WO2021047046A1 - Microinterface-enhanced system and process for preparing ethylene oxide from ethylene - Google Patents

Microinterface-enhanced system and process for preparing ethylene oxide from ethylene Download PDF

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WO2021047046A1
WO2021047046A1 PCT/CN2019/120185 CN2019120185W WO2021047046A1 WO 2021047046 A1 WO2021047046 A1 WO 2021047046A1 CN 2019120185 W CN2019120185 W CN 2019120185W WO 2021047046 A1 WO2021047046 A1 WO 2021047046A1
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gas
micro
ethylene
reactor
hypochlorous acid
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French (fr)
Chinese (zh)
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张志炳
张锋
周政
李磊
孟为民
王宝荣
杨高东
罗华勋
杨国强
田洪舟
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南京延长反应技术研究院有限公司
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    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07D—HETEROCYCLIC COMPOUNDS
    • C07D303/00—Compounds containing three-membered rings having one oxygen atom as the only ring hetero atom
    • C07D303/02—Compounds containing oxirane rings
    • C07D303/04—Compounds containing oxirane rings containing only hydrogen and carbon atoms in addition to the ring oxygen atoms
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
    • B01D3/007—Energy recuperation; Heat pumps
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
    • B01D3/009—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping in combination with chemical reactions
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
    • B01D3/14—Fractional distillation or use of a fractionation or rectification column
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/0093—Microreactors, e.g. miniaturised or microfabricated reactors
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J8/00—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J8/00—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
    • B01J8/08—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with moving particles
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J8/00—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
    • B01J8/18—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with fluidised particles
    • B01J8/20—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with fluidised particles with liquid as a fluidising medium
    • B01J8/22—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with fluidised particles with liquid as a fluidising medium gas being introduced into the liquid
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B11/00—Oxides or oxyacids of halogens; Salts thereof
    • C01B11/04—Hypochlorous acid
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C29/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
    • C07C29/64—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring by simultaneous introduction of -OH groups and halogens
    • C07C29/66—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring by simultaneous introduction of -OH groups and halogens by addition of hypohalogenous acids, which may be formed in situ, to carbon-to-carbon unsaturated bonds
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C31/00—Saturated compounds having hydroxy or O-metal groups bound to acyclic carbon atoms
    • C07C31/34—Halogenated alcohols
    • C07C31/36—Halogenated alcohols the halogen not being fluorine
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07D—HETEROCYCLIC COMPOUNDS
    • C07D301/00—Preparation of oxiranes
    • C07D301/02—Synthesis of the oxirane ring
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07D—HETEROCYCLIC COMPOUNDS
    • C07D301/00—Preparation of oxiranes
    • C07D301/02—Synthesis of the oxirane ring
    • C07D301/24—Synthesis of the oxirane ring by splitting off HAL—Y from compounds containing the radical HAL—C—C—OY
    • C07D301/26—Y being hydrogen
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07D—HETEROCYCLIC COMPOUNDS
    • C07D301/00—Preparation of oxiranes
    • C07D301/32—Separation; Purification
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07D—HETEROCYCLIC COMPOUNDS
    • C07D303/00—Compounds containing three-membered rings having one oxygen atom as the only ring hetero atom
    • C07D303/02—Compounds containing oxirane rings
    • C07D303/12—Compounds containing oxirane rings with hydrocarbon radicals, substituted by singly or doubly bound oxygen atoms

Definitions

  • the invention relates to the technical field of preparing ethylene oxide from ethylene, in particular to a micro-interface strengthening system and process for preparing ethylene oxide from ethylene.
  • Ethylene oxide is one of the simplest cyclic ethers. It is a heterocyclic compound. It is a colorless and transparent liquid at a low temperature below 10.7°C, and a colorless gas at room temperature and pressure. It is irritating to eyes, throat and nose when exposed to ethylene oxide gas. Its lively nature is an important organic chemical product second only to polyethylene and polyvinyl chloride in the ethylene industry derivatives. It is a versatile organic synthesis intermediate. The ethylene oxide produced in the industry can be divided into bulk rings according to its purity. Ethylene oxide and high-purity ethylene oxide are mainly used in the production of ethylene glycol and ethoxylates in the detergent industry.
  • ethylene oxide has the characteristics of broad-spectrum, high-efficiency, and low-temperature sterilization, it is also used as a fumigant, insecticide, fungicide, and disinfectant for disposable medical devices. Due to its wide range of uses, it leads to epoxy The ethane market is in strong demand.
  • the main production methods of ethylene oxide are the chlorohydrin method and the direct ethylene oxidation method.
  • the chlorohydrin method is the earliest industrial method for preparing ethylene oxide.
  • the chlorohydrin method includes two reactions:
  • the first step is to pass ethylene and chlorine into the water to generate 2-chloroethanol
  • the second step is to react with alkali (usually milk of lime) and 2-chloroethanol to produce ethylene oxide.
  • alkali usually milk of lime
  • 2-chloroethanol to produce ethylene oxide.
  • the ethylene is hypochlorous acidified to produce chloroethanol, and then saponified with calcium hydroxide to produce crude ethylene oxide. Fractional distillation produces ethylene oxide.
  • Cipheral Patent Publication Number: CN103896882A discloses a method for preparing ethylene oxide by the chlorohydrin method. Ethylene and chlorine are used as raw materials. The main process is divided into two steps. The first step is the reaction of chlorine and water to form hypochlorous acid.
  • the reaction molar ratio of hypochlorous acid and ethylene is 1:0.5-1; produces chloroethanol; the second step chloroethanol is saponified to produce ethylene oxide; reactor for producing ethylene oxide by chlorohydrin method
  • the most resident organization uses the tower type, water and chlorine enter from the bottom of the tower to generate hypochlorous acid; ethylene is passed in from a high place, reacts with hypochlorous acid to produce chloroethanol, and overflows from the top of the tower
  • the aqueous solution of chloroethanol, the reaction temperature is 10-50 degrees, normal pressure; the saponification process can be carried out in a kettle or tower reactor, using lime milk as the saponifying agent, the reaction temperature is 100-102 degrees, and the residence time is about 30 It can be saponified completely within minutes; the tower reactor is used as a distillation tower.
  • the chloroethanol solution and the lime milk are added into the tower at the same time, and the light component ethylene oxide is steamed from the top of the tower, and the calcium chloride containing organic matter is discharged from the tower.
  • Aqueous solution It can be seen that the method has the following problems:
  • the reaction rate of ethylene and hypochlorous acid is reduced, which leads to a decrease in ethylene utilization rate, which largely causes a waste of raw materials, increases the production cost of ethylene oxide, and does not meet the requirements of the existing circular economy.
  • the present invention provides a micro-interface strengthening system and process for preparing ethylene oxide from ethylene to overcome the problem of low system reaction efficiency caused by uneven mixing of materials and by-products in the prior art.
  • the present invention provides a micro-interface strengthening system for preparing ethylene oxide from ethylene, which includes:
  • the hypochlorous acid synthesis unit is used to provide a reaction place for chlorine and water, and to separate the generated materials;
  • the chlorohydrinization reaction unit is connected to the hypochlorous acid synthesis unit to provide a reaction place for the output material of the hypochlorous acid synthesis unit and ethylene;
  • the saponification reaction unit is connected to the chlorohydrin reaction unit and is used to provide a reaction place for the chlorohydrin reaction unit to output liquid phase materials and lime milk;
  • a separation and purification unit connected to the saponification reaction unit, for rectifying and separating the output liquid phase materials
  • the number of micro-interface generators is two, which are respectively installed in the hypochlorous acid synthesis unit and the chlorohydrin reaction unit, and convert the pressure energy of the gas and/or the kinetic energy of the liquid into the surface energy of the bubble and transfer it to
  • the gas phase component breaks the gas phase gas to form micron-sized bubbles with a diameter of ⁇ 1 ⁇ m and ⁇ 1mm to increase the mass transfer area of the gas phase component and the liquid phase component, reduce the thickness of the liquid film, and reduce the mass transfer resistance, and after crushing
  • the liquid phase component is mixed with micron-sized bubbles to form a gas-liquid emulsion to enhance the mass transfer efficiency and reaction efficiency of the gas-liquid component within the preset operating condition range.
  • micro-interface generator is a pneumatic micro-interface generator, and the micro-interface generator includes a first micro-interface generator and a second micro-interface generator;
  • the first micro-interface generator is arranged at the bottom of the reaction zone of the hypochlorous acid synthesis unit, and is used to crush the chlorine gas to form micron-scale micron-scale bubbles and output the micron-scale bubbles to the hypochlorous acid synthesis unit after the crushing is completed It is mixed with water to form a gas-liquid emulsion;
  • the second micro-interface generator is arranged at the bottom of the reaction zone of the chlorohydrin reaction unit, and is used to crush ethylene to form micron-sized micro-sized bubbles and output the micro-sized bubbles to the chlorohydrin reaction unit after the crushing is completed.
  • the output liquid phase material of the hypochlorous acid synthesis unit is mixed to form a gas-liquid emulsion.
  • hypochlorous acid synthesis unit includes:
  • the gas-phase feed pipeline is arranged on the side wall of the hypochlorous acid reactor and connected to the first micro-interface generator, and is used to transport chlorine gas into the first micro-interface generator and make the micro-interface generator Crush the chlorine gas;
  • a liquid-phase feed pipe which is arranged on the side wall of the hypochlorous acid reactor and above the gas-phase feed pipe, to transport water into the hypochlorous acid reactor;
  • hypochlorous acid synthesis unit further includes:
  • a first gas-phase reflux pipe which is arranged on the hypochlorous acid reactor and connected to the first micro-interface generator, for returning the gas phase components to the hypochlorous acid reactor;
  • the gas-liquid separator is connected with the hypochlorous acid reactor and is used for gas-liquid separation of the output materials of the hypochlorous acid reactor.
  • chlorohydrin reaction unit includes:
  • the chlorohydrinization reactor is connected to the gas-liquid separator to provide a reaction place for hypochlorous acid and ethylene;
  • the ethylene feed pipe is arranged on the side wall of the chlorohydrin reactor and connected to the second micro-interface generator, and is used to transport ethylene into the second micro-interface generator and make the micro-interface generator pair Ethylene is crushed;
  • chlorohydrin reaction unit further includes:
  • the second gas-phase reflux pipe is arranged on the chlorohydrin reactor and connected with the second micro-interface generator, and is used for returning the gas-phase components to the chlorohydrin reactor.
  • the saponification reaction unit includes:
  • the saponification reactor is connected to the chlorohydrinization reactor and is used to provide a reaction place for the chlorohydrinization reaction unit to output liquid phase materials and lime milk;
  • the lime milk feed pipe is arranged on the side wall of the saponification reactor to transport the lime milk into the saponification reactor.
  • the separation and purification unit includes:
  • a heat exchanger which is connected to the saponification reaction unit, and is used to exchange energy between the output material of the saponification reaction unit and ethylene oxide;
  • a rectification tower which is connected with the heat exchanger, is used for rectifying and separating the output materials of the saponification reaction unit.
  • a micro-interface strengthening process for preparing ethylene oxide from ethylene includes:
  • Step 1 Transport water into the hypochlorous acid reactor through the liquid-phase feed pipeline
  • Step 2 Transport chlorine gas into the hypochlorous acid reactor through the gas-phase feed pipe, the gas-phase feed pipe will transport the chlorine gas to the first micro-interface generator, and the first micro-interface
  • the device crushes the chlorine gas to form micron-sized bubbles.
  • the first micro-interface generator outputs the micron-sized bubbles to the hypochlorous acid reactor and mixes with water to form a gas-liquid emulsion.
  • the liquid emulsion reacts to form a mixture of hypochlorous acid;
  • Step 3 The under-reacted chlorine gas in the hypochlorous acid reactor flows back into the first micro-interface generator along the first gas-phase reflux pipe on the top of the hypochlorous acid reactor, and passes through the first micro-interface The generator breaks the chlorine gas and further reacts with water;
  • Step 4 The liquid phase components in the hypochlorous acid reactor flow into the gas-liquid separator. After gas-liquid separation, the tail gas is discharged along the gas-phase outlet at the top of the gas-liquid separator, and the hypochlorous acid solution flows along the gas-liquid separator. The liquid phase outlet at the bottom of the separator is discharged and transferred to the chlorohydrin reaction unit;
  • Step 5 The hypochlorous acid solution enters the chlorohydrinization reactor, and ethylene is transported into the chlorohydrinization reactor through the ethylene feed pipe, and the ethylene feed pipe will transport ethylene gas to the second micro An interface generator, wherein the second micro-interface generator breaks ethylene to form micro-scale bubbles of micron scale;
  • Step 6 After the crushing is completed, the second micro-interface generator outputs micron-sized bubbles to the chlorohydrinization reactor and mixes them with the hypochlorous acid solution to form a gas-liquid emulsion, and the gas-liquid emulsion reacts to produce chloroethanol Solution, the chloroethanol solution in the chlorohydrinization reactor flows out and is transferred to the saponification reaction unit;
  • Step 7 Under-reacted ethylene in the chlorohydrinization reactor flows back into the second micro-interface generator along the second gas-phase reflux pipe on the top of the chlorohydrin reactor, and passes through the second micro-interface generator Crush the ethylene and further react with the hypochlorous acid solution;
  • Step 8 The chloroethanol solution flows into the saponification reaction unit, and the lime milk is transferred into the saponification reaction unit through the lime milk feed pipe.
  • the lime milk and the chloroethanol solution undergo a saponification reaction in the saponification reaction unit to produce a ring Oxyethane mixture, where the ethylene oxide mixture flows out in the saponification reaction and is transferred to the separation and purification unit;
  • Step 9 The ethylene oxide mixture flows into the separation and purification unit, where the ethylene oxide mixture flows through the heat exchanger and enters the rectification tower for rectification, and the gas phase material output from the rectification tower is ethylene oxide Alkane gas and other waste water are discharged along the bottom of the rectification tower, wherein the ethylene oxide gas exchanges heat with the ethylene oxide mixture in the heat exchanger and is discharged to obtain an ethylene oxide product.
  • reaction temperature in the hypochlorous acid reactor is 10-20°C and normal pressure
  • gas-liquid ratio in the first micro-interface generator is 120-130:1;
  • the reaction temperature in the chlorohydrinization reactor is 37-47°C
  • the reaction pressure is 0.13-0.19MPa
  • the gas-liquid ratio in the second micro-interface generator is 115-125:1;
  • the reaction temperature in the saponification reactor is 87-97°C and normal pressure.
  • the beneficial effect of the present invention is that the main structure of the system of the present invention is formed by the chlorohydrin reaction unit, the chlorohydrin reaction unit, the saponification reaction unit, the separation and purification unit, the micro-interface generator and the intelligent control unit.
  • the chlorine gas is broken to form micron-sized bubbles, and the micron-sized bubbles are mixed with water to form a gas-liquid emulsion to increase the area of the gas-liquid phase boundary, improve the synthesis efficiency of hypochlorous acid, improve the efficiency of chlorine reaction, and save Cost:
  • a hypochlorous acid synthesis unit is used to provide a reaction place for chlorine and water, and to separate the generated materials.
  • the chlorohydrin reaction unit is connected to the hypochlorous acid synthesis unit to output the hypochlorous acid synthesis unit
  • the material and ethylene provide a reaction place
  • the saponification reaction unit is connected to the chlorohydrin reaction unit to provide a reaction place for the chlorohydrin reaction unit to output liquid phase materials and lime milk
  • the separation and purification unit is connected to the saponification reaction unit to output the liquid phase.
  • the materials are separated by rectification. According to different product requirements, the chlorine gas can be flexibly adjusted in the range of preset operating conditions to ensure that the reaction is fully and effectively carried out, thereby ensuring the reaction rate, and achieving the purpose of strengthening the reaction.
  • the hypochlorous acid synthesis unit of the present invention is provided with a hypochlorous acid reactor, a gas-phase feed pipe, a liquid-phase feed pipe, a first gas-phase return pipe and a gas-liquid separator, so as to improve the hypochlorous acid reactor for chlorine and water.
  • a reaction place transport the chlorine gas into the first micro-interface generator through the gas-phase feed pipe, and make the micro-interface generator break the chlorine gas, and transport the water to the hypochlorous acid reactor through the liquid-phase feed pipe.
  • the first gas-phase reflux pipe returns the gas-phase components to the hypochlorous acid reactor, and performs gas-liquid separation of the output materials of the hypochlorous acid reactor through a gas-liquid separator to realize the efficient reaction of water and chlorine gas and improve the utilization rate of chlorine gas raw materials.
  • the chlorohydrin reaction unit of the present invention is equipped with a chlorohydrin reactor, an ethylene feed pipeline and a second gas phase return pipe.
  • the chlorohydrin reactor provides a reaction place for hypochlorous acid and ethylene, and the ethylene is fed through the ethylene feed pipeline. It is transported to the second micro-interface generator, and the micro-interface generator is used to crush the ethylene.
  • the gas-phase components are returned to the chlorohydrinization reactor through the second gas-phase reflux pipe to realize the high-efficiency reaction of ethylene and hypochlorous acid and improve the utilization rate of ethylene raw materials.
  • the saponification reaction unit of the present invention is provided with a saponification reactor and a lime milk feeding pipeline.
  • the saponification reactor provides a reaction place for the chlorohydrin reaction unit to output liquid phase materials and lime milk, and the lime milk is transported through the lime milk feeding pipeline.
  • ethylene oxide is obtained through the saponification reaction of chloroethanol and lime milk.
  • the separation and purification unit of the present invention is equipped with a heat exchanger and a rectification tower; the heat exchanger is used to exchange energy between the output material of the saponification reaction unit and ethylene oxide, and the output material of the saponification reaction unit is rectified through the rectification tower. Separation, in which the ethylene oxide gas exchanges heat with the ethylene oxide mixture in the heat exchanger, which improves energy utilization and saves energy consumption.
  • Fig. 1 is a schematic structural diagram of the system of the micro-interface strengthening system for preparing ethylene oxide from ethylene 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 micro-interface strengthening system for preparing ethylene oxide from ethylene according to the present invention, including a chlorohydrin reaction unit 1, a chlorohydrin reaction unit 2, a saponification reaction unit 3, and a separation and purification unit 4.
  • Micro-interface generator 5 The hypochlorous acid synthesis unit 1 is used to provide a reaction place for chlorine and water and separate the produced materials.
  • the chlorohydrin reaction unit 2 is connected to the hypochlorous acid synthesis unit 1 to synthesize hypochlorous acid
  • the unit output material and ethylene provide a reaction place.
  • the saponification reaction unit 3 is connected to the chlorohydrin reaction unit 2 to provide a reaction place for the liquid phase material output from the chlorohydrin reaction unit and lime milk.
  • the separation and purification unit 4 Connected to the saponification reaction unit for rectifying and separating the output liquid phase materials, and the micro-interface generator 5 is respectively arranged at the designated positions of the hypochlorous acid synthesis unit 1 and the chlorohydrin reaction unit 2, and The pressure energy of the gas and/or the kinetic energy of the liquid is transformed into the surface energy of the bubbles and transferred to the gas phase components, so that the gas phase gas is broken to form micron-sized bubbles with a diameter of ⁇ 1 ⁇ m and ⁇ 1mm.
  • the gas-phase components of the micro-interface generator 5 are broken to form micro-sized micro-sized bubbles and the mixture of the micro-sized bubbles and the liquid-phase components are mixed to form a gas-liquid emulsion.
  • the micro-interface generator 5 of the present invention can also be used in other multiphase reactions, such as via micro-interface, micro-nano interface, ultra-micro interface, micro-bubble biochemical reactor or micro-bubble biological Reactor and other equipment, 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-
  • the micro-interface generator 5 is a pneumatic micro-interface generator, and the micro-interface generator 5 includes a first micro-interface generator 51 and a second micro-interface generator 52;
  • the first micro-interface generator 51 is arranged at the bottom of the reaction zone of the hypochlorous acid synthesis unit 1, and is used to break the chlorine gas into micron-sized micro-sized bubbles and output the micro-sized bubbles to the hypochlorous acid after the crushing is completed. Mix with water in the synthesis unit to form a gas-liquid emulsion;
  • the gas-phase component chlorine of the first micro-interface generator 51 is broken to form micro-scale micro-sized bubbles, and the mixture of the micro-scale bubbles and the liquid-phase component water is mixed to form a gas-liquid emulsion;
  • the second micro-interface generator 52 is arranged at the bottom of the reaction zone of the chlorohydrin reaction unit 2, and is used to crush ethylene to form micro-scale micro-sized bubbles and output the micro-scale bubbles to the chlorohydrin reaction unit after the crushing is completed. It is mixed with the output liquid phase material of hypochlorous acid synthesis unit to form gas-liquid emulsion;
  • the gas-phase component ethylene of the second micro-interface generator 52 is broken to form micro-sized micro-sized bubbles and the mixture of the micro-sized bubbles and the liquid component hypochlorous acid is mixed to form a gas-liquid emulsion.
  • the hypochlorous acid synthesis unit 1 includes: a hypochlorous acid reactor 11, a gas-phase feed pipe 12, a liquid-phase feed pipe 13, a first gas-phase reflux pipe 14 and a gas-liquid separator 15;
  • the hypochlorous acid reactor 11 is used to provide a reaction place for chlorine and water;
  • the gas-phase feed pipe 12 is arranged on the side wall of the hypochlorous acid reactor 1 and is connected to the first micro-interface generator 51, and is used to transport chlorine gas into the first micro-interface generator and make the micro
  • the interface generator breaks the chlorine gas
  • the liquid-phase feed pipe 13 is arranged on the side wall of the hypochlorous acid reactor 1 and above the gas-phase feed pipe 11 to transport water into the hypochlorous acid reactor;
  • the first gas-phase reflux pipe 14 is arranged on the hypochlorous acid reactor 1 and connected to the first micro-interface generator 51 for returning the gas-phase components to the hypochlorous acid reactor;
  • the gas-liquid separator 15 is connected to the hypochlorous acid reactor 1 and is used for gas-liquid separation of the output material of the hypochlorous acid reactor;
  • the hypochlorous acid reactor 11 When the system is running, the hypochlorous acid reactor 11 is used as a reactor of chlorine and water, and the water is transported into the hypochlorous acid reactor 11 through the liquid-phase feed pipe 13 while the chlorine is transported through the gas-phase feed pipe 12 Into the first micro-interface generator 51, and make the first micro-interface generator 51 crush the chlorine gas to form micro-scale micro-scale bubbles.
  • the first micro-interface generator 51 outputs micro-scale bubbles To the hypochlorous acid reactor 11 and mix with water to form a gas-liquid emulsion, the gas-liquid emulsion reacts to form a hypochlorous acid mixture, and the insufficiently reacted chlorine in the hypochlorous acid reactor 1 follows the hypochlorous acid
  • the first gas phase return pipe 14 at the top of the acid reactor 1 flows back into the first micro-interface generator 51, and the chlorine gas is broken by the first micro-interface generator 51, and further reacts with water.
  • the liquid phase components in the acid reactor 1 flow into the gas-liquid separator 15.
  • the tail gas is discharged along the gas-phase outlet at the top of the gas-liquid separator 15, and the hypochlorous acid solution is discharged along the bottom of the gas-liquid separator 15
  • the liquid phase outlet is discharged and transferred to the chlorohydrin reaction unit 2.
  • the materials and dimensions of the gas phase feed pipe 12, the liquid phase feed pipe 13 and the first gas phase return pipe 14 are all in this embodiment. There is no specific limitation, as long as it is satisfied that the gas-phase feed pipe 12, the liquid-phase feed pipe 13 and the first gas-phase return pipe 14 can transport a specified volume of material within a specified time.
  • the chlorohydrin reaction unit 2 includes: a chlorohydrin reactor 21, an ethylene feed pipe 22, and a second gas phase return pipe 23;
  • the chlorohydrinization reactor 21 is connected to the gas-liquid separator 15 to provide a reaction place for hypochlorous acid and ethylene;
  • the ethylene feed pipe 22 is arranged on the side wall of the chlorohydrinization reactor 2 and is connected to the second micro-interface generator 52 to transport ethylene into the second micro-interface generator and make the micro-interface The generator crushes ethylene;
  • the second gas-phase reflux pipe 23 is arranged on the chlorohydrin reactor 2 and is connected to the second micro-interface generator 52 for returning the gas-phase components to the chlorohydrin reactor;
  • the hypochlorous acid solution enters the chlorohydrinization reactor 21, and transports ethylene into the chlorohydrinization reactor 21 through the ethylene feed pipe 22, and the ethylene feed pipe 22 will transport ethylene gas
  • the second micro-interface generator 52 crushes ethylene to form micro-scale bubbles. After the crushing is completed, the second micro-interface generator 52 removes the micro-scale bubbles.
  • the chlorohydrin solution in the chlorohydrinization reactor 21 flows out and is transferred to the saponification In reaction unit 3, under-reacted ethylene in the chlorohydrin reactor 21 flows back into the second micro-interface generator 52 along the second gas phase reflux pipe 23 at the top of the chlorohydrin reactor 21, and passes through the second micro-interface generator 52.
  • the second micro-interface generator 52 crushes ethylene and further reacts with the hypochlorous acid solution. It can be understood that the material and size of the ethylene feed pipe 22 and the second gas phase return pipe 23 are not used in this embodiment. The specific limitation is as long as it is satisfied that the ethylene feed pipe 22 and the second gas phase return pipe 23 can transport a specified volume of material within a specified time.
  • the saponification reaction unit 3 includes: a saponification reactor 31 and a lime milk feed pipe 32;
  • the saponification reactor 31 is connected to the chlorohydrinization reactor 21, and is used to provide a reaction place for the liquid phase material output from the chlorohydrinization reaction unit and the milk of lime;
  • the lime milk feed pipe 32 is arranged on the side wall of the saponification reactor 31 to transport the lime milk into the saponification reactor.
  • the chloroethanol solution flows into the saponification reaction unit 3, and transfers the milk of lime into the saponification reaction unit 31 through the milk of lime feed pipe 32.
  • the main component of the milk of lime is calcium hydroxide and has a strong alkali. Therefore, the lime milk and the chloroethanol solution undergo a saponification reaction in the saponification reaction unit 3 to produce an ethylene oxide mixture. In the saponification reaction, the ethylene oxide mixture flows out and is transferred to the separation and purification unit 4.
  • the separation and purification unit 4 includes: a heat exchanger 41 and a rectification tower 42;
  • the heat exchanger 41 is connected to the saponification reaction unit 3, and is used to exchange energy between the output material of the saponification reaction unit and ethylene oxide;
  • the rectification tower 42 is connected to the heat exchanger 41 for rectifying and separating the output materials of the saponification reaction unit;
  • the ethylene oxide mixture flows into the separation and purification unit 4, and the ethylene oxide mixture flows through the heat exchanger 41 and enters the rectification tower 42 for rectification.
  • the components have different volatility, that is, at the same temperature, the vapor pressure of each component is different, so that the light components in the liquid phase (low boilers) are transferred to the gas phase, while the heavy components in the gas phase (high boilers) are transferred to the gas phase.
  • the gas phase material output from the rectification tower 42 is ethylene oxide gas, and other waste water is discharged along the bottom of the rectification tower 42.
  • the ethylene oxide gas is discharged in the heat exchange
  • the heat exchange between the ethylene oxide mixture and the ethylene oxide mixture is carried out in the vessel 41.
  • the heat exchanger 41 realizes the heat transfer between the two fluids of the ethylene oxide product at different temperatures and the output material of the saponification reaction unit, so that the heat is transferred from the higher temperature.
  • the fluid is transferred to the fluid with a lower temperature, so that the fluid temperature reaches the target specified in the process, energy saving and emission reduction, that is, the ethylene oxide product is obtained.
  • the model and power of the heat exchanger 41 in this embodiment are both There is no specific limitation, as long as the heat exchanger 41 can reach its designated working state.
  • the rectification tower 42 can be of any kind of tray type and packed type, and the type and model of the rectification tower 42 are in this embodiment. There are no specific restrictions, as long as the rectification tower 42 can reach its designated working state.
  • a micro-interface strengthening process for preparing ethylene oxide from ethylene including:
  • Step 1 Transport water into the hypochlorous acid reactor through the liquid-phase feed pipeline
  • Step 2 Transport chlorine gas into the hypochlorous acid reactor through the gas-phase feed pipe, the gas-phase feed pipe will transport the chlorine gas to the first micro-interface generator, and the first micro-interface
  • the device crushes the chlorine gas to form micron-sized bubbles.
  • the first micro-interface generator outputs the micron-sized bubbles to the hypochlorous acid reactor and mixes with water to form a gas-liquid emulsion.
  • the liquid emulsion reacts to form a mixture of hypochlorous acid;
  • Step 3 The under-reacted chlorine gas in the hypochlorous acid reactor flows back into the first micro-interface generator along the first gas-phase reflux pipe on the top of the hypochlorous acid reactor, and passes through the first micro-interface The generator breaks the chlorine gas and further reacts with water;
  • Step 4 The liquid phase components in the hypochlorous acid reactor flow into the gas-liquid separator. After gas-liquid separation, the tail gas is discharged along the gas-phase outlet at the top of the gas-liquid separator, and the hypochlorous acid solution flows along the gas-liquid separator. The liquid phase outlet at the bottom of the separator is discharged and transferred to the chlorohydrin reaction unit;
  • Step 5 The hypochlorous acid solution enters the chlorohydrinization reactor, and ethylene is transported into the chlorohydrinization reactor through the ethylene feed pipe, and the ethylene feed pipe will transport ethylene gas to the second micro An interface generator, wherein the second micro-interface generator breaks ethylene to form micro-scale bubbles of micron scale;
  • Step 6 After the crushing is completed, the second micro-interface generator outputs micron-sized bubbles to the chlorohydrinization reactor and mixes them with the hypochlorous acid solution to form a gas-liquid emulsion, and the gas-liquid emulsion reacts to produce chloroethanol Solution, the chloroethanol solution in the chlorohydrinization reactor flows out and is transferred to the saponification reaction unit;
  • Step 7 Under-reacted ethylene in the chlorohydrinization reactor flows back into the second micro-interface generator along the second gas-phase reflux pipe on the top of the chlorohydrin reactor, and passes through the second micro-interface generator Crush the ethylene and further react with the hypochlorous acid solution;
  • Step 8 The chloroethanol solution flows into the saponification reaction unit, and the lime milk is transferred into the saponification reaction unit through the lime milk feed pipe.
  • the lime milk and the chloroethanol solution undergo a saponification reaction in the saponification reaction unit to produce a ring Oxyethane mixture, where the ethylene oxide mixture flows out in the saponification reaction and is transferred to the separation and purification unit;
  • Step 9 The ethylene oxide mixture flows into the separation and purification unit, where the ethylene oxide mixture flows through the heat exchanger and enters the rectification tower for rectification, and the gas phase material output from the rectification tower is ethylene oxide Alkane gas and other waste water are discharged along the bottom of the rectification tower, wherein the ethylene oxide gas exchanges heat with the ethylene oxide mixture in the heat exchanger and is discharged to obtain an ethylene oxide product.
  • reaction temperature in the hypochlorous acid reactor is 10°C and normal pressure
  • the gas-liquid ratio in the first micro-interface generator is 120:1;
  • the reaction temperature in the chlorohydrin reactor is 37°C, 0.13MPa;
  • the gas-liquid ratio in the second micro-interface generator is 115:1;
  • the reaction temperature in the saponification reactor is 89°C and atmospheric pressure.
  • the ethylene conversion rate is 98.7%, and the synthesis efficiency of the process is increased by 3.7%.
  • reaction temperature in the hypochlorous acid reactor is 12°C and normal pressure
  • the gas-liquid ratio in the first micro-interface generator is 123:1;
  • the reaction temperature in the chlorohydrin reactor is 39°C, 0.16MPa;
  • the gas-liquid ratio in the second micro-interface generator is 118:1;
  • the reaction temperature in the saponification reactor is 89°C and atmospheric pressure.
  • the ethylene conversion rate is 98.6%, and the synthesis efficiency of the process is increased by 3.8%.
  • reaction temperature in the hypochlorous acid reactor is 17°C and normal pressure
  • the gas-liquid ratio in the first micro-interface generator is 127:1;
  • the reaction temperature in the chlorohydrin reactor is 41°C, 0.18MPa;
  • the gas-liquid ratio in the second micro-interface generator is 123:1;
  • the reaction temperature in the saponification reactor is 93°C and atmospheric pressure.
  • the ethylene conversion rate is 98.8%, and the synthesis efficiency of the process is increased by 3.8%.
  • reaction temperature in the hypochlorous acid reactor is 19°C and normal pressure
  • the gas-liquid ratio in the first micro-interface generator is 128:1;
  • the reaction temperature in the chlorohydrin reactor is 45°C, 0.19MPa;
  • the gas-liquid ratio in the second micro-interface generator is 124:1;
  • the reaction temperature in the saponification reactor is 96°C and atmospheric pressure.
  • the ethylene conversion rate is 98.9%, and the synthesis efficiency of the process is increased by 3.9%.
  • reaction temperature in the hypochlorous acid reactor is 20°C and normal pressure
  • the gas-liquid ratio in the first micro-interface generator is 130:1;
  • the reaction temperature in the chlorohydrin reactor is 47°C, 0.19MPa;
  • the gas-liquid ratio in the second micro-interface generator is 125:1;
  • the reaction temperature in the saponification reactor is 97°C and atmospheric pressure.
  • the ethylene conversion rate is 99.0%, and the synthesis efficiency of the process is increased by 4.0%.
  • the prior art is used to prepare ethylene oxide from ethylene, wherein the process parameters selected in this embodiment are the same as those in the fifth embodiment.
  • the ethylene conversion rate is 73.3%.

Abstract

Disclosed are a microinterface-enhanced system and process for preparing ethylene oxide from ethylene. The microinterface-enhanced system comprises a chlorohydrination reaction unit, a chlorohydrination reaction unit, a saponification reaction unit, a separation and purification unit, and a microinterface generator. By installing the microinterface generator for treating chlorine gas and ethylene, the chlorine gas or ethylene is broken into micron-scale bubbles on the micrometer scale, the micron-scale bubbles of chlorine gas are mixed with water to form a gas-liquid emulsion, and the micron-scale bubbles of ethylene are mixed with hypochlorous acid to form a gas-liquid emulsion, in order to increase the area of the phase interface between a gas phase and a liquid phase, decrease the thickness of a liquid film, and decrease the mass transfer resistance; in order to enhance the mass transfer efficiency and reaction efficiency of the gas and liquid components within a preset operation condition range to improve the reaction efficiency of the chlorine gas or ethylene; and in order to ensure that the reaction is carried out adequately and efficiently, and increase the utilization rates of the chlorine gas or ethylene, thus ensuring the reaction rate, achieving the aim of enhancing the reaction and reducing the production cost of ethylene oxide.

Description

一种乙烯制备环氧乙烷的微界面强化系统及工艺Micro-interface strengthening system and process for preparing ethylene oxide from ethylene 技术领域Technical field
本发明涉及乙烯制备环氧乙烷技术领域，尤其涉及一种乙烯制备环氧乙烷的微界面强化系统及工艺。The invention relates to the technical field of preparing ethylene oxide from ethylene, in particular to a micro-interface strengthening system and process for preparing ethylene oxide from ethylene.
背景技术Background technique
环氧乙烷是一种最简单的环醚，属于杂环类化合物，在低温10.7℃以下时为无色透明液体，常温常压下为无色气体。暴露在环氧乙烷气体下，对眼、喉、鼻有刺激性。其性质活泼，是乙烯工业衍生物中仅次于聚乙烯和聚氯乙烯的重要有机化工产品，是用途广泛的有机合成中间体，工业中生产的环氧乙烷根据纯度划分可分为大宗环氧乙烷和高纯环氧乙烷，主要用于生产乙二醇和洗涤剂工业的乙氧基化物，其中大约3/4的环氧乙烷用于生产乙二醇，其特殊的三元环结构决定了环氧乙烷的特殊反应活性，由环氧乙烷衍生可得到一系列非常重要的精细化工产品，如其它醇类如聚乙二醇、二甘醇和三甘醇等、乙醇胺、乙二醇醚类、非离子表面活性剂、防冻剂、增塑剂、添加剂、溶剂、香料、高能燃料、推进剂等。另外由于环氧乙烷有广谱、高效、低温灭菌的特点,因此也用作熏蒸剂、杀虫剂、杀菌剂以及一次性医疗器械的消毒剂等，由于其广泛的用途，导致环氧乙烷市场需求旺盛。Ethylene oxide is one of the simplest cyclic ethers. It is a heterocyclic compound. It is a colorless and transparent liquid at a low temperature below 10.7°C, and a colorless gas at room temperature and pressure. It is irritating to eyes, throat and nose when exposed to ethylene oxide gas. Its lively nature is an important organic chemical product second only to polyethylene and polyvinyl chloride in the ethylene industry derivatives. It is a versatile organic synthesis intermediate. The ethylene oxide produced in the industry can be divided into bulk rings according to its purity. Ethylene oxide and high-purity ethylene oxide are mainly used in the production of ethylene glycol and ethoxylates in the detergent industry. About 3/4 of the ethylene oxide is used in the production of ethylene glycol, and its special three-membered ring structure determines In view of the special reactivity of ethylene oxide, a series of very important fine chemical products can be derived from ethylene oxide, such as other alcohols such as polyethylene glycol, diethylene glycol and triethylene glycol, ethanolamine, ethylene glycol, etc. Ethers, non-ionic surfactants, antifreeze, plasticizers, additives, solvents, fragrances, high-energy fuels, propellants, etc. In addition, because ethylene oxide has the characteristics of broad-spectrum, high-efficiency, and low-temperature sterilization, it is also used as a fumigant, insecticide, fungicide, and disinfectant for disposable medical devices. Due to its wide range of uses, it leads to epoxy The ethane market is in strong demand.
环氧乙烷的主要生产方法有氯醇法和乙烯直接氧化法，其中，氯醇法最早制备环氧乙烷的工业方法，氯醇法中包括两部反应：The main production methods of ethylene oxide are the chlorohydrin method and the direct ethylene oxidation method. Among them, the chlorohydrin method is the earliest industrial method for preparing ethylene oxide. The chlorohydrin method includes two reactions:
第一步是将乙烯和氯气通入水中，生成2-氯乙醇；The first step is to pass ethylene and chlorine into the water to generate 2-chloroethanol;
第二步是用碱(通常为石灰乳)与2-氯乙醇反应，生成环氧乙烷，乙烯经次氯酸化生成氯乙醇，然后与氢氧化钙皂化生成环氧乙烷粗产品，再经分馏，制得环氧乙烷。The second step is to react with alkali (usually milk of lime) and 2-chloroethanol to produce ethylene oxide. The ethylene is hypochlorous acidified to produce chloroethanol, and then saponified with calcium hydroxide to produce crude ethylene oxide. Fractional distillation produces ethylene oxide.
中国专利公开号：CN103896882A公开了一种采用氯醇法制备环氧乙烷的方法，乙烯和氯气为原料，主要工艺分为两步，第一步是氯气与水反应成次氯酸，摩尔比为1:1-2；次氯酸与乙烯反应摩尔比为1:0.5-1；生成氯乙醇；第二步氯乙醇经皂化生成环氧乙烷；氯醇法生产环氧乙烷的反应器有多种形式，最常驻机构用的为塔式，水和氯气从塔的底部进入，生成次氯酸；乙烯则在高处通入，与 次氯酸反应生成氯乙醇，由塔顶溢出氯乙醇的水溶液，反应温度为10～50度，常压；皂化过程可在釜式或塔式反应器中进行，采用石灰乳做皂化剂，反应温度为100～102度，停留时间约三十分钟，可皂化完全；采用塔式反应器，兼作蒸馏塔用，氯乙醇溶液与石灰乳同时加入塔内，由塔顶蒸出轻组分环氧乙烷，塔釜排放含有有机物的氯化钙水溶液。由此可见，所述方法存在以下问题：Chinese Patent Publication Number: CN103896882A discloses a method for preparing ethylene oxide by the chlorohydrin method. Ethylene and chlorine are used as raw materials. The main process is divided into two steps. The first step is the reaction of chlorine and water to form hypochlorous acid. It is 1:1-2; the reaction molar ratio of hypochlorous acid and ethylene is 1:0.5-1; produces chloroethanol; the second step chloroethanol is saponified to produce ethylene oxide; reactor for producing ethylene oxide by chlorohydrin method There are many forms, the most resident organization uses the tower type, water and chlorine enter from the bottom of the tower to generate hypochlorous acid; ethylene is passed in from a high place, reacts with hypochlorous acid to produce chloroethanol, and overflows from the top of the tower The aqueous solution of chloroethanol, the reaction temperature is 10-50 degrees, normal pressure; the saponification process can be carried out in a kettle or tower reactor, using lime milk as the saponifying agent, the reaction temperature is 100-102 degrees, and the residence time is about 30 It can be saponified completely within minutes; the tower reactor is used as a distillation tower. The chloroethanol solution and the lime milk are added into the tower at the same time, and the light component ethylene oxide is steamed from the top of the tower, and the calcium chloride containing organic matter is discharged from the tower. Aqueous solution. It can be seen that the method has the following problems:
第一，所述方法中仅通过乙烯在高处通入，与次氯酸反应生成氯乙醇，气相组分乙烯进入反应器形成大气泡，然而由于气泡体积过大，无法与液相组分充分接触，降低了系统的反应效率。First, in the method, only ethylene is passed in at a high place, and it reacts with hypochlorous acid to generate chloroethanol. The gas phase component ethylene enters the reactor to form large bubbles. However, because the volume of the bubbles is too large, it cannot fully interact with the liquid phase components. Contact reduces the reaction efficiency of the system.
第二，所述方法中乙烯与次氯酸反应速率降低，导致乙烯利用率降低，很大程度上造成原料的浪费，增加了环氧乙烷的生产成本，不符合现有的循环经济的要求。Second, in the method, the reaction rate of ethylene and hypochlorous acid is reduced, which leads to a decrease in ethylene utilization rate, which largely causes a waste of raw materials, increases the production cost of ethylene oxide, and does not meet the requirements of the existing circular economy. .
发明内容Summary of the invention
为此，本发明提供一种乙烯制备环氧乙烷的微界面强化系统及工艺，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。To this end, the present invention provides a micro-interface strengthening system and process for preparing ethylene oxide from ethylene to overcome the problem of low system reaction efficiency caused by uneven mixing of materials and by-products in the prior art.
一方面，本发明提供一种乙烯制备环氧乙烷的微界面强化系统，包括：In one aspect, the present invention provides a micro-interface strengthening system for preparing ethylene oxide from ethylene, which includes:
次氯酸合成单元，用以为氯气和水提供反应场所，并对生成物料进行分离；The hypochlorous acid synthesis unit is used to provide a reaction place for chlorine and water, and to separate the generated materials;
氯醇化反应单元，与所述次氯酸合成单元相连，用以为次氯酸合成单元输出物料与乙烯提供反应场所；The chlorohydrinization reaction unit is connected to the hypochlorous acid synthesis unit to provide a reaction place for the output material of the hypochlorous acid synthesis unit and ethylene;
皂化反应单元，与所述氯醇化反应单元相连，用以为氯醇化反应单元输出液相物料与石灰乳提供反应场所；The saponification reaction unit is connected to the chlorohydrin reaction unit and is used to provide a reaction place for the chlorohydrin reaction unit to output liquid phase materials and lime milk;
分离纯化单元，与所述皂化反应单元相连，用以为输出液相物料进行精馏分离；A separation and purification unit, connected to the saponification reaction unit, for rectifying and separating the output liquid phase materials;
微界面发生器，其设置个数为两个，分别设置在所述次氯酸合成单元和所述氯醇化反应单元，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气相组分，使气相气破碎形成直径≥1μm、且＜1mm的微米级气泡以提高气相组分与液相组分的传质面积，减小液膜厚度，降低传质阻力，并在破碎后将液相组分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气液组分的传质效率和反应效率。The number of micro-interface generators is two, which are respectively installed in the hypochlorous acid synthesis unit and the chlorohydrin reaction unit, and convert the pressure energy of the gas and/or the kinetic energy of the liquid into the surface energy of the bubble and transfer it to The gas phase component breaks the gas phase gas to form micron-sized bubbles with a diameter of ≥1μm and <1mm to increase the mass transfer area of the gas phase component and the liquid phase component, reduce the thickness of the liquid film, and reduce the mass transfer resistance, and after crushing The liquid phase component is mixed with micron-sized bubbles to form a gas-liquid emulsion to enhance the mass transfer efficiency and reaction efficiency of the gas-liquid component within the preset operating condition range.
进一步地，所述微界面发生器为气动式微界面发生器，所述微界面发生器包括第一微界面发生器和第二微界面发生器；Further, the micro-interface generator is a pneumatic micro-interface generator, and the micro-interface generator includes a first micro-interface generator and a second micro-interface generator;
所述第一微界面发生器设置在所述次氯酸合成单元的反应区底部，用以将氯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次氯酸合成单元内与水混合形成气液乳化物；The first micro-interface generator is arranged at the bottom of the reaction zone of the hypochlorous acid synthesis unit, and is used to crush the chlorine gas to form micron-scale micron-scale bubbles and output the micron-scale bubbles to the hypochlorous acid synthesis unit after the crushing is completed It is mixed with water to form a gas-liquid emulsion;
所述第二微界面发生器设置在所述氯醇化反应单元的反应区底部，用以将乙烯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氯醇化反应单元内与次氯酸合成单元输出液相物料混合形成气液乳化物。The second micro-interface generator is arranged at the bottom of the reaction zone of the chlorohydrin reaction unit, and is used to crush ethylene to form micron-sized micro-sized bubbles and output the micro-sized bubbles to the chlorohydrin reaction unit after the crushing is completed. The output liquid phase material of the hypochlorous acid synthesis unit is mixed to form a gas-liquid emulsion.
进一步地，所述次氯酸合成单元包括：Further, the hypochlorous acid synthesis unit includes:
次氯酸反应器，用以为氯气和水提供反应场所；Hypochlorous acid reactor to provide a reaction place for chlorine and water;
气相进料管道，其设置在所述次氯酸反应器的侧壁并与所述第一微界面发生器相连，用以将氯气输送至第一微界面发生器内，并使微界面发生器对氯气进行破碎；The gas-phase feed pipeline is arranged on the side wall of the hypochlorous acid reactor and connected to the first micro-interface generator, and is used to transport chlorine gas into the first micro-interface generator and make the micro-interface generator Crush the chlorine gas;
液相进料管道，其设置在所述次氯酸反应器的侧壁并位于所述气相进料管道上方，用以将水输送至次氯酸反应器内；A liquid-phase feed pipe, which is arranged on the side wall of the hypochlorous acid reactor and above the gas-phase feed pipe, to transport water into the hypochlorous acid reactor;
进一步地，所述次氯酸合成单元还包括：Further, the hypochlorous acid synthesis unit further includes:
第一气相回流管，其设置在所述次氯酸反应器上并与所述第一微界面发生器相连，用以将气相组分回输至次氯酸反应器内；A first gas-phase reflux pipe, which is arranged on the hypochlorous acid reactor and connected to the first micro-interface generator, for returning the gas phase components to the hypochlorous acid reactor;
气液分离器，其与所述次氯酸反应器相连，用以对次氯酸反应器输出物料进行气液分离。The gas-liquid separator is connected with the hypochlorous acid reactor and is used for gas-liquid separation of the output materials of the hypochlorous acid reactor.
进一步地，所述氯醇化反应单元包括：Further, the chlorohydrin reaction unit includes:
氯醇化反应器，其与所述气液分离器相连，用以为次氯酸和乙烯提供反应场所；The chlorohydrinization reactor is connected to the gas-liquid separator to provide a reaction place for hypochlorous acid and ethylene;
乙烯进料管道，其设置在所述氯醇化反应器的侧壁并与所述第二微界面发生器相连，用以将乙烯输送至第二微界面发生器内，并使微界面发生器对乙烯进行破碎；The ethylene feed pipe is arranged on the side wall of the chlorohydrin reactor and connected to the second micro-interface generator, and is used to transport ethylene into the second micro-interface generator and make the micro-interface generator pair Ethylene is crushed;
进一步地，所述氯醇化反应单元还包括：Further, the chlorohydrin reaction unit further includes:
第二气相回流管，其设置在所述氯醇化反应器上并与所述第二微界面发生器相连，用以将气相组分回输至氯醇化反应器内。The second gas-phase reflux pipe is arranged on the chlorohydrin reactor and connected with the second micro-interface generator, and is used for returning the gas-phase components to the chlorohydrin reactor.
进一步地，所述皂化反应单元包括：Further, the saponification reaction unit includes:
皂化反应器，与所述氯醇化反应器相连，用以为氯醇化反应单元输出液相物料与石灰乳提供反应场所；The saponification reactor is connected to the chlorohydrinization reactor and is used to provide a reaction place for the chlorohydrinization reaction unit to output liquid phase materials and lime milk;
石灰乳进料管道，其设置在所述皂化反应器的侧壁，用以将石灰乳输送至皂化反应器内。The lime milk feed pipe is arranged on the side wall of the saponification reactor to transport the lime milk into the saponification reactor.
进一步地，所述分离纯化单元包括：Further, the separation and purification unit includes:
换热器，其与所述皂化反应单元相连，用以为皂化反应单元输出物料与环氧乙烷进行能量交换；A heat exchanger, which is connected to the saponification reaction unit, and is used to exchange energy between the output material of the saponification reaction unit and ethylene oxide;
精馏塔，其与所述换热器相连，用以对皂化反应单元输出物料进行精馏分离。A rectification tower, which is connected with the heat exchanger, is used for rectifying and separating the output materials of the saponification reaction unit.
另一方面，一种乙烯制备环氧乙烷的微界面强化工艺，包括：On the other hand, a micro-interface strengthening process for preparing ethylene oxide from ethylene includes:
次氯酸合成工序：Hypochlorous acid synthesis process:
步骤1：通过所述液相进料管道向所述次氯酸反应器内输送水；Step 1: Transport water into the hypochlorous acid reactor through the liquid-phase feed pipeline;
步骤2：通过所述气相进料管道向所述次氯酸反应器内输送氯气，所述气相进料管道会将氯气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氯气进行破碎，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次氯酸反应器并与水混合形成气液乳化物，气液乳化物进反应，生成次氯酸混合物；Step 2: Transport chlorine gas into the hypochlorous acid reactor through the gas-phase feed pipe, the gas-phase feed pipe will transport the chlorine gas to the first micro-interface generator, and the first micro-interface The device crushes the chlorine gas to form micron-sized bubbles. After the crushing is completed, the first micro-interface generator outputs the micron-sized bubbles to the hypochlorous acid reactor and mixes with water to form a gas-liquid emulsion. The liquid emulsion reacts to form a mixture of hypochlorous acid;
步骤3：所述次氯酸反应器内未充分反应氯气沿所述次氯酸反应器顶部所述第一气相回流管回流入所述第一微界面发生器，并通过所述第一微界面发生器对氯气进行破碎，与水进一步反应；Step 3: The under-reacted chlorine gas in the hypochlorous acid reactor flows back into the first micro-interface generator along the first gas-phase reflux pipe on the top of the hypochlorous acid reactor, and passes through the first micro-interface The generator breaks the chlorine gas and further reacts with water;
步骤4：所述次氯酸反应器内液相组分流入所述气液分离器，气液分离后，尾气沿所述气液分离器顶部气相出口排出，次氯酸溶液沿所述气液分离器底部液相出口排出，并传输至氯醇化反应单元；Step 4: The liquid phase components in the hypochlorous acid reactor flow into the gas-liquid separator. After gas-liquid separation, the tail gas is discharged along the gas-phase outlet at the top of the gas-liquid separator, and the hypochlorous acid solution flows along the gas-liquid separator. The liquid phase outlet at the bottom of the separator is discharged and transferred to the chlorohydrin reaction unit;
氯醇化反应工序：Chlorohydrin reaction process:
步骤5：次氯酸溶液进入所述氯醇化反应器，通过所述乙烯进料管道向所述氯醇化反应器内输送乙烯，所述乙烯进料管道会将乙烯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乙烯进行破碎，形成微米尺度的微米级气泡；Step 5: The hypochlorous acid solution enters the chlorohydrinization reactor, and ethylene is transported into the chlorohydrinization reactor through the ethylene feed pipe, and the ethylene feed pipe will transport ethylene gas to the second micro An interface generator, wherein the second micro-interface generator breaks ethylene to form micro-scale bubbles of micron scale;
步骤6：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氯醇化反应器并与次氯酸溶液混合形成气液乳化物，气液乳化物进反应，生成氯乙醇 溶液，所述氯醇化反应器内氯乙醇溶液流出并传输至皂化反应单元；Step 6: After the crushing is completed, the second micro-interface generator outputs micron-sized bubbles to the chlorohydrinization reactor and mixes them with the hypochlorous acid solution to form a gas-liquid emulsion, and the gas-liquid emulsion reacts to produce chloroethanol Solution, the chloroethanol solution in the chlorohydrinization reactor flows out and is transferred to the saponification reaction unit;
步骤7：所述氯醇化反应器内未充分反应乙烯沿所述氯醇化反应器顶部所述第二气相回流管回流入所述第二微界面发生器，并通过所述第二微界面发生器对乙烯进行破碎，与次氯酸溶液进一步反应；Step 7: Under-reacted ethylene in the chlorohydrinization reactor flows back into the second micro-interface generator along the second gas-phase reflux pipe on the top of the chlorohydrin reactor, and passes through the second micro-interface generator Crush the ethylene and further react with the hypochlorous acid solution;
皂化工序：Saponification process:
步骤8：氯乙醇溶液流入所述皂化反应单元内，通过石灰乳进料管道向所述皂化反应单元内传输石灰乳，石灰乳与氯乙醇溶液在所述皂化反应单元内发生皂化反应，产生环氧乙烷混合物，所述皂化反应内环氧乙烷混合物流出并传输至分离纯化单元；Step 8: The chloroethanol solution flows into the saponification reaction unit, and the lime milk is transferred into the saponification reaction unit through the lime milk feed pipe. The lime milk and the chloroethanol solution undergo a saponification reaction in the saponification reaction unit to produce a ring Oxyethane mixture, where the ethylene oxide mixture flows out in the saponification reaction and is transferred to the separation and purification unit;
分离纯化工序：Separation and purification process:
步骤9：环氧乙烷混合物流入所述分离纯化单元内，其中环氧乙烷混合物流经所述换热器进入所述精馏塔内进行精馏，精馏塔输出气相物料为环氧乙烷气体，其他废水沿精馏塔塔底排出，其中环氧乙烷气体在所述换热器内与环氧乙烷混合物进行热交换并排出，即获得环氧乙烷产品。Step 9: The ethylene oxide mixture flows into the separation and purification unit, where the ethylene oxide mixture flows through the heat exchanger and enters the rectification tower for rectification, and the gas phase material output from the rectification tower is ethylene oxide Alkane gas and other waste water are discharged along the bottom of the rectification tower, wherein the ethylene oxide gas exchanges heat with the ethylene oxide mixture in the heat exchanger and is discharged to obtain an ethylene oxide product.
进一步地，所述工艺中次氯酸反应器内反应温度为10-20℃，常压，所述第一微界面发生器内的气液比为120-130:1；Further, in the process, the reaction temperature in the hypochlorous acid reactor is 10-20°C and normal pressure, and the gas-liquid ratio in the first micro-interface generator is 120-130:1;
所述工艺中氯醇化反应器内反应温度为37-47℃，反应压强为0.13-0.19MPa，所述第二微界面发生器内的气液比为115-125:1；In the process, the reaction temperature in the chlorohydrinization reactor is 37-47°C, the reaction pressure is 0.13-0.19MPa, and the gas-liquid ratio in the second micro-interface generator is 115-125:1;
所述工艺中皂化反应器内反应温度为87-97℃，常压。In the process, the reaction temperature in the saponification reactor is 87-97°C and normal pressure.
与现有技术相比，本发明的有益效果在于，通过氯醇化反应单元、氯醇化反应单元、皂化反应单元、分离纯化单元、微界面发生器和智能控制单元构成本发明系统的主体结构，通过破碎氯气使其形成微米尺度的微米级气泡，使微米级气泡与水混合形成气液乳化物，以增大气液两相的相界面积，提高次氯酸的合成效率，提高氯气反应效率，节约成本；本发明系统中通过次氯酸合成单元，用以为氯气和水提供反应场所，并对生成物料进行分离，氯醇化反应单元，与次氯酸合成单元相连，用以为次氯酸合成单元输出物料与乙烯提供反应场所，皂化反应单元，与氯醇化反应单元相连，用以为氯醇化反应单元输出液相物料与石灰乳提供反应场所，分离纯化单元，与皂化反应单元相连，用以为输出液相物料进行精馏分离。可以根据不同的产品要求，而灵活地对氯气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。Compared with the prior art, the beneficial effect of the present invention is that the main structure of the system of the present invention is formed by the chlorohydrin reaction unit, the chlorohydrin reaction unit, the saponification reaction unit, the separation and purification unit, the micro-interface generator and the intelligent control unit. The chlorine gas is broken to form micron-sized bubbles, and the micron-sized bubbles are mixed with water to form a gas-liquid emulsion to increase the area of the gas-liquid phase boundary, improve the synthesis efficiency of hypochlorous acid, improve the efficiency of chlorine reaction, and save Cost: In the system of the present invention, a hypochlorous acid synthesis unit is used to provide a reaction place for chlorine and water, and to separate the generated materials. The chlorohydrin reaction unit is connected to the hypochlorous acid synthesis unit to output the hypochlorous acid synthesis unit The material and ethylene provide a reaction place, the saponification reaction unit is connected to the chlorohydrin reaction unit to provide a reaction place for the chlorohydrin reaction unit to output liquid phase materials and lime milk, and the separation and purification unit is connected to the saponification reaction unit to output the liquid phase. The materials are separated by rectification. According to different product requirements, the chlorine gas can be flexibly adjusted in the range of preset operating conditions to ensure that the reaction is fully and effectively carried out, thereby ensuring the reaction rate, and achieving the purpose of strengthening the reaction.
尤其，本发明的次氯酸合成单元内设置了次氯酸反应器、气相进料管道、液相进料管道、第一气相回流管和气液分离器，提高次氯酸反应器为氯气和水提供反应场所，通过气相进料管道将氯气输送至第一微界面发生器内，并使微界面发生器对氯气进行破碎，通过液相进料管将水输送至次氯酸反应器内，通过第一气相回流管将气相组分回输至次氯酸反应器内，通过气液分离器对次氯酸反应器输出物料进行气液分离，实现水和氯气高效反应，提高氯气原料利用率。In particular, the hypochlorous acid synthesis unit of the present invention is provided with a hypochlorous acid reactor, a gas-phase feed pipe, a liquid-phase feed pipe, a first gas-phase return pipe and a gas-liquid separator, so as to improve the hypochlorous acid reactor for chlorine and water. Provide a reaction place, transport the chlorine gas into the first micro-interface generator through the gas-phase feed pipe, and make the micro-interface generator break the chlorine gas, and transport the water to the hypochlorous acid reactor through the liquid-phase feed pipe. The first gas-phase reflux pipe returns the gas-phase components to the hypochlorous acid reactor, and performs gas-liquid separation of the output materials of the hypochlorous acid reactor through a gas-liquid separator to realize the efficient reaction of water and chlorine gas and improve the utilization rate of chlorine gas raw materials.
尤其，本发明的氯醇化反应单元设置了氯醇化反应器、乙烯进料管道和第二气相回流管，通过氯醇化反应器，为次氯酸和乙烯提供反应场所，通过乙烯进料管道将乙烯输送至第二微界面发生器内，并使微界面发生器对乙烯进行破碎。通过第二气相回流管将气相组分回输至氯醇化反应器内，实现乙烯和次氯酸的高效反应，提高乙烯原料利用率。In particular, the chlorohydrin reaction unit of the present invention is equipped with a chlorohydrin reactor, an ethylene feed pipeline and a second gas phase return pipe. The chlorohydrin reactor provides a reaction place for hypochlorous acid and ethylene, and the ethylene is fed through the ethylene feed pipeline. It is transported to the second micro-interface generator, and the micro-interface generator is used to crush the ethylene. The gas-phase components are returned to the chlorohydrinization reactor through the second gas-phase reflux pipe to realize the high-efficiency reaction of ethylene and hypochlorous acid and improve the utilization rate of ethylene raw materials.
尤其，本发明的皂化反应单元设置了皂化反应器和石灰乳进料管道，通过皂化反应器为氯醇化反应单元输出液相物料与石灰乳提供反应场所，通过石灰乳进料管道将石灰乳输送至皂化反应器内，通过氯乙醇与石灰乳的皂化反应获得环氧乙烷。In particular, the saponification reaction unit of the present invention is provided with a saponification reactor and a lime milk feeding pipeline. The saponification reactor provides a reaction place for the chlorohydrin reaction unit to output liquid phase materials and lime milk, and the lime milk is transported through the lime milk feeding pipeline. In the saponification reactor, ethylene oxide is obtained through the saponification reaction of chloroethanol and lime milk.
尤其，本发明的分离纯化单元设置了换热器和精馏塔；通过换热器为皂化反应单元输出物料与环氧乙烷进行能量交换，通过精馏塔对皂化反应单元输出物料进行精馏分离，其中环氧乙烷气体在换热器内与环氧乙烷混合物进行热交换，提高能源利用率，节约能耗。In particular, the separation and purification unit of the present invention is equipped with a heat exchanger and a rectification tower; the heat exchanger is used to exchange energy between the output material of the saponification reaction unit and ethylene oxide, and the output material of the saponification reaction unit is rectified through the rectification tower. Separation, in which the ethylene oxide gas exchanges heat with the ethylene oxide mixture in the heat exchanger, which improves energy utilization and saves energy consumption.
附图说明Description of the drawings
图1为本发明所述的乙烯制备环氧乙烷的微界面强化系统的系统的结构示意图。Fig. 1 is a schematic structural diagram of the system of the micro-interface strengthening system for preparing ethylene oxide from ethylene according to the present invention.
具体实施方式detailed description
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。The preferred embodiments of the present invention will be described below with reference to the drawings. Those skilled in the art should understand that these embodiments are only used to explain the technical principles of the present invention, and are not intended to limit the protection scope of the present invention.
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。It should be noted that in the description of the present invention, the terms "upper", "lower", "left", "right", "inner", "outer" and other terms indicating directions or positional relationships are based on the attached drawings. The direction or position relationship shown is only for ease of description, and does not indicate or imply that the device or element must have a specific orientation, be configured and operated in a specific orientation, and therefore cannot be understood as a limitation of the present invention.
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。In addition, it should be noted that, in the description of the present invention, unless otherwise clearly specified and limited, 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. For those skilled in the art, the specific meaning of the above-mentioned terms in the present invention can be understood according to specific circumstances.
请参阅图1所示，其为本发明所述的乙烯制备环氧乙烷的微界面强化系统的结构示意图，包括氯醇化反应单元1、氯醇化反应单元2、皂化反应单元3、分离纯化单元4、微界面发生器5。所述次氯酸合成单元1，用以为氯气和水提供反应场所，并对生成物料进行分离，所述氯醇化反应单元2，与所述次氯酸合成单元1相连，用以为次氯酸合成单元输出物料与乙烯提供反应场所，所述皂化反应单元3，与所述氯醇化反应单元2相连，用以为氯醇化反应单元输出液相物料与石灰乳提供反应场所，所述分离纯化单元4，与所述皂化反应单元相连，用以为输出液相物料进行精馏分离，所述微界面发生器5分别设置在所述次氯酸合成单元1和所述氯醇化反应单元2的制定位置，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气相组分，使气相气破碎形成直径≥1μm、且＜1mm的微米级气泡。Please refer to Figure 1, which is a schematic structural diagram of the micro-interface strengthening system for preparing ethylene oxide from ethylene according to the present invention, including a chlorohydrin reaction unit 1, a chlorohydrin reaction unit 2, a saponification reaction unit 3, and a separation and purification unit 4. Micro-interface generator 5. The hypochlorous acid synthesis unit 1 is used to provide a reaction place for chlorine and water and separate the produced materials. The chlorohydrin reaction unit 2 is connected to the hypochlorous acid synthesis unit 1 to synthesize hypochlorous acid The unit output material and ethylene provide a reaction place. The saponification reaction unit 3 is connected to the chlorohydrin reaction unit 2 to provide a reaction place for the liquid phase material output from the chlorohydrin reaction unit and lime milk. The separation and purification unit 4, Connected to the saponification reaction unit for rectifying and separating the output liquid phase materials, and the micro-interface generator 5 is respectively arranged at the designated positions of the hypochlorous acid synthesis unit 1 and the chlorohydrin reaction unit 2, and The pressure energy of the gas and/or the kinetic energy of the liquid is transformed into the surface energy of the bubbles and transferred to the gas phase components, so that the gas phase gas is broken to form micron-sized bubbles with a diameter of ≥1μm and <1mm.
当所述系统运行时，微界面发生器5气相组分破碎形成微米尺度的微米级气泡并使微米级气泡与液相组分的混合物混合形成气液乳化物。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5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。When the system is running, the gas-phase components of the micro-interface generator 5 are broken to form micro-sized micro-sized bubbles and the mixture of the micro-sized bubbles and the liquid-phase components are mixed to form a gas-liquid emulsion. Those skilled in the art can understand that the micro-interface generator 5 of the present invention can also be used in other multiphase reactions, such as via micro-interface, micro-nano interface, ultra-micro interface, micro-bubble biochemical reactor or micro-bubble biological Reactor and other equipment, 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, microbubble flow, microbubble, microbubble flow, micro-nano bubble and micro-nano bubble flow and other multi-phase fluids formed by micro-scale particles, or multi-phase fluids formed by micro-nano-scale particles (abbreviated as Micro-interface fluid), thereby effectively increasing the mass transfer area of the phase boundary between the gas and/or liquid phase and the liquid and/or solid phase during the reaction.
请继续参阅图1所示，所述微界面发生器5为气动式微界面发生器，所述微界面发生器5包括第一微界面发生器51和第二微界面发生器52；Please continue to refer to FIG. 1, the micro-interface generator 5 is a pneumatic micro-interface generator, and the micro-interface generator 5 includes a first micro-interface generator 51 and a second micro-interface generator 52;
所述第一微界面发生器51设置在所述次氯酸合成单元1的反应区底部，用以将氯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次氯酸合成单元内与水混合形成气液乳化物；The first micro-interface generator 51 is arranged at the bottom of the reaction zone of the hypochlorous acid synthesis unit 1, and is used to break the chlorine gas into micron-sized micro-sized bubbles and output the micro-sized bubbles to the hypochlorous acid after the crushing is completed. Mix with water in the synthesis unit to form a gas-liquid emulsion;
当系统运行时，所述第一微界面发生器51的气相组分氯气破碎形成微米尺度的微米级气泡并使微米级气泡与液相组分水的混合物混合形成气液乳化物；When the system is running, the gas-phase component chlorine of the first micro-interface generator 51 is broken to form micro-scale micro-sized bubbles, and the mixture of the micro-scale bubbles and the liquid-phase component water is mixed to form a gas-liquid emulsion;
所述第二微界面发生器52设置在所述氯醇化反应单元2的反应区底部，用以将乙烯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氯醇化反应单元内与次氯酸合成单元输出液相物料混合形成气液乳化物；The second micro-interface generator 52 is arranged at the bottom of the reaction zone of the chlorohydrin reaction unit 2, and is used to crush ethylene to form micro-scale micro-sized bubbles and output the micro-scale bubbles to the chlorohydrin reaction unit after the crushing is completed. It is mixed with the output liquid phase material of hypochlorous acid synthesis unit to form gas-liquid emulsion;
当系统运行时，所述第二微界面发生器52的气相组分乙烯破碎形成微米尺度的微米级气泡并使微米级气泡与液相组分次氯酸的混合物混合形成气液乳化物。When the system is running, the gas-phase component ethylene of the second micro-interface generator 52 is broken to form micro-sized micro-sized bubbles and the mixture of the micro-sized bubbles and the liquid component hypochlorous acid is mixed to form a gas-liquid emulsion.
请继续参阅图1所示，所述次氯酸合成单元1包括：次氯酸反应器11、气相进料管道12、液相进料管道13、第一气相回流管14和气液分离器15；Please continue to refer to FIG. 1, the hypochlorous acid synthesis unit 1 includes: a hypochlorous acid reactor 11, a gas-phase feed pipe 12, a liquid-phase feed pipe 13, a first gas-phase reflux pipe 14 and a gas-liquid separator 15;
次氯酸反应器11，用以为氯气和水提供反应场所；The hypochlorous acid reactor 11 is used to provide a reaction place for chlorine and water;
气相进料管道12，其设置在所述次氯酸反应器1的侧壁并与所述第一微界面发生器51相连，用以将氯气输送至第一微界面发生器内，并使微界面发生器对氯气进行破碎；The gas-phase feed pipe 12 is arranged on the side wall of the hypochlorous acid reactor 1 and is connected to the first micro-interface generator 51, and is used to transport chlorine gas into the first micro-interface generator and make the micro The interface generator breaks the chlorine gas;
液相进料管道13，其设置在所述次氯酸反应器1的侧壁并位于所述气相进料管道11上方，用以将水输送至次氯酸反应器内；The liquid-phase feed pipe 13 is arranged on the side wall of the hypochlorous acid reactor 1 and above the gas-phase feed pipe 11 to transport water into the hypochlorous acid reactor;
第一气相回流管14，其设置在所述次氯酸反应器1上并与所述第一微界面发生器51相连，用以将气相组分回输至次氯酸反应器内；The first gas-phase reflux pipe 14 is arranged on the hypochlorous acid reactor 1 and connected to the first micro-interface generator 51 for returning the gas-phase components to the hypochlorous acid reactor;
气液分离器15，其与所述次氯酸反应器1相连，用以对次氯酸反应器输出物料进行气液分离；The gas-liquid separator 15 is connected to the hypochlorous acid reactor 1 and is used for gas-liquid separation of the output material of the hypochlorous acid reactor;
当所述系统运行时，次氯酸反应器11作为氯气与水的反应器，通过液相进 料管道13将水输送至次氯酸反应器11内，同时通过气相进料管道12将氯气输送至第一微界面发生器51内，并使第一微界面发生器51对氯气进行破碎，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51将微米级气泡输出至所述次氯酸反应器11并与水混合形成气液乳化物，气液乳化物进反应，生成次氯酸混合物，所述次氯酸反应器1内未充分反应氯气沿所述次氯酸反应器1顶部所述第一气相回流管14回流入所述第一微界面发生器51，并通过所述第一微界面发生器51对氯气进行破碎，与水进一步反应，所述次氯酸反应器1内液相组分流入所述气液分离器15，气液分离后，尾气沿所述气液分离器15顶部气相出口排出，次氯酸溶液沿所述气液分离器15底部液相出口排出，并传输至氯醇化反应单元2，可以理解的是，所述气相进料管道12、所述液相进料管道13和第一气相回流管14的材质和尺寸本实施例均不做具体限制，只要满足气相进料管道12、所述液相进料管道13和第一气相回流管14能够在指定时间内输送指定体积的物料即可。When the system is running, the hypochlorous acid reactor 11 is used as a reactor of chlorine and water, and the water is transported into the hypochlorous acid reactor 11 through the liquid-phase feed pipe 13 while the chlorine is transported through the gas-phase feed pipe 12 Into the first micro-interface generator 51, and make the first micro-interface generator 51 crush the chlorine gas to form micro-scale micro-scale bubbles. After the crushing is completed, the first micro-interface generator 51 outputs micro-scale bubbles To the hypochlorous acid reactor 11 and mix with water to form a gas-liquid emulsion, the gas-liquid emulsion reacts to form a hypochlorous acid mixture, and the insufficiently reacted chlorine in the hypochlorous acid reactor 1 follows the hypochlorous acid The first gas phase return pipe 14 at the top of the acid reactor 1 flows back into the first micro-interface generator 51, and the chlorine gas is broken by the first micro-interface generator 51, and further reacts with water. The liquid phase components in the acid reactor 1 flow into the gas-liquid separator 15. After gas-liquid separation, the tail gas is discharged along the gas-phase outlet at the top of the gas-liquid separator 15, and the hypochlorous acid solution is discharged along the bottom of the gas-liquid separator 15 The liquid phase outlet is discharged and transferred to the chlorohydrin reaction unit 2. It can be understood that the materials and dimensions of the gas phase feed pipe 12, the liquid phase feed pipe 13 and the first gas phase return pipe 14 are all in this embodiment. There is no specific limitation, as long as it is satisfied that the gas-phase feed pipe 12, the liquid-phase feed pipe 13 and the first gas-phase return pipe 14 can transport a specified volume of material within a specified time.
请继续参阅图1所示，所述氯醇化反应单元2包括：氯醇化反应器21、乙烯进料管道22和第二气相回流管23；Please continue to refer to FIG. 1, the chlorohydrin reaction unit 2 includes: a chlorohydrin reactor 21, an ethylene feed pipe 22, and a second gas phase return pipe 23;
氯醇化反应器21，其与所述气液分离器15相连，用以为次氯酸和乙烯提供反应场所；The chlorohydrinization reactor 21 is connected to the gas-liquid separator 15 to provide a reaction place for hypochlorous acid and ethylene;
乙烯进料管道22，其设置在所述氯醇化反应器2的侧壁并与所述第二微界面发生器52相连，用以将乙烯输送至第二微界面发生器内，并使微界面发生器对乙烯进行破碎；The ethylene feed pipe 22 is arranged on the side wall of the chlorohydrinization reactor 2 and is connected to the second micro-interface generator 52 to transport ethylene into the second micro-interface generator and make the micro-interface The generator crushes ethylene;
第二气相回流管23，其设置在所述氯醇化反应器2上并与所述第二微界面发生器52相连，用以将气相组分回输至氯醇化反应器内；The second gas-phase reflux pipe 23 is arranged on the chlorohydrin reactor 2 and is connected to the second micro-interface generator 52 for returning the gas-phase components to the chlorohydrin reactor;
当系统运行时，次氯酸溶液进入所述氯醇化反应器21，通过所述乙烯进料管道22向所述氯醇化反应器21内输送乙烯，所述乙烯进料管道22会将乙烯气输送至所述第二微界面发生器52，所述第二微界面发生器52对乙烯进行破碎，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52将微米级气泡输出至所述氯醇化反应器21并与次氯酸溶液混合形成气液乳化物，气液乳化物进反应，生成氯乙醇溶液，所述氯醇化反应器21内氯乙醇溶液流出并传输至皂化反应单元3，所述氯醇化反应器21内未充分反应乙烯沿所述氯醇化反应 器21顶部所述第二气相回流管23回流入所述第二微界面发生器52，并通过所述第二微界面发生器52对乙烯进行破碎，与次氯酸溶液进一步反应，可以理解的是，所述乙烯进料管道22和所述第二气相回流管23的材质和尺寸本实施例均不做具体限制，只要满足乙烯进料管道22和所述第二气相回流管23能够在指定时间内输送指定体积的物料即可。When the system is running, the hypochlorous acid solution enters the chlorohydrinization reactor 21, and transports ethylene into the chlorohydrinization reactor 21 through the ethylene feed pipe 22, and the ethylene feed pipe 22 will transport ethylene gas To the second micro-interface generator 52, the second micro-interface generator 52 crushes ethylene to form micro-scale bubbles. After the crushing is completed, the second micro-interface generator 52 removes the micro-scale bubbles. Output to the chlorohydrinization reactor 21 and mix with hypochlorous acid solution to form a gas-liquid emulsion. The gas-liquid emulsion reacts to generate a chloroethanol solution. The chlorohydrin solution in the chlorohydrinization reactor 21 flows out and is transferred to the saponification In reaction unit 3, under-reacted ethylene in the chlorohydrin reactor 21 flows back into the second micro-interface generator 52 along the second gas phase reflux pipe 23 at the top of the chlorohydrin reactor 21, and passes through the second micro-interface generator 52. The second micro-interface generator 52 crushes ethylene and further reacts with the hypochlorous acid solution. It can be understood that the material and size of the ethylene feed pipe 22 and the second gas phase return pipe 23 are not used in this embodiment. The specific limitation is as long as it is satisfied that the ethylene feed pipe 22 and the second gas phase return pipe 23 can transport a specified volume of material within a specified time.
请继续参阅图1所示，所述皂化反应单元3包括：皂化反应器31和石灰乳进料管道32；Please continue to refer to FIG. 1, the saponification reaction unit 3 includes: a saponification reactor 31 and a lime milk feed pipe 32;
皂化反应器31，与所述氯醇化反应器21相连，用以为氯醇化反应单元输出液相物料与石灰乳提供反应场所；The saponification reactor 31 is connected to the chlorohydrinization reactor 21, and is used to provide a reaction place for the liquid phase material output from the chlorohydrinization reaction unit and the milk of lime;
石灰乳进料管道32，其设置在所述皂化反应器31的侧壁，用以将石灰乳输送至皂化反应器内。The lime milk feed pipe 32 is arranged on the side wall of the saponification reactor 31 to transport the lime milk into the saponification reactor.
当系统运行时，氯乙醇溶液流入所述皂化反应单元3内，通过石灰乳进料管道32向所述皂化反应单元31内传输石灰乳，其中石灰乳的主要成分为氢氧化钙，具有强碱性，石灰乳与氯乙醇溶液在所述皂化反应单元3内发生皂化反应，产生环氧乙烷混合物，所述皂化反应内环氧乙烷混合物流出并传输至分离纯化单元4。When the system is running, the chloroethanol solution flows into the saponification reaction unit 3, and transfers the milk of lime into the saponification reaction unit 31 through the milk of lime feed pipe 32. The main component of the milk of lime is calcium hydroxide and has a strong alkali. Therefore, the lime milk and the chloroethanol solution undergo a saponification reaction in the saponification reaction unit 3 to produce an ethylene oxide mixture. In the saponification reaction, the ethylene oxide mixture flows out and is transferred to the separation and purification unit 4.
请继续参阅图1所示，所述分离纯化单元4包括：换热器41和精馏塔42；Please continue to refer to FIG. 1, the separation and purification unit 4 includes: a heat exchanger 41 and a rectification tower 42;
换热器41，其与所述皂化反应单元3相连，用以为皂化反应单元输出物料与环氧乙烷进行能量交换；The heat exchanger 41 is connected to the saponification reaction unit 3, and is used to exchange energy between the output material of the saponification reaction unit and ethylene oxide;
精馏塔42，其与所述换热器41相连，用以对皂化反应单元输出物料进行精馏分离；The rectification tower 42 is connected to the heat exchanger 41 for rectifying and separating the output materials of the saponification reaction unit;
当系统运行时，环氧乙烷混合物流入所述分离纯化单元4内，其中环氧乙烷混合物流经所述换热器41进入所述精馏塔42内进行精馏，利用混合物中各组分具有不同的挥发度，即在同一温度下各组分的蒸气压不同这一性质，使液相中的轻组分(低沸物)转移到气相中，而气相中的重组分(高沸物)转移到液相中，从而实现分离的目的，精馏塔42输出气相物料为环氧乙烷气体，其他废水沿精馏塔42塔底排出，其中环氧乙烷气体在所述换热器41内与环氧乙烷混合物进行热交换，通过换热器41在不同温度的环氧乙烷产品与皂化反应单元输出物料两种流体间实现物料之间热量传递，使热量由温度较高的流体传递给温度较低的流体， 使流体温度达到流程规定的指标，节能减排，即获得环氧乙烷产品，可以理解的是，所述换热器41的型号及功率本实施例均不作具体限制，只要满足所述换热器41能够达到其指定的工作状态即可，所述精馏塔42可以为塔板式和填料式任意种类，且精馏塔42的类型及型号本实施例均不作具体限制，只要满足所述精馏塔42能够达到其指定的工作状态即可。When the system is running, the ethylene oxide mixture flows into the separation and purification unit 4, and the ethylene oxide mixture flows through the heat exchanger 41 and enters the rectification tower 42 for rectification. The components have different volatility, that is, at the same temperature, the vapor pressure of each component is different, so that the light components in the liquid phase (low boilers) are transferred to the gas phase, while the heavy components in the gas phase (high boilers) are transferred to the gas phase. In order to achieve the purpose of separation, the gas phase material output from the rectification tower 42 is ethylene oxide gas, and other waste water is discharged along the bottom of the rectification tower 42. The ethylene oxide gas is discharged in the heat exchange The heat exchange between the ethylene oxide mixture and the ethylene oxide mixture is carried out in the vessel 41. The heat exchanger 41 realizes the heat transfer between the two fluids of the ethylene oxide product at different temperatures and the output material of the saponification reaction unit, so that the heat is transferred from the higher temperature. The fluid is transferred to the fluid with a lower temperature, so that the fluid temperature reaches the target specified in the process, energy saving and emission reduction, that is, the ethylene oxide product is obtained. It is understandable that the model and power of the heat exchanger 41 in this embodiment are both There is no specific limitation, as long as the heat exchanger 41 can reach its designated working state. The rectification tower 42 can be of any kind of tray type and packed type, and the type and model of the rectification tower 42 are in this embodiment. There are no specific restrictions, as long as the rectification tower 42 can reach its designated working state.
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。In order to make the purpose and advantages of the present invention clearer, the following further describes the present invention in conjunction with the embodiments; it should be understood that the specific embodiments described here are only used to explain the present invention, not to limit the present invention.
一种乙烯制备环氧乙烷的微界面强化工艺，包括：A micro-interface strengthening process for preparing ethylene oxide from ethylene, including:
次氯酸合成工序：Hypochlorous acid synthesis process:
步骤1：通过所述液相进料管道向所述次氯酸反应器内输送水；Step 1: Transport water into the hypochlorous acid reactor through the liquid-phase feed pipeline;
步骤2：通过所述气相进料管道向所述次氯酸反应器内输送氯气，所述气相进料管道会将氯气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氯气进行破碎，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次氯酸反应器并与水混合形成气液乳化物，气液乳化物进反应，生成次氯酸混合物；Step 2: Transport chlorine gas into the hypochlorous acid reactor through the gas-phase feed pipe, the gas-phase feed pipe will transport the chlorine gas to the first micro-interface generator, and the first micro-interface The device crushes the chlorine gas to form micron-sized bubbles. After the crushing is completed, the first micro-interface generator outputs the micron-sized bubbles to the hypochlorous acid reactor and mixes with water to form a gas-liquid emulsion. The liquid emulsion reacts to form a mixture of hypochlorous acid;
步骤3：所述次氯酸反应器内未充分反应氯气沿所述次氯酸反应器顶部所述第一气相回流管回流入所述第一微界面发生器，并通过所述第一微界面发生器对氯气进行破碎，与水进一步反应；Step 3: The under-reacted chlorine gas in the hypochlorous acid reactor flows back into the first micro-interface generator along the first gas-phase reflux pipe on the top of the hypochlorous acid reactor, and passes through the first micro-interface The generator breaks the chlorine gas and further reacts with water;
步骤4：所述次氯酸反应器内液相组分流入所述气液分离器，气液分离后，尾气沿所述气液分离器顶部气相出口排出，次氯酸溶液沿所述气液分离器底部液相出口排出，并传输至氯醇化反应单元；Step 4: The liquid phase components in the hypochlorous acid reactor flow into the gas-liquid separator. After gas-liquid separation, the tail gas is discharged along the gas-phase outlet at the top of the gas-liquid separator, and the hypochlorous acid solution flows along the gas-liquid separator. The liquid phase outlet at the bottom of the separator is discharged and transferred to the chlorohydrin reaction unit;
氯醇化反应工序：Chlorohydrin reaction process:
步骤5：次氯酸溶液进入所述氯醇化反应器，通过所述乙烯进料管道向所述氯醇化反应器内输送乙烯，所述乙烯进料管道会将乙烯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乙烯进行破碎，形成微米尺度的微米级气泡；Step 5: The hypochlorous acid solution enters the chlorohydrinization reactor, and ethylene is transported into the chlorohydrinization reactor through the ethylene feed pipe, and the ethylene feed pipe will transport ethylene gas to the second micro An interface generator, wherein the second micro-interface generator breaks ethylene to form micro-scale bubbles of micron scale;
步骤6：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氯醇化反应器并与次氯酸溶液混合形成气液乳化物，气液乳化物进反应，生成氯乙醇溶液，所述氯醇化反应器内氯乙醇溶液流出并传输至皂化反应单元；Step 6: After the crushing is completed, the second micro-interface generator outputs micron-sized bubbles to the chlorohydrinization reactor and mixes them with the hypochlorous acid solution to form a gas-liquid emulsion, and the gas-liquid emulsion reacts to produce chloroethanol Solution, the chloroethanol solution in the chlorohydrinization reactor flows out and is transferred to the saponification reaction unit;
步骤7：所述氯醇化反应器内未充分反应乙烯沿所述氯醇化反应器顶部所述第二气相回流管回流入所述第二微界面发生器，并通过所述第二微界面发生器对乙烯进行破碎，与次氯酸溶液进一步反应；Step 7: Under-reacted ethylene in the chlorohydrinization reactor flows back into the second micro-interface generator along the second gas-phase reflux pipe on the top of the chlorohydrin reactor, and passes through the second micro-interface generator Crush the ethylene and further react with the hypochlorous acid solution;
皂化工序：Saponification process:
步骤8：氯乙醇溶液流入所述皂化反应单元内，通过石灰乳进料管道向所述皂化反应单元内传输石灰乳，石灰乳与氯乙醇溶液在所述皂化反应单元内发生皂化反应，产生环氧乙烷混合物，所述皂化反应内环氧乙烷混合物流出并传输至分离纯化单元；Step 8: The chloroethanol solution flows into the saponification reaction unit, and the lime milk is transferred into the saponification reaction unit through the lime milk feed pipe. The lime milk and the chloroethanol solution undergo a saponification reaction in the saponification reaction unit to produce a ring Oxyethane mixture, where the ethylene oxide mixture flows out in the saponification reaction and is transferred to the separation and purification unit;
分离纯化工序：Separation and purification process:
步骤9：环氧乙烷混合物流入所述分离纯化单元内，其中环氧乙烷混合物流经所述换热器进入所述精馏塔内进行精馏，精馏塔输出气相物料为环氧乙烷气体，其他废水沿精馏塔塔底排出，其中环氧乙烷气体在所述换热器内与环氧乙烷混合物进行热交换并排出，即获得环氧乙烷产品。Step 9: The ethylene oxide mixture flows into the separation and purification unit, where the ethylene oxide mixture flows through the heat exchanger and enters the rectification tower for rectification, and the gas phase material output from the rectification tower is ethylene oxide Alkane gas and other waste water are discharged along the bottom of the rectification tower, wherein the ethylene oxide gas exchanges heat with the ethylene oxide mixture in the heat exchanger and is discharged to obtain an ethylene oxide product.
实施例1Example 1
使用上述系统及工艺进行乙烯制备环氧乙烷，其中：Use the above system and process to prepare ethylene oxide from ethylene, where:
所述工艺中次氯酸反应器内反应温度为10℃，常压；In the process, the reaction temperature in the hypochlorous acid reactor is 10°C and normal pressure;
第一微界面发生器内气液比为120:1；The gas-liquid ratio in the first micro-interface generator is 120:1;
氯醇化反应器内反应温度为37℃，0.13MPa；The reaction temperature in the chlorohydrin reactor is 37°C, 0.13MPa;
第二微界面发生器内的气液比为115：1；The gas-liquid ratio in the second micro-interface generator is 115:1;
皂化反应器内反应温度89℃，常压。The reaction temperature in the saponification reactor is 89°C and atmospheric pressure.
经检测，使用所述系统及工艺后，乙烯转化率98.7％，工艺的合成效率提升3.7％。After testing, after using the system and process, the ethylene conversion rate is 98.7%, and the synthesis efficiency of the process is increased by 3.7%.
实施例2Example 2
使用上述系统及工艺进行乙烯制备环氧乙烷，其中：Use the above system and process to prepare ethylene oxide from ethylene, where:
所述工艺中次氯酸反应器内反应温度为12℃，常压；In the process, the reaction temperature in the hypochlorous acid reactor is 12°C and normal pressure;
第一微界面发生器内气液比为123:1；The gas-liquid ratio in the first micro-interface generator is 123:1;
氯醇化反应器内反应温度为39℃，0.16MPa；The reaction temperature in the chlorohydrin reactor is 39°C, 0.16MPa;
第二微界面发生器内的气液比为118：1；The gas-liquid ratio in the second micro-interface generator is 118:1;
皂化反应器内反应温度89℃，常压。The reaction temperature in the saponification reactor is 89°C and atmospheric pressure.
经检测，使用所述系统及工艺后，乙烯转化率98.6％，工艺的合成效率提升3.8％。After testing, after using the system and process, the ethylene conversion rate is 98.6%, and the synthesis efficiency of the process is increased by 3.8%.
实施例3Example 3
使用上述系统及工艺进行乙烯制备环氧乙烷，其中：Use the above system and process to prepare ethylene oxide from ethylene, where:
所述工艺中次氯酸反应器内反应温度为17℃，常压；In the process, the reaction temperature in the hypochlorous acid reactor is 17°C and normal pressure;
第一微界面发生器内气液比为127:1；The gas-liquid ratio in the first micro-interface generator is 127:1;
氯醇化反应器内反应温度为41℃，0.18MPa；The reaction temperature in the chlorohydrin reactor is 41℃, 0.18MPa;
第二微界面发生器内的气液比为123：1；The gas-liquid ratio in the second micro-interface generator is 123:1;
皂化反应器内反应温度93℃，常压。The reaction temperature in the saponification reactor is 93°C and atmospheric pressure.
经检测，使用所述系统及工艺后，乙烯转化率98.8％，工艺的合成效率提升3.8％。After testing, after using the system and process, the ethylene conversion rate is 98.8%, and the synthesis efficiency of the process is increased by 3.8%.
实施例4Example 4
使用上述系统及工艺进行乙烯制备环氧乙烷，其中：Use the above system and process to prepare ethylene oxide from ethylene, where:
所述工艺中次氯酸反应器内反应温度为19℃，常压；In the process, the reaction temperature in the hypochlorous acid reactor is 19°C and normal pressure;
第一微界面发生器内气液比为128:1；The gas-liquid ratio in the first micro-interface generator is 128:1;
氯醇化反应器内反应温度为45℃，0.19MPa；The reaction temperature in the chlorohydrin reactor is 45°C, 0.19MPa;
第二微界面发生器内的气液比为124：1；The gas-liquid ratio in the second micro-interface generator is 124:1;
皂化反应器内反应温度96℃，常压。The reaction temperature in the saponification reactor is 96°C and atmospheric pressure.
经检测，使用所述系统及工艺后，乙烯转化率98.9％，工艺的合成效率提升3.9％。After testing, after using the system and process, the ethylene conversion rate is 98.9%, and the synthesis efficiency of the process is increased by 3.9%.
实施例5Example 5
使用上述系统及工艺进行乙烯制备环氧乙烷，其中：Use the above system and process to prepare ethylene oxide from ethylene, where:
所述工艺中次氯酸反应器内反应温度为20℃，常压；In the process, the reaction temperature in the hypochlorous acid reactor is 20°C and normal pressure;
第一微界面发生器内气液比为130:1；The gas-liquid ratio in the first micro-interface generator is 130:1;
氯醇化反应器内反应温度为47℃，0.19MPa；The reaction temperature in the chlorohydrin reactor is 47°C, 0.19MPa;
第二微界面发生器内的气液比为125：1；The gas-liquid ratio in the second micro-interface generator is 125:1;
皂化反应器内反应温度97℃，常压。The reaction temperature in the saponification reactor is 97°C and atmospheric pressure.
经检测，使用所述系统及工艺后，乙烯转化率99.0％，工艺的合成效率提升4.0％。After testing, after using the system and process, the ethylene conversion rate is 99.0%, and the synthesis efficiency of the process is increased by 4.0%.
对比例Comparison
使用现有技术进行乙烯制备环氧乙烷，其中，本实施例选用的工艺参数与所述实施例5中的工艺参数相同。The prior art is used to prepare ethylene oxide from ethylene, wherein the process parameters selected in this embodiment are the same as those in the fifth embodiment.
经检测，使用所述系统及工艺后，乙烯转化率73.3％。After testing, after using the system and process, the ethylene conversion rate is 73.3%.
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。So far, the technical solutions of the present invention have been described in conjunction with the preferred embodiments shown in the drawings. However, it is easy for those skilled in the art to understand that the protection scope of the present invention is obviously not limited to these specific embodiments. Without departing from the principle of the present invention, those skilled in the art can make equivalent changes or substitutions to the relevant technical features, and the technical solutions after these changes or substitutions will fall within the protection scope of the present invention.
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。The above descriptions are only preferred embodiments of the present invention and are not used to limit the present invention; for those skilled in the art, the present invention can have various modifications and changes. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present invention should be included in the protection scope of the present invention.

Claims (10)

  1. 一种乙烯制备环氧乙烷的微界面强化系统，其特征在于，包括：A micro-interface strengthening system for preparing ethylene oxide from ethylene, which is characterized in that it comprises:
    次氯酸合成单元，用以为氯气和水提供反应场所，并对生成物料进行分离；The hypochlorous acid synthesis unit is used to provide a reaction place for chlorine and water, and to separate the generated materials;
    氯醇化反应单元，与所述次氯酸合成单元相连，用以为次氯酸合成单元输出物料与乙烯提供反应场所；The chlorohydrinization reaction unit is connected to the hypochlorous acid synthesis unit to provide a reaction place for the output material of the hypochlorous acid synthesis unit and ethylene;
    皂化反应单元，与所述氯醇化反应单元相连，用以为氯醇化反应单元输出液相物料与石灰乳提供反应场所；The saponification reaction unit is connected to the chlorohydrin reaction unit and is used to provide a reaction place for the chlorohydrin reaction unit to output liquid phase materials and lime milk;
    分离纯化单元，与所述皂化反应单元相连，用以为输出液相物料进行精馏分离；A separation and purification unit, connected to the saponification reaction unit, for rectifying and separating the output liquid phase materials;
    微界面发生器，其设置个数为两个，分别设置在所述次氯酸合成单元和所述氯醇化反应单元，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气相组分，使气相气破碎形成直径≥1μm、且＜1mm的微米级气泡以提高气相组分与液相组分的传质面积，减小液膜厚度，降低传质阻力，并在破碎后将液相组分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气液组分的传质效率和反应效率。The number of micro-interface generators is two, which are respectively installed in the hypochlorous acid synthesis unit and the chlorohydrin reaction unit, and convert the pressure energy of the gas and/or the kinetic energy of the liquid into the surface energy of the bubble and transfer it to The gas phase component breaks the gas phase gas to form micron-sized bubbles with a diameter of ≥1μm and <1mm to increase the mass transfer area of the gas phase component and the liquid phase component, reduce the thickness of the liquid film, and reduce the mass transfer resistance, and after crushing The liquid phase component is mixed with micron-sized bubbles to form a gas-liquid emulsion to enhance the mass transfer efficiency and reaction efficiency of the gas-liquid component within the preset operating condition range.
  2. 根据权利要求1所述的乙烯制备环氧乙烷的微界面强化系统，其特征在于，所述微界面发生器为气动式微界面发生器，所述微界面发生器包括第一微界面发生器和第二微界面发生器；The micro-interface strengthening system for preparing ethylene oxide from ethylene according to claim 1, wherein the micro-interface generator is a pneumatic micro-interface generator, and the micro-interface generator includes a first micro-interface generator and The second micro-interface generator;
    所述第一微界面发生器设置在所述次氯酸合成单元的反应区底部，用以将氯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次氯酸合成单元内与水混合形成气液乳化物；The first micro-interface generator is arranged at the bottom of the reaction zone of the hypochlorous acid synthesis unit, and is used to crush the chlorine gas to form micron-scale micron-scale bubbles and output the micron-scale bubbles to the hypochlorous acid synthesis unit after the crushing is completed It is mixed with water to form a gas-liquid emulsion;
    所述第二微界面发生器设置在所述氯醇化反应单元的反应区底部，用以将乙烯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氯醇化反应单元内与次氯酸合成单元输出液相物料混合形成气液乳化物。The second micro-interface generator is arranged at the bottom of the reaction zone of the chlorohydrin reaction unit, and is used to crush ethylene to form micron-sized micro-sized bubbles and output the micro-sized bubbles to the chlorohydrin reaction unit after the crushing is completed. The output liquid phase material of the hypochlorous acid synthesis unit is mixed to form a gas-liquid emulsion.
  3. 根据权利要求1所述的乙烯制备环氧乙烷的微界面强化系统，其特征在于，所述次氯酸合成单元包括：The micro-interface strengthening system for preparing ethylene oxide from ethylene according to claim 1, wherein the hypochlorous acid synthesis unit comprises:
    次氯酸反应器，用以为氯气和水提供反应场所；Hypochlorous acid reactor to provide a reaction place for chlorine and water;
    气相进料管道，其设置在所述次氯酸反应器的侧壁并与所述第一微界面发生器相连，用以将氯气输送至第一微界面发生器内，并使微界面发生器对氯气进行破碎；The gas-phase feed pipeline is arranged on the side wall of the hypochlorous acid reactor and connected to the first micro-interface generator, and is used to transport chlorine gas into the first micro-interface generator and make the micro-interface generator Crush the chlorine gas;
    液相进料管道，其设置在所述次氯酸反应器的侧壁并位于所述气相进料管道上方，用以将水输送至次氯酸反应器内；A liquid-phase feed pipe, which is arranged on the side wall of the hypochlorous acid reactor and above the gas-phase feed pipe, to transport water into the hypochlorous acid reactor;
  4. 根据权利要求3所述的乙烯制备环氧乙烷的微界面强化系统，其特征在于，所述次氯酸合成单元还包括：The micro-interface strengthening system for preparing ethylene oxide from ethylene according to claim 3, wherein the hypochlorous acid synthesis unit further comprises:
    第一气相回流管，其设置在所述次氯酸反应器上并与所述第一微界面发生器相连，用以将气相组分回输至次氯酸反应器内；A first gas-phase reflux pipe, which is arranged on the hypochlorous acid reactor and connected to the first micro-interface generator, for returning the gas phase components to the hypochlorous acid reactor;
    气液分离器，其与所述次氯酸反应器相连，用以对次氯酸反应器输出物料进行气液分离。The gas-liquid separator is connected with the hypochlorous acid reactor and is used for gas-liquid separation of the output materials of the hypochlorous acid reactor.
  5. 根据权利要求1所述的乙烯制备环氧乙烷的微界面强化系统，其特征在于，所述氯醇化反应单元包括：The micro-interface strengthening system for preparing ethylene oxide from ethylene according to claim 1, wherein the chlorohydrin reaction unit comprises:
    氯醇化反应器，其与所述气液分离器相连，用以为次氯酸和乙烯提供反应场所；The chlorohydrinization reactor is connected to the gas-liquid separator to provide a reaction place for hypochlorous acid and ethylene;
    乙烯进料管道，其设置在所述氯醇化反应器的侧壁并与所述第二微界面发生器相连，用以将乙烯输送至第二微界面发生器内，并使微界面发生器对乙烯进行破碎。An ethylene feed pipe, which is arranged on the side wall of the chlorohydrin reactor and connected to the second micro-interface generator, is used to transport ethylene into the second micro-interface generator and make the micro-interface generator to The ethylene is broken.
  6. 根据权利要求5所述的乙烯制备环氧乙烷的微界面强化系统，其特征在于，所述氯醇化反应单元还包括：The micro-interface strengthening system for preparing ethylene oxide from ethylene according to claim 5, wherein the chlorohydrin reaction unit further comprises:
    第二气相回流管，其设置在所述氯醇化反应器上并与所述第二微界面发生器相连，用以将气相组分回输至氯醇化反应器内。The second gas-phase reflux pipe is arranged on the chlorohydrin reactor and connected with the second micro-interface generator, and is used for returning the gas-phase components to the chlorohydrin reactor.
  7. 根据权利要求1所述的乙烯制备环氧乙烷的微界面强化系统，其特征在于，所述皂化反应单元包括：The micro-interface strengthening system for preparing ethylene oxide from ethylene according to claim 1, wherein the saponification reaction unit comprises:
    皂化反应器，与所述氯醇化反应器相连，用以为氯醇化反应单元输出液相物料与石灰乳提供反应场所；The saponification reactor is connected to the chlorohydrinization reactor and is used to provide a reaction place for the chlorohydrinization reaction unit to output liquid phase materials and lime milk;
    石灰乳进料管道，其设置在所述皂化反应器的侧壁，用以将石灰乳输送至皂化反应器内。The lime milk feed pipe is arranged on the side wall of the saponification reactor to transport the lime milk into the saponification reactor.
  8. 根据权利要求1所述的乙烯制备环氧乙烷的微界面强化系统，其特征在于，所述分离纯化单元包括：The micro-interface strengthening system for preparing ethylene oxide from ethylene according to claim 1, wherein the separation and purification unit comprises:
    换热器，其与所述皂化反应单元相连，用以为皂化反应单元输出物料与环氧乙烷进行能量交换；A heat exchanger, which is connected to the saponification reaction unit, and is used to exchange energy between the output material of the saponification reaction unit and ethylene oxide;
    精馏塔，其与所述换热器相连，用以对皂化反应单元输出物料进行精馏分离。A rectification tower, which is connected with the heat exchanger, is used for rectifying and separating the output materials of the saponification reaction unit.
  9. 一种乙烯制备环氧乙烷的微界面强化工艺，其特征在于，包括：A micro-interface strengthening process for preparing ethylene oxide from ethylene, which is characterized in that it comprises:
    次氯酸合成工序：Hypochlorous acid synthesis process:
    步骤1：通过所述液相进料管道向所述次氯酸反应器内输送水；Step 1: Transport water into the hypochlorous acid reactor through the liquid-phase feed pipeline;
    步骤2：通过所述气相进料管道向所述次氯酸反应器内输送氯气，所述气相进料管道会将氯气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氯气进行破碎，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次氯酸反应器并与水混合形成气液乳化物，气液乳化物进反应，生成次氯酸混合物；Step 2: Transport chlorine gas into the hypochlorous acid reactor through the gas-phase feed pipe, the gas-phase feed pipe will transport the chlorine gas to the first micro-interface generator, and the first micro-interface The device crushes the chlorine gas to form micron-sized bubbles. After the crushing is completed, the first micro-interface generator outputs the micron-sized bubbles to the hypochlorous acid reactor and mixes with water to form a gas-liquid emulsion. The liquid emulsion reacts to form a mixture of hypochlorous acid;
    步骤3：所述次氯酸反应器内未充分反应氯气沿所述次氯酸反应器顶部所述第一气相回流管回流入所述第一微界面发生器，并通过所述第一微界面发生器对氯气进行破碎，与水进一步反应；Step 3: The under-reacted chlorine gas in the hypochlorous acid reactor flows back into the first micro-interface generator along the first gas-phase reflux pipe on the top of the hypochlorous acid reactor, and passes through the first micro-interface The generator breaks the chlorine gas and further reacts with water;
    步骤4：所述次氯酸反应器内液相组分流入所述气液分离器，气液分离后，尾气沿所述气液分离器顶部气相出口排出，次氯酸溶液沿所述气液分离器底部液相出口排出，并传输至氯醇化反应单元；Step 4: The liquid phase components in the hypochlorous acid reactor flow into the gas-liquid separator. After gas-liquid separation, the tail gas is discharged along the gas-phase outlet at the top of the gas-liquid separator, and the hypochlorous acid solution flows along the gas-liquid separator. The liquid phase outlet at the bottom of the separator is discharged and transferred to the chlorohydrin reaction unit;
    氯醇化反应工序：Chlorohydrin reaction process:
    步骤5：次氯酸溶液进入所述氯醇化反应器，通过所述乙烯进料管道向所述氯醇化反应器内输送乙烯，所述乙烯进料管道会将乙烯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乙烯进行破碎，形成微米尺度的微米级气泡；Step 5: The hypochlorous acid solution enters the chlorohydrinization reactor, and ethylene is transported into the chlorohydrinization reactor through the ethylene feed pipe, and the ethylene feed pipe will transport ethylene gas to the second micro An interface generator, wherein the second micro-interface generator breaks ethylene to form micro-scale bubbles of micron scale;
    步骤6：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氯醇化反应器并与次氯酸溶液混合形成气液乳化物，气液乳化物进反应，生成氯乙醇溶液，所述氯醇化反应器内氯乙醇溶液流出并传输至皂化反应单元；Step 6: After the crushing is completed, the second micro-interface generator outputs micron-sized bubbles to the chlorohydrinization reactor and mixes them with the hypochlorous acid solution to form a gas-liquid emulsion, and the gas-liquid emulsion reacts to produce chloroethanol Solution, the chloroethanol solution in the chlorohydrinization reactor flows out and is transferred to the saponification reaction unit;
    步骤7：所述氯醇化反应器内未充分反应乙烯沿所述氯醇化反应器顶部所述第二气相回流管回流入所述第二微界面发生器，并通过所述第二微界面发生器对乙烯进行破碎，与次氯酸溶液进一步反应；Step 7: Under-reacted ethylene in the chlorohydrinization reactor flows back into the second micro-interface generator along the second gas-phase reflux pipe on the top of the chlorohydrin reactor, and passes through the second micro-interface generator Crush the ethylene and further react with the hypochlorous acid solution;
    皂化工序：Saponification process:
    步骤8：氯乙醇溶液流入所述皂化反应单元内，通过石灰乳进料管道向所述皂化反应单元内传输石灰乳，石灰乳与氯乙醇溶液在所述皂化反应单元内发生皂化反应，产生环氧乙烷混合物，所述皂化反应内环氧乙烷混合物流出并传输至分 离纯化单元；Step 8: The chloroethanol solution flows into the saponification reaction unit, and the lime milk is transferred into the saponification reaction unit through the lime milk feed pipe. The lime milk and the chloroethanol solution undergo a saponification reaction in the saponification reaction unit to produce a ring Oxyethane mixture, where the ethylene oxide mixture flows out in the saponification reaction and is transferred to the separation and purification unit;
    分离纯化工序：Separation and purification process:
    步骤9：环氧乙烷混合物流入所述分离纯化单元内，其中环氧乙烷混合物流经所述换热器进入所述精馏塔内进行精馏，精馏塔输出气相物料为环氧乙烷气体，其他废水沿精馏塔塔底排出，其中环氧乙烷气体在所述换热器内与环氧乙烷混合物进行热交换并排出，即获得环氧乙烷产品。Step 9: The ethylene oxide mixture flows into the separation and purification unit, where the ethylene oxide mixture flows through the heat exchanger and enters the rectification tower for rectification, and the gas phase material output from the rectification tower is ethylene oxide Alkane gas and other waste water are discharged along the bottom of the rectification tower, wherein the ethylene oxide gas exchanges heat with the ethylene oxide mixture in the heat exchanger and is discharged to obtain an ethylene oxide product.
  10. 根据权利要求9所述的乙烯制备环氧乙烷的微界面强化工艺，其特征在于，所述工艺中次氯酸反应器内反应温度为10-20℃，常压，所述第一微界面发生器内的气液比为120-130:1；The micro-interface strengthening process for preparing ethylene oxide from ethylene according to claim 9, wherein the reaction temperature in the hypochlorous acid reactor in the process is 10-20° C. and atmospheric pressure, and the first micro-interface The gas-liquid ratio in the generator is 120-130:1;
    所述工艺中氯醇化反应器内反应温度为37-47℃，反应压强为0.13-0.19MPa，所述第二微界面发生器内的气液比为115-125:1；In the process, the reaction temperature in the chlorohydrinization reactor is 37-47°C, the reaction pressure is 0.13-0.19MPa, and the gas-liquid ratio in the second micro-interface generator is 115-125:1;
    所述工艺中皂化反应器内反应温度为87-97℃，常压。In the process, the reaction temperature in the saponification reactor is 87-97°C and normal pressure.
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