WO2021047044A1 - 一种基于蒽醌法制备双氧水的系统及工艺 - Google Patents

一种基于蒽醌法制备双氧水的系统及工艺 Download PDF

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WO2021047044A1
WO2021047044A1 PCT/CN2019/120126 CN2019120126W WO2021047044A1 WO 2021047044 A1 WO2021047044 A1 WO 2021047044A1 CN 2019120126 W CN2019120126 W CN 2019120126W WO 2021047044 A1 WO2021047044 A1 WO 2021047044A1
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tower
hydrogenation
micro
liquid
gas
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PCT/CN2019/120126
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English (en)
French (fr)
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张志炳
黄传峰
周政
张锋
李磊
孟为民
王宝荣
杨高东
罗华勋
杨国强
田洪舟
曹宇
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南京延长反应技术研究院有限公司
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Publication of WO2021047044A1 publication Critical patent/WO2021047044A1/zh

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    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B15/00Peroxides; Peroxyhydrates; Peroxyacids or salts thereof; Superoxides; Ozonides
    • C01B15/01Hydrogen peroxide
    • C01B15/022Preparation from organic compounds
    • C01B15/023Preparation from organic compounds by the alkyl-anthraquinone process
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D47/00Separating dispersed particles from gases, air or vapours by liquid as separating agent
    • B01D47/02Separating dispersed particles from gases, air or vapours by liquid as separating agent by passing the gas or air or vapour over or through a liquid bath

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  • the invention relates to the technical field of hydrogen peroxide preparation by an anthraquinone method, in particular to a system and process for preparing hydrogen peroxide based on an anthraquinone method.
  • Hydrogen peroxide is an aqueous solution of hydrogen peroxide (H 2 O 2 ). It is an important inorganic peroxide. It has the characteristics of oxidizing, bleaching, and environmental protection during use. It can be used in fabrics, pulp decolorization, chemical synthesis, and wastewater. In processing, medical, metallurgy, military, food processing and other fields, it acts as an oxidant, bleaching agent, disinfectant, polymer initiator and crosslinking agent, propellant, etc. With the increasingly stringent environmental regulations, the production capacity of products such as propylene oxide and green caprolactam by the hydrogen peroxide direct oxidation method (HPPO method) has increased, resulting in a strong market demand for H 2 O 2.
  • HPPO method hydrogen peroxide direct oxidation method
  • the production methods of hydrogen peroxide include anthraquinone method, electrolysis method, isopropanol oxidation method, inorganic reaction method, hydrogen and oxygen direct synthesis method and so on.
  • the anthraquinone method is currently the mainstream method for producing hydrogen peroxide at home and abroad.
  • the anthraquinone hydrogen peroxide production process uses 2-ethylanthraquinone (EAQ) as a carrier, heavy aromatic hydrocarbons (AR) and trioctyl phosphate (TOP) as mixed solvents, and is formulated into a solution with a certain composition (working fluid)
  • EAQ 2-ethylanthraquinone
  • AR heavy aromatic hydrocarbons
  • TOP trioctyl phosphate
  • the anthraquinone method is mainly divided into four processes: hydrogenation, oxidation, extraction, and post-treatment.
  • hydrogenation is a key step in the production of hydrogen peroxide by the anthraquinone method.
  • the activity and selectivity of the anthraquinone hydrogenation catalyst largely determine the efficiency and unit consumption of the hydrogenation process.
  • a hydrogenation catalyst with high activity and high selectivity can increase the yield of hydrogen peroxide, reduce the degradation of anthraquinone, reduce production costs, and create Better economic efficiency.
  • Chinese Patent Publication No.: CN106395755A discloses a method for preparing hydrogen peroxide by the anthraquinone method.
  • a working fluid containing anthraquinone derivatives and hydrogen in the fiber catalyst in the fiber catalyst reactor contact, in the fiber catalyst Under the action of the active components, it reacts to generate hydrogenation liquid; then the alkylhydroanthraquinone is oxidized by air to generate an oxidizing liquid containing hydrogen peroxide and alkylanthraquinone, and then the hydrogen peroxide in the oxidizing liquid is extracted with water, and the hydrogen peroxide is purified and concentrated to a certain extent.
  • the concentration of hydrogen peroxide product, the working solution containing alkyl anthraquinone after extraction is recycled. It can be seen that the method has the following problems:
  • the method only introduces air through an air distributor, and oxidizes the alkylhydroanthraquinone through the air to generate an oxidizing solution containing hydrogen peroxide and alkylanthraquinone.
  • the volume of the bubbles is too large to be fully compatible with the alkylhydroanthraquinone. Contact reduces the reaction efficiency of the system.
  • the present invention provides a system and process for preparing hydrogen peroxide based on the anthraquinone method to overcome the problem of low system reaction efficiency caused by uneven mixing of materials in the prior art and resulting by-products.
  • the present invention provides a system for preparing hydrogen peroxide based on the anthraquinone method, including:
  • the hydrogenation tower is used to provide a reaction place for the working liquid containing anthraquinone derivatives and hydrogen;
  • the micro-interface generator is equipped with a hydrogenation tower to provide a reaction place for the working liquid containing anthraquinone derivatives and hydrogen;
  • a filtering and cooling unit which is arranged on the side wall of the hydrogenation tower to filter and cool the hydrogenated material output from the hydrogenation tower;
  • the oxidation tower is connected to the filtering and cooling unit, and is used to provide a reaction place for the material output by the filtering and cooling unit and oxygen;
  • the extraction tower is used to extract and separate the materials output from the oxidation tower
  • a micro-interface generator which is set at a designated position in the hydrogenation tower and the oxidation tower, converts the pressure energy of the gas and/or the kinetic energy of the liquid into the surface energy of the bubbles and transfers it to the hydrogen, so that the hydrogen is broken to form a diameter of ⁇ 1 ⁇ m , And ⁇ 1mm micron-level bubbles to increase the mass transfer area between the anthraquinone derivative-containing working fluid and hydrogen, reduce the thickness of the liquid film, reduce the mass transfer resistance, and combine the anthraquinone derivative-containing working fluid with the micron after being broken
  • the gas-liquid emulsion is formed by mixing the first-stage bubbles to enhance the mass transfer efficiency and reaction efficiency between the anthraquinone derivative-containing working liquid and hydrogen within the preset operating conditions.
  • micro-interface generator includes:
  • the first micro-interface generator which is arranged at the bottom of the reaction zone of the hydrogenation tower, is used to crush hydrogen gas to form micro-scale micro-scale bubbles and output the micro-scale bubbles to the hydrogenation tower after the crushing is completed , And mixed with the anthraquinone derivative working liquid in the hydrogenation tower to form a gas-liquid emulsion;
  • the second micro-interface generator which is arranged at the bottom of the reaction zone of the oxidation tower, is used to crush oxygen to form micro-scale micro-scale bubbles and output the micro-scale bubbles to the hydrogenation tower after the crushing is completed , And mixed with the 2-ethylhydroanthraquinone solution in the oxidation tower to form a gas-liquid emulsion.
  • the hydrogenation tower includes:
  • a hydrogen feed pipeline which is arranged on the side wall of the hydrogenation tower and is connected to the first micro-interface generator, and is used to transport hydrogen to the first micro-interface generator so that the first micro-interface generator can break the hydrogen ;
  • the working fluid feed pipe is arranged on the side wall of the hydrogen tower and above the hydrogen feed pipe, and is used to transport the working fluid containing anthraquinone derivatives to the inside of the hydrogenation tower;
  • a catalyst feed port which is arranged on the side wall of the hydrogenation tower and above the working fluid feed pipe, and is used to put the catalyst into the hydrogenation tower;
  • the first tail gas outlet is set at the top of the hydrogenation tower to discharge tail gas.
  • the oxidation tower includes:
  • An air feed pipe which is arranged on the side wall of the oxidation tower and connected to the second micro-interface generator, and used to transport air to the second micro-interface generator so that the second micro-interface generator can break the air ;
  • the hydrogenation liquid feed pipe is arranged on the side wall of the oxidation tower and above the air feed pipe, and is used to transport the 2-ethylhydroanthraquinone solution to the inside of the oxidation tower;
  • a reflux pipe which is arranged on the side wall of the oxidation tower, is used to return the material output from the oxidation tower to the oxidation tower, so that the 2-ethylhydroanthraquinone solution in the material is fully reacted;
  • a circulating pump which is connected to the return pipe, and is used to provide return power to the material output by the return pipe;
  • the second tail gas outlet is arranged at the top of the oxidation tower to discharge air;
  • the discharge port is arranged on the side wall of the oxidation tower to discharge the mixture of 2-ethylanthraquinone and hydrogen peroxide.
  • the filtering and cooling unit includes:
  • a filter which is arranged on the upper part of the side wall of the hydrogenation tower and is connected to the liquid output end of the gas-liquid separator, and is used to filter the hydrogenated material output from the hydrogenation tower to filter out solid impurities entrained in the material;
  • a heat exchanger which is connected to the filter, and is used to exchange heat between the material output from the filter and the anthraquinone derivative-containing working liquid to maintain the anthraquinone derivative-containing working liquid within a preset temperature range;
  • the hydrogenation cooler is arranged in the middle of the side wall of the hydrogenation tower and is connected with the heat exchanger to cool the materials after heat exchange.
  • the extraction tower includes:
  • a pure water feed pipe which is arranged at the top of the extraction tower and is used to transfer pure water to the inside of the extraction tower;
  • a heater which is connected to the pure water feed pipe for preheating the pure water
  • a pure water plus acid metering pump which is connected to the pure water feed pipe and is located below the heater, and is used to add phosphoric acid to adjust the acidity of the pure water;
  • a pure water pump which is connected to the pure water feed pipe and is located below the pure water plus acid metering pump, and is used to transmit pure water;
  • the hydrogen peroxide discharge pipe is arranged at the bottom of the extraction tower to output hydrogen peroxide.
  • a process for preparing hydrogen peroxide based on the anthraquinone method includes:
  • Step 1 Transport the working liquid containing anthraquinone derivatives into the hydrogenation tower through the working liquid feed pipe, and transport the catalyst into the hydrogenation tower through the catalyst feed port;
  • Step 2 Transport hydrogen into the hydrogenation tower through the hydrogen feed pipe.
  • the hydrogen feed pipe will transport hydrogen to the first micro-interface generator, and the first micro-interface generator performs hydrogen Crushing to form micron-scale micron-scale bubbles. After the crushing is completed, the first micro-interface generator outputs the micron-scale bubbles to the hydrogenation tower and mixes with the working liquid containing anthraquinone derivatives to form a gas-liquid emulsion;
  • Step 3 The gas-liquid emulsion undergoes a hydrogenation reaction under the action of a catalyst to produce a mixture containing 2-ethylhydroanthraquinone solution. After the reaction is completed, the mixture flows upward into the gas-liquid separator;
  • Step 4 After the mixture enters the gas-liquid separator, the tail gas is discharged from the top of the gas-liquid separator, and the hydrogenated liquid containing 2-ethylhydroanthraquinone is discharged from the side of the gas-liquid separator and enters the filter cooling unit ;
  • Step 5 After the hydrogenated liquid containing 2-ethylhydroanthraquinone enters the filter, solid impurities entrained in the hydrogenated liquid containing 2-ethylhydroanthraquinone remain in the filter, containing 2-ethylhydroanthracene
  • the filtrate in the quinone hydrogenation liquid is discharged from the bottom of the filter and enters the heat exchanger.
  • the heat exchanger contains 2-ethylhydroanthraquinone hydrogenation liquid and the working liquid containing anthraquinone derivatives for heat exchange.
  • the exchanged working liquid containing anthraquinone derivatives flows into the working liquid feed pipe, the heat-exchanged hydrogenated liquid containing 2-ethylhydroanthraquinone enters the hydrogenation cooler, and the cooled containing 2-ethyl
  • the hydrogenated hydroanthraquinone solution enters the oxidation tower;
  • Step 6 Transport the hydrogenation liquid containing 2-ethylhydroanthraquinone into the oxidation tower through the hydrogenation liquid feed pipe, and the air feed pipe will transport air to the second micro-interface generator, so The second micro-interface generator crushes the air to form micron-scale bubbles. After the crushing is completed, the second micro-interface generator outputs the micron-scale bubbles to the oxidation tower and mixes them with 2-ethyl hydrogen. The anthraquinone hydrogenation liquid is mixed to form a gas-liquid emulsion;
  • Step 7 The gas-liquid emulsion undergoes oxidation reaction to produce a mixture containing 2-ethylanthraquinone and hydrogen peroxide. After the reaction is completed, the mixture flows upwards and flows back to the oxidation tower along the reflux pipe, and a small amount of tail gas moves upwards and passes through The second tail gas outlet is discharged, and the mixture of 2-ethylanthraquinone and hydrogen peroxide after the tail gas is discharged is output to the oxidation tower through the discharge port;
  • Step 8 The mixture of 2-ethylanthraquinone and hydrogen peroxide is transferred to the bottom of the extraction tower through the discharge port, pure water is transferred to the heater through the pure water pump, and acid is added through the pure water The metering pump is adjusted to adjust the acidity of the pure water.
  • the preheated pure water enters the extraction tower along the pure water feed pipe and is extracted with the mixture of 2-ethylanthraquinone and hydrogen peroxide.
  • the hydrogen peroxide is output to the extraction tower along the hydrogen peroxide discharge pipe.
  • the reaction temperature in the hydrogenation tower is 20-40° C.
  • the reaction pressure is 0.05-0.50 MPa.
  • the reaction temperature in the oxidation tower is 20-45°C, and the reaction pressure is 0.10-0.20 MPa.
  • gas-liquid ratio in the first micro-interface generator is 300-500:1
  • gas-liquid ratio in the second micro-interface generator is 400-500:1.
  • the beneficial effect of the present invention is that the present invention breaks hydrogen gas to form micron-scale bubbles, and mixes the micron-scale bubbles with the working liquid containing anthraquinone derivatives to form a gas-liquid emulsion.
  • the phase boundary area of the two phases of the atmosphere and liquid improve the hydrogenation efficiency of the working fluid containing anthraquinone derivatives, increase the hydrogen reaction rate, save costs, and reduce the risk;
  • the air is broken to form micron-sized bubbles, and the micron-sized bubbles are mixed with the hydrogenated liquid containing 2-ethylhydroanthraquinone to form a gas-liquid emulsion, so as to increase the area of the gas-liquid phase boundary and achieve a lower
  • the mixture of 2-ethylanthraquinone and hydrogen peroxide is extracted through the extraction tower, and the water phase is from the top
  • the bottom and bottom-up mixtures are subjected to countercurrent extraction to achieve rapid extraction; at the same time, the system of the present invention filters, heats and cool
  • the 2-ethylhydroanthraquinone-containing hydrogenation fluid is cooled to reach the preset temperature range.
  • the range of preset operating conditions can be flexibly adjusted according to different product requirements or different catalysts, which further ensures the full and effective progress of the reaction, thereby ensuring the reaction rate, and achieving the purpose of strengthening the reaction.
  • the present invention also installs a gas-liquid separator in the hydrogenation tower, through the gas-liquid separator, the produced 2-ethylhydroanthraquinone hydrogenation liquid is separated and degassed, and the 2-ethylhydroanthraquinone hydrogenation liquid is further oxidized. effectiveness.
  • the unreacted raw material liquid in the materials is fully used by refluxing the materials after the reaction, thereby improving the utilization rate of the materials, thereby further improving the reaction efficiency of the system.
  • the hydrogenation tower and the oxidation tower of the present invention are respectively provided with a first micro-interface generator and a second micro-interface generator.
  • a first micro-interface generator By using different types of micro-interface generators, the mixing of micro-sized bubbles and materials is more effective. Uniformity, thereby improving the mixing efficiency of the materials in the reactor and the micron-level bubbles, so as to further improve the reaction efficiency of the system.
  • the extraction tower of the present invention extracts the mixture of 2-ethylanthraquinone and hydrogen peroxide, and the top-down and bottom-up mixtures of the water phase are subjected to countercurrent extraction, which improves the extraction efficiency and realizes rapid extraction.
  • the pure water plus acid metering pump adjusts the acidity of the pure water to ensure the acidity of the extractant, and the heater preheats the pure water so that the pure water enters the extraction tower within a predetermined temperature range to improve extraction efficiency.
  • the filtering and cooling unit of the present invention performs filtering, heat exchange and cooling treatments on the hydrogenated liquid containing 2-ethylhydroanthraquinone output from the hydrogenation tower to filter out solid impurities entrained in the material and work with anthraquinone derivatives. Liquid heat exchange saves energy consumption.
  • the 2-ethylhydroanthraquinone hydrogenated liquid is cooled to reach a preset temperature range to further improve the reaction efficiency of the system.
  • Fig. 1 is a schematic diagram of the structure of the system for preparing hydrogen peroxide based on the anthraquinone method according to the present invention.
  • the terms “installed”, “connected”, and “connected” should be understood in a broad sense. For example, they can be fixed or fixed. It is a detachable connection or an integral connection; it can be a mechanical connection or an electrical connection; it can be directly connected or indirectly connected through an intermediate medium, and it can be the internal communication between two components.
  • installed e.g., they can be fixed or fixed. It is a detachable connection or an integral connection; it can be a mechanical connection or an electrical connection; it can be directly connected or indirectly connected through an intermediate medium, and it can be the internal communication between two components.
  • the specific meaning of the above-mentioned terms in the present invention can be understood according to specific circumstances.
  • Figure 1 is a schematic structural diagram of the system for preparing hydrogen peroxide based on the anthraquinone method according to the present invention, including a hydrogenation tower 1, a micro-interface generator 2 (not shown in the figure), a filter cooling unit 3, and an oxidation Tower 4 and extraction column 5.
  • the micro-interface generator 2 is arranged inside the hydrogenation tower 1 and the oxidation tower 4, and is used to crush hydrogen and oxygen to form micron-scale micron-scale bubbles and mix the micron-scale bubbles with the materials in the hydrogenation tower and the oxidation tower. The formation of gas-liquid emulsions.
  • the filtering and cooling unit 3 is connected to the hydrogenation tower 1 and the oxidation tower 4 to filter and cool the hydrogenated material output from the hydrogenation tower.
  • the oxidation tower 4 is used to filter and cool the material output from the cooling unit and oxygen.
  • a reaction place is provided, and the extraction tower 5 and the oxidation tower 4 are used to extract and separate the materials output from the oxidation tower.
  • the working fluid containing anthraquinone derivatives and the catalyst are first delivered to the hydrogenation tower 1, and hydrogen is delivered to the hydrogenation tower 1.
  • the hydrogen enters the micro-interface generator 2, and the micro-interface generator 2 breaks the hydrogen.
  • the gas-liquid emulsion undergoes a hydrogenation reaction under the action of a catalyst to produce a solution containing 2-ethylhydroanthraquinone
  • the hydrogenation tower 1 will exhaust the exhaust gas during the reaction process, and output the reaction mixture containing the 2-ethylhydroanthraquinone solution to the filter cooling unit 3, and the filter cooling unit 3 filters and cools the mixture.
  • the air will enter the micro-interface generator 2 and the micro-interface generator 2 will break the air to form micro-sized micro-sized bubbles and make the micro-sized bubbles and containing 2-ethyl
  • the mixture of hydroanthraquinone solutions is mixed to form a gas-liquid emulsion, and the gas-liquid emulsion undergoes an oxidation reaction to generate a mixture containing 2-ethylanthraquinone and hydrogen peroxide, which is transferred to extraction tower 5, containing 2-ethylanthraquinone
  • the mixture of hydrogen peroxide and hydrogen peroxide and pure water are extracted in the extraction tower 5, and the extracted hydrogen peroxide is output to the extraction tower 5.
  • micro-interface generator 2 of the present invention can also be used in other multi-phase reactions, such as via micro-interface, micro-nano interface, ultra-micro interface, micro-bubble biochemical reactor or micro-bubble biological reaction.
  • micro-mixing using micro-mixing, micro-fluidization, ultra-micro-fluidization, micro-bubble fermentation, micro-bubble bubbling, micro-bubble mass transfer, micro-bubble transfer, micro-bubble reaction, micro-bubble absorption, micro-bubble oxygenation, micro-bubble Bubble contact and other processes or methods to make materials form multi-phase micro-mixed flow, multi-phase micro-nano flow, multi-phase emulsified flow, multi-phase micro-structured flow, gas-liquid-solid micro-mixed flow, gas-liquid-solid micro-nano flow, gas-liquid-solid emulsification Flow, gas-liquid-solid microstructure flow, micro-bubble, micro-bubble flow, micro-foam, micro-foam flow, micro-gas-liquid flow, gas-liquid micro-nano emulsion flow, ultra-micro flow, micro-dispersion flow, two micro-mixed flows, Micro-turbulent flow, micro-bubble flow, micro-turbul
  • the hydrogenation tower 1 of the present invention includes a hydrogen feed pipe 11, a working fluid feed pipe 12, a catalyst feed port 13 and a first tail gas outlet 14.
  • the hydrogen feed pipe 11 is arranged on the side wall of the hydrogenation tower 1 and is connected to the micro-interface generator 2 to transmit hydrogen.
  • the working fluid feed pipe 12 is arranged on the side wall of the hydrogen tower 1 and above the hydrogen feed pipe 11 to transport the working fluid containing anthraquinone derivatives to the inside of the hydrogenation tower.
  • the catalyst feed inlet 13 is arranged on the side wall of the hydrogenation tower 1 and above the working fluid feed pipe 12 to put the catalyst into the hydrogenation tower.
  • the first tail gas outlet 114 is arranged at the The top of the hydrogenation tower is used to discharge tail gas.
  • the hydrogenation tower 1 When the hydrogenation tower 1 is in operation, hydrogen is delivered into the hydrogenation tower 1 through the hydrogen feed pipe 11, and the hydrogen feed pipe 11 will deliver hydrogen to the micro-interface generator 2.
  • a micro-interface 21 generator breaks the hydrogen gas to form micro-scale micro-sized bubbles.
  • the micro-interface generator 2 After the crushing is completed, the micro-interface generator 2 outputs the micro-scale bubbles to the hydrogenation tower 1 and mixes them with a working liquid containing anthraquinone derivatives.
  • the gas-liquid emulsion is mixed in the hydrogenation tower to form a gas-liquid emulsion, and the gas-liquid emulsion undergoes a hydrogenation reaction under the action of a catalyst to form a mixture containing a 2-ethylhydroanthraquinone solution.
  • the hydrogen feed pipe 11 is arranged on the side wall of the hydrogenation tower 1 and is connected to the micro-interface generator 2 to deliver hydrogen to the first micro-interface generator so that the first micro-interface
  • the generator crushes the hydrogen to form micron-scale micron-scale bubbles, which are mixed with the working fluid containing anthraquinone derivatives.
  • the material and size of the hydrogen feed pipe 11 are not specifically limited in this embodiment. , As long as it is satisfied that the hydrogen feed pipe 11 can transport a specified volume of hydrogen within a specified time.
  • the micro-interface generator 2 of the present invention includes a first micro-interface generator 21 and a second micro-interface generator 22.
  • the first micro-interface generator 21 is arranged at the bottom of the reaction zone, and is used to break the hydrogen gas to form micro-scale micro-sized bubbles.
  • the second micro-interface generator 22 is arranged at the bottom of the reaction zone for breaking oxygen to form micro-sized micro-sized bubbles.
  • the first micro-interface generator 21 will break the hydrogen gas to form micro-sized micro-sized bubbles, and mix the micro-sized bubbles with the working liquid containing anthraquinone derivatives to form a gas-liquid emulsion.
  • the second micro-interface generator 22 is used to break the oxygen to form micro-sized micro-sized bubbles, and mix it with the 2-ethylhydroanthraquinone solution in the oxidation tower to form a gas-liquid emulsion.
  • the first micro-interface generator 21 of the present invention is a pneumatic micro-interface generator, which is connected to the hydrogen feed pipe 11 to crush the hydrogen delivered by the hydrogen feed pipe 11 and form a micron scale. Of micron-sized bubbles.
  • the hydrogen feed pipe 11 will transport hydrogen to the first micro-interface generator 21, and the first micro-interface generator 21 will break the hydrogen into a micron-sized micron scale.
  • the micron-sized bubbles are output to the hydrogenation tower, and mixed with the anthraquinone derivative working liquid in the hydrogenation tower to form a gas-liquid emulsion to fully react.
  • the second micro-interface generator 22 of the present invention is a pneumatic micro-interface generator, which is connected to the air feed pipe and is used to crush the air conveyed by the air feed pipe and form a micron-sized micron. Level bubbles.
  • the air feed pipe will transport air to the second micro-interface generator 22, and the second micro-interface generator 22 will break the air and form micro-scale micro-sized bubbles
  • the micron-sized bubbles are output to the oxidation tower, and mixed with the hydrogenation liquid containing 2-ethylhydroanthraquinone in the oxidation tower to form a gas-liquid emulsion to fully react.
  • the filtering and cooling unit 3 of the present invention includes a filter 31, a heat exchanger 32 and a hydrogenation cooler 33.
  • the filter 31 is arranged on the upper part of the side wall of the hydrogenation tower 1 and is connected to the liquid output end of the gas-liquid separator 12, and is used to filter the hydrogenated material output from the hydrogenation tower to filter out entrained materials in the hydrogenation tower.
  • Solid impurities, the heat exchanger 32 is connected to the filter 31 to exchange heat between the material output from the filter and the working liquid containing anthraquinone derivatives, so that the working liquid containing anthraquinone derivatives is maintained at a preset value Within the temperature range.
  • the hydrogenation cooler 33 is arranged in the middle of the side wall of the hydrogenation tower 1 and is connected to the heat exchanger 32 to cool the material after heat exchange.
  • the filter 31 It will receive the liquid phase components discharged from the gas-liquid separator 12 and filter the solid impurities in the liquid phase components.
  • the filtrate containing 2-ethylhydroanthraquinone enters the heat exchanger 32 and exchanges with the working fluid containing anthraquinone derivatives.
  • the hydrogenation cooler 33 will receive the 2-ethylhydroanthraquinone hydrogenation liquid discharged from the heat exchanger 32 and cool the solution.
  • the filter 31, the heat exchanger 32, and the The model and power of the hydrogen cooler 33 are not specifically limited in this embodiment, as long as the filter 31, the heat exchanger 32 and the hydrogen cooler 33 can reach their designated working conditions.
  • the oxidation tower 4 of the present invention includes an air feed pipe 41, a hydrogenated liquid feed pipe 42, a return pipe 43, a circulating pump 44, a second tail gas outlet 45 and a discharge port 46.
  • the air feed pipe 41 is arranged on the side wall of the oxidation tower 4 and is connected to the second micro-interface generator 22 for conveying air to the second micro-interface generator so that the second micro-interface generator can interact with each other. The air is broken.
  • the hydrogenation liquid feed pipe 42 is arranged on the side wall of the oxidation tower 4 and above the air feed pipe 41, and is used to transport the 2-ethylhydroanthraquinone solution to the inside of the oxidation tower 4;
  • the reflux pipe 43 is arranged on the side wall of the oxidation tower 4 to reflux the material output from the oxidation tower into the oxidation tower so as to fully react the 2-ethylhydroanthraquinone solution in the material.
  • the circulation pump 44 is connected to the return pipe 43 to provide return power to the material output by the return pipe.
  • the second tail gas outlet 45 is arranged at the top of the oxidation tower to discharge air.
  • the feed port 46 is arranged on the side wall of the oxidation tower to discharge the mixture of 2-ethylanthraquinone and hydrogen peroxide.
  • the air is transported into the oxidation tower 4 through the air feed pipe 41.
  • the air feed pipe 41 is connected to the second micro-interface generator 22.
  • the second micro-interface generator 22 crushes the air to form Micron-scale micron-scale bubbles.
  • the second micro-interface generator 22 outputs the micron-scale bubbles to the oxidation tower 4 and mixes them with the 2-ethylhydroanthraquinone solution in the oxidation tower to form a gas-liquid Emulsions, gas-liquid emulsions are fully reacted to produce a mixture containing 2-ethylanthraquinone and hydrogen peroxide.
  • the extraction tower 5 of the present invention includes a pure water feed pipe 51, a heater 52, a pure water plus acid metering pump 53, a pure water pump 54 and a hydrogen peroxide discharge pipe 55.
  • the pure water feed pipe 51 is arranged at the top of the extraction tower to transmit pure water to the inside of the extraction tower.
  • the heater 52 is connected to the pure water feed pipe for preheating the pure water.
  • the pure water plus acid metering pump 53 is connected to the pure water feed pipe and located below the heater, and is used to add phosphoric acid to adjust the acidity of the pure water.
  • the pure water pump 54 is connected to the pure water feed pipe and is located below the pure water plus acid metering pump, and is used for transmitting pure water.
  • the hydrogen peroxide discharge pipe 55 is arranged at the bottom of the extraction tower to output hydrogen peroxide.
  • pure water is transmitted to the heater 52 through the pure water pump 54, and the acidity of the pure water is adjusted by the pure water plus acid metering pump 53.
  • the preheated pure water is The pure water feed pipe 51 enters the extraction tower 5 and extracts with the mixture of 2-ethylanthraquinone and hydrogen peroxide, and the extracted hydrogen peroxide is output to the extraction tower 5 along the hydrogen peroxide discharge pipe 55.
  • the models and powers of the heater 52, the pure water plus acid metering pump 53, and the pure water pump 54 are not specifically limited in this embodiment, as long as they meet the requirements of the heater 52, pure water plus acid metering pump 53 and pure water pump. 54 can reach its designated working state.
  • a process for preparing hydrogen peroxide based on the anthraquinone method includes:
  • Step 1 Transport the working liquid containing anthraquinone derivatives into the hydrogenation tower through the working liquid feed pipe, and transport the catalyst into the hydrogenation tower through the catalyst feed port;
  • Step 2 Transport hydrogen into the hydrogenation tower through the hydrogen feed pipe.
  • the hydrogen feed pipe will transport hydrogen to the first micro-interface generator, and the first micro-interface generator performs hydrogen Crushing to form micron-scale micron-scale bubbles. After the crushing is completed, the first micro-interface generator outputs the micron-scale bubbles to the hydrogenation tower and mixes with the working liquid containing anthraquinone derivatives to form a gas-liquid emulsion;
  • Step 3 The gas-liquid emulsion undergoes a hydrogenation reaction under the action of a catalyst to produce a mixture containing 2-ethylhydroanthraquinone solution. After the reaction is completed, the mixture flows upward into the gas-liquid separator;
  • Step 4 After the mixture enters the gas-liquid separator, the tail gas is discharged from the top of the gas-liquid separator, and the hydrogenated liquid containing 2-ethylhydroanthraquinone is discharged from the side of the gas-liquid separator and enters the filter cooling unit ;
  • Step 5 After the hydrogenated liquid containing 2-ethylhydroanthraquinone enters the filter, solid impurities entrained in the hydrogenated liquid containing 2-ethylhydroanthraquinone remain in the filter, containing 2-ethylhydroanthracene
  • the filtrate in the quinone hydrogenation liquid is discharged from the bottom of the filter and enters the heat exchanger.
  • the heat exchanger contains 2-ethylhydroanthraquinone hydrogenation liquid and the working liquid containing anthraquinone derivatives for heat exchange.
  • the exchanged working liquid containing anthraquinone derivatives flows into the working liquid feed pipe, the heat-exchanged hydrogenated liquid containing 2-ethylhydroanthraquinone enters the hydrogenation cooler, and the cooled containing 2-ethyl
  • the hydrogenated hydroanthraquinone solution enters the oxidation tower;
  • Step 6 Transport the hydrogenation liquid containing 2-ethylhydroanthraquinone into the oxidation tower through the hydrogenation liquid feed pipe, and the air feed pipe will transport air to the second micro-interface generator, so The second micro-interface generator crushes the air to form micron-scale bubbles. After the crushing is completed, the second micro-interface generator outputs the micron-scale bubbles to the oxidation tower and mixes them with 2-ethyl hydrogen. The anthraquinone hydrogenation liquid is mixed to form a gas-liquid emulsion;
  • Step 7 The gas-liquid emulsion undergoes oxidation reaction to produce a mixture containing 2-ethylanthraquinone and hydrogen peroxide. After the reaction is completed, the mixture flows upwards and flows back to the oxidation tower along the reflux pipe, and a small amount of tail gas moves upwards and passes through The second tail gas outlet is discharged, and the mixture of 2-ethylanthraquinone and hydrogen peroxide after the tail gas is discharged is output to the oxidation tower through the discharge port;
  • Step 8 The mixture of 2-ethylanthraquinone and hydrogen peroxide is transferred to the bottom of the extraction tower through the discharge port, pure water is transferred to the heater through the pure water pump, and acid is added through the pure water The metering pump is adjusted to adjust the acidity of the pure water.
  • the preheated pure water enters the extraction tower along the pure water feed pipe and is extracted with the mixture of 2-ethylanthraquinone and hydrogen peroxide.
  • the hydrogen peroxide is output to the extraction tower along the hydrogen peroxide discharge pipe.
  • the working solution containing anthraquinone derivatives is composed of 2-ethylanthraquinone (EAQ), heavy aromatic hydrocarbons (AR) and trioctyl phosphate.
  • EAQ 2-ethylanthraquinone
  • AR heavy aromatic hydrocarbons
  • trioctyl phosphate 2-ethylanthraquinone
  • the range of preset operating conditions can be adjusted flexibly according to different product requirements or different catalysts to ensure the full and effective progress of the reaction, thereby ensuring the reaction rate, and achieving the purpose of strengthening the reaction.
  • the type of catalyst is not specifically limited in this embodiment, as long as it can ensure the smooth progress of the strengthening reaction.
  • the reaction temperature in the hydrogenation tower is 38° C.
  • the reaction pressure is 0.05 MPa
  • the anthraquinone content is 220 g/L
  • the flow rate of the working liquid containing anthraquinone derivatives is 130 h -1
  • the gas in the first micro-interface generator The liquid ratio is 300:1.
  • the reaction temperature in the oxidation tower is 35°C
  • the reaction pressure is 0.10 MPa
  • the flow rate of the hydrogenation liquid containing 2-ethylhydroanthraquinone is 140h -1
  • the gas-liquid ratio in the second micro-interface generator is 400 :1.
  • the hydrogenation efficiency is 14.2 g/L
  • the oxidation efficiency is 13.9 g/L
  • the oxidation reaction conversion rate is 97.9%.
  • the reaction temperature in the hydrogenation tower is 39°C
  • the reaction pressure is 0.15MPa
  • the anthraquinone content is 235g/L
  • the flow rate of the working liquid containing anthraquinone derivatives is 135h -1
  • the gas in the first micro-interface generator The liquid ratio is 350:1.
  • the reaction temperature in the oxidation tower is 37°C
  • the reaction pressure is 0.13 MPa
  • the flow rate of the hydrogenation liquid containing 2-ethylhydroanthraquinone is 145h -1
  • the gas-liquid ratio in the second micro-interface generator is 420 :1.
  • the hydrogenation efficiency is 14.6 g/L
  • the oxidation efficiency is 14.3 g/L
  • the oxidation reaction conversion rate is 97.9%.
  • the reaction temperature in the hydrogenation tower is 42° C.
  • the reaction pressure is 0.30 MPa
  • the anthraquinone content is 245 g/L
  • the flow rate of the working liquid containing anthraquinone derivatives is 147 h -1
  • the gas in the first micro-interface generator The liquid ratio is 400:1.
  • the reaction temperature in the oxidation tower is 40° C.
  • the reaction pressure is 0.15 MPa
  • the flow rate of the hydrogenation liquid containing 2-ethylhydroanthraquinone is 152 h -1
  • the gas-liquid ratio in the second micro-interface generator is 450 :1.
  • the hydrogenation efficiency is 14.7 g/L
  • the oxidation efficiency is 14.4 g/L
  • the oxidation reaction conversion rate is 98.0%.
  • the reaction temperature in the hydrogenation tower is 45° C.
  • the reaction pressure is 0.40 MPa
  • the anthraquinone content is 248 g/L
  • the flow rate of the working liquid containing anthraquinone derivatives is 150 h -1
  • the gas in the first micro-interface generator The liquid ratio is 470:1.
  • the reaction temperature in the oxidation tower is 43° C.
  • the reaction pressure is 0.18 MPa
  • the flow rate of the hydrogenation liquid containing 2-ethylhydroanthraquinone is 154 h -1
  • the gas-liquid ratio in the second micro-interface generator is 460 :1.
  • the hydrogenation efficiency is 14.8 g/L
  • the oxidation efficiency is 14.6 g/L
  • the oxidation reaction conversion rate is 98.6%.
  • the reaction temperature in the hydrogenation tower is 48°C
  • the reaction pressure is 0.50MPa
  • the anthraquinone content is 260g/L
  • the flow rate of the working liquid containing anthraquinone derivatives is 160h -1
  • the gas in the first micro-interface generator The liquid ratio is 500:1.
  • the reaction temperature in the oxidation tower is 45° C.
  • the reaction pressure is 0.20 MPa
  • the flow rate of the hydrogenation liquid containing 2-ethylhydroanthraquinone is 160 h -1
  • the gas-liquid ratio in the second micro-interface generator is 500 :1.
  • the hydrogenation efficiency is 14.9 g/L
  • the oxidation efficiency is 14.7 g/L
  • the oxidation reaction conversion rate is 98.6%.
  • the anthraquinone method is used to prepare hydrogen peroxide using the existing technology, wherein the process parameters selected in this embodiment are the same as those in the fourth embodiment.
  • the hydrogenation efficiency is 10.7 g/L
  • the oxidation efficiency is 9.9 g/L
  • the oxidation reaction conversion rate is 73.8%.

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Abstract

一种基于蒽醌法制备双氧水的系统及工艺,包括:氢化塔(1)、微界面发生器(2)、过滤冷却单元(3)、氧化塔(4)和萃取塔(5)。通过破碎氢气使其形成微米尺度的微米级气泡,使微米级气泡与含蒽醌衍生物工作液或含2-乙基氢蒽醌氢化液混合形成气液乳化物,以增大气液两相的相界面积,并达到在较低预设操作条件范围内强化传质的效果,提高含蒽醌衍生物工作液氢化、氧化效率,提高氢气反应率,节约成本,降低危险性,通过萃取塔(5)对2-乙基蒽醌和过氧化氢的混合物进行萃取,水相自上而下与自下而上的混合物进行逆流萃取,实现快速萃取。

Description

一种基于蒽醌法制备双氧水的系统及工艺 技术领域
本发明涉及蒽醌法制双氧水技术领域,尤其涉及一种基于蒽醌法制备双氧水的系统及工艺。
背景技术
双氧水为过氧化氢(H 2O 2)的水溶液,是一种重要的无机过氧化物,具有氧化性、漂白性和使用过程绿色环保等特点,可应用于织物、纸浆脱色、化工合成、废水处理、医疗、冶金、军工、食品加工等领域,充当氧化剂、漂白剂、消毒剂、聚合物引发剂和交联剂、推进剂等。随着环保法规的日益严格,过氧化氢直接氧化法(HPPO法)生产环氧丙烷、绿色己内酰胺等产品产能增加,导致H 2O 2的市场需求旺盛。
过氧化氢的生产方法有蒽醌法、电解法、异丙醇氧化法,无机反应法、氢氧直接合成法等。其中,蒽醌法是目前国内外生产过氧化氢的主流方法。
蒽醌法过氧化氢生产工艺是以2-乙基蒽醌(EAQ)为载体,重芳烃(AR)及磷酸三辛酯(TOP)为混合溶剂,配制成具有一定组成的溶液(工作液),在钯或镍催化剂的催化作用下,交替进行烷基蒽醌的催化加氢和空气氧化,氧化生成的过氧化氢用水萃取出来成粗品双氧水,烷基蒽醌可以循环使用。相当于H 2和O 2合成H 2O 2。蒽醌法主要分为氢化、氧化、萃取、后处理四个工序。其中,氢化是蒽醌法生产过氧化氢的关键步骤。蒽醌加氢催化剂的活性和选择性很大程度上决定了氢化过程的效率和单耗,高活性和高选择性的氢化催化剂可以提高双氧水的产率,减少蒽醌降解,降低生产成本,创造更好的经济效益。
中国专利公开号:CN106395755A公开了一种蒽醌法制备过氧化氢的方法,通过采用一种将含蒽醌衍生物工作液和氢气在纤维催化反应器中的纤维催化剂接触,在纤维催化剂的催化活性组分作用下反应生成氢化液;再通过空气氧化烷基氢蒽醌生成含有过氧化氢和烷基蒽醌的氧化液,然后用水萃取氧化液中的过氧化氢,经净化、浓缩得一定浓度的过氧化氢产品,萃取后的含烷基蒽醌的工作液循环使用。由此可见,所述方法存在以下问题:
第一,所述方法中仅通过纤维催化反应器使纤维催化剂与含蒽醌衍生物工作液和氢气接触,氢气通过氢气分布器进入纤维催化反应器内,形成大气泡,然而由于气泡体积过大,无法与纤维催化剂和蒽醌衍生物工作液充分接触,降低了所述系统的氢化效率。
第二,所述方法在氢气与纤维催化剂和蒽醌衍生物工作液接触不充分情况下,氢化程度降低,直接影响后续氧化、萃取效率,且系统内易燃易爆原料氢气含量增加,剩余氢气沿氢气第二尾气出口流出,既增加了生产成本,又具有一定为危险性。
第三,所述方法仅通过空气分布器通入空气,通过空气氧化烷基氢蒽醌生成含有过氧化氢和烷基蒽醌的氧化液,气泡体积过大,无法与烷基氢蒽醌充分接触,降低了所述系统的反应效率。
发明内容
为此,本发明提供一种基于蒽醌法制备双氧水的系统及工艺,用以克服现有技术中物料间混合不均匀产生副产物导致的系统反应效率低的问题。
一方面,本发明提供一种基于蒽醌法制备双氧水的系统,包括:
氢化塔,用以为含蒽醌衍生物工作液与氢气提供反应场所;
微界面发生器,其设置氢化塔,用以为含蒽醌衍生物工作液与氢气提供反应场所;
过滤冷却单元,其设置在所述氢化塔侧壁,用以对氢化塔输出的氢化物料进行过滤并进行冷却;
氧化塔,与所述过滤冷却单元相连,用以为过滤冷却单元输出的物料与氧气提供反应场所;
萃取塔,用以对氧化塔输出的物料进行萃取分离;
微界面发生器,其设置在所述氢化塔和所述氧化塔内的指定位置,将气体的压力能和/或液体的动能转变为气泡表面能并传递给氢气,使氢气破碎形成直径≥1μm、且<1mm的微米级气泡以提高含蒽醌衍生物工作液与氢气间的传质面积,减小液膜厚度,降低传质阻力,并在破碎后将含蒽醌衍生物工作液与微米级气泡混合形成气液乳化物,以在预设操作条件范围内强化含蒽醌衍生物工作液与 氢气间的传质效率和反应效率。
进一步地,所述微界面发生器包括:
第一微界面发生器,所述第一微界面发生器设置在所述氢化塔反应区底部,用以将氢气破碎形成微米尺度的微米级气泡并在破碎完成后将微米级气泡输出至氢化塔、并与氢化塔内的含蒽醌衍生物工作液混合形成气液乳化物;
第二微界面发生器,所述第二微界面发生器设置在所述氧化塔反应区底部,用以将氧气破碎形成微米尺度的微米级气泡并在破碎完成后将微米级气泡输出至氢化塔、并与氧化塔内的2-乙基氢蒽醌溶液混合形成气液乳化物。
进一步地,所述氢化塔包括:
氢气进料管道,其设置在所述氢化塔侧壁且与所述第一微界面发生器相连,用以将氢气输送至第一微界面发生器以使第一微界面发生器对氢气进行破碎;
工作液进料管道,其设置在所述氢气塔侧壁并位于所述氢气进料管道上方,用以将含蒽醌衍生物工作液输送至氢化塔内部;
催化剂进料口,其设置在所述氢化塔侧壁并位于所述工作液进料管道上方,用以将催化剂放至氢化塔内;
第一尾气出口,其设置在所述氢化塔顶部,用以排出尾气。
进一步地,所述氧化塔包括:
空气进料管道,其设置在所述氧化塔侧壁且与所述第二微界面发生器相连,用以将空气输送至第二微界面发生器以使第二微界面发生器对空气进行破碎;
氢化液进料管道,其设置在所述氧化塔侧壁并位于所述空气进料管道上方,用以将2-乙基氢蒽醌溶液输送至氧化塔内部;
回流管,其设置在所述氧化塔侧壁,用以对氧化塔输出的物料回流至氧化塔内,以使物料中2-乙基氢蒽醌溶液充分反应;
循环泵,其与所述回流管相连,用以对回流管输出的物料提供回输动力;
第二尾气出口,设置在所述氧化塔顶部,用以排出空气;
出料口,设置在所述氧化塔侧壁,用以将2-乙基蒽醌和过氧化氢的混合物排出。
进一步地,所述过滤冷却单元包括:
过滤器,其设置在所述氢化塔侧壁上部且与所述气液分离器的液体输出端相 连,用以对氢化塔输出的氢化物料进行过滤,以滤除物料中夹带的固体杂质;
换热器,其与所述过滤器相连,用以对过滤器输出的物料与含蒽醌衍生物工作液进行换热以使含蒽醌衍生物工作液维持在预设温度范围内;
氢化冷却器,其设置在所述氢化塔侧壁中部且与所述换热器相连,用以对换热后物料进行冷却处理。
进一步地,所述萃取塔包括:
纯水进料管道,其设置在所述萃取塔顶部,用以将纯水传输至萃取塔内部;
加热器,其与所述纯水进料管道相连,用以对纯水进行预热处理;
纯水加酸计量泵,其与所述纯水进料管道相连且位于所述加热器下方,用以加入磷酸对纯水酸度进行调节;
纯水泵,其与所述纯水进料管道相连且位于所述纯水加酸计量泵下方,用以对纯水进行传输;
双氧水出料管道,其设置在所述萃取塔底部,用以输出双氧水。
另一方面,一种基于蒽醌法制备双氧水的工艺,包括:
步骤1:通过所述工作液进料管道向所述氢化塔内输送含蒽醌衍生物工作液,并通过所述催化剂进料口将催化剂输送至所述氢化塔内;
步骤2:通过所述氢气进料管道向所述氢化塔内输送氢气,所述氢气进料管道会将氢气输送至所述第一微界面发生器,所述第一微界面发生器对氢气进行破碎,形成微米尺度的微米级气泡,破碎完成后,所述第一微界面发生器将微米级气泡输出至所述氢化塔并与含蒽醌衍生物工作液混合形成气液乳化物;
步骤3:气液乳化物在催化剂的作用下发生氢化反应,生成含2-乙基氢蒽醌溶液的混合物,反应完成后,混合物向上流动进入所述气液分离器;
步骤4:混合物进入所述气液分离器后,尾气由所述气液分离器顶部排出,含2-乙基氢蒽醌氢化液由所述气液分离器侧面排出并进入所述过滤冷却单元;
步骤5:含2-乙基氢蒽醌氢化液进入所述过滤器后,含2-乙基氢蒽醌氢化液中夹带的固体杂质残留在所述过滤器内,含2-乙基氢蒽醌氢化液中滤液由所述过滤器底部排出并进入所述换热器内,所述换热器内含2-乙基氢蒽醌氢化液与含蒽醌衍生物工作液进行热交换,热交换后的含蒽醌衍生物工作液并流入所述工作液进料管道,热交换后的含2-乙基氢蒽醌氢化液进入所述氢化冷却器内, 冷却后的含2-乙基氢蒽醌氢化液进入所述氧化塔;
步骤6:通过所述氢化液进料管道向所述氧化塔内输送含2-乙基氢蒽醌氢化液,所述空气进料管道会将空气输送至所述第二微界面发生器,所述第二微界面发生器对空气进行破碎,形成微米尺度的微米级气泡,破碎完成后,所述第二微界面发生器将微米级气泡输出至所述氧化塔并与含2-乙基氢蒽醌氢化液混合形成气液乳化物;
步骤7:气液乳化物发生氧化反应,生成含2-乙基蒽醌和过氧化氢的混合物,反应完成后,混合物向上流动并沿所述回流管回流至氧化塔,少量尾气向上运动并通过所述第二尾气出口排出,排出尾气后的2-乙基蒽醌和过氧化氢的混合物通过所述出料口输出所述氧化塔;
步骤8:2-乙基蒽醌和过氧化氢的混合物通过出料口传输至所述萃取塔底部,纯水通过所述纯水泵传输至所述加热器内,并通过所述纯水加酸计量泵调节对纯水酸度进行调节,预热后的纯水沿所述纯水进料管道进入所述萃取塔内部,与2-乙基蒽醌和过氧化氢的混合物发生萃取,萃取后的双氧水沿所述双氧水出料管道输出所述萃取塔。
进一步地,所述工艺中氢化塔内的反应温度为20-40℃,反应压强为0.05-0.50MPa。
进一步地,所述工艺中氧化塔内的反应温度为20-45℃,反应压强为0.10-0.20MPa。
进一步地,所述第一微界面发生器内的气液比为300-500:1,所述第二微界面发生器内的气液比为400-500:1。
与现有技术相比,本发明的有益效果在于,本发明通过破碎氢气使其形成微米尺度的微米级气泡,使微米级气泡与含蒽醌衍生物工作液混合形成气液乳化物,以增大气液两相的相界面积,并达到在较低预设操作条件范围内强化传质的效果,提高含蒽醌衍生物工作液氢化效率,提高氢气反应率,节约成本,降低危险性;通过破碎空气使其形成微米尺度的微米级气泡,使微米级气泡与含2-乙基氢蒽醌氢化液混合形成气液乳化物,以增大气液两相的相界面积,并达到在较低预设操作条件范围内强化传质的效果,提高含2-乙基氢蒽醌氢化液的氧化效率;通过萃取塔对2-乙基蒽醌和过氧化氢的混合物进行萃取,水相自上而下与 自下而上的混合物进行逆流萃取,实现快速萃取;同时,本发明所述系统通过过滤冷却单元对氢化塔输出的含2-乙基氢蒽醌氢化液进行过滤、换热和冷却处理,以滤除物料中夹带的固体杂质,与含蒽醌衍生物工作液换热,节约能耗,对的含2-乙基氢蒽醌氢化液冷却使其达到预设温度范围。此外,可以根据不同的产品要求或不同的催化剂,而对预设操作条件的范围进行灵活调整,进一步确保了反应的充分有效进行,进而保证了反应速率,达到了强化反应的目的。
尤其,本发明还在氢化塔中设置气液分离器,通过气液分离器,对生产的2-乙基氢蒽醌氢化液进行分离除气,提高2-乙基氢蒽醌氢化液进一步氧化效率。
进一步地,通过对反应完成的物料进行回流以充分使用物料中的未反应原料液,从而提高物料的利用率,从而进一步提高了所述系统的反应效率。
进一步地,本发明所述氢化塔和所述氧化塔内分别设有第一微界面发生器和第二微界面发生器,通过使用不同种类的微界面发生器,使微米级气泡与物料混合更加均匀,从而提高反应器内物料与微米级气泡的混合效率,以进一步提高所述系统的反应效率。
尤其,本发明所述萃取塔对2-乙基蒽醌和过氧化氢的混合物进行萃取,水相自上而下与自下而上的混合物进行逆流萃取,提高萃取效率,实现快速萃取。
进一步地,所述纯水加酸计量泵对纯水进行酸度调节,保证萃取剂的酸度,所述加热器对纯水进行预热,使纯水为预定温度范围进入萃取塔,提高萃取效率。
尤其,本发明所述过滤冷却单元对氢化塔输出的含2-乙基氢蒽醌氢化液进行过滤、换热和冷却处理,以滤除物料中夹带的固体杂质,与含蒽醌衍生物工作液换热,节约能耗,对的含2-乙基氢蒽醌氢化液冷却使其达到预设温度范围,以进一步提高系统的反应效率。
附图说明
图1为本发明所述的基于蒽醌法制备双氧水的系统的结构示意图。
具体实施方式
下面参照附图来描述本发明的优选实施方式。本领域技术人员应当理解的是,这些实施方式仅仅用于解释本发明的技术原理,并非在限制本发明的保护范 围。
需要说明的是,在本发明的描述中,术语“上”、“下”、“左”、“右”、“内”、“外”等指示的方向或位置关系的术语是基于附图所示的方向或位置关系,这仅仅是为了便于描述,而不是指示或暗示所述装置或元件必须具有特定的方位、以特定的方位构造和操作,因此不能理解为对本发明的限制。
此外,还需要说明的是,在本发明的描述中,除非另有明确的规定和限定,术语“安装”、“相连”、“连接”应做广义理解,例如,可以是固定连接,也可以是可拆卸连接,或一体地连接;可以是机械连接,也可以是电连接;可以是直接相连,也可以通过中间媒介间接相连,可以是两个元件内部的连通。对于本领域技术人员而言,可根据具体情况理解上述术语在本发明中的具体含义。
请参阅图1所示,其为本发明所述的基于蒽醌法制备双氧水的系统的结构示意图,包括氢化塔1、微界面发生器2(图中未标出)、过滤冷却单元3、氧化塔4和萃取塔5。所述微界面发生器2设置在所述氢化塔1和氧化塔4内部,分别用以将氢气和氧气破碎形成微米尺度的微米级气泡并将微米级气泡与氢化塔和氧化塔内的物料混合形成气液乳化物。所述过滤冷却单元3与所述氢化塔1和所述氧化塔4相连,用以对氢化塔输出的氢化物料进行过滤并进行冷却,所述氧化塔4用以为过滤冷却单元输出的物料与氧气提供反应场所,所述萃取塔5与所述氧化塔4,用以对氧化塔输出的物料进行萃取分离。
当所述系统运行时,先向氢化塔1内输送含蒽醌衍生物工作液和催化剂,同时向氢化塔1内输送氢气,氢气会进入微界面发生器2,微界面发生器2将氢气破碎形成微米尺度的微米级气泡并使微米级气泡与含蒽醌衍生物工作液混合形成气液乳化物,气液乳化物在催化剂作用下进行氢化反应,生成含2-乙基氢蒽醌溶液的混合物,氢化塔1会将反应过程中尾气排出系统,并将反应后的含2-乙基氢蒽醌溶液的混合物输出至过滤冷却单元3,过滤冷却单元3对混合物进行进行过滤并进行冷却,并传输至氧化塔4,向氧化塔4内输送空气,空气会进入微界面发生器2,微界面发生器2将空气破碎形成微米尺度的微米级气泡并使微米级气泡与含2-乙基氢蒽醌溶液的混合物混合形成气液乳化物,气液乳化物进行氧化反应,生成含2-乙基蒽醌和过氧化氢的混合物,并传输至萃取塔5,含2-乙基蒽醌和过氧化氢的混合物与纯水在萃取塔5内进行萃取,萃取后的双氧水 输出萃取塔5。本领域的技术人员可以理解的是,本发明所述微界面发生器2还可用于其它多相反应中,如通过微界面、微纳界面、超微界面、微泡生化反应器或微泡生物反应器等设备,使用微混合、微流化、超微流化、微泡发酵、微泡鼓泡、微泡传质、微泡传递、微泡反应、微泡吸收、微泡增氧、微泡接触等工艺或方法,以使物料形成多相微混流、多相微纳流、多相乳化流、多相微结构流、气液固微混流、气液固微纳流、气液固乳化流、气液固微结构流、微米级气泡、微米级气泡流、微泡沫、微泡沫流、微气液流、气液微纳乳化流、超微流、微分散流、两项微混流、微湍流、微泡流、微鼓泡、微鼓泡流、微纳鼓泡以及微纳鼓泡流等由微米尺度颗粒形成的多相流体、或由微纳尺度颗粒形成的多相流体(简称微界面流体),从而有效地增大了反应过程中所述气相和/或液相与液相和/或固相之间的相界传质面积。
请继续参阅图1所示,本发明所述氢化塔1包括氢气进料管道11、工作液进料管道12、催化剂进料口13和第一尾气出口14。其中,所述氢气进料管道11设置在在所述氢化塔1侧壁且与所述微界面发生器2相连,用以传输氢气。所述工作液进料管道12设置在所述氢气塔1侧壁并位于所述氢气进料管道11上方,用以将含蒽醌衍生物工作液输送至氢化塔内部。所述催化剂进料口13设置在所述氢化塔1侧壁并位于所述工作液进料管道12上方,用以将催化剂放至氢化塔内,所述第一尾气出口114,设置在所述氢化塔顶部,用以排出尾气。
当所述氢化塔1运行时,通过所述氢气进料管道11向所述氢化塔1内输送氢气,所述氢气进料管道11会将氢气输送至所述微界面发生器2,所述第一微界面21发生器对氢气进行破碎,形成微米尺度的微米级气泡,破碎完成后,所述微界面发生器2将微米级气泡输出至所述氢化塔1并与含蒽醌衍生物工作液在所述氢化塔混合形成气液乳化物,气液乳化物在催化剂的作用下发生氢化反应,生成含2-乙基氢蒽醌溶液的混合物。
具体而言,所述氢气进料管道11设置在在所述氢化塔1侧壁且与所述微界面发生器2相连,用以将氢气输送至第一微界面发生器以使第一微界面发生器对氢气进行破碎,形成微米尺度的微米级气泡,并与含蒽醌衍生物工作液混合,可以理解的是,所述氢气进料管道11的材质和尺寸本实施例均不做具体限制,只要满足所述氢气进料管道11能够在指定时间内输送指定体积的氢气即可。
请继续参阅图1所示,本发明所述微界面发生器2包括第一微界面发生器21和第二微界面发生器22。其中所述第一微界面发生器21设置在所述反应区底部,用以将氢气破碎形成微米尺度的微米级气泡。所述第二微界面发生器22设置在所述反应区底部,用以将氧气破碎形成微米尺度的微米级气泡。当氢化塔1运行时,所述第一微界面发生器21会将氢气破碎形成微米尺度的微米级气泡,并将微米级气泡与含蒽醌衍生物工作液混合形成气液乳化物,所述第二微界面发生器22用以将氧气破碎形成微米尺度的微米级气泡,并与氧化塔内的2-乙基氢蒽醌溶液混合形成气液乳化物。
具体而言,本发明所述第一微界面发生器21为气动式微界面发生器,其与所述氢气进料管道11相连,用以对氢气进料管道11输送的氢气进行破碎并形成微米尺度的微米级气泡。当所述氢化塔1在运行时,所述氢气进料管道11会将氢气输送至所述第一微界面发生器21,第一微界面发生器21会将氢气破碎并形成微米尺度的微米级气泡,并在破碎完成后将微米级气泡输出至氢化塔、并与氢化塔内的含蒽醌衍生物工作液混合形成气液乳化物以充分反应。
具体而言,本发明所述第二微界面发生器22为气动式微界面发生器,其与所述空气进料管道相连,用以对空气进料管道输送的空气进行破碎并形成微米尺度的微米级气泡。当所述氧化塔2在运行时,所述空气进料管道会将空气输送至所述第二微界面发生器22,第二微界面发生器22会将空气破碎并形成微米尺度的微米级气泡,并在破碎完成后将微米级气泡输出至氧化塔、并与氧化塔内的含2-乙基氢蒽醌氢化液混合形成气液乳化物以充分反应。
请继续参阅图1所示,本发明所述过滤冷却单元3包括过滤器31、换热器32和氢化冷却器33。其中所述过滤器31设置在所述氢化塔1侧壁上部且与所述气液分离器12的液体输出端相连,用以对氢化塔输出的氢化物料进行过滤,以滤除物料中夹带的固体杂质,所述换热器32与所述过滤器31相连,用以对过滤器输出的物料与含蒽醌衍生物工作液进行换热,以使含蒽醌衍生物工作液维持在预设温度范围内。所述氢化冷却器33设置在所述氢化塔1侧壁中部且与所述换热器32相连,用以对换热后物料进行冷却处理,当过滤冷却单元3运行时,所述过滤器31会接收气液分离器12排出的液相组分,并将液相组分内固体杂质过滤,含2-乙基氢蒽醌的滤液进入换热器32与含蒽醌衍生物工作液进行换热,然 后所述氢化冷却器33会接收换热器32排出的2-乙基氢蒽醌氢化液,并对溶液进行冷却处理,可以理解的是,所述过滤器31、换热器32和氢化冷却器33的型号及功率本实施例均不作具体限制,只要满足过滤器31、换热器32和氢化冷却器33能够达到其指定的工作状态即可。
请继续参阅图1所示,本发明所述氧化塔4包括空气进料管道41、氢化液进料管道42、回流管43、循环泵44、第二尾气出口45和出料口46。所述空气进料管道41设置在所述氧化塔4侧壁且与所述第二微界面发生器22相连,用以将空气输送至第二微界面发生器以使第二微界面发生器对空气进行破碎。所述氢化液进料管道42设置在所述氧化塔4侧壁并位于所述空气进料管道41上方,用以将2-乙基氢蒽醌溶液输送至氧化塔4内部;所述回流管43设置在所述氧化塔4侧壁,用以对氧化塔输出的物料回流至氧化塔内,以使物料中2-乙基氢蒽醌溶液充分反应。所述循环泵44与所述回流管43相连,用以对回流管输出的物料提供回输动力,所述第二尾气出口45,设置在所述氧化塔顶部,用以排出空气,所述出料口46,设置在所述氧化塔侧壁,用以将2-乙基蒽醌和过氧化氢的混合物排出。通过所述空气进料管道41向氧化塔4内输送空气,所述空气进料管道41与所述第二微界面发生器22相连,所述第二微界面22发生器对空气进行破碎,形成微米尺度的微米级气泡,破碎完成后,所述第二微界面发生器22将微米级气泡输出至所述氧化塔4并与2-乙基氢蒽醌溶液在所述氧化塔混合形成气液乳化物,气液乳化物充分反应,生产含2-乙基蒽醌和过氧化氢的混合物。
请继续参阅图1所示,本发明所述萃取塔5包括纯水进料管道51、加热器52、纯水加酸计量泵53、纯水泵54和双氧水出料管道55。其中所述纯水进料管道51设置在所述萃取塔顶部,用以将纯水传输至萃取塔内部。所述加热器52与所述纯水进料管道相连,用以对纯水进行预热处理。所述纯水加酸计量泵53,与所述纯水进料管道相连且位于所述加热器下方,用以加入磷酸对纯水酸度进行调节。所述纯水泵54与所述纯水进料管道相连且位于所述纯水加酸计量泵下方,用以对纯水进行传输。所述双氧水出料管道55设置在所述萃取塔底部,用以输出双氧水。萃取塔5运行时,纯水通过所述纯水泵54传输至所述加热器52内,并通过所述纯水加酸计量泵53调节对纯水酸度进行调节,预热后的纯水沿所述纯水进料管道51进入所述萃取塔5内部,与2-乙基蒽醌和过氧化氢的混合物发 生萃取,萃取后的双氧水沿所述双氧水出料管道55输出所述萃取塔5。可以理解的是,所述加热器52、纯水加酸计量泵53和纯水泵54的型号及功率本实施例均不作具体限制,只要满足加热器52、纯水加酸计量泵53和纯水泵54能够达到其指定的工作状态即可。
为了使本发明的目的和优点更加清楚明白,下面结合实施例对本发明作进一步描述;应当理解,此处所描述的具体实施例仅仅用于解释本发明,并不用于限定本发明。
一种基于蒽醌法制备双氧水的工艺,包括:
步骤1:通过所述工作液进料管道向所述氢化塔内输送含蒽醌衍生物工作液,并通过所述催化剂进料口将催化剂输送至所述氢化塔内;
步骤2:通过所述氢气进料管道向所述氢化塔内输送氢气,所述氢气进料管道会将氢气输送至所述第一微界面发生器,所述第一微界面发生器对氢气进行破碎,形成微米尺度的微米级气泡,破碎完成后,所述第一微界面发生器将微米级气泡输出至所述氢化塔并与含蒽醌衍生物工作液混合形成气液乳化物;
步骤3:气液乳化物在催化剂的作用下发生氢化反应,生成含2-乙基氢蒽醌溶液的混合物,反应完成后,混合物向上流动进入所述气液分离器;
步骤4:混合物进入所述气液分离器后,尾气由所述气液分离器顶部排出,含2-乙基氢蒽醌氢化液由所述气液分离器侧面排出并进入所述过滤冷却单元;
步骤5:含2-乙基氢蒽醌氢化液进入所述过滤器后,含2-乙基氢蒽醌氢化液中夹带的固体杂质残留在所述过滤器内,含2-乙基氢蒽醌氢化液中滤液由所述过滤器底部排出并进入所述换热器内,所述换热器内含2-乙基氢蒽醌氢化液与含蒽醌衍生物工作液进行热交换,热交换后的含蒽醌衍生物工作液并流入所述工作液进料管道,热交换后的含2-乙基氢蒽醌氢化液进入所述氢化冷却器内,冷却后的含2-乙基氢蒽醌氢化液进入所述氧化塔;
步骤6:通过所述氢化液进料管道向所述氧化塔内输送含2-乙基氢蒽醌氢化液,所述空气进料管道会将空气输送至所述第二微界面发生器,所述第二微界面发生器对空气进行破碎,形成微米尺度的微米级气泡,破碎完成后,所述第二微界面发生器将微米级气泡输出至所述氧化塔并与含2-乙基氢蒽醌氢化液混合形成气液乳化物;
步骤7:气液乳化物发生氧化反应,生成含2-乙基蒽醌和过氧化氢的混合物,反应完成后,混合物向上流动并沿所述回流管回流至氧化塔,少量尾气向上运动并通过所述第二尾气出口排出,排出尾气后的2-乙基蒽醌和过氧化氢的混合物通过所述出料口输出所述氧化塔;
步骤8:2-乙基蒽醌和过氧化氢的混合物通过出料口传输至所述萃取塔底部,纯水通过所述纯水泵传输至所述加热器内,并通过所述纯水加酸计量泵调节对纯水酸度进行调节,预热后的纯水沿所述纯水进料管道进入所述萃取塔内部,与2-乙基蒽醌和过氧化氢的混合物发生萃取,萃取后的双氧水沿所述双氧水出料管道输出所述萃取塔。
其中,所述含蒽醌衍生物工作液由2-乙基蒽醌(EAQ)、重芳烃(AR)和及磷酸三辛酯组成。可以理解的是,可以根据不同的产品要求或不同的催化剂,而灵活地进行预设操作条件的范围调整,以确保反应的充分有效进行,进而保证反应速率,达到了强化反应的目的。同时,本实施例中不具体限定催化剂的种类,只要能够确保强化反应顺利进行即可。
实施例1
使用上述系统及工艺进行蒽醌法制备双氧水,其中:
所述工艺中氢化塔内的反应温度为38℃,反应压强为0.05MPa,蒽醌含量220g/L,含蒽醌衍生物工作液流速130h -1,所述第一微界面发生器内的气液比为300:1。
所述工艺中氧化塔内的反应温度为35℃,反应压强为0.10MPa,含2-乙基氢蒽醌氢化液流速140h -1,所述第二微界面发生器内的气液比为400:1。
经检测,使用所述系统及工艺后,氢化效率14.2g/L,氧化效率13.9g/L,氧化反应转化率97.9%。
实施例2
使用上述系统及工艺进行蒽醌法制备双氧水,其中:
所述工艺中氢化塔内的反应温度为39℃,反应压强为0.15MPa,蒽醌含量235g/L,含蒽醌衍生物工作液流速135h -1,所述第一微界面发生器内的气液比为 350:1。
所述工艺中氧化塔内的反应温度为37℃,反应压强为0.13MPa,含2-乙基氢蒽醌氢化液流速145h -1,所述第二微界面发生器内的气液比为420:1。
经检测,使用所述系统及工艺后,氢化效率14.6g/L,氧化效率14.3g/L,氧化反应转化率97.9%。
实施例3
使用上述系统及工艺进行蒽醌法制备双氧水,其中:
所述工艺中氢化塔内的反应温度为42℃,反应压强为0.30MPa,蒽醌含量245g/L,含蒽醌衍生物工作液流速147h -1,所述第一微界面发生器内的气液比为400:1。
所述工艺中氧化塔内的反应温度为40℃,反应压强为0.15MPa,含2-乙基氢蒽醌氢化液流速152h -1,所述第二微界面发生器内的气液比为450:1。
经检测,使用所述系统及工艺后,氢化效率14.7g/L,氧化效率14.4g/L,氧化反应转化率98.0%。
实施例4
使用上述系统及工艺进行蒽醌法制备双氧水,其中:
所述工艺中氢化塔内的反应温度为45℃,反应压强为0.40MPa,蒽醌含量248g/L,含蒽醌衍生物工作液流速150h -1,所述第一微界面发生器内的气液比为470:1。
所述工艺中氧化塔内的反应温度为43℃,反应压强为0.18MPa,含2-乙基氢蒽醌氢化液流速154h -1,所述第二微界面发生器内的气液比为460:1。
经检测,使用所述系统及工艺后,氢化效率14.8g/L,氧化效率14.6g/L,氧化反应转化率98.6%。
实施例5
使用上述系统及工艺进行蒽醌法制备双氧水,其中:
所述工艺中氢化塔内的反应温度为48℃,反应压强为0.50MPa,蒽醌含量 260g/L,含蒽醌衍生物工作液流速160h -1,所述第一微界面发生器内的气液比为500:1。
所述工艺中氧化塔内的反应温度为45℃,反应压强为0.20MPa,含2-乙基氢蒽醌氢化液流速160h -1,所述第二微界面发生器内的气液比为500:1。
经检测,使用所述系统及工艺后,氢化效率14.9g/L,氧化效率14.7g/L,氧化反应转化率98.6%。
对比例
使用现有技术进行蒽醌法制备双氧水,其中,本实施例选用的工艺参数与所述实施例4中的工艺参数相同。
经检测,使用所述系统及工艺后,使用所述系统及工艺后,氢化效率10.7g/L,氧化效率9.9g/L,氧化反应转化率73.8%。
至此,已经结合附图所示的优选实施方式描述了本发明的技术方案,但是,本领域技术人员容易理解的是,本发明的保护范围显然不局限于这些具体实施方式。在不偏离本发明的原理的前提下,本领域技术人员可以对相关技术特征做出等同的更改或替换,这些更改或替换之后的技术方案都将落入本发明的保护范围之内。
以上所述仅为本发明的优选实施例,并不用于限制本发明;对于本领域的技术人员来说,本发明可以有各种更改和变化。凡在本发明的精神和原则之内,所作的任何修改、等同替换、改进等,均应包含在本发明的保护范围之内。

Claims (10)

  1. 一种基于蒽醌法制备双氧水的系统,其特征在于,包括:
    氢化塔,用以为含蒽醌衍生物工作液与氢气提供反应场所;
    过滤冷却单元,其设置在所述氢化塔侧壁,用以对氢化塔输出的氢化物料进行过滤并进行冷却;
    氧化塔,与所述过滤冷却单元相连,用以为过滤冷却单元输出的物料与氧气提供反应场所;
    萃取塔,用以对氧化塔输出的物料进行萃取分离;
    微界面发生器,其设置在所述氢化塔和所述氧化塔内的指定位置,将气体的压力能和/或液体的动能转变为气泡表面能并传递给氢气,使氢气破碎形成直径≥1μm、且<1mm的微米级气泡以提高含蒽醌衍生物工作液与氢气间的传质面积,减小液膜厚度,降低传质阻力,并在破碎后将含蒽醌衍生物工作液与微米级气泡混合形成气液乳化物,以在预设操作条件范围内强化含蒽醌衍生物工作液与氢气间的传质效率和反应效率。
  2. 根据权利要求1所述的基于蒽醌法制备双氧水的系统,其特征在于,所述微界面发生器包括:
    第一微界面发生器,所述第一微界面发生器设置在所述氢化塔反应区底部,用以将氢气破碎形成微米尺度的微米级气泡并在破碎完成后将微米级气泡输出至氢化塔、并与氢化塔内的含蒽醌衍生物工作液混合形成气液乳化物;
    第二微界面发生器,所述第二微界面发生器设置在所述氧化塔反应区底部,用以将氧气破碎形成微米尺度的微米级气泡并在破碎完成后将微米级气泡输出至氢化塔、并与氧化塔内的2-乙基氢蒽醌溶液混合形成气液乳化物。
  3. 根据权利要求1所述的基于蒽醌法制备双氧水的系统,其特征在于,所述氢化塔包括:
    氢气进料管道,其设置在所述氢化塔侧壁且与所述第一微界面发生器相连,用以将氢气输送至第一微界面发生器以使第一微界面发生器对氢气进行破碎;
    工作液进料管道,其设置在所述氢气塔侧壁并位于所述氢气进料管道上方,用以将含蒽醌衍生物工作液输送至氢化塔内部;
    催化剂进料口,其设置在所述氢化塔侧壁并位于所述工作液进料管道上方,用以将催化剂放至氢化塔内;
    第一尾气出口,其设置在所述氢化塔顶部,用以排出尾气。
  4. 根据权利要求1所述的基于蒽醌法制备双氧水的系统,其特征在于,所述氧化塔包括:
    空气进料管道,其设置在所述氧化塔侧壁且与所述第二微界面发生器相连,用以将空气输送至第二微界面发生器以使第二微界面发生器对空气进行破碎;
    氢化液进料管道,其设置在所述氧化塔侧壁并位于所述空气进料管道上方,用以将2-乙基氢蒽醌溶液输送至氧化塔内部;
    回流管,其设置在所述氧化塔侧壁,用以对氧化塔输出的物料回流至氧化塔内,以使物料中2-乙基氢蒽醌溶液充分反应;
    循环泵,其与所述回流管相连,用以对回流管输出的物料提供回输动力;
    第二尾气出口,设置在所述氧化塔顶部,用以排出空气;
    出料口,设置在所述氧化塔侧壁,用以将2-乙基蒽醌和过氧化氢的混合物排出。
  5. 根据权利要求1所述的基于蒽醌法制备双氧水的系统,其特征在于,所述过滤冷却单元包括:
    过滤器,其设置在所述氢化塔侧壁上部且与所述气液分离器的液体输出端相连,用以对氢化塔输出的氢化物料进行过滤,以滤除物料中夹带的固体杂质;
    换热器,其与所述过滤器相连,用以对过滤器输出的物料与含蒽醌衍生物工作液进行换热以使含蒽醌衍生物工作液维持在预设温度范围内;
    氢化冷却器,其设置在所述氢化塔侧壁中部且与所述换热器相连,用以对换热后物料进行冷却处理。
  6. 根据权利要求1所述的基于蒽醌法制备双氧水的系统,其特征在于,所述萃取塔包括:
    纯水进料管道,其设置在所述萃取塔顶部,用以将纯水传输至萃取塔内部;
    加热器,其与所述纯水进料管道相连,用以对纯水进行预热处理;
    纯水加酸计量泵,其与所述纯水进料管道相连且位于所述加热器下方,用以加入磷酸对纯水酸度进行调节;
    纯水泵,其与所述纯水进料管道相连且位于所述纯水加酸计量泵下方,用以对纯水进行传输;
    双氧水出料管道,其设置在所述萃取塔底部,用以输出双氧水。
  7. 一种基于蒽醌法制备双氧水的工艺,其特征在于,包括:
    步骤1:通过所述工作液进料管道向所述氢化塔内输送含蒽醌衍生物工作液,并通过所述催化剂进料口将催化剂输送至所述氢化塔内;
    步骤2:通过所述氢气进料管道向所述氢化塔内输送氢气,所述氢气进料管道会将氢气输送至所述第一微界面发生器,所述第一微界面发生器对氢气进行破碎,形成微米尺度的微米级气泡,破碎完成后,所述第一微界面发生器将微米级气泡输出至所述氢化塔并与含蒽醌衍生物工作液混合形成气液乳化物;
    步骤3:气液乳化物在催化剂的作用下发生氢化反应,生成含2-乙基氢蒽醌溶液的混合物,反应完成后,混合物向上流动进入所述气液分离器;
    步骤4:混合物进入所述气液分离器后,尾气由所述气液分离器顶部排出,含2-乙基氢蒽醌氢化液由所述气液分离器侧面排出并进入所述过滤冷却单元;
    步骤5:含2-乙基氢蒽醌氢化液进入所述过滤器后,含2-乙基氢蒽醌氢化液中夹带的固体杂质残留在所述过滤器内,含2-乙基氢蒽醌氢化液中滤液由所述过滤器底部排出并进入所述换热器内,所述换热器内含2-乙基氢蒽醌氢化液与含蒽醌衍生物工作液进行热交换,热交换后的含蒽醌衍生物工作液并流入所述工作液进料管道,热交换后的含2-乙基氢蒽醌氢化液进入所述氢化冷却器内,冷却后的含2-乙基氢蒽醌氢化液进入所述氧化塔;
    步骤6:通过所述氢化液进料管道向所述氧化塔内输送含2-乙基氢蒽醌氢化液,所述空气进料管道会将空气输送至所述第二微界面发生器,所述第二微界面发生器对空气进行破碎,形成微米尺度的微米级气泡,破碎完成后,所述第二微界面发生器将微米级气泡输出至所述氧化塔并与含2-乙基氢蒽醌氢化液混合形成气液乳化物;
    步骤7:气液乳化物发生氧化反应,生成含2-乙基蒽醌和过氧化氢的混合物,反应完成后,混合物向上流动并沿所述回流管回流至氧化塔,少量尾气向上运动并通过所述第二尾气出口排出,排出尾气后的2-乙基蒽醌和过氧化氢的混合物通过所述出料口输出所述氧化塔;
    步骤8:2-乙基蒽醌和过氧化氢的混合物通过出料口传输至所述萃取塔底部,纯水通过所述纯水泵传输至所述加热器内,并通过所述纯水加酸计量泵调节 对纯水酸度进行调节,预热后的纯水沿所述纯水进料管道进入所述萃取塔内部,与2-乙基蒽醌和过氧化氢的混合物发生萃取,萃取后的双氧水沿所述双氧水出料管道输出所述萃取塔。
  8. 根据权利要求7所述的基于蒽醌法制备双氧水的工艺,其特征在于,所述工艺中氢化塔内的反应温度为38-48℃,反应压强为0.05-0.50MPa。
  9. 根据权利要求7所述的基于蒽醌法制备双0氧水的工艺,其特征在于,所述工艺中氧化塔内的反应温度为35-45℃,反应压强为0.10-0.20MPa。
  10. 根据权利要求7所述的基于蒽醌法制备双氧水的工艺,其特征在于,所述第一微界面发生器内的气液比为300-500:1,所述第二微界面发生器内的气液比为400-500:1。
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