CN111056537A - Spray reaction device for preparing insoluble sulfur by box-type closed cycle - Google Patents

Spray reaction device for preparing insoluble sulfur by box-type closed cycle Download PDF

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Publication number
CN111056537A
CN111056537A CN202010040782.7A CN202010040782A CN111056537A CN 111056537 A CN111056537 A CN 111056537A CN 202010040782 A CN202010040782 A CN 202010040782A CN 111056537 A CN111056537 A CN 111056537A
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China
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communicated
insoluble sulfur
cooling chamber
cooling
gas
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CN202010040782.7A
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Chinese (zh)
Inventor
蒋邦彦
王益庆
蒋中昕
王晓平
沈家锋
王凯
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Jiangsu Aidi Intelligent Equipment Co ltd
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Changzhou Lingyu Drying Engineering Co Ltd
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Priority to CN202010040782.7A priority Critical patent/CN111056537A/en
Publication of CN111056537A publication Critical patent/CN111056537A/en
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    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B17/00Sulfur; Compounds thereof
    • C01B17/02Preparation of sulfur; Purification
    • C01B17/12Insoluble sulfur (mu-sulfur)

Abstract

The invention discloses a box-type spray reaction device for preparing insoluble sulfur in a closed cycle manner, and relates to the technical field of preparation equipment for insoluble sulfur for rubber tires and rubber products. The inert gas can effectively reduce the oxidation of the sulfur and improve the product quality. The quenching section process effectively restrains the reverse reaction, thereby directly influencing the content of insoluble sulfur in the product. The insoluble sulfur is obtained by adopting a low-temperature melting reaction method, the process is environment-friendly, and the spray reaction equipment can play a role in saving resources and reducing cost, and has good market prospect.

Description

Spray reaction device for preparing insoluble sulfur by box-type closed cycle
Technical Field
The invention relates to the technical field of preparation equipment of insoluble sulfur for rubber tires and rubber products, in particular to a spray reaction device for preparing insoluble sulfur in a box-type closed cycle manner.
Background
The spray reaction equipment is an advanced novel high-efficiency process equipment, and is characterized in that an atomizer is utilized to atomize solution, emulsion, pasty liquid and suspension liquid materials, micronized fog drops have extremely large surface area, and the materials are promoted to carry out drying, decomposition or cracking reaction under a certain high-temperature atmosphere condition to produce required powdery products or generate brand new materials. The lithium iron phosphate is widely applied to liquids, suspensions and viscous fluids in the fields of petrochemical industry, aviation industry and military industry at present, such as superconducting materials, lithium iron phosphate, graphite, propellants, negative electrode materials, petroleum catalysts, medicines and the like; can also be used for lithium battery materials, intermediates and inorganic salt products, and is ideal process equipment in the industries of chemical engineering, new energy, advanced materials and the like.
With the rapid development of the automobile industry in China, the annual output of tires is increased year by year, and the demand of sulfur as a main vulcanizing agent of rubber is increased year by year.
However, the solubility of ordinary sulfur in rubber is limited, and the solubility of the ordinary sulfur increases with the increase of temperature in the rubber mixing process, and precipitates in a crystalline form on the surface of the rubber compound when the temperature is reduced, so that the ordinary sulfur migrates to the surface of the rubber compound, namely, the phenomenon of so-called 'blooming' in the production of tires and rubber products is formed, the appearance of the products is seriously influenced, and the adhesiveness of the products is reduced.
In order to solve the problems of common sulfur blooming and the like, an Insoluble Sulfur (IS) product IS produced due to transportation, the Insoluble Sulfur (IS) IS a linear long-chain high-molecular polymer for deep processing of sulfur (S), the number of sulfur atoms on a molecular chain IS up to more than 108, and the insoluble sulfur IS insoluble in carbon disulfide, so that the insoluble sulfur IS called as the insoluble sulfur at present, the IS IS a recognized optimal rubber vulcanizing agent with the characteristic of no blooming, and the insoluble sulfur has the advantages that ① enables a rubber material to have good self-adhesiveness, can improve the adhesive strength among layers of a multi-layer rubber product, particularly can improve the adhesive property of a steel wire and rubber during manufacturing of a tire, ② insoluble sulfur IS uniformly distributed in the rubber material, effectively reduces the phenomenon of scorching during storage of the rubber material, prolongs the storage period of the rubber material, ensures uniform vulcanization, improves the quality of the rubber product, does not migrate to the surface of the rubber material to generate blooming due to the insoluble sulfur, ensures the appearance quality of a light-color product.
For technical reasons, insoluble sulfur products produced by domestic enterprises have the problems of low purity, high ash content, poor heat resistance and the like, and the difference is still larger compared with products of companies such as Flexsys and the like abroad.
Although the insoluble sulfur has outstanding performance, the technology for producing the insoluble sulfur at home and abroad has the problems of high production cost, high energy consumption, serious equipment corrosion, easy accident generation due to high pressure, instability in the storage process of the insoluble sulfur, easy conversion into common sulfur and the like. Therefore, in recent years, development of new environmentally-friendly and safe insoluble sulfur production processes is also sought, but at present, most of the new processes are still in the laboratory stage, and industrialization is not realized.
The key technology of gasification or melting is the selection of stabilizer, the determination of quench liquid and quench mode. However, most manufacturers and some Chinese patents in China adopt a method of using water as quenching liquid, and some Chinese patents also adopt a method of matching carbon disulfide and a composite stabilizer in different proportions. The insoluble sulfur produced by using water as a quenching liquid has poor dispersibility, high-temperature thermal stability cannot meet the requirements of radial tires, the amount of wastewater in the production process is large, and the environmental protection problem is prominent, and Chinese patent 01101968.9 specially provides a production method of melting anhydrous insoluble sulfur. The insoluble sulfur produced by using carbon disulfide as quenching liquid can basically meet the requirements of radial tires, but the boiling point is only 42.7 ℃, the flash point is-30 ℃, and the production process is extremely inflammable and explosive. The method for preparing insoluble sulfur by atomization is mentioned in Chinese patent 201310511371.1 and Chinese patent 201310511388.7, but the method is only an explanation on the process and does not mention a specific reaction device.
In addition, the liquid flow is quenched basically in a pouring mode or a dropping mode, the quenching effect is poor, the conversion rate is low, and the reason why the insoluble sulfur content produced by the melting method is lower than that produced by the gasification method is also provided. Meanwhile, the generated insoluble sulfur crude product is blocky or granular and is not easy to crush after being solidified.
Disclosure of Invention
In order to solve the technical problems, the invention provides a box-type spray reaction device for preparing insoluble sulfur in a closed cycle manner, which can complete two processes of high-temperature ring-opening reaction and low-temperature crystallization of sulfur by one device.
In order to achieve the purpose, the invention provides the following scheme:
the invention provides a box-type spray reaction device for preparing insoluble sulfur in a closed cycle manner, which comprises a melting system, a feeding system, a high-temperature reaction furnace, a cooling chamber, a separation system, a gas analysis system, a cooling system, a pressure balance system and a discharging system, wherein the feeding system is connected with the high-temperature reaction furnace; the outlet end of the melting system is communicated with the inlet end of the feeding system, the outlet end of the feeding system is provided with an atomizing nozzle, the atomizing nozzle is communicated with the high-temperature reaction furnace, the high-temperature reaction furnace is communicated with the cooling chamber, and the outlet end of the cooling system is communicated with the inside of the cooling chamber; the bottom of the cooling chamber is provided with the discharging system, the inlet end of the separating system is communicated with the cooling chamber, and the gas outlet end of the separating system is communicated with the inlet end of the cooling system; and the gas analysis system and the pressure balance system are arranged between the gas outlet end of the separation system and the inlet end of the cooling system.
Optionally, the cooling system includes a fan, a heat exchanger, a filter and a gas distributor which are sequentially communicated; the inlet end of the fan is communicated with the gas outlet end of the separation system; the gas distributor is used for introducing cooling gas into the cooling chamber.
Optionally, the separation system includes a separator and a tail gas purifier, the inlet end of the separator is communicated with the cooling chamber, the gas outlet end of the separator is communicated with the tail gas purifier, and the gas outlet end of the tail gas purifier is communicated with the inlet end of the fan.
Optionally, the cooling chamber is of a box-type structure, a cleaning device is arranged at the bottom in the box-type structure, the high-temperature reaction furnace is arranged on one side of the cooling chamber, and the gas distributor is arranged between the high-temperature reaction furnace and the cooling chamber; the discharging system is arranged at the bottom of the other side of the cooling cavity.
Optionally, the separation system comprises an exhaust purifier.
Optionally, the discharging system is a quantitative discharging device or a spiral discharging device.
Compared with the prior art, the invention has the following technical effects:
(1) the insoluble sulfur spray reaction device has high stability, and the process characteristics are suitable for large-scale industrialized and continuous production.
(2) The insoluble sulfur spray reaction device relies on the traditional spray drying mechanism and has high feasibility.
(3) The production process of the insoluble sulfur has high safety, is environment-friendly and does not discharge three wastes.
(4) The product has high stability, can effectively improve the thermal stability, and does not have the blooming phenomenon in rubber compound.
(5) The insoluble sulfur product prepared by the invention can be uniformly distributed in the rubber material, effectively reduces scorching of the rubber material during storage, prolongs the storage period of the rubber material and improves the quality of rubber products.
(6) The product has outstanding comprehensive performance, improves the self-adhesiveness of rubber materials, improves the adhesive property of steel wires and rubber during manufacturing tires, and endows rubber products with good comprehensive performance.
(7) The process reduces the high requirement of insoluble sulfur on equipment in production and the high risk in the subsequent treatment process.
(8) The insoluble sulfur product prepared by the invention has high quality stability, strong market competitiveness and good economic benefit.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings needed in the embodiments will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art to obtain other drawings without creative efforts.
FIG. 1 is a schematic structural diagram of a spray reaction device for preparing insoluble sulfur by a box-type closed cycle of the present invention;
FIG. 2 is a schematic sectional view of a linear laminar flow air-homogenizing gas distributor in a spray reaction device for preparing insoluble sulfur by closed cycle according to the present invention;
FIG. 3 is a schematic top view of a linear laminar flow air-homogenizing distributor in a spray reactor for producing insoluble sulfur by closed cycle according to the present invention;
FIG. 4 is a schematic structural diagram of a volute type gas distributor in a spray reaction device for preparing insoluble sulfur by closed cycle according to the present invention.
Description of reference numerals: 1. a melting system; 2. a feed pump; 3. an atomizing spray head; 4. a high-temperature reaction furnace; 5. a gas distributor; 6. a cooling chamber; 7. a cleaning device; 8. a tail gas purifier; 9. a gas analysis system; 10. a fan; 11. a heat exchanger; 12. a filter; 14. a pressure equalization system; 15. a discharge system; 16. laminar flow orifice plates.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The first embodiment is as follows:
as shown in fig. 1, the present embodiment provides a box-type spray reaction apparatus for preparing insoluble sulfur by closed cycle, which includes a melting system 1, a feeding system, a high-temperature reaction furnace 4, a cooling chamber 6, a separation system, a gas analysis system 9, a cooling system, a pressure balancing system 14, and a discharging system 15; the outlet end of the melting system 1 is communicated with the inlet end of the feeding system, the outlet end of the feeding system is provided with an atomizing nozzle 3, the atomizing nozzle 3 is communicated with the high-temperature reaction furnace 4, the high-temperature reaction furnace 4 is communicated with the cooling chamber 6, and the outlet end of the cooling system is communicated with the inside of the cooling chamber 6; the discharging system 15 is arranged at the bottom of the cooling chamber 6, the inlet end of the separation system is communicated with the cooling chamber 6, and the gas outlet end of the separation system is communicated with the inlet end of the cooling system; the gas analysis system 9 and the pressure equalization system 14 are arranged between the gas outlet end of the separation system and the inlet end of the cooling system.
In this embodiment, as shown in fig. 1, the cooling system includes a fan 10, a heat exchanger 11, a filter 12 and a gas distributor 5, which are sequentially connected; the inlet end of the fan 10 is communicated with the gas outlet end of the separation system; the gas distributor 5 is used for introducing cooling gas into the cooling chamber 6.
The cooling chamber 6 is of a box type structure, a cleaning device 7 is arranged at the bottom in the box type structure, the high-temperature reaction furnace 4 is arranged on one side of the cooling chamber 6, and the gas distributor 5 is arranged between the high-temperature reaction furnace 4 and the cooling chamber 6; the discharging system 15 is arranged at the bottom of the other side of the cooling chamber 6. The separation system includes an exhaust purifier 8.
Cleaning device 7 includes the chain of two parallel settings, two chains set up in the both sides of bottom in the box formula structure are provided with a plurality of scrapers between two chains, the both ends of scraper blade are connected with the chain of one side respectively, and the chain is by motor drive, and the chain rotates the in-process and drives the solid particle that the scraper blade will drop the box formula structure bottom and push away discharge system 15 and discharge.
The discharge system 15 includes a quantitative discharge device, and may also be a spiral discharge device.
The spraying reaction device for preparing insoluble sulfur by box-type closed cycle in the embodiment mainly comprises the following working processes:
the material is melted in the melting system 1, and the melted material is sprayed into the high-temperature reaction furnace 4 through the feeding pump 2 and the atomizing nozzle 3, the high-temperature reaction furnace 4 is communicated with the cooling chamber 6, the material entering the cooling chamber 6 is rapidly cooled into solid particles by cooling gas from the gas distributor 5, the solid particles fall onto the cleaning device 7 at the bottom of the cooling chamber 6 and are discharged through the discharging system 15, a small amount of the solid particles enter the tail gas purifier 8 along with gas flow, the clean gas is discharged from the top and enters the cooling system through the dust removing cloth bag, and the solid particles remained in the tail gas purifier 8 are discharged from the bottom; in the cooling system, the air flow passes through a fan 10, a heat exchanger 11 and a filter 12 in sequence, and finally flows into the cooling chamber 6 through the gas distributor 5.
The gas analysis system 9 arranged between the tail gas purifier 8 and the fan 10 can analyze the components in the circulating gas flow, mainly detecting the oxygen concentration, thereby being convenient for the operators to adjust the materials and the gas introduced into the system.
The pressure balancing system 14 includes a safety valve, i.e. an automatic pressure relief valve, for controlling the gas pressure in the system, preventing the gas pressure from being too large to affect the operation of the device, and ensuring safe production.
The whole process of the spray reaction device for preparing the insoluble sulfur in a box-type closed cycle mode comprises the steps of utilizing the atomization process of the spray drying reaction device to carry out rapid reaction and utilizing cold nitrogen to carry out rapid cooling on the insoluble sulfur, effectively inhibiting the reverse reaction from being carried out, and avoiding the method of obtaining the insoluble sulfur by using inflammable and explosive carbon disulfide as an extracting agent. In the production process of insoluble sulfur by adopting a spray drying reaction device, quenching is one of very critical processes, plays a role in instantly terminating a reversible reaction, and further directly influences the content of the insoluble sulfur in a product. The required raw materials are simple and easy to obtain, the process is environment-friendly and pollution-free, and good social and economic benefits are achieved.
The spray reaction equipment atomizes certain liquid materials by using an atomizer, and micronized fog drops have extremely large surface area, promote the materials to generate drying, decomposition or cracking reaction under certain high-temperature atmosphere conditions, and are the most widely applied process in high-end new material industries. It is especially suitable for preparing powdery and granular solid products from solution, emulsion, suspension and pasty liquid raw materials. Therefore, the sulfur can be melted at high temperature and solidified at low temperature, when the sulfur is in a melting state above 120 ℃, the sulfur can be sprayed into a reaction chamber above 200 ℃ by adopting a spraying process, the sulfur can be subjected to polymerization reaction above the temperature to obtain polymeric sulfur, a cooling device is added at the rear part of the device, the polymeric sulfur can be rapidly cooled to below 60 ℃, so that the polymeric sulfur is converted into insoluble sulfur, the conversion rate of the sulfur is improved, and the use of inflammable and explosive carbon disulfide as a solvent is avoided, and the process has the characteristics of environmental friendliness and the like.
The device of the invention is used for preparing insoluble sulfur, and gases such as inert gas, superheated steam and the like are adopted to effectively reduce the oxidation of sulfur and improve the product quality. The quenching section process effectively restrains the reverse reaction, thereby directly influencing the content of insoluble sulfur in the product. The obtained product has the performance reaching the product level of companies such as Flexsys and the like abroad, has environment-friendly process, can play the roles of saving resources and reducing cost, and has good market prospect.
The principle and the implementation mode of the present invention are explained by applying specific examples in the present specification, and the above descriptions of the examples are only used to help understanding the method and the core idea of the present invention; meanwhile, for a person skilled in the art, according to the idea of the present invention, the specific embodiments and the application range may be changed. In view of the above, the present disclosure should not be construed as limiting the invention.

Claims (6)

1. A box-type spray reaction device for preparing insoluble sulfur in a closed cycle manner is characterized by comprising a melting system, a feeding system, a high-temperature reaction furnace, a cooling chamber, a separation system, a gas analysis system, a cooling system, a pressure balance system and a discharging system; the outlet end of the melting system is communicated with the inlet end of the feeding system, the outlet end of the feeding system is provided with an atomizing nozzle, the atomizing nozzle is communicated with the high-temperature reaction furnace, the high-temperature reaction furnace is communicated with the cooling chamber, and the outlet end of the cooling system is communicated with the inside of the cooling chamber; the bottom of the cooling chamber is provided with the discharging system, the inlet end of the separating system is communicated with the cooling chamber, and the gas outlet end of the separating system is communicated with the inlet end of the cooling system; and the gas analysis system and the pressure balance system are arranged between the gas outlet end of the separation system and the inlet end of the cooling system.
2. The spray reactor apparatus for preparing insoluble sulfur according to claim 1, wherein the cooling system comprises a blower, a heat exchanger, a filter and a gas distributor which are communicated in sequence; the inlet end of the fan is communicated with the gas outlet end of the separation system; the gas distributor is used for introducing cooling gas into the cooling chamber.
3. The spray reactor apparatus according to claim 2, wherein the separation system comprises a separator and an exhaust gas purifier, the inlet of the separator is communicated with the cooling chamber, the gas outlet of the separator is communicated with the exhaust gas purifier, and the gas outlet of the exhaust gas purifier is communicated with the inlet of the fan.
4. The spray reaction device for preparing insoluble sulfur through the box-type closed cycle according to claim 2, wherein the cooling chamber is of a box-type structure, a cleaning device is arranged at the bottom in the box-type structure, the high-temperature reaction furnace is arranged at one side of the cooling chamber, and the gas distributor is arranged between the high-temperature reaction furnace and the cooling chamber; the discharging system is arranged at the bottom of the other side of the cooling cavity.
5. The spray reactor apparatus for closed loop insoluble sulfur production according to claim 4 wherein said separation system comprises an exhaust gas purifier.
6. The spray reactor apparatus for preparing insoluble sulfur according to claim 1, wherein the discharge system is a quantitative discharge device or a spiral discharge device.
CN202010040782.7A 2020-01-15 2020-01-15 Spray reaction device for preparing insoluble sulfur by box-type closed cycle Pending CN111056537A (en)

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Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB727206A (en) * 1952-04-28 1955-03-30 Bayer Ag Production of carbon disulphide-insoluble sulphur
CN103539078A (en) * 2013-10-25 2014-01-29 北京化工大学 Method for preparation of insoluble sulfur
CN103539079A (en) * 2013-10-25 2014-01-29 北京化工大学 Method for one-step preparation of insoluble sulfur
CN105688778A (en) * 2016-03-29 2016-06-22 常州市先导干燥设备有限公司 Closed-cycle high-temperature airflow reaction device
CN106744707A (en) * 2017-03-06 2017-05-31 杨松 One kind prepares insoluble sulfur process unit
CN207435026U (en) * 2017-11-14 2018-06-01 浙江海洋大学 A kind of insoluble sulfur quenching device with quick chilling atomizing

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB727206A (en) * 1952-04-28 1955-03-30 Bayer Ag Production of carbon disulphide-insoluble sulphur
CN103539078A (en) * 2013-10-25 2014-01-29 北京化工大学 Method for preparation of insoluble sulfur
CN103539079A (en) * 2013-10-25 2014-01-29 北京化工大学 Method for one-step preparation of insoluble sulfur
CN105688778A (en) * 2016-03-29 2016-06-22 常州市先导干燥设备有限公司 Closed-cycle high-temperature airflow reaction device
CN106744707A (en) * 2017-03-06 2017-05-31 杨松 One kind prepares insoluble sulfur process unit
CN207435026U (en) * 2017-11-14 2018-06-01 浙江海洋大学 A kind of insoluble sulfur quenching device with quick chilling atomizing

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Effective date of registration: 20220908

Address after: No. 30, Zhennan Road, Xiaoji Town, Jiangdu District, Yangzhou City, Jiangsu Province, 225000

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Application publication date: 20200424