotary air lock valve 7.4 and the second rotary air lock valve 7.5 respectively.

[0048] The first-level thin-walled material receiver 1, the second-level thin-walled material receiver 2, the first-level screw conveyor 3, and the second-level screw conveyor 4 are all provided with cooling water jackets on the outside, and the materials inside the first-level thin-walled material receiver and the second-level thin-walled material receiver as well as the first-level screw conveyor, the second-level screw conveyor and their conveyed materials are cooled by circulating cooling water inside the cooling jackets.

[0049] The primary atomizing device 1.1 and the secondary atomizing device 2.1 both include an atomizing tube and an atomizing nozzle; the atomizing tube and the atomizing nozzle spray and atomize the ultrafine powder by controlling the atomizing pressure through high-pressure gas.

[0050] The secondary gas phase outlet is connected to a pulse dust collector.

[0051] The ultrafine pulverizer is equipped with a classifier. After the ultrafine pulverizer pulverizes the transformation material, the particle size after pulverization is adjusted by the classifier through frequency conversion to obtain the transformation ultrafine powder.

[0052] On the other hand, Example 1 of the present invention provides a chlorothalonil lattice transformation process in a chlorination reaction gas collection process, comprising the following steps:

[0053] S1: Manually put the transformation material into the transformation silo for the first time, control the frequency of the rotary valve to transport the transformation material to the ultrafine grinder through the discharge port of the transformation silo, and after the ultrafine grinder grinds the transformation material, the particle size after grinding is adjusted by the frequency conversion of the classifier to obtain the transformation ultrafine powder;

[0054] S2: The transformation ultrafine powder is transported to the cyclone separator and the bag dust collector by the negative pressure of the induced draft fan, and the frequencies of the first rotary air lock valve and the second rotary air lock valve are controlled to transport the transformation ultrafine powder to the tube chain conveyor through the bottom discharge port of the cyclone separator and the bottom discharge port of the bag dust collector, and the transformation ultrafine powder is transported to the primary atomization equipment and the secondary atomization equipment by the tube chain conveyor, and the transformation ultrafine powder is sprayed and atomized by controlling the atomization pressure by high-pressure gas to obtain atomized type I lattice thiophanate-methyl;

[0055] S3: The atomized Type I crystal lattice thiophanate-methyl enters the primary thin-walled receiver and the secondary thin-walled receiver, and the chlorination reaction gas is introduced into the primary thin-walled receiver. The chlorination reaction gas passes through the primary thin-walled receiver and then the secondary thin-walled receiver, and contacts with the atomized Type I crystal lattice thiophanate-methyl to undergo lattice transformation and precipitate Type I crystal lattice thiophanate-methyl product;

[0056] S4: Start the first-stage screw conveyor and the second-stage screw conveyor to transport the Type I lattice thiophanate-methyl product obtained in the first-stage thin-walled receiver and the second-stage thin-walled receiver to the transformation silo for recycling, thus establishing a material collection and transformation cycle.

[0057] The particle size of the transformation material is 20-100 μm, and the bulk density is 900-1050 kg / m 3 .

[0058] The input amount of the transformation material accounts for 50% of the volume of the transformation silo.

[0059] The frequency of the rotary valve is 5 Hz.

[0060] The frequency of the superfine grinder is 30HZ.

[0061] The frequency of the classifier is 20HZ, and the particle size of the transformed ultrafine powder is 325 meshes.

[0062] The frequency of the first rotary air lock valve and the second rotary air lock valve is 30HZ, and the flow rate of the transformed ultrafine powder is 300kg / h.

[0063] The high-pressure gas is high-pressure nitrogen, and the atomization pressure is 1.0 MPa.

[0064] The temperature of the chlorination reaction gas is 250° C. and theoretically contains 200 kg of thiophanate-methyl gas.

[0065] The mass ratio of the chlorination reaction gas to the atomized type I lattice thiophanate-methyl is 2:3.

[0066] The temperature of the lattice transformation is 120°C.

[0067] The temperature of the Type I lattice thiophanate-methyl product is 120°C.

[0068] The temperature of the Type I lattice thiophanate-methyl product transported to the transformation silo by a primary screw conveyor and a secondary screw conveyor is 50°C.

[0069] The material level in the transition material bin reaches 70% (v / v) and is transported to the transition material storage system. The material level in the transition material bin reaches 50% (v / v) and the transport is stopped (sampling is performed at this time).

[0070] Example 2

[0071] Embodiment 2 of the present invention provides a device and process for thiophanate-methyl lattice transformation in the process of collecting chlorination reaction gas. The specific implementation method is the same as that of embodiment 1, except that the frequency of the rotary valve is 10HZ, the frequency of the first rotary air lock valve and the second rotary air lock valve is 35HZ, and the flow rate of the transformed ultrafine powder is 400kg / h. The high-pressure gas is high-pressure nitrogen, and the atomization pressure is 1.1MPa. The mass ratio of the chlorination reaction gas to the atomized type I lattice thiophanate-methyl is 1:2. The temperature of the lattice transformation is 110°C, and the temperature of the type I lattice thiophanate-methyl product is 110°C.

[0072] Example 3

[0073] Embodiment 3 of the present invention provides a device and process for thiophanate-methyl lattice transformation in the process of collecting chlorination reaction gas. The specific implementation method is the same as that of embodiment 1, except that the frequency of the rotary valve is 20HZ, the frequency of the first rotary air lock valve and the second rotary air lock valve is 40HZ, and the flow rate of the transformed ultrafine powder is 500kg / h. The high-pressure gas is high-pressure nitrogen, and the atomization pressure is 1.2MPa. The mass ratio of the chlorination reaction gas to the atomized type I lattice thiophanate-methyl is 2:5. The temperature of the lattice transformation is 100°C, and the temperature of the type I lattice thiophanate-methyl product is 100°C.

[0074] Example 4

[0075] Embodiment 4 of the present invention provides a device and process for thiophanate-methyl lattice transformation in the process of collecting chlorination reaction gas. The specific implementation method is the same as that of embodiment 1, except that the frequency of the rotary valve is 30HZ, the frequency of the first rotary air lock valve and the second rotary air lock valve is 45HZ, and the flow rate of the transformed ultrafine powder is 600kg / h. The high-pressure gas is high-pressure nitrogen, and the atomization pressure is 1.3MPa. The mass ratio of the chlorination reaction gas to the atomized type I lattice thiophanate-methyl is 1:3. The temperature of the lattice transformation is 95°C, and the temperature of the type I lattice thiophanate-methyl product is 95°C.

[0076] Example 5

[0077] Embodiment 5 of the present invention provides a device and process for thiophanate-methyl lattice transformation in the process of collecting chlorination reaction gas. The specific implementation method is the same as that of embodiment 1, except that the frequency of the rotary valve is 40HZ, the frequency of the first rotary air lock valve and the second rotary air lock valve is 50HZ, and the flow rate of the transformed ultrafine powder is 800kg / h. The high-pressure gas is high-pressure nitrogen, and the atomization pressure is 1.5MPa. The mass ratio of the chlorination reaction gas to the atomized type I lattice thiophanate-methyl is 1:4. The temperature of the lattice transformation is 90°C, and the temperature of the type I lattice thiophanate-methyl product is 90°C.

[0078] Performance Testing

[0079] The type I lattice thiophanate-methyl product obtained in Examples 1-5 was sampled and analyzed. The results are shown in Tables 1, Figure 2 For the comparative XRD pattern of type II lattice thiophanate-methyl, see Figure 3 The characteristic diffraction peaks of the product Type I crystal lattice thiophanate-methyl were analyzed by X-ray diffraction. The characteristic diffraction peak 2-Theta of Type I crystal lattice thiophanate-methyl appeared at 25.5±0.2°, and the characteristic diffraction peak 2-Theta of Type II crystal lattice thiophanate-methyl appeared at 26.3±0.2°. The corresponding diffraction peaks of Type I and Type II thiophanate-methyl will appear during the detection process. When 2-Theta has the strongest diffraction peak at 25.5±0.2° and Area% reaches 100%, it means that the collected thiophanate-methyl is all Type I crystal lattice.

[0080] Table 1

[0081] Type I lattice Area% Type II lattice Area% Example 1 100 7.2 Example 2 100 7.3 Example 3 100 7.6 Example 4 100 6.5 Example 5 100 5.6

[0082] From the analysis of Table 1, we can see that:

[0083] (1) It can be seen from Examples 1 to 5 that the chlorothalonil lattice transformation production device for the chlorination reaction gas collection process provided by the present invention realizes the synchronous transformation of the chlorination reaction gas collection process, and finally obtains a Type I chlorothalonil product with a transformation rate of more than 99%.

[0084] (2) Based on Examples 1 to 5, it can be seen that the smaller the mass ratio of chlorothalonil gas to chlorothalonil powder is, the greater the mass of the ultrafinely ground atomized type I lattice chlorothalonil feed material is, and the more conducive it is to the collection, cooling and transformation of the high-temperature chlorination reaction gas.

[0085] (3) According to the embodiment, the entire process of ultrafine grinding, negative pressure conveying and high pressure atomization can ensure that the type I lattice thiophanate-methyl and the chlorination reaction gas collected to obtain thiophanate-methyl are continuously recycled in the entire system, ensuring the temperature and transformation effect of the collected materials. The cooling effect of the ultrafinely ground cold solid thiophanate-methyl in contact with the reaction gas after atomization exceeds that of the partition cooling water cooling.

[0086] In addition to the above embodiments, the present invention also includes other implementation modes. Any technical solution formed by equivalent transformation or equivalent replacement should fall within the protection scope of the claims of the present invention.

Claims

1. A chlorothalonil crystal transformation device in a chlorination reaction gas collection process, characterized in that: It at least includes a primary thin-walled material receiver, a secondary thin-walled material receiver, a primary screw conveyor, a secondary screw conveyor, a transformation silo, a rotary valve, an ultrafine grinder, and a tube chain conveyor. The primary thin-walled material receiver is provided with a primary gas phase inlet and a primary atomizing device at the upper end, a primary gas phase outlet is provided at the lower end to be connected with the secondary thin-walled material receiver, and a primary solid discharge port is provided at the lower end to be connected with the primary screw conveyor; the secondary thin-walled material receiver is provided with a secondary gas phase inlet and a secondary solid discharge port at the lower end, the secondary solid discharge port is connected with the secondary screw conveyor, and a secondary atomizing device and a secondary gas phase outlet are provided at the upper end; the primary screw conveyor and the secondary screw conveyor are both connected with the transformation silo, the discharge port of the transformation silo is connected with a rotary valve, and the outlet of the rotary valve is divided into two streams, one stream is connected with the ultrafine grinder and the tube chain conveyor in sequence, and the tube chain conveyor is respectively connected with the primary thin-walled material receiver and the secondary thin-walled material receiver; the other stream is connected with the transformation material storage system through a third rotary air lock valve.

2. The device for chlorothalonil crystal transformation in the chlorination reaction gas collection process according to claim 1, characterized in that: A cyclone separator is arranged between the ultrafine grinder and the tube chain conveyor, the top outlet of the cyclone separator is connected to the bag dust collector, the top outlet of the bag dust collector is connected to the induced draft fan, the bottom discharge port of the cyclone separator and the bottom discharge port of the bag dust collector are connected to the tube chain conveyor through the first rotary air lock valve and the second rotary air lock valve respectively.

3. The device for chlorothalonil crystal transformation in the chlorination reaction gas collection process according to claim 2, characterized in that: The ultrafine pulverizer is equipped with a classifier. After the ultrafine pulverizer pulverizes the transformation material, the particle size after pulverization is adjusted by the classifier through frequency conversion to obtain the transformation ultrafine powder.

4. The device for chlorothalonil crystal transformation in the chlorination reaction gas collection process according to claim 3, characterized in that: The first-stage thin-walled material receiver, the second-stage thin-walled material receiver, the first-stage screw conveyor and the second-stage screw conveyor are all provided with cooling elements outside.

5. A chlorothalonil lattice transformation process in the chlorination reaction gas collection process using the device according to claim 3 or 4, characterized in that: At least the following steps are included: S1: Manually put the transformation material into the transformation silo for the first time, control the frequency of the rotary valve to transport the transformation material to the ultrafine grinder through the discharge port of the transformation silo, and after the ultrafine grinder grinds the transformation material, the particle size after grinding is adjusted by the frequency conversion of the classifier to obtain the transformation ultrafine powder; S2: The transformation ultrafine powder is transported to the cyclone separator and the bag dust collector by the negative pressure of the induced draft fan, and the frequencies of the first rotary air lock valve and the second rotary air lock valve are controlled to transport the transformation ultrafine powder to the tube chain conveyor through the bottom discharge port of the cyclone separator and the bottom discharge port of the bag dust collector, and the transformation ultrafine powder is transported to the primary atomization equipment and the secondary atomization equipment by the tube chain conveyor, and the transformation ultrafine powder is sprayed and atomized by controlling the atomization pressure by high-pressure gas to obtain atomized type I lattice thiophanate-methyl; S3: The atomized Type I crystal lattice thiophanate-methyl enters the primary thin-walled material receiver and the secondary thin-walled material receiver, and the chlorination reaction gas is introduced into the primary thin-walled material receiver. The chlorination reaction gas passes through the primary thin-walled material receiver and then the secondary thin-walled material receiver, and contacts with the atomized Type I crystal lattice thiophanate-methyl to undergo lattice transformation and precipitate Type I crystal lattice thiophanate-methyl product; S4: Start the first-stage screw conveyor and the second-stage screw conveyor to transport the Type I lattice thiophanate-methyl product obtained in the first-stage thin-walled receiver and the second-stage thin-walled receiver to the transformation silo for recycling, thus establishing a material collection and transformation cycle.

6. The chlorothalonil lattice transformation process in the chlorination reaction gas collection process according to claim 5, characterized in that: The frequency of the rotary valve is 5-40HZ.

7. The chlorothalonil lattice transformation process in the chlorination reaction gas collection process according to claim 5, characterized in that: The frequencies of the first rotary air lock valve and the second rotary air lock valve are 30-50 Hz.

8. The chlorothalonil lattice transformation process in the chlorination reaction gas collection process according to claim 5, characterized in that: The high-pressure gas is high-pressure nitrogen, and the atomization pressure is 1.0-1.5 MPa.

9. The chlorothalonil lattice transformation process in the chlorination reaction gas collection process according to claim 5, characterized in that: The mass ratio of the chlorination reaction gas to the atomized type I lattice thiophanate-methyl is (1-2): (2-5).

10. The device for chlorothalonil crystal transformation in the chlorination reaction gas collection process according to claim 5, characterized in that: The temperature of the lattice transformation is 90-120°C.

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