CN216605220U - Apparatus for producing of hydroxyethylidene/propyl ethylenediamine - Google Patents
Apparatus for producing of hydroxyethylidene/propyl ethylenediamine Download PDFInfo
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- CN216605220U CN216605220U CN202123440893.6U CN202123440893U CN216605220U CN 216605220 U CN216605220 U CN 216605220U CN 202123440893 U CN202123440893 U CN 202123440893U CN 216605220 U CN216605220 U CN 216605220U
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Abstract
The utility model provides a production device of hydroxyethyl/propyl ethylenediamine, which comprises a continuous conveying unit, a mixing unit, a reaction unit and a rectifying unit which are communicated in sequence; the mixing unit is a micro mixer; the rectification unit comprises a light component removal rectification tower and a heavy component removal rectification tower which are sequentially communicated, the light component removal rectification tower is provided with a reaction liquid inlet, an ethylene diamine outlet and a light component removal mother liquid outlet, the heavy component removal rectification tower is provided with a light component removal mother liquid inlet, a heavy component outlet and a hydroxyethyl/propyl ethylene diamine product outlet, and the light component removal mother liquid outlet is communicated with the light component removal mother liquid inlet of the heavy component removal rectification tower; the production device of hydroxyethylethylene/propylethylenediamine comprises a back pressure system. According to the utility model, the back pressure system is arranged, and materials are quickly mixed in a liquid state in the mixing unit before entering the reaction unit, so that the volume of the reactor can be reduced, the situation that the polyhydroxy compounds are increased is avoided, the product yield is improved, the energy consumption is reduced, and the safety is improved.
Description
Technical Field
The utility model belongs to the technical field of organic chemical industry, and particularly relates to a production device of hydroxyethyl/propyl ethylenediamine.
Background
Hydroxyethyl ethylenediamine and hydroxypropyl ethylenediamine are important chemical raw materials, and the hydroxyethyl ethylenediamine can be used for producing dyes, resins, rubber, flotation agents, insecticides, surfactants, corrosion inhibitors and the like, can also be used as a curing agent of epoxy resin, has excellent performance, low toxicity and environmental protection; the hydroxypropyl ethylenediamine can be used for producing zwitterionic and cationic oxazoline surfactants, and can be used for producing various shampoos, bath lotions and personal and industrial detergents; the compound is used as a raw material in the pharmaceutical industry to produce a pharmaceutical intermediate 2-methylpiperazine, an antituberculotic drug pyrazinamide and the like.
The production device of hydroxyethyl ethylenediamine and hydroxypropyl ethylenediamine can be shared, and the synthesis device of hydroxyethyl ethylenediamine is taken as an example to illustrate the prior art and the problems existing in the prior art.
Because the boiling points of ethylene oxide and propylene oxide are both low, a device suitable for gas-liquid reaction is generally adopted in industrial production. CN102617363A discloses a novel process for synthesizing hydroxyethyl ethylenediamine from ethylenediamine and ethylene oxide, wherein a reaction zone is formed by designing a set of novel gas-liquid reaction device and placing the novel gas-liquid reaction device between the rectification section and the stripping section of a rectification tower, and a gas distribution disc is arranged at an inlet of the reaction zone.
The tower-type gas-liquid reactor can not completely avoid the generation of ethylene oxide waste gas, for example, in the environmental evaluation disclosed by a certain enterprise, 2.14kg of ethylene oxide waste gas can be generated when one batch of hydroxyethyl ethylenediamine is produced, because ethylene oxide belongs to a flammable dangerous material, the explosion limit range is very wide (3-100), the combustion heat is very high (1262.8kJ/mol), and if the ethylene oxide is not properly treated, the safety of the production process can be threatened.
CN102786425B discloses a method for producing beta-hydroxyethyl ethylenediamine, which adopts a micro-reactor, utilizes the micro-mixing principle to distribute dispersed phase ethylene oxide in parallel in a micro-channel continuous phase through micro-scale micropores so as to achieve the aim of uniform dispersion, and simultaneously reacts partial raw materials to reduce the feeding ratio of ethylenediamine and ethylene oxide and the amount of byproducts. According to the description in the patent example, after the ethylene oxide and the ethylenediamine are in contact reaction in the microreactor, the conversion rate of the ethylene oxide only reaches about 25 percent, and the space velocity of the ethylene oxide described in the patent can be 4-40 ten thousand kg.h-1·m-3When the space velocity of ethylene oxide is 40 ten thousand kg.h-1·m-3In order to ensure the conversion rate of the ethylene oxide, heat-insulating curing equipment with the volume of two hundred cubes needs to be matched, the size is large, the safety is poor, and the production efficiency is not improved due to the fact that a micro-reactor is adopted at the front end. In addition, in CN102786425B, in order to realize gas-liquid mixing of ethylene oxide and ethylenediamine, the ethylene oxide is output to a heater in a liquid form through back pressure of a pump, heated and gasified, and then enters into a microreactor, and energy waste is also caused by heat absorption in the process of converting the ethylene oxide from a liquid state to a gas state.
SUMMERY OF THE UTILITY MODEL
The utility model aims to provide a production device of hydroxyethyl/propyl ethylenediamine, wherein the volume of a reactor is obviously reduced, the production efficiency is obviously improved, the energy consumption is reduced, and the safety is improved.
The utility model provides a production device of hydroxyethyl/propyl ethylenediamine, which is characterized by comprising a continuous conveying unit, a mixing unit, a reaction unit and a rectifying unit which are sequentially communicated;
the mixing unit is a micro mixer and is used for mixing liquid ethylenediamine and liquid ethylene oxide/propane;
the reaction unit is a microchannel reactor, a tubular reactor or a combination of the microchannel reactor and the tubular reactor;
the rectification unit comprises a light component removal rectification tower and a heavy component removal rectification tower which are communicated in sequence,
the heavy component removal rectifying tower is provided with a heavy component removal rectifying tower, a heavy component removal rectifying tower and a hydroxyethyl/propyl ethylenediamine product outlet, and the light component removal rectifying tower is provided with a reaction liquid inlet, an ethylenediamine outlet and a light component removal mother liquid outlet which is communicated with the light component removal mother liquid inlet of the heavy component removal rectifying tower.
Preferably, the continuous feed unit comprises at least two feed pumps for feeding ethylenediamine and ethylene/propane oxide.
Preferably, the characteristic size of the mixing channel of the mixing unit is 1-10 mm.
Preferably, the mixing unit is provided with a heat exchange channel.
Preferably, a preheating unit is further arranged between the mixing unit and the continuous conveying unit.
Preferably, the volume of the reaction unit is 1-200L.
Preferably, the front section of the continuous conveying unit is further provided with a storage unit, and the storage unit comprises a device for storing or temporarily storing ethylenediamine and a device for storing or temporarily storing ethylene oxide/propane.
Preferably, an ethylenediamine outlet of the light component removal rectifying tower is communicated with a device for storing or temporarily storing ethylenediamine in the storage unit, or is communicated with a separate ethylenediamine collecting tank.
Preferably, the mixing unit can also be a reaction plate in a microchannel reactor.
Preferably, the apparatus for producing hydroxyethylene/propylethylenediamine further comprises a back pressure system.
The utility model provides a production device of hydroxyethyl/propyl ethylenediamine, which comprises a continuous conveying unit, a mixing unit, a reaction unit and a rectifying unit which are communicated in sequence; the mixing unit is a micro mixer; the reaction unit is a microchannel reactor, a tubular reactor or a combination of the microchannel reactor and the tubular reactor; the rectification unit comprises a light component removal rectification tower and a heavy component removal rectification tower which are sequentially communicated, the light component removal rectification tower is provided with a reaction liquid inlet, an ethylene diamine outlet and a light component removal mother liquid outlet, the heavy component removal rectification tower is provided with a light component removal mother liquid inlet, a heavy component outlet and a hydroxyethyl/propyl ethylene diamine product outlet, and the light component removal mother liquid outlet is communicated with the light component removal mother liquid inlet of the heavy component removal rectification tower; the production device of hydroxyethylethylene/propylethylenediamine comprises a back pressure system. In addition, the utility model can realize that the ethylene oxide/propane and the ethylenediamine are mixed in the mixing unit in a liquid form and enter the reaction unit for reaction by arranging a back pressure system, so that the volume of the reactor is reduced, the product yield is improved, the energy consumption is reduced, and the safety is improved.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the provided drawings without creative efforts.
FIG. 1 is a schematic view of an apparatus for producing hydroxyethylene/propylethylenediamine used in example 1 of the present invention;
FIG. 2 is a schematic view of an apparatus for producing hydroxyethylene/propylethylenediamine used in example 2 of the present invention;
in fig. 1-2, 1-1 is an ethylenediamine feeding pump, 1-2 is an ethylene oxide/propane feeding pump, 2 is a mixing unit, 3 is a reaction unit, 4-1 is a light component removal rectifying tower, 4-2 is a heavy component removal rectifying tower, 5-1 is an ethylenediamine heat exchanger, and 5-2 is an ethylene oxide/propane heat exchanger.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The utility model provides a production device of hydroxyethyl/propyl ethylenediamine, which is characterized by comprising a continuous conveying unit, a mixing unit, a reaction unit and a rectifying unit which are sequentially communicated;
the mixing unit is a micro mixer;
the reaction unit is a microchannel reactor, a tubular reactor or a combination of the microchannel reactor and the tubular reactor;
the rectification unit comprises a light component removal rectification tower and a heavy component removal rectification tower which are communicated in sequence,
the light component removal rectifying tower is provided with a reaction liquid inlet, an ethylenediamine outlet and a light component removal mother liquid outlet, the heavy component removal rectifying tower is provided with a light component removal mother liquid inlet, a heavy component outlet and a hydroxyethyl ethylene/propyl ethylenediamine product outlet, and the light component removal mother liquid outlet is communicated with the light component removal mother liquid inlet of the heavy component removal rectifying tower.
In the utility model, the production device of the hydroxyethylene/propylethylenediamine is a continuous production device and comprises a continuous conveying unit, a mixing unit, a reaction unit and a rectifying unit.
In the utility model, the continuous conveying unit is used for realizing the continuous conveying of the materials of the ethylenediamine and the ethylene oxide/propane and providing power for the flowing of the materials in the continuous production device, and in order to realize the continuous and safe conveying of the materials to the mixing unit and into the reaction unit by overcoming the pressure resistance, the continuous conveying system comprises at least two feeding pumps with the upper pressure limit not lower than 2MPa, the feeding pumps are used for respectively conveying the ethylenediamine and the ethylene oxide/propane, and the feeding pumps are provided with an ethylenediamine outlet and an ethylene oxide/propane outlet which are communicated with the inlet of the mixing unit. If the upper pressure limit of the feed pump is lower than 2MPa, the power provided in the process of conveying materials is limited, so that the product cannot smoothly enter the mixing unit and the subsequent reaction unit, or the feeding is stopped because the pressure of the reaction system is higher than the upper pressure limit of the feed pump.
In the utility model, the mixing unit is preferably a micro mixer, provided with an ethylenediamine inlet and an ethylene oxide/propane inlet which are respectively communicated with an ethylenediamine outlet and an ethylene oxide/propane outlet of the continuous conveying unit, and further provided with a mixed liquid outlet which is communicated with a mixed liquid inlet of the reaction unit. The mixing unit has the function of realizing the rapid mixing of the ethylenediamine and the ethylene oxide/propane in a liquid state. In order to ensure that the ethylenediamine and the ethylene oxide/propane are uniformly mixed before entering the reaction unit and realize industrial mass production, the characteristic dimension (width or depth) of the mixing channel is preferably 1-10 mm. And a micro mixer with a heat exchange channel is preferred, so that the condition that the reaction of the ethylenediamine and the ethylene oxide/propane is accelerated due to the fact that the temperature of a mixing unit is increased because the heat released by the reaction of the ethylenediamine and the ethylene oxide/propane during mixing cannot be removed in time is avoided.
Preferably, a preheating unit is further arranged before the mixing unit, and the preheating unit is preferably a heat exchanger and is used for preheating the ethylenediamine and the ethylene oxide/propane to the required temperature.
In the utility model, the reaction unit is used for providing a place for mixing and reacting ethylene diamine and ethylene oxide/propane, the reaction unit is provided with a mixed liquid inlet and a reaction liquid outlet, and the reaction liquid outlet is communicated with an inlet of the light component removal rectifying tower.
The reaction unit can be a microchannel reactor, a tubular reactor, or a combination of a microchannel reactor and a tubular reactor, preferably a combination of a microchannel reactor and a tubular reactor; the microchannel reactor is a reactor consisting of a plurality of micro reaction sheets with reaction channels and heat exchange channels, and the micro mixer of the mixing unit can also be replaced by the reaction sheets of the microchannel reactor. The tubular reactor is a tubular reactor which is provided with a mixing element playing a role of turbulent flow in a reaction cavity, a reactor provided with a heat exchange jacket outside the reaction cavity or a tubular reactor capable of exchanging heat, both of which have the advantages of high mass transfer efficiency, good heat transfer effect and the like, can ensure that ethylene oxide/propane and ethylenediamine can quickly and stably react in a flowing process in a reaction unit, reduce the contact probability of products and raw materials, reduce the occurrence of side reactions and realize that the conversion rate of ethylene oxide/propane reaches 100%. In the utility model, the volume of the microchannel reactor or the tubular reactor is preferably 1-200L, and more preferably 10-150L.
In the utility model, the rectifying unit comprises a light-component removal rectifying tower and a heavy-component removal rectifying tower which are sequentially communicated, the light-component removal rectifying tower is provided with a reaction liquid inlet, an ethylenediamine outlet and a light-component removal mother liquid outlet, the heavy-component removal rectifying tower is provided with a light-component removal mother liquid inlet, a heavy-component removal outlet and a hydroxyethyl/propyl ethylenediamine product outlet, and the light-component removal mother liquid outlet is communicated with the light-component removal mother liquid inlet of the heavy-component removal rectifying tower.
The utility model adopts a backpressure system to carry out backpressure on a reaction system, a pressure regulating valve is arranged on a connecting pipeline between a reaction unit and a separation unit, the pressure of the system is fed back in real time through pressure sensing, and the pressure regulation and control of the reaction system are realized through automatic regulating systems such as feeding control, temperature control, discharge control and the like.
In the utility model, for the device with larger capacity, a material storage unit is preferably arranged at the front section of the continuous conveying unit, wherein the material storage unit comprises a storage tank, a temporary storage tank and a tank for storing or temporarily storing ethylenediamine, and a storage tank, a temporary storage tank and a tank for storing or temporarily storing ethylene oxide/propane.
In the utility model, an ethylenediamine outlet of the light component removal rectifying tower is communicated with an ethylenediamine storage tank or an independent ethylenediamine collecting tank stored or temporarily stored in the storage unit, and the ethylenediamine outlet is used for cooling and recovering ethylenediamine obtained by separation of the light component removal rectifying tower and then returning the ethylenediamine to the continuous production device for production of hydroxyethylene/propylethylenediamine so as to improve the utilization rate of the ethylenediamine.
Because the rapid reaction of the ethylenediamine and the ethylene oxide requires a certain temperature to be provided in advance, and the reaction of the ethylenediamine and the ethylene oxide is an exothermic reaction, in the specific embodiment of the utility model, the temperature required for the reaction of the ethylenediamine and the ethylene oxide is provided by the heat exchange system, and the heat released by the reaction is removed in time. The heat exchange system can be an independent heat exchange device, such as a high-low temperature cold-hot integrated machine, is connected with a heat exchange channel of the device in the reaction unit, and adjusts the temperature through an ACS automatic control system; the heat exchange system can also adopt public works, a flow regulating valve group is arranged on an outlet pipeline of a steam system or a heat conduction oil system, and the temperature of materials is detected through a thermal resistor, so that the flow of the public works is regulated to realize the temperature control of the mixing unit, the reaction unit and the separation unit.
In the continuous production device for producing the hydroxyethyl ethylene diamine, all systems and units are connected with the automatic control system for automatic operation, so that the continuous automatic production of the hydroxyethyl ethylene diamine can be realized. In the utility model, the continuous production device of the hydroxyethyl ethylenediamine is provided with the detection and control of flow, pressure and temperature, and overpressure and overtemperature safety interlock. The overpressure safety interlock is arranged in the continuous conveying system, when any one parameter reaches a set value, the ESD emergency stop system is executed, a protection interlock signal is sent out, the feeding pump is closed, the equipment is safely protected, and serious loss caused by danger diffusion is avoided. The over-temperature safety interlock is characterized in that a temperature alarm interlock (high-temperature alarm value: 250 ℃) is arranged on the reactor, when the temperature exceeds the high-temperature alarm value, the system increases the public work consumption through an adjusting valve, and simultaneously executes an ESD emergency shutdown system to send out a protection interlock signal, close a feed pump, perform safety protection on equipment and avoid serious loss caused by dangerous diffusion. In addition, the continuous production device has four working modes: the production mode, the cleaning mode, the trial run mode and the shutdown mode are controlled by remote operation, so that the safety of automation and production processes is greatly improved.
In the present invention, unless otherwise explicitly specified or limited, the connection means between the systems/devices such as "communicate" and "connect" should be understood in a broad sense. For example, the connection may be direct pipe connection, or may be pipe connection connected with conventional conveying, metering, controlling, and temporary storage equipment such as pumping equipment, metering equipment, valve pipe fittings, and storage tanks, or may be fixed connection or detachable connection. The specific meaning of the above terms in the present invention can be understood by those skilled in the art according to specific situations.
Based on the production device of the hydroxyethylene/propylethylenediamine, the utility model also provides a production process of the hydroxyethylene/propylethylenediamine, which comprises the following steps:
A) conveying ethylenediamine and ethylene oxide/propane to a mixing unit through a continuous conveying unit for mixing to obtain a mixed solution;
B) conveying the mixed solution to a reaction unit for reaction to obtain a reaction solution;
the reaction temperature is 80-200 ℃;
C) and conveying the reaction liquid to a rectification unit, and separating unreacted raw material ethylenediamine to obtain a hydroxyethyl/propyl ethylenediamine product.
The term "ethylene oxide/propylene oxide" as used herein refers to ethylene oxide or propylene oxide; "hydroxyethylethylene/propylethylenediamine" refers to hydroxyethylethylenediamine or hydroxypropylethylenediamine.
In the utility model, the ethylenediamine and the ethylene oxide/propane are respectively conveyed to the mixing unit through the continuous conveying unit, so that the ethylenediamine and the ethylene oxide/propane are uniformly mixed in a liquid state to obtain a mixed solution, then the obtained mixed solution enters the reaction unit for reaction, and the generated reaction solution is continuously removed and transferred to the rectifying unit for separation. The ethylenediamine and the ethylene oxide/propane are mixed in a liquid state in the mixing unit, so that the condition of uneven mixing caused by great volume difference of gas phase and liquid phase is avoided, and the contact between the hydroxyethylene/propylethylenediamine and the ethylene oxide/propane is avoided to a certain extent by timely removing the reaction liquid containing the hydroxyethylene/propylethylenediamine.
In the utility model, materials are quickly mixed in the mixing unit at a lower temperature before entering the reaction unit, so that the situation that polyhydroxy compounds such as dihydroxyethylene/propylethylenediamine and the like generated by the hydroxyethylene/propylethylenediamine and the ethylene oxide/propane are increased due to the reaction of the oxyethylene/propane and the ethylenediamine under the condition of insufficient mixing can be avoided, and the product yield is improved.
In the utility model, the mixing unit is preferably a micro mixer, the mixing temperature is not more than 80 ℃, preferably 0-80 ℃, such as 10-70 ℃, such as 0 ℃, 10 ℃, 20 ℃, 30 ℃, 40 ℃, 50 ℃, 60 ℃, 70 ℃ and 80 ℃, and preferably ranges with any value as an upper limit or a lower limit; the ethylenediamine and the ethylene oxide/propane are mixed under the condition that the temperature is not higher than 80 ℃, so that the instant violent reaction between the ethylenediamine and the ethylene oxide/propane can be avoided, but when the ethylenediamine and the ethylene oxide/propane contact, part of raw materials react and release heat, in the utility model, in order to ensure that the raw materials are fully and uniformly mixed and control the conversion rate of the raw materials, the mixing time is preferably not longer than 5 s; the mixing pressure is preferably 1 to 8MPa, more preferably 1.3 to 6MPa, most preferably 1.8 to 4MPa, such as 1MPa, 1.3MPa, 1.5MPa, 1.8MPa, 2MPa, 2.5MPa, 3MPa, 3.5MPa, 4MPa, 4.5MPa, 5MPa, 5.5MPa, 6MPa, 6.5MPa, 7MPa, 7.5MPa, 8MPa, preferably any of the above values is the upper limit or the lower limit. Under the pressure, the ethylene oxide/propane and the ethylenediamine in the mixing unit can be ensured to be cyclized and reacted in a liquid state, and meanwhile, the materials are ensured to be balanced in proportion and fully mixed.
Preferably, in one embodiment of the present invention, the ethylene diamine and ethylene/propane oxide are first preheated to a desired temperature in a preheating unit and then mixed in a feeding unit to a mixing unit. In order to avoid the instant violent reaction of ethylene diamine and ethylene oxide/propane after preheating and mixing, the temperature of ethylene diamine and ethylene oxide/propane after preheating is not higher than 80 ℃.
The obtained mixed liquid flows out of the mixing unit and enters the reaction unit for reaction to obtain reaction liquid.
In the present invention, the reaction temperature is preferably 80 to 200 ℃, more preferably 100 to 180 ℃, such as 80 ℃, 90 ℃, 100 ℃, 110 ℃, 120 ℃, 130 ℃, 140 ℃, 150 ℃, 160 ℃, 170 ℃, 180 ℃, 190 ℃ and 200 ℃, preferably any of the above values is used as the upper limit or the lower limit of the range value. If the reaction temperature is too high, the reaction rate of the ethylenediamine and the ethylene oxide/propane is accelerated, but the rate of the side reaction of the product of the hydroxyethylene/propylethylenediamine and the ethylene oxide/propane is also accelerated, and in addition, the energy consumption and the safety risk are increased due to too high reaction temperature; if the reaction temperature is low, the reaction rate of ethylenediamine and ethylene oxide/propane will be reduced, the reaction time will be prolonged, the production efficiency will be reduced, the conversion rate of ethylene oxide/propane will be reduced within a certain reaction time,
in the present invention, the pressure of the reaction is preferably 1 to 8MPa, more preferably 1.3 to 6MPa, most preferably 1.8 to 4MPa, such as 1MPa, 1.3MPa, 1.5MPa, 1.8MPa, 2MPa, 2.5MPa, 3MPa, 3.5MPa, 4MPa, 4.5MPa, 5MPa, 5.5MPa, 6MPa, 6.5MPa, 7MPa, 7.5MPa, 8MPa, and is preferably a range value having any of the above values as an upper limit or a lower limit. If the pressure is too low, the mixture ratio of materials is unbalanced and the mixing is insufficient, and the residence time is insufficient due to the increase of the volume of the reactants, so that the conversion rate of ethylene oxide/propane is reduced, and the product yield is reduced.
In the present invention, the residence time of the material in the reaction unit is preferably 3 to 180s, more preferably 8 to 120s, such as 3s, 5s, 8s, 10s, 15s, 20s, 25s, 30s, 35s, 40s, 45s, 50s, 55s, 60s, 65s, 70s, 75s, 80s, 85s, 90s, 95s, 100s, 110s, 120s, 130s, 140s, 150s, 160s, 170s, 180s, and preferably any of the above values is used as an upper limit or a lower limit. If the retention time is too long, the generated hydroxyethylene/propylethylenediamine is not timely removed from the reaction system, and the hydroxyethylene/propylethylenediamine and ethylene oxide/propane generate side reaction to generate polyhydroxy compounds, so that the production efficiency is also reduced; if the residence time is too short, part of the ethylene oxide/propane is not completely reacted and is removed from the reaction system together with the reaction liquid, which lowers the yield of hydroxyethylene/propylethylenediamine and also lowers the safety.
In the utility model, the molar ratio of the ethylenediamine to the ethylene oxide/propane is (5-15): 1, more preferably (7-14): 1, such as 6:1, 7:1, 8:1, 9:1, 10:1, 11:1, 12:1, 13:1, 14:1, 15:1, preferably any of the above values is used as an upper or lower limit. By increasing the molar ratio of ethylene diamine to ethylene oxide/propane feed, the probability of contact between the product hydroxyethylene/propylethylene diamine and ethylene oxide/propane is reduced, so that the reaction of ethylene diamine with ethylene oxide/propane takes advantage of competing reactions with the hydroxyethylene/propylethylene diamine and ethylene oxide/propane, thereby reducing the probability of side reactions occurring. The higher the molar ratio of ethylenediamine to ethylene oxide/propane is when feeding, the lower the probability that hydroxyethylene/propylethylenediamine contacts with ethylene oxide/propane and causes side reaction, the higher the yield of hydroxyethylene/propylethylenediamine is, but the too high molar ratio of ethylenediamine to ethylene oxide/propane when feeding results in large handling capacity but small yield of a single set of production equipment in the production process, and the large circulation amount of ethylenediamine and high energy consumption; the lower molar ratio of ethylene diamine to ethylene oxide/propane feed, while reducing the amount of ethylene diamine recycled and reducing energy consumption, increases the probability of side reactions and decreases product yield when ethylene/propylene glycol contacts ethylene oxide/propane.
After the reaction is finished, the obtained reaction liquid contains ethylenediamine, hydroxyethyl/propyl ethylenediamine and a small amount of dihydroxyethylene/propyl ethylenediamine, the reaction liquid flows out of the reaction unit and enters a rectification unit, and unreacted ethylenediamine and polyhydroxy compounds in the reaction liquid are sequentially separated through rectification, so that a hydroxyethyl/propyl ethylenediamine product is obtained.
In the utility model, the rectifying unit comprises a light removal rectifying tower and a heavy removal rectifying tower, wherein the light removal rectifying tower is used for removing unreacted ethylenediamine, light removal mother liquor flowing out of the light removal rectifying tower enters the heavy removal rectifying tower, and the heavy removal rectifying tower is used for removing heavy components containing polyhydroxy compounds so as to purify hydroxyethyl ethylene/propyl ethylenediamine products.
In the utility model, the temperature of the bottom of the light component removal rectifying tower is preferably 100-200 ℃, more preferably 120-180 ℃, such as 100 ℃, 110 ℃, 120 ℃, 130 ℃, 140 ℃, 150 ℃, 160 ℃, 170 ℃, 180 ℃, 190 ℃ and 200 ℃, and is preferably a range value taking any value as an upper limit or a lower limit; the pressure of the light ends removal rectification column is preferably 1 to 100kPa, more preferably 10 to 90kPa, such as 1kPa, 10kPa, 20kPa, 30kPa, 40kPa, 50kPa, 60kPa, 70kPa, 80kPa, 90kPa, 100kPa, and preferably ranges in which any of the above values is an upper limit or a lower limit.
In the utility model, the temperature of the tower bottom of the de-heavy rectifying tower is preferably 130-250 ℃, more preferably 150-220 ℃, such as 130 ℃, 140 ℃, 150 ℃, 160 ℃, 170 ℃, 180 ℃, 190 ℃, 200 ℃, 210 ℃, 220 ℃, 230 ℃, 240 ℃ and 250 ℃, and preferably ranges with any value as the upper limit or the lower limit; the pressure in the heavy component removal and rectification column is preferably 0.5 to 15kPa, more preferably 1 to 10kPa, such as 0.5kPa, 1kPa, 1.5kPa, 2kPa, 2.5kPa, 3kPa, 3.5kPa, 4kPa, 4.5kPa, 5kPa, 5.5kPa, 6kPa, 6.5kPa, 7kPa, 7.5kPa, 8kPa, 8.5kPa, 9kPa, 9.5kPa, 10kPa, and preferably is in the range of any of the above values as the upper limit or the lower limit.
In one embodiment of the utility model, the continuous production device of hydroxyethylidene/propylethylenediamine is shown in figure 1 and comprises a continuous conveying system, a mixing unit, a reaction unit and a rectification unit, wherein the continuous conveying system comprises at least two feed pumps 1-1 and 1-2, and the feed pumps are respectively provided with an ethylenediamine outlet and an ethylene oxide/propane outlet; the mixing unit 2 is a micro mixer, the mixing unit is provided with an ethylenediamine inlet and an ethylene oxide/propane inlet which are respectively communicated with an ethylenediamine outlet and an ethylene oxide/propane outlet of the feeding pump, and the mixing unit 2 is also provided with a mixed liquid outlet which is communicated with an inlet of the reaction unit; the reaction unit 3 is a micro-channel reactor and/or a tubular reactor and is provided with an inlet and a reaction liquid outlet, the rectifying unit is provided with a light-component removal rectifying tower 4-1 and a heavy-component removal rectifying tower 4-2, the reaction liquid outlet of the reaction unit is communicated with the inlet of the light-component removal rectifying tower 4-1, and the kettle outlet of the light-component removal rectifying tower is communicated with the inlet of the heavy-component removal rectifying tower.
Preferably, as shown in FIG. 2, an ethylenediamine heat exchanger 5-1 and an ethylene oxide/propane heat exchanger 5-2 are further provided between the mixing unit 2 and the continuous feed system.
In the continuous production device, ethylenediamine and ethylene oxide/propane are respectively conveyed to a mixing unit through two feed pumps of a continuous conveying system according to a molar ratio of 5-15: 1, the ethylene diamine and the ethylene oxide/propane are uniformly mixed in a liquid state at a temperature of not higher than 80 ℃, the obtained mixed solution enters a reaction unit, the reaction unit reacts for 3-180 s at a temperature of 80-200 ℃ and a pressure of 1-8 MPa to obtain a reaction solution, the reaction solution enters a light component removal rectification tower of a rectification unit while the reaction solution is hot, the ethylenediamine is separated at a heating temperature of 100-200 ℃ and a pressure of 1-100 kPa in the tower kettle, the mother solution from which the ethylenediamine is removed enters a heavy component removal rectification tower, and the hydroxyethyl/propyl ethylenediamine is separated at a temperature of 130-250 ℃ and a pressure of 0.5-15 kPa to obtain the hydroxyethyl/propyl ethylenediamine.
According to the utility model, ethylene oxide/propane and ethylenediamine are mixed in a liquid state in a continuous production device and react to produce hydroxyethylene/propylethylenediamine, so that energy waste caused by heating and gasifying ethylene oxide/propane is avoided, energy can be saved by 569.87kJ when ethylene oxide per kilogram participates in production of hydroxyethylethylenediamine, namely, 8.23 tons of standard coal can be saved when every 1000 tons of hydroxyethylethylenediamine is produced, and energy can be saved by 454.2kJ when propylene oxide per kilogram participates in production of hydroxypropylethylenediamine, namely, 6.56 tons of standard coal can be saved when every 1000 tons of hydroxypropylethylenediamine is produced.
Comparative example 1
Adding ethylenediamine into a DN1200L tower reactor, heating to 100-130 ℃, carrying out two-stage condensation reflux at the top, allowing the ethylenediamine to fall into a gas-liquid contactor, carrying out gas-liquid contact with ethylene oxide gas entering at 1.19kg/min to generate hydroxyethyl ethylenediamine, allowing the generated hydroxyethyl ethylenediamine to fall into the bottom of the tower, continuously evaporating the ethylenediamine at the bottom of the tower, transferring feed liquid into a rectifying tower after the reaction is finished, carrying out reduced pressure rectification, collecting 136-139 ℃ fraction with 2133Pa to obtain hydroxyethyl ethylenediamine, and the annual output is 1214 tons.
Example 1
The continuous conveying system in the hydroxyethylene/propylethylenediamine production device shown in fig. 1 comprises two feed pumps which can respectively convey ethylenediamine and ethylene oxide/propane, the mixing unit is a micro mixer with a heat exchange channel, the reaction unit is a micro-channel reactor, and the rectification units are a light-component removal rectification tower and a heavy-component removal rectification tower which are sequentially connected.
Ethylene oxide is conveyed into a microchannel reactor of a mixing unit through a feed pump of a continuous conveying system at a flow rate of 2.28kg/min, ethylene diamine and ethylene oxide enter the microchannel reactor at the same time in a molar ratio of 5:1 with ethylene oxide, the ethylene diamine and the ethylene oxide are mixed in a liquid state at a temperature of 80 ℃ to obtain a mixed solution, the mixed solution enters a microchannel reactor with a liquid holding capacity of 1L in a reaction unit and reacts for 3s at a temperature of 200 ℃ and a pressure of 8MPa to obtain a reaction solution, the reaction solution enters a light component removal rectifying tower while being hot, the heating temperature of a tower kettle is 200 ℃, ethylene diamine is separated by normal pressure rectification, and a mother solution from which ethylene diamine is removed enters a heavy component removal rectifying tower and is separated at the temperature of the tower kettle of 200 ℃ and the pressure of 15kPa to obtain a product of hydroxyethyl ethylene diamine.
The purity of the hydroxyethyl ethylenediamine obtained by gas phase detection is 99.5%, the product yield is 95.1%, the continuous and stable production is 7200h, the annual output can reach 2218 tons, compared with comparative example 1, the production efficiency is improved by 83%, the reaction volume is reduced by 1200 times, and at least 1301kJ/h of energy is saved.
Example 2
As shown in fig. 2, the continuous conveying system in the apparatus for producing hydroxyethylidene/propylethylenediamine comprises two feed pumps, which are respectively connected with two heat exchangers of a preheating unit, and can respectively convey and preheat ethylenediamine and ethylene oxide/propane, the mixing unit is a micro mixer with a heat exchange channel, the reaction unit is a micro channel reactor, and the rectification units are a light component removal rectification column and a heavy component removal rectification column which are sequentially connected.
Ethylene oxide is conveyed into a micro mixer of a mixing unit through a feed pump of a continuous conveying system at the flow speed of 2.78kg/min, ethylene diamine and ethylene oxide are preheated to 50 ℃ through a preheater respectively according to the molar ratio of 15:1, then the ethylene diamine and the ethylene oxide enter the micro mixer at the same time, the ethylene diamine and the ethylene oxide are mixed at the temperature of 50 ℃ in a liquid state to obtain a mixed solution, the mixed solution enters a combined reactor of a microchannel reactor and a tubular reactor with the liquid holdup of 200L in a reaction unit and reacts for 180s at the temperature of 80 ℃ and under the pressure of 1MPa to obtain a reaction solution, the reaction solution enters a light-end removal rectifying tower while the reaction solution is hot, the ethylene diamine is rectified and separated at the temperature of 100 ℃ and under the pressure of 1kPa, and the mother solution without the ethylene diamine enters a heavy-end rectifying tower and is separated at the temperature of 140 ℃ and the pressure of 1kPa to obtain the product of hydroxyethyl ethylene diamine.
The purity of the hydroxyethyl ethylenediamine obtained by gas phase detection is 99.3%, the product yield is 95%, continuous and stable production is 7200h, the annual output can reach 2698 tons, compared with comparative example 1, the production efficiency is improved by 122%, the reaction volume is reduced by 6 times, and energy is saved by 1585kJ/h at least.
Claims (10)
1. The production device of hydroxyethyl/propyl ethylenediamine is characterized by comprising a continuous conveying unit, a mixing unit, a reaction unit and a rectification unit which are communicated in sequence;
the mixing unit is a micro mixer and is used for mixing liquid ethylenediamine and liquid ethylene oxide/propane;
the reaction unit is a microchannel reactor, a tubular reactor or a combination of the microchannel reactor and the tubular reactor;
the rectification unit comprises a light component removal rectification tower and a heavy component removal rectification tower which are communicated in sequence,
the heavy component removal rectifying tower is provided with a heavy component removal rectifying tower, a heavy component removal rectifying tower and a hydroxyethyl/propyl ethylenediamine product outlet, and the light component removal rectifying tower is provided with a reaction liquid inlet, an ethylenediamine outlet and a light component removal mother liquid outlet which is communicated with the light component removal mother liquid inlet of the heavy component removal rectifying tower.
2. The production apparatus as claimed in claim 1, wherein the continuous feed unit comprises at least two feed pumps for feeding ethylenediamine and ethylene/propane oxide.
3. The production device according to claim 2, wherein the mixing channel of the mixing unit has a characteristic dimension of 1-10 mm.
4. A production device according to claim 3, characterized in that the mixing unit is provided with heat exchange channels.
5. The production device according to claim 4, wherein a preheating unit is further provided between the mixing unit and the continuous conveying unit.
6. The production device according to claim 5, wherein the volume of the reaction unit is 1-200L.
7. The production device according to claim 6, wherein a storage unit is further arranged at the front section of the continuous conveying unit, and the storage unit comprises a device for storing or temporarily storing ethylenediamine and a device for storing or temporarily storing ethylene oxide/propane.
8. The production device according to claim 7, wherein the ethylene diamine outlet of the light ends removal rectification column is communicated with a device for storing or temporarily storing ethylene diamine in the storage unit or communicated with a separate ethylene diamine collecting tank.
9. The production device of claim 8, wherein the mixing unit is also a reaction plate in a microchannel reactor.
10. The apparatus for producing according to any one of claims 1 to 9, wherein the apparatus for producing hydroxyethylene/propylethylenediamine further comprises a back pressure system.
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| CN114213259B (en) * | 2021-12-31 | 2024-07-02 | 山东友泉新材料有限公司 | Production process of hydroxyethyl/propylethylenediamine |
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