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CN-121972114-A - Chlorosulfonic acid preparation system and method based on plasma pretreatment sulfur

CN121972114ACN 121972114 ACN121972114 ACN 121972114ACN-121972114-A

Abstract

The invention relates to the technical field of chlorosulfonic acid preparation, in particular to a chlorosulfonic acid preparation system and a chlorosulfonic acid preparation method based on plasma pretreatment sulfur, wherein an air inlet of a plasma reactor is connected with an inert gas pipeline, a feed inlet of the plasma reactor is connected with a feed pipeline, and a discharge outlet of the plasma reactor is connected with a feed inlet of a reaction kettle through a discharge pipeline; the discharge port of the reaction kettle is connected with the feed inlet of the heat exchanger, the discharge port of the heat exchanger is connected with the feed inlet of the rectifying tower, and the discharge port of the rectifying tower is connected with the chlorosulfonic acid pipeline. According to the method, the sulfur is pretreated by the plasma, the low-temperature plasma is utilized to bombard and activate the surface of the sulfur, so that the reactivity of the sulfur is effectively improved, the subsequent synthesis reaction with chlorine is more complete, and the preparation efficiency and the product purity of chlorosulfonic acid are remarkably improved.

Inventors

  • LI YAWEN
  • FENG YONGJUN
  • PEI YINGGE
  • ZHANG WENXUE
  • LIU YING
  • WU YUANMIN

Assignees

  • 金川集团股份有限公司
  • 金川集团化工新材料有限责任公司

Dates

Publication Date
20260505
Application Date
20251228

Claims (7)

  1. 1. A chlorosulfonic acid preparation system based on plasma pretreatment sulfur is characterized by comprising a plasma reactor (1), an inert gas pipeline (3), a drying tower (5), a chlorine pipeline (5 a), a filter (6), a reaction kettle (7), a heat exchanger (9), a rectifying tower (10), a chlorosulfonic acid pipeline (10 a), a recovery pipe (10 b) and a chlorine pump (11), wherein the air inlet of the plasma reactor (1) is connected with the inert gas pipeline (3), the feed inlet of the plasma reactor (1) is connected with the feed pipeline, the discharge outlet of the plasma reactor (1) is connected with the feed inlet of the reaction kettle (7) through the discharge pipeline, the air inlet of the drying tower (5) is connected with the chlorine pipeline (5 a), the air outlet of the drying tower (5) is connected with the air inlet of the filter (6), the air outlet of the filter (6) is connected with the air inlet of the reaction kettle (7), the discharge outlet of the reaction kettle (7) is connected with the feed inlet of the heat exchanger (9), the discharge outlet of the heat exchanger (9) is connected with the feed inlet of the rectifying tower (10) through the discharge pipe (10 a), the chlorine pump (10) is connected with the discharge outlet of the rectifying tower (10), the output end of the chlorine pump (11) is connected with the air inlet of the reaction kettle (7).
  2. 2. The chlorosulfonic acid preparation system based on the plasma pretreatment sulfur according to claim 1, wherein a feeding device (4) is arranged on the feeding pipeline, and a discharging device (8) is arranged on the discharging pipeline.
  3. 3. The chlorosulfonic acid production system based on plasma pretreatment sulfur according to claim 1, wherein the plasma reactor (1) is connected with a power supply system (2).
  4. 4. The chlorosulfonic acid preparation system based on the plasma pretreatment sulfur according to claim 1, wherein a stirring device is arranged in the reaction kettle (7), and stirring blades of the stirring device are of an anchor type, a paddle type or a push type structure.
  5. 5. The chlorosulfonic acid production system based on plasma pretreatment sulfur according to claim 1, wherein a drying agent is filled in the drying tower (5), and the drying agent is one of anhydrous calcium chloride, silica gel or molecular sieve.
  6. 6. The chlorosulfonic acid production system based on the plasma pretreatment sulfur according to claim 1, wherein the inert gas conveyed by the inert gas pipeline (3) is one or more mixed gases of nitrogen, argon or helium.
  7. 7. A method for preparing chlorosulfonic acid based on plasma pretreated sulfur using the system of any one of claims 1-6, comprising the steps of: Firstly, pretreating the sulfur powder in a plasma reactor (1), introducing inert gas through an inert gas pipeline (3), supplying power to the plasma reactor (1) by a power supply system (2) to generate low-temperature plasma, and carrying out bombardment activation on the surface of the sulfur to obtain pretreated sulfur, wherein the flow rate of the inert gas in the plasma pretreatment is 100-300mL/min, the pressure is 0.1-0.3MPa, the plasma power is 50-150W, the treatment time is 10-30 min, and the temperature is 40-60 ℃; Step two, a synthesis reaction, namely conveying the pretreated sulfur obtained in the step one to a reaction kettle (7) through a discharge pipeline and a discharge device (8), introducing chlorine into a drying tower (5) through a chlorine pipeline (5 a) for drying, purifying the chlorine through a filter (6), introducing the purified chlorine into the reaction kettle (7), mixing the pretreated sulfur and the chlorine in the reaction kettle (7) according to a molar ratio of 1:1.02-1.08, and stirring the mixture by a stirring device for reaction, wherein the reaction temperature in the reaction kettle (7) is 180-220 ℃, and the reaction pressure is 0.3-0.5MPa; And thirdly, condensing and recycling, namely conveying product steam generated by the reaction to a heat exchanger (9) from a discharge hole of a reaction kettle (7), cooling, separating the cooled material in a rectifying tower (10), collecting finished chlorosulfonic acid through a chlorosulfonic acid pipeline (10 a), conveying unreacted chlorine to a chlorine pump (11) through an air outlet of the rectifying tower (10) and a recycling pipe (10 b), pressurizing by the chlorine pump (11), and recycling to the reaction kettle (7), wherein the temperature of the heat exchanger (9) is between-10 ℃ and 0 ℃.

Description

Chlorosulfonic acid preparation system and method based on plasma pretreatment sulfur Technical Field The invention relates to the technical field of chlorosulfonic acid preparation, in particular to a chlorosulfonic acid preparation system and method based on plasma pretreatment sulfur. Background Chlorosulfonic acid is an important basic chemical raw material, and is widely applied to organic synthesis industries such as dyes, medicines, pesticides, saccharin, detergents and the like, and is mainly used as a sulfonating agent and a chlorosulfonating agent. With the rapid development of the fine chemical industry, the demand of chlorosulfonic acid in the market is continuously increasing, and meanwhile, the green, low energy consumption and high quality requirements of the production process are also increasingly stringent. Currently, the mainstream process for industrially preparing chlorosulfonic acid is realized by directly combining hydrogen chloride gas with sulfur trioxide in liquid phase or gas phase. Chinese patent CN101100289A discloses a typical mainstream synthesis method, which adopts liquid sulfur trioxide with concentration higher than 99% to react with dry hydrogen chloride in a reaction tower, and has the advantage of relatively simple equipment structure, but has obvious technical shortboards that the reaction process is a strong exothermic reaction, the requirement on temperature control precision is extremely high, and once the temperature fluctuation is easy to cause product decomposition or side reaction, meanwhile, the process is severely dependent on high-purity sulfur trioxide and hydrogen chloride raw materials, the purification and preparation links of the raw materials increase the overall production cost, and the economy of large-scale application of the process is limited. In addition to the main flow route, the direct chlorination of sulfur is used for preparing sulfur-containing chlorides (such as sulfur monochloride, sulfur dichloride and the like), and the sulfur-containing chlorides are used as a source for synthesizing chlorosulfonic acid or a precursor thereof for reaction, so that the method is another important technical path. However, in the traditional chlorination reaction using sulfur as a starting material, sulfur molecules (S 8) have a stable annular structure, and have strong chemical property and inertia at normal temperature, so that the reaction kinetic resistance of the sulfur molecules and chlorine is high, and the reaction activity is insufficient. The prior art generally needs to maintain the reaction temperature above 200 ℃ and match with high pressure conditions to achieve the ideal reaction rate and conversion rate. The high-temperature high-pressure operation mode not only ensures that the energy consumption of a unit product is up to 1.5kWh/kg and greatly increases the production cost, but also can aggravate the corrosion of reaction equipment, promote the occurrence of side reactions and influence the purity of the product. In addition, the recycling rate of the traditional technology to the unreacted chlorine is lower, and the traditional technology is mostly treated by adopting a simple liquid seal or alkali liquor absorption mode, so that not only is the waste of raw materials caused, but also chlorine-containing and sulfur-containing waste gas emission is easy to generate, and the traditional technology does not meet the current increasingly strict environmental protection standard. In recent years, low-temperature plasma technology has been applied to the surface activation treatment of sulfur powder as an efficient material surface modification means. Related researches show that the surface defects and active sites of the sulfur powder can be obviously increased by non-thermal plasma treatment, and the reactivity is improved. However, in the prior art, no disclosure has been made on applying the plasma activation technology to the chemical synthesis reaction of chlorosulfonic acid or its precursor, and the core problems of low reactivity and high production energy consumption of sulfur raw materials cannot be solved by means of the technology. Disclosure of Invention Aiming at the problems in the prior art, the invention provides a chlorosulfonic acid preparation system and a chlorosulfonic acid preparation method based on plasma pretreatment sulfur. In order to achieve the above purpose, the technical scheme of the invention is as follows: a chlorosulfonic acid preparation system based on plasma pretreatment sulfur comprises a plasma reactor, an inert gas pipeline, a drying tower, a chlorine pipeline, a filter, a reaction kettle, a heat exchanger, a rectifying tower, a chlorosulfonic acid pipeline, a recovery pipe and a chlorine pump, wherein an air inlet of the plasma reactor is connected with the inert gas pipeline, a feed inlet of the plasma reactor is connected with the feed inlet of the reaction kettle through the discharge pipeline, an