WO2015020277A1 - High-efficiency chemical reaction method and apparatus - Google Patents

High-efficiency chemical reaction method and apparatus Download PDF

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Publication number
WO2015020277A1
WO2015020277A1 PCT/KR2013/011499 KR2013011499W WO2015020277A1 WO 2015020277 A1 WO2015020277 A1 WO 2015020277A1 KR 2013011499 W KR2013011499 W KR 2013011499W WO 2015020277 A1 WO2015020277 A1 WO 2015020277A1
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Prior art keywords
reaction
reaction system
reactor
batch
reactants
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PCT/KR2013/011499
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French (fr)
Korean (ko)
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이만식
백재호
김지선
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한국생산기술연구원
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    • 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
    • B01J19/18—Stationary reactors having moving elements inside
    • 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
    • C07C29/60—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring by elimination of -OH groups, e.g. by dehydration
    • 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
    • B01J19/18—Stationary reactors having moving elements inside
    • B01J19/1856—Stationary reactors having moving elements inside placed in parallel
    • 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
    • B01J19/18—Stationary reactors having moving elements inside
    • B01J19/1862—Stationary reactors having moving elements inside placed in series
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C201/00—Preparation of esters of nitric or nitrous acid or of compounds containing nitro or nitroso groups bound to a carbon skeleton
    • C07C201/06—Preparation of nitro compounds
    • C07C201/12—Preparation of nitro compounds by reactions not involving the formation of nitro groups
    • 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
    • C07C31/18—Polyhydroxylic acyclic alcohols
    • C07C31/20—Dihydroxylic alcohols
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C69/00—Esters of carboxylic acids; Esters of carbonic or haloformic acids
    • C07C69/96—Esters of carbonic or haloformic acids
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07D—HETEROCYCLIC COMPOUNDS
    • C07D317/00—Heterocyclic compounds containing five-membered rings having two oxygen atoms as the only ring hetero atoms
    • C07D317/08—Heterocyclic compounds containing five-membered rings having two oxygen atoms as the only ring hetero atoms having the hetero atoms in positions 1 and 3
    • C07D317/10—Heterocyclic compounds containing five-membered rings having two oxygen atoms as the only ring hetero atoms having the hetero atoms in positions 1 and 3 not condensed with other rings
    • C07D317/32—Heterocyclic compounds containing five-membered rings having two oxygen atoms as the only ring hetero atoms having the hetero atoms in positions 1 and 3 not condensed with other rings with hetero atoms or with carbon atoms having three bonds to hetero atoms with at the most one bond to halogen, e.g. ester or nitrile radicals, directly attached to ring carbon atoms
    • C07D317/34—Oxygen atoms
    • C07D317/36—Alkylene carbonates; Substituted alkylene carbonates

Definitions

  • the present invention relates to a high efficiency chemical reaction method and apparatus, and more particularly, to high efficiency chemistry that can be easily applied to various chemical reactions to obtain products by reacting different liquids or adding a gas such as hydrogen to the reactants. It relates to a reaction method and apparatus.
  • This chemical reaction proceeds using a reactor.
  • the reactor is made free to control the reaction.
  • Reactors are classified into batch type, batch type, continuous type (flow type, flow type, continues type) and semi-batch type according to the operating method.
  • Batch is a method of adding raw materials once and continuing the reaction until the purpose is achieved
  • continuous is a method of continuously supplying raw materials and drawing out products
  • semi-batch is different from the beginning when raw materials are added and the reaction proceeds. It is a method of adding a raw material.
  • Registration No. 10-0830718 "Method for Producing Alkyl ⁇ -lactone by Hydrogenation of Alkylketene Dimers" uses a fixed bed reactor equipped with a granular metal catalyst in place of a conventional batch reactor for the hydrogenation of alkyl ketendimers. It is proposed a technique for performing a continuous process.
  • the addition reaction in a chemical reaction is a reaction in which another molecule is bonded to an unsaturated bond, and a compound having a double bond or a triple bond can react with an addition, and is useful for making a polymer, which is useful in our lives.
  • Produces widely used polymers include ethene (ethylene) having a double bond, and examples of reactions when hydrogen is added, halogen is added, and water is added.
  • Korean Laid-Open Patent Publication No. 10-2012-0102055 “Method for producing polyamide” uses a batch reactor equipped with a condenser to provide 20 mole% or more of paraxylylenediamine in the dicarboxylic acid component.
  • the batch production method of polyamide in which polyamine is condensed by adding a diamine component containing 70 mol% or more of silylenediamine the diamine component is added under pressure while maintaining the flow state throughout the reaction system, and the addition is continued between specific molar ratios.
  • a method for producing a polyamide that lowers the pressure has been proposed.
  • Patent Publication No. 10-0685535 "Method for preparing polyamide,” accurately adjusts the molar balance between the diamine component and the dicarboxylic acid component in an appropriate balance in a batch-wise adjustment tank. And preparing a slurry liquid in which substantially no amidation reaction occurs, and the slurry liquid thus prepared is fed to a batch or continuous polymerization reactor, without causing problems such as foaming and solidification. A technique for advancing the amidation reaction to easily produce a polyamide having a desired diamine component and a dicarboxylic acid component is proposed.
  • Such a chemical reaction according to the prior art is performed using one reactor of a batch reactor, a continuous reactor and a semi-batch reactor, or by connecting several kinds of reactors in a row to increase the productivity by the reaction process sequentially I'm sleeping.
  • it is difficult to use the existing equipment and the cost of the equipment is increased, the occupancy area of the equipment is increased, there is a problem of being limited in the installation space, and there are problems such as a limitation in increasing the processing speed.
  • the present invention has been proposed to solve the problems of the prior art, and is a novel method that can be easily applied to various chemical reactions to obtain products by reacting different liquids or adding a gas such as hydrogen to the reactants. It is an object to provide a high efficiency chemical reaction method and apparatus in the form.
  • the present invention improves the reaction speed of the prior art to increase the reaction rate to reduce the formation of impurities, improve productivity, reduce the maintenance cost, if necessary, a new form of high efficiency to facilitate the increase of the reaction rate It is an object to provide a chemical reaction method and apparatus.
  • the present invention is difficult to use the existing equipment in the chemical reaction equipment in the prior art, the cost of the equipment is increased, the occupied area of the equipment is limited in the installation space, there is a problem that there is a limit to increase or decrease the treatment capacity It is an object of the present invention to provide a new type of high efficiency chemical reaction method and apparatus that can solve the problem.
  • the high-efficiency chemical reaction method according to the characteristics of the present invention for achieving the above object is a batch reaction process step of putting a reactant in the batch reaction system 12, and proceeds the reaction process to obtain a product; Circulation to make the reaction process while circulating the reactants in which the batch reaction process proceeds in the batch reaction system 12 to the circulating reaction system 13 installed to form a closed circuit with the batch reaction system 12 A reaction process step; Stopping circulation to the circulating reaction system 13 and discharging the product in the batch reaction system 12 to the outside.
  • the batch reaction step is carried out in the batch reaction system 12, and then the reaction step to obtain the product by adding the reactant, the cyclic reaction step
  • the reaction may be performed by putting the additive reactant into the reactant supplied from the batch reaction system 12.
  • the additive reactant may be a gas.
  • the circulating reaction step may be performed so that the internal pressure of the cyclic reaction system 13 is greater than the internal pressure of the batch reaction system 12.
  • the reactants may be formed in a plurality of liquid phases.
  • the circulating reaction process step is performed through a continuous reactor 14 disposed on the connection line 15 installed to form a closed circuit with the batch reaction system 12. Can be lost.
  • the continuous reactor 14 is provided with a stirred reactor 40 having a mixing (mixing) function
  • the circulation reaction step is the reactant is the stirred reactor (40)
  • Continuous stirring may be achieved during the passage.
  • the continuous reactor 14 includes a diffusion reactor 50 having a dispersion function, and the circulation reaction step includes the diffusion reactor 50. Through the dispersion of the reactants can be made.
  • the continuous reactor 14 includes a plurality of reactors installed in series on the connection line 15, and the circulation reaction step includes the plurality of reactors sequentially. You can make it through.
  • the plurality of reactors of the continuous reactor 14 are agitated reactor 40 having a mixing function and a diffusion reactor 50 having a dispersion function.
  • the circulating reaction step may be a continuous agitation while the reactant is passed through the stirred reactor 40, the dispersion of the reactant is made through the diffusion reactor (50).
  • the high-efficiency chemical reaction device for achieving the above object is a batch reaction that is configured to add a reactant and continue the process until the reaction process is completed, and to discharge the finished product at once System 12;
  • the circulating reaction system 13 is installed to form a closed circuit with the batch reaction system 12, and is accommodated in the batch reaction system 12 to circulate the reactants through which the reaction process proceeds. It can be provided.
  • the circulation type reaction system 13 includes a connection line 15 installed to form a closed circuit with the batch type reaction system 12; It may be provided with a continuous reactor (14) installed on the connection line (15).
  • the continuous reactor 14 may include a stirred reactor 40 having a mixing function to allow continuous agitation while the reactants pass through.
  • the continuous reactor 14 may be provided with a diffusion type reactor 50 having a dispersion function for dispersing the reactants.
  • the continuous reactor 14 may include a plurality of reactors which are installed on the connection line 15 in series.
  • the continuous reactor 14 is a stirred reactor (40) having a mixing (mixing) function to make a continuous stirring while the reactants pass, and the continuous reactor ( 14 may be equipped with a diffusion reactor 50 having a dispersion function to allow dispersion of the reactants.
  • the batch reaction system 12 and the circulation reaction system 13 further include an addition reactant supply unit 16 installed to supply the addition reactant after the addition of the reactant. It can be provided.
  • the circulation type reaction system 13 includes a pump 30 installed at the front end of the continuous reactor 14 on the connection line 15 and a liquid level installed at the rear end.
  • a regulator 34 may further be provided such that the internal pressure of the circulating reaction system 13 is set higher than the internal pressure of the batch reaction system 12.
  • connection line 15 connects the front end and the rear end of each reactor to each of the plurality of reactors, so that the reactants flowing through the connection line 15 pass through each reactor. It may further include a bypass line to flow.
  • the high-efficiency chemical reaction method and apparatus by combining the batch reaction system 12 and the circulation reaction system 13 to perform a variety of chemical reactions, compared to the conventional batch reactor
  • the speed can be increased, so productivity can be easily increased.
  • it is basically made by installing a cyclic reaction system 13 applying the continuous reactor 14 to the batch reaction system 12 applying the batch reactor, it is possible to utilize the existing chemical reaction equipment, No additional utility is required to reduce maintenance costs, and the formation of impurities is reduced by increasing the reaction rate.
  • the multi-stage design of the continuous reactor 14 is possible in the cyclic reaction system 13, it is easy to increase the reaction rate, and various chemical reactions for reacting different liquids or adding a gas such as hydrogen to the reactants to obtain a product. It can be easily applied to, and the productivity is improved by increasing the reaction rate, so that the installation of the chemical reaction device 10 can be made small while reducing the space constraint.
  • FIG. 1 is a view for explaining a high efficiency chemical reaction method and apparatus according to the technical idea of the present invention
  • FIG. 2 is a view for explaining a high efficiency chemical reaction method and apparatus according to a preferred embodiment of the present invention
  • FIG. 3 is a view for explaining a modification of the high efficiency chemical reaction method and apparatus according to a preferred embodiment of the present invention shown in FIG.
  • FIG. 4 is a view for explaining a high efficiency chemical reaction method and apparatus according to another embodiment of the present invention.
  • FIG. 5 is a view for explaining a high efficiency chemical reaction method and apparatus according to another embodiment of the present invention.
  • FIG. 6 is a view for explaining a high efficiency chemical reaction method and apparatus according to a preferred embodiment of the present invention configured for the hydrogenation reaction.
  • FIG. 2 is a view for explaining a high efficiency chemical reaction method and apparatus according to a preferred embodiment of the present invention.
  • the high-efficiency chemical reaction method is to put the reactants in the batch reaction system 12, a batch reaction process step of proceeding the reaction process to obtain a product, batch reaction system ( 12) and a circulating reaction process step, the product is formed to circulate the reactants undergoing the batch reaction process in the batch reaction system 12 to the circulating reaction system 13 installed to form a closed circuit, the product is formed When it stops, the circulation to the circulating reaction system 13 is stopped, and the product in the batch reaction system 12 is discharged to the outside.
  • the reactants consist of a plurality of liquid phases.
  • the high-efficiency chemical reaction method according to the present embodiment is such that the circulating reaction process step is made through the continuous reactor 14 disposed on the connection line 15 installed to form a closed circuit with the batch reaction system 12 By doing so, the reactants flowing from the batch reaction system 12 can be carried out through the connection line 15 to perform various reaction processes to increase the reaction efficiency.
  • the cyclic reaction process step is performed through the continuous reactor 14 and the stirred reactor 40 and the diffusion reactor 50.
  • the stirred reactor 40 is a reactor having a mixing (mixing) function
  • the circulating reaction step is to convert the laminar flow fluid into turbulent fluid through the stirred reactor 40 so that continuous stirring is performed during the passage. do.
  • the diffusion reactor 50 is a reactor having a dispersion function, and the circulating reaction process step allows dispersion of reactants to facilitate contact of different fluids through the diffusion reactor 50.
  • the cyclic reaction step may be applied to a single continuous reactor 14, a plurality of continuous reactor 14 is installed in series on the connection line 15 It may be made of the above reactor, it may be made while sequentially passing through a plurality of reactors. That is, the cyclic reaction process step is agitated so that the above-mentioned stirring reactor 40 having the mixing function and the diffusion reactor 50 having the dispersion function are installed on the connection line 15 in succession.
  • the order, number of reactors forming the continuous reactor 14 can be configured in various ways according to the needs of the installation.
  • the high efficiency chemical reaction device 10 is a batch reaction system 12 and a circulating reaction system in order to be able to perform the chemical reaction process as described above. (13) is provided.
  • the batch reaction system 12 is configured to put the reactants and to continue the process until the reaction process is completed, and to discharge the finished product at once.
  • the circulating reaction system 13 is installed to form a closed circuit with the batch reaction system 12, and is accommodated in the batch reaction system 12 to circulate the reactants through which the reaction process proceeds.
  • the circulating reaction system 13 includes a continuous reactor 14 and a connection line 15, and the connection line 15 is a batch reaction system 12. And to form a closed circuit, and a continuous reactor 14 is installed on the connecting line 15.
  • the continuous reactor 14 may typically be a stirred reactor 40 and a diffusion reactor 50.
  • the stirred reactor 40 has a mixing function to convert the laminar fluid into a turbulent fluid while allowing continuous stirring to be performed during the passage, and the diffusion reactor 50 is capable of contacting different fluids. It has a dispersion function that facilitates dispersion of the reactants.
  • the reactors 40 and 50 constituting the continuous reactor 14 may be used separately, or may be installed in series on the connection line 15, and a plurality or more thereof may be used.
  • the present embodiment showed the stirred reactor 40 and the diffused reactor 50 as an example of the continuous reactor 14, each of which may be applied in plural or different kinds of continuous reactors.
  • FIG. 3 is a view for explaining a modification of the high efficiency chemical reaction method and apparatus according to a preferred embodiment of the present invention shown in FIG.
  • the high efficiency chemical reaction device 10 may include a bypass line 15a on the connection line 15 of the high efficiency chemical reaction device 10 according to the preferred embodiment of the present invention shown in FIG. 2.
  • 15b is additionally installed.
  • the bypass lines 15a and 15b connect the front and rear ends of each reactor to each of a plurality of reactors (agitated reactor 40 and diffusion reactor 50 in this embodiment), thereby connecting the connection line 15. The reactant flowing through the flow through each reactor.
  • Such bypass lines 15a and 15b may be usefully applied when it is necessary to selectively apply the processes of the two reactors.
  • FIG. 4 is a view for explaining a high efficiency chemical reaction method and apparatus according to another embodiment of the present invention.
  • a reaction process for adding an added reactant to obtain a product and performing a cyclic reaction involves adding reactants to the reactants supplied from the batch reaction system 12 so that the reaction process takes place.
  • the high-efficiency chemical reaction device 10 includes an additive reactant supply unit 16 installed to supply an additive reactant after placing a reactant in the batch reaction system 12 and the circulating reaction system 13. ) Is installed.
  • the additive reactant supply unit 16 in the circulating reaction system 13 may be configured in various forms so that the additive reactants may be uniformly supplied to each of the stirred reactor 40 and the diffusion reactor 50. .
  • the high-efficiency chemical reaction method according to this embodiment is a liquid-liquid reaction by mixing two or more liquid reactants, such as hydrogen (H 2 ), carbon dioxide (CO 2 ), methane (CH 4 ) to the liquid reactants Various addition reaction processes, such as gas-liquid reaction to add gas, can be performed.
  • liquid reactants such as hydrogen (H 2 ), carbon dioxide (CO 2 ), methane (CH 4 )
  • FIG. 5 is a view for explaining a high efficiency chemical reaction method and apparatus according to another embodiment of the present invention.
  • the high-efficiency chemical reaction method allows the internal pressure of the circulating reaction system 13 to be greater than the internal pressure of the batch reaction system 12 so that the cyclic reaction process may be performed. Make the reaction more efficient.
  • This high-efficiency chemical reaction method by applying a cyclic reaction system 13 that can make the pressure relatively easily compared to the batch reaction system 12, while reducing the manufacturing cost and maintenance cost of the reaction apparatus Higher reaction efficiency can be expected.
  • the high-efficiency chemical reaction device 10 is formed by installing a pump 30 and a liquid level regulator 34 in a circulating reaction system 13.
  • the pump 30 is installed at the front end of the continuous reactor 14 of the circulating reaction system 13 on the connection line 15 to allow the reactants to flow from the batch reaction system 12 to the connection line 15.
  • a valve 32 for controlling the flow rate and pressure is installed at the rear end of the pump 30.
  • the reactants introduced into the continuous reactor 14 by the pump 30 through the connecting line 15 are supplied with an additive reactant such as hydrogen gas by the additive reactant supply unit 16 to supply the reactant in the circulating reaction system 13.
  • the pressure is raised and maintained at high pressure.
  • the high pressure in the circulating reaction system 13 is applied from the valve 32 at the rear end of the pump 30 to the valve 36 at the rear end of the liquid level regulator 34.
  • the liquid level regulator 34 is installed at the rear end of the continuous reactor 14 on the connecting line 15 so as to adjust the flow rate and pressure while maintaining the internal pressure of the circulating reaction system 13. Open to allow reactants to flow into batch reaction system 12.
  • the high-efficiency chemical reaction device 10 is a batch reaction system 12 allows the reaction process to proceed at low pressure (relative pressure relative to the cyclic reaction system 13), the circulation
  • the type reaction system 13 allows the reaction process to proceed at a high pressure, but in order to maintain the high pressure of the circulating reaction system 13 (that is, a gas such as toil gas supplied to the circulating reaction system 13 is arranged.
  • the control of the flow rate and pressure control valve 36 that is linked to the liquid level regulator 34
  • the flow and pressure of the control valve 36 will be made by the controller of the reactor 10, to prevent the flow of the fluid by the reaction liquid collected in the liquid level regulator 34, one independent Made into a system All.
  • the circulation type reaction system 13 maintains a high pressure state
  • the batch type reaction system 12 maintains a low pressure state and is independent of each other. It becomes a system closed to space.
  • the reaction pressure is controlled by the hydrogen pressure entering each reactor, and the pressures can be used separately because they are independent systems.
  • the liquid level regulator 34 should always adjust the height of the reaction liquid, so that the reaction liquid is always filled to a predetermined height or more, and when the height of the reaction liquid increases as the process proceeds, the liquid level regulator 34 interworks with it. By using the valve 36 is maintained a constant liquid level.
  • FIG. 6 is a view for explaining a high efficiency chemical reaction method and apparatus according to a preferred embodiment of the present invention configured for the hydrogenation reaction.
  • the high-efficiency chemical reaction method is a liquid-liquid reaction made by mixing two or more liquid reactants, hydrogen (H 2 ), carbon dioxide (CO 2 ), Various reaction processes such as a gas-liquid reaction in which a gas such as methane (CH 4 ) is added may be performed.
  • Such a high-efficiency chemical reaction method is basically a batch reaction process step of putting the reactants in the batch reaction system 12, and proceeds with the reaction process to obtain a product, the batch reaction system 12 and the closed circuit
  • the stirring line 40, the diffusion type reactor 50 is installed in the connection line 15 to form a closed circuit so that the reactant flows out from the batch reaction system 12 according to the present embodiment.
  • two stirred dispersion reactors 40a and 40b are installed continuously on the connecting line 15.
  • the connecting line 15 at the front end of the stirred reactor 40 includes a pump 30 for flowing the reactants into the circulating reaction system 13, and a high pressure in the circulating reaction system 13 at the front of the pump 30.
  • Valve 32 for controlling the flow of reactants while maintaining, level gauge 72 for checking the flow of reactants, and pressure cage 70 for checking the pressure in front of the stirred reactor 40 are installed.
  • the connection line 15 at the rear end of the diffusion reactor 50 has a liquid level regulator 34 and a flow of reactants into the batch reaction system 12 while maintaining a high pressure in the circulation reaction system 13.
  • the valve 36 to control the is installed.
  • the high-efficiency chemical reaction device 10 is provided with bypass lines 15a and 15b in the stirred reactor 40 and the diffused reactor 50, and if necessary, diffused with the stirred reactor 40.
  • Selective reactor 50 is selectively applied to allow the reaction process to proceed.
  • the high-efficiency chemical reaction device 10 is a batch reaction system 12 and a circulating reaction system 13 to add a reactant after the addition of the reactant so as to enable a gas addition reaction
  • the supply unit 16 is installed.
  • the nitrogen supply unit 18 for supplying nitrogen for the hydrogenation reaction is configured together.
  • the additive reactant supply unit 16 and the nitrogen reactant supply unit 16 are connected to the reactor (not shown), the stirred reactor 40 and the diffusion reactor 50 of the batch reaction system 12, respectively, to form hydrogen and nitrogen. Supply each.
  • a vent unit 60 including a capacitor 62, a collector 64, and the like is installed to safely discharge hydrogen.
  • the high-efficiency chemical reaction method according to the present embodiment is such that the cyclic reaction step is performed through a plurality of continuous reactors 14 installed in succession. That is, the above-described stirred reactor 40 and the diffusion reactor 50 are continuously arranged so that the stream of the reactant is continuously stirred and dispersed, thereby shortening the reaction time to increase production efficiency.
  • the high-efficiency chemical reaction method allows the reaction process made by adding a gas, such as hydrogenation reaction.
  • the batch reaction step may include a reactant in a batch reaction system 12, and then proceed with a reaction step to obtain a product by adding an additional reactant, and the cyclic reaction step may include a batch reaction system 12.
  • the reaction product is added to the reactant supplied from the reaction mixture.
  • the cyclic reaction process step allows the internal pressure of the cyclic reaction system 13 to be greater than the internal pressure of the batch reaction system 12, thereby reducing the operating cost. Reduce time to increase production efficiency.
  • the valve of the batch reaction system is opened and a pump is used to circulate the reactants of the batch reaction system to the stirred reactor and the diffusion reactor of the circulation reaction system, wherein the circulation
  • the amount of reactant to be controlled was maintained at 10-15 L / min by flow meter valve. Nitrogen is pushed into the batch and circulating reaction system to circulate the dissolved reactants to remove oxygen remaining in each reactor and reactant, and then hydrogen is pushed into the nitrogen to make the inside of the batch and circulating reaction system into a hydrogen atmosphere. Was removed.
  • the reactor temperature was set to 300 ° C., the reaction temperature, and then the hydrogen pressure in the batch and circulating reaction system was raised to 5 bar, and the hydrogen pressure in the batch and circulating reaction system. After reaching 5 bar, the hydrogen pressure in the circulating reaction system was raised to 14 bar. At 300 ° C., the hydrogen pressure in the reactor was maintained at 5 bar in the batch reaction system and 14 bar in the circulating reaction system. Hydrogenation reaction was performed.
  • the reactants in the circulating reaction system were drained into the batch reaction system.
  • the product produced after the reaction was mixed with the catalyst, and the product was transferred to a filter vessel (not shown) for separation of the catalyst to separate the product from the catalyst.
  • the temperature of the product inside the batch reaction system and the filter vessel temperature is maintained at 90 °C and transferred to the filter vessel in a liquid state, after the catalyst separation, the propylene glycol product is dissolved in H 2 O in the filtrate obtained in the filter vessel. Exists in a state. At this time, the time required to complete the reaction was 12 hours in total.
  • the reactor temperature was set to 300 ° C.
  • the reaction temperature was raised, and the internal hydrogen pressure was raised to 14 bar to maintain the batch reaction system at 14 bar, and the glycerol was stirred under a stirring speed of 300 rpm.
  • Hydrogenation reaction was carried out.
  • the product produced after the reaction was mixed with the catalyst, and the product was transferred to a filter vessel to separate the catalyst and the product was separated from the catalyst.
  • the temperature of the product inside the batch reaction system and the filter vessel temperature are maintained at 90 ° C. and transferred to the filter vessel in a liquid state.
  • propylene glycol as a product is present in a state where the product is dissolved in H 2 O in the filtrate obtained in the filter vessel.
  • the time required to complete the reaction was 17 hours in total.
  • a circulating reaction is introduced by introducing a circulating reaction system into an existing batch reaction system.
  • the reaction rate is improved by the improvement of the pressure and the stirring speed, and thus, the conversion and the reaction yield are markedly improved, as well as the selectivity is increased, so that impurities can be reduced to obtain a high purity product. I could confirm it.
  • 75 kg of propylene oxide was added to a batch reaction system of a high-efficiency chemical reaction apparatus according to a preferred embodiment of the present invention, and the temperature of the batch reaction system was set to 110 ° C., followed by stirring at 300 rpm. While stirring the reaction, 26.2 kg of the catalyst (ZnCl 2 ) was added, and after the catalyst was added, the batch reaction system was completely sealed. After the catalyst is sufficiently dispersed in the reactant, the valve of the batch reaction system is opened and a pump is used to circulate the reactants of the batch reaction system into the stirred reactor and the diffusion reactor of the circulating reaction system, wherein The amount was controlled by a flow meter valve to maintain 10-15 L / min.
  • the hydrogen pressure inside the reactor was maintained at 15 bar at 110 ° C., and CO 2 addition reaction of propylene oxide was carried out under a stirring speed of 300 rpm. After the reaction was completed, the resulting product was mixed with the catalyst. The product propylene carbonate was obtained. At this time, the time required to complete the reaction was 6 hours in total.
  • nitromethane and 3.3 kg of propionaldehyde are added to a batch reaction system of a high-efficiency chemical reaction device according to a preferred embodiment of the present invention, and the temperature of the batch reaction system is set to 25 ° C.
  • the reaction mixture was thoroughly mixed with 100 rpm, and 11.3 kg of a catalyst (chloroaluminate ionic liquid) was added while stirring the reaction mixture.
  • the catalyst is added, the batch reaction system is completely sealed and the catalyst is sufficiently dispersed in the reactant, and then the valves of the batch reaction system are opened to pump the reactants of the batch reaction system using a pump. Circulated to the reactor.
  • the amount of reactant circulated was controlled by a flow meter valve and maintained at 10-15 L / min. Nitrogen was pushed into the batch and circulating reaction systems while circulating the dissolved reactants to remove oxygen remaining in each reactor and reactants, and then the reaction was performed at atmospheric pressure. After completion of the reaction, the reactants in the circulating reaction system were drained into the batch reaction system. The product produced after the reaction was 1-nitro-2-butanol, and phase-separated with water and ethyl acetate to separate it, and purified pure 1-nitro-2 on the ethyl acetate layer. Butanol was obtained. At this time, the time required to complete the reaction was 11 hours in total.
  • the product produced after the reaction was 1-nitro-2-butanol, and to separate it, phase separation was performed using water and ethyl acetate to obtain pure 1-nitro-2-butanol on an ethyl acetate layer. At this time, the time required to complete the reaction was 16 hours in total.
  • the method and apparatus for high-efficiency chemical reaction circulates the reactants for the reaction process through the batch reaction system 12 to the circulation type reaction system 13 so that an additional reaction process is performed. Increasing the rate can significantly improve productivity while reducing the formation of impurities.
  • the high-efficiency chemical reaction method and apparatus according to the present invention by circulating the reactant to the reaction process through the batch reaction system 12 to the circulating reaction system 13 to make an additional reaction process, reaction Increased speed improves productivity while reducing the formation of impurities, reduces maintenance costs by eliminating the need for additional utilities, and reduces the size of the reaction facility while improving processing efficiency, making it easier to install with less space constraints. do.
  • using the conventional batch reaction method and reactor can see the same effect as the high efficiency chemical reaction method and apparatus according to the present invention, but with the high efficiency chemical reaction method and apparatus according to the present invention with the conventional batch reaction method and reactor In order to see the same efficiency, the cost of the equipment and the process cost to be added will be increased.
  • the prior art should design a batch reactor of 10 bar, while the present invention is 5 bar to the reactor (corresponding to the general batch reactor) of the batch reaction system 12
  • the reactor of the batch reaction system 12 is designed.
  • the material and design costs for the reactor will be lowered.
  • the reactor of the batch reaction system 12 is manufactured at a high allowable pressure, and the reactor of the batch reaction system 12 is manufactured at a low pressure, and the continuous reactor of the circulating reaction system 13 is manufactured. Producing only 14 at high pressure has many advantages in terms of manufacturing cost.
  • the key to improving the reactivity in the chemical reaction can be seen as an improvement that comes from maximizing the contact efficiency of the reactants to be mixed, which can be improved by improving the stirring speed of the reactor.
  • the current industrially applicable stirring speed is up to about 300rpm, but may be higher than 300rpm, but the production cost increases accordingly.
  • the high-efficiency chemical reaction device 10 according to the present invention sets the reactor of the batch type reaction system 12 to 300 rpm and proceeds the reaction process while circulating to the continuous reactor 14 of the circulating type reaction system 13. The effect is much better than the stirring speed of the conventional batch reactor.
  • the conventional batch reactor should produce 1 to 1.5 batches per day using three 10-ton reactors, but using the high-efficiency chemical reaction method and apparatus according to the present invention As the speed increases, 2.5 to 3 batches can be produced per day using two 10-ton reactors. Then, the production cost can be saved by one reactor for the initial equipment investment cost, and the operation cost of one reactor can be saved even during operation.
  • the pretreatment equipment and the aftertreatment equipment may also be equipped with pretreatment equipment and post-treatment equipment suitable for the number of reactors, thereby reducing the overall process cost, and thus can obtain an advantage in price competitiveness for the final product.
  • the high-efficiency chemical reaction device 10 according to the present invention can reduce the maintenance cost because no additional utility.
  • the additional utility refers to the additional equipment required for operating the reaction equipment.
  • there is a typical addition utility heating and cooling system Heat & Cooling system
  • Heating & Cooling system in the case of the high-efficiency chemical reaction device 10 according to the present invention is heated in the reactor of the batch reaction system 12
  • a cooling system it is not necessary to install a heating and cooling system in the circulating reaction system 13, and the flow rate of the liquid can be determined in consideration of the capacity of the circulating reaction system 13, so that the circulating reaction system 13 ) Eliminates the need for additional utilities to control reaction conditions.
  • FIG. 1 is a view for explaining a high efficiency chemical reaction method and apparatus according to the technical idea of the present invention.
  • the high-efficiency chemical reaction device 10 includes a batch reaction system 12 that includes a circulating reaction system 13 for allowing a reactant contained in the batch reaction system 12 to circulate. And is formed to form a closed circuit.
  • the batch reaction system 12 is configured to contain the reactants and to allow the process to continue until the reaction process is completed, and to discharge the finished products at once.
  • the circulation type reaction system 13 is installed to form a closed circuit with the batch type reaction system 12 so as to be accommodated in the batch type reaction system 12 to circulate the reactants through which the reaction process proceeds.
  • connection line 15 may be installed in various paths and lengths according to the needs of the circulating reaction system 13, and circulates various kinds of reactants such as liquid-liquid chemical reactions and gas-liquid chemical reactions. And various valves, measuring instruments, sensors, safety devices, etc. will be installed to control the flow.
  • the high-efficiency chemical reaction device 10 will be configured to be controlled through a controller (control unit) like a general chemical reaction device.
  • a controller control unit
  • a centralized controller may be applied to monitor and control all the necessary things for the operation of the reaction apparatus in one place.
  • the control unit is configured to control the liquid level control, the valve on / off for the gas vent, and the like in one place.
  • Such a control unit may set the maximum pressure value so that the gas vent valve is automatically opened when the pressure exceeds a predetermined value for safety, and to set the stirring speed, reaction temperature, etc. to set the reaction conditions.
  • the batch reaction system 12 is configured to add a reactant and to continue the process until the reaction process is completed, and to discharge the finished products at once.
  • the circulating reaction system 13 is installed to form a closed circuit with the batch reaction system 12, and is accommodated in the batch reaction system 12 to circulate the reactants through which the reaction process proceeds.
  • the circulating reaction system 13 has a concept similar to that of a general continuous reactor, which is a method of continuously supplying raw materials and extracting products when viewed independently.
  • the reactant is placed in a batch reaction system 12, and a batch reaction step (1) of proceeding with a reaction process for obtaining a product, and a batch reaction system 12 and a closed circuit are formed.
  • Circulating reaction process step (2) to circulate the reactants undergoing the batch reaction process in the batch reaction system 12 to the circulating reaction system 13 installed so as to perform the reaction process, and when the product is formed. Stopping circulation to the circulation reaction system 13 and discharging the product in the batch reaction system 12 to the outside.
  • Such a high-efficiency chemical reaction method according to the present invention is configured to allow the addition of liquid-liquid reaction, as well as (gas; in particular, hydrogen) addition reaction as in the preferred embodiment of the present invention, and in the cyclic reaction system 13
  • the continuous reactor 14 is installed in multiple stages sequentially on the connection line 15 to increase the reaction rate through various circulation reaction processes to improve productivity.
  • the continuous reactor 14 of the circulating reaction system 13 in the high-efficiency chemical reaction device 10 as a reactor to proceed the reaction process in the stream (stream), various forms are Can be applied.
  • the continuous reactor 14 of the circulating reaction system 13 includes a stirred dispersion reactor 40 (see FIGS. 2 to 4 and 6) and a tower dispersion reactor 50 (FIG. 2). 4 to 6), the cyclic reaction system 13 of the high-efficiency chemical reaction device 10 of the present invention allows the reaction to flow in a continuous stream of reactants.
  • Various reactors may be applied to allow the process to proceed.
  • the stirred reactor 40 is installed inside the pipe through which the fluid flows, and does not interfere with the flow of the liquid to increase the stirring efficiency of the liquid, the reactants pass through the reaction efficiency between the reactants, high speed, Stirring causes the reaction to occur smoothly.
  • Representative structure of the stirred reactor 40 is a spiral (screw-type) structure of the inside of the tube, the reaction liquid has a form that the reactants are mixed while passing through the spiral, the spiral is the width that the liquid can pass and The stirring speed changes according to the rotation speed of the spiral. Therefore, the stirred reactor 40 according to the present invention can be applied to various kinds of reactors to smoothly stir the reaction liquid without disturbing the flow of the fluid.
  • the diffusion reactor 50 increases the retention time of the reactants circulated through the column internals such as packing, and expands the surface area of the reactants in the liquid phase to facilitate reactant distribution. In addition, the contact area between the reactants is increased to allow the reaction to occur smoothly.
  • Inside the diffusion type reactor 50 is configured to include a liquid dispersing device that can increase the liquid droplets of the liquid reactant, a device for expanding the surface area, a device that can increase the retention time.
  • the high-efficiency chemical reaction method and apparatus by combining the batch reaction system 12 and the circulation reaction system 13 to perform a variety of chemical reactions, compared to the conventional batch reactor
  • the speed can be increased, so productivity can be easily increased.
  • it is basically made by installing a cyclic reaction system 13 applying the continuous reactor 14 to the batch reaction system 12 applying the batch reactor, it is possible to utilize the existing chemical reaction equipment, No additional utility is required to reduce maintenance costs, and the formation of impurities is reduced by increasing the reaction rate.
  • the multi-stage design of the continuous reactor 14 is possible in the cyclic reaction system 13, it is easy to increase the reaction rate, and various chemical reactions for reacting different liquids or adding a gas such as hydrogen to the reactants to obtain a product. It can be easily applied to, and the productivity is improved by increasing the reaction rate, so that the installation of the chemical reaction device 10 can be made small while reducing the space constraint.

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Abstract

The present invention provides a high-efficiency chemical reaction method and apparatus which are easily applicable to various chemical reactions for obtaining a product by reacting different liquids or by adding a gas, such as hydrogen or the like, to a reactant. The present invention enables various types of chemical reactions to be carried out by combining a batch-type reaction system and a circulation-type reaction system, and is capable of increasing reaction rate in comparison to conventional batch-type reactors, and thus easily improving productivity. In addition, because the present invention is configured to install a circulation-type reaction system in a batch-type reaction system, it is possible to utilize conventional chemical reaction facilities, reduce maintenance costs as additional utilities are unnecessary, and reduce the formation of impurities by increasing the reaction rate. Furthermore, the present invention easily increases the reaction rate because a multistage design of a continuous reactor is possible in a circulation-type reaction system, and the whole system is configured on a small scale, thereby simplifying the installation thereof while reducing spatial constraints.

Description

고효율 화학반응 방법 및 장치High efficiency chemical reaction method and apparatus
본 발명은 고효율 화학반응 방법 및 장치에 관한 것으로, 좀 더 구체적으로는 서로 다른 액체를 반응시키거나 반응물에 수소 등의 기체를 첨가하여 생성물을 얻는 다양한 화학반응에 용이하게 적용할 수 있도록 하는 고효율 화학반응 방법 및 장치에 관한 것이다. The present invention relates to a high efficiency chemical reaction method and apparatus, and more particularly, to high efficiency chemistry that can be easily applied to various chemical reactions to obtain products by reacting different liquids or adding a gas such as hydrogen to the reactants. It relates to a reaction method and apparatus.
인류는 오래전부터 화학반응(Chemical reaction)을 이용하여 유용한 물질을 만들고자 노력해 왔다. 고대의 제련, 주조 기술에서부터 값싼 금속에서 금을 만들고자 했던 중세의 연금술에 이르기까지 축적된 화학 지식을 바탕으로 현대의 화학이 발전했다. 인공적인 화학반응으로 원하는 물질을 만드는 화학 합성을 통해 의약품, 플라스틱과 같은 물질을 만들어내거나, 연소를 이용하여 에너지를 얻는다. Humans have long tried to make useful materials using chemical reactions. Modern chemistry has evolved based on accumulated chemistry knowledge, from ancient smelting and casting techniques to medieval alchemy that sought to make gold from cheap metals. Artificial chemical reactions produce the desired substances, producing chemicals, plastics and other materials, or burning them for energy.
이와 같은 화학반응은 반응기(reactor)를 사용하여 진행된다. 이 반응기는 반응을 자유롭게 제어할 수 있게 만들어져 있다. 반응기는 조작방식에 따라 회분식(回分式, 배치식, batch type), 연속식(유통식, 플로식, continues type) 및 반회분식 등으로 분류된다. 회분식은 한 번 원료를 넣으면 목적을 달성할 때까지 반응을 계속하는 방식이고, 연속식은 계속해서 원료를 공급하고, 제품을 끌어내는 방식이며, 반회분식은 처음에 원료를 넣고 반응이 진행됨에 따라 다른 원료를 첨가하는 방법이다. This chemical reaction proceeds using a reactor. The reactor is made free to control the reaction. Reactors are classified into batch type, batch type, continuous type (flow type, flow type, continues type) and semi-batch type according to the operating method. Batch is a method of adding raw materials once and continuing the reaction until the purpose is achieved, and continuous is a method of continuously supplying raw materials and drawing out products, and semi-batch is different from the beginning when raw materials are added and the reaction proceeds. It is a method of adding a raw material.
이와 같은 반응기를 사용한 기술과 관련하여 대한민국 등록특허공보 등록번호 제10-0349476호 "연속 3상 슬러리 가수소화 반응용 2단계 반응기 및 작업 방법"은 연속 교반 탱크 반응기와 버블 칼럼 반응기가 쌍을 이루어 연속 공정, 예컨대 가수소화 공정(이때, 기체 반응물은 액체와 혼합됨)의 전환율을 향상시키기 위한 기술을 제안하고 있다. Regarding the technology using such a reactor, Republic of Korea Patent Publication No. 10-0349476 "Two-stage reactor and operation method for continuous three-phase slurry hydrogenation reaction" is a continuous stirred tank reactor and a bubble column reactor in pairs Techniques have been proposed for improving the conversion of processes, such as hydrogenation processes, wherein the gaseous reactants are mixed with the liquid.
등록번호 제10-0830718호 "알킬케텐다이머의 수소화 반응에 의한 알킬 β-락톤의제조방법"은 알킬케텐다이머의 수소화 반응시 종래의 회분식 반응기 대신에 입상형의 금속촉매가 장착된 고정층 반응기를 사용하는 연속공정을 수행하는 기술을 제안하고 있다. Registration No. 10-0830718 "Method for Producing Alkyl β-lactone by Hydrogenation of Alkylketene Dimers" uses a fixed bed reactor equipped with a granular metal catalyst in place of a conventional batch reactor for the hydrogenation of alkyl ketendimers. It is proposed a technique for performing a continuous process.
등록번호 제10-0926854호 "수소화 방향족 폴리카르복시산의 제조방법 및 수소화 방향족 폴리카르복시산 무수물의 제조방법"은 (1) 방향족 폴리카르복시산을 로듐 혹은 팔라듐 또는 이들 양쪽을 모두 포함하는 귀금속이 방향족 폴리카르복시산 100중량부당 0.5 내지 10중량부의 비율로 함유된 촉매의 존재하에 회분식 시스템에서 1MPa이상의 수소분압에서 수소화하고, 또한 (2) 방향족 폴리카르복시산을 로듐 혹은 팔라듐 또는 이들 양쪽을 모두 포함하는 귀금속이 함유된 촉매가 충전된 충전층에 1 내지 100h-1 WHSV로 공급하여 상기 폴리카르복시산을 연속유동식 시스템에서 1MPa 이상의 수소분압하에 수소화함으로써 수소화 방향족 폴리카르복시산을 제조하는 방법, 및 상술한 방법으로 수득된 수소화 방향족 폴리카르복시산을 수소화 방향족 폴리카르복시산의 카르복시기에 대해 0.64 내지 5.7배 몰의 무수 아세트산을 이용하여 탈수반응시켜 수소화 방향족 폴리카르복시산 무수물을 제조하는 방법을 제안하고 있다. No. 10-0926854 "Method for producing hydrogenated aromatic polycarboxylic acid and method for producing hydrogenated aromatic polycarboxylic anhydride" (1) 100 weight of aromatic polycarboxylic acid is a precious metal containing aromatic polycarboxylic acid rhodium or palladium or both Hydrogenated at a hydrogen partial pressure of at least 1 MPa in a batch system in the presence of a catalyst contained in a proportion of 0.5 to 10 parts by weight per part, and (2) an aromatic polycarboxylic acid is charged with a catalyst containing a noble metal comprising rhodium or palladium or both To produce a hydrogenated aromatic polycarboxylic acid by supplying the packed bed at 1 to 100 h −1 WHSV to hydrogenate the polycarboxylic acid under a hydrogen partial pressure of 1 MPa or more in a continuous flow system, and to hydrogenate the hydrogenated aromatic polycarboxylic acid obtained by the above-described method. Of aromatic polycarboxylic acids Using acetic anhydride of 0.64 to 5.7 times mole based on a time reubok proposes a method for producing a hydrogenated aromatic polycarboxylic anhydride by dehydration reaction.
등록번호 제10-1038724호 "1-부텐의 제조방법"은 납사 크래커에서 생산되는 C4-유분으로부터 이소부텐을 추출하여 t-부탄올(tert-butyl alcohol, TBA)을 제조하는 공정에서 얻은 7% 이상의 이소부텐을 함유하는 C4 유분인 라피네이트-II를 이용하여 적절한 수화반응 및 수소첨가반응을 통해, t-부탄올을 추가적으로 생산하고 동시에 1-부텐을 최적 조건으로 생산 가능한 1-부텐의 제조방법을 제안하고 있다. Registration No. 10-1038724 "Manufacturing method of 1-butene" is more than 7% obtained in the process for producing t-butanol (TBA) by extracting isobutene from the C4- fraction produced in naphtha crackers. Proposing a method for producing 1-butene that can additionally produce t-butanol and produce 1-butene under optimum conditions through appropriate hydration and hydrogenation using raffinate-II, a C4 fraction containing isobutene. Doing.
한편, 화학반응에서 첨가반응(addition reaction)은 불포화 결합에 다른 분자가 결합하는 반응으로, 이중 결합이나 삼중 결합이 있는 화합물은 첨가반응을 할 수 있으며, 고분자를 만드는 데에도 유용하게 쓰여 우리 생활에 널리 사용되는 고분자를 생산하고 있다. 이와 같은 첨가반응은 이중 결합이 있는 에텐(에틸렌)을 예로 들어 수소가 첨가될 때, 할로젠이 첨가될 때, 물이 첨가될 때의 반응 실례를 들 수 있다. On the other hand, the addition reaction in a chemical reaction is a reaction in which another molecule is bonded to an unsaturated bond, and a compound having a double bond or a triple bond can react with an addition, and is useful for making a polymer, which is useful in our lives. Produces widely used polymers. Examples of such an addition reaction include ethene (ethylene) having a double bond, and examples of reactions when hydrogen is added, halogen is added, and water is added.
이와 같은 첨가 반응과 관련하여 대한민국 공개특허공보 공개번호 특1995-0014046호 "CCl₄를 이용한 CHCl₃제조방법"은 Pt나 Pd 지지촉매와 하나 이상의 용매존재하에서 액상으로 CCI4를 촉매 수소첨가 반응하여 CHCI3를 제조하고, 환원반응은 연속식 및 회분식으로 실행하며 CHCI3 공업생산에도 응용할 수 있도록 하는 기술을 제안하고 있다.In this regard and as reaction Republic of Korea Patent Application Laid-Open Publication No. 1995-0014046 Patent No. "CHCl₃ method using CCl₄" is Pt or Pd supported catalysts with a liquid with CHCI 3 in response to the CCI 4 hydrogenation catalyst in the presence one or more solvents Is proposed, and the reduction reaction is carried out continuously and batchwise, and proposes a technique that can be applied to industrial production of CHCI 3 .
공개특허공보 공개번호 제10-2012-0102055호 "폴리아미드의 제조방법"은 분축기를 구비한 회분식 반응조를 이용하여, 디카르복실산 성분에 파라크실릴렌디아민을 20몰% 이상 포함하는 크실릴렌디아민을 70몰% 이상 포함하는 디아민 성분을 첨가하여 중축합시키는 폴리아미드의 회분식 제조방법과 관련하여 반응계 전체가 유동 상태를 유지하면서 가압 하에서 디아민 성분을 첨가하고, 첨가를 계속하면서 특정한 몰비 사이로 압력을 저하시키는 폴리아미드의 제조방법을 제안하고 있다. Korean Laid-Open Patent Publication No. 10-2012-0102055 "Method for producing polyamide" uses a batch reactor equipped with a condenser to provide 20 mole% or more of paraxylylenediamine in the dicarboxylic acid component. Regarding the batch production method of polyamide in which polyamine is condensed by adding a diamine component containing 70 mol% or more of silylenediamine, the diamine component is added under pressure while maintaining the flow state throughout the reaction system, and the addition is continued between specific molar ratios. A method for producing a polyamide that lowers the pressure has been proposed.
등록특허공보 등록번호 제10-0685535호 "폴리아미드의 제조방법"은 배치식(batch-wise) 조정탱크 내에서 적절한 밸런스로 디아민 성분과 디카르복실산 성분 간의 몰밸런스(molar balance)를 정확히 조정하는 단계와, 실질적으로 아미드화 반응이 일어나지 않는 슬러리액을 제조하는 단계를 포함하고, 이렇게 제조된 슬러리액은 배치식 또는 연속식 중합반응기에 공급되고, 발포, 고체화 등과 같은 문제를 발생시키는 일 없이 아미드화 반응이 진행되어 원하는 밸런스의 디아민 성분과 디카르복실산 성분을 갖는 폴리아미드가 용이하게 제조되도록 하는 기술을 제안하고 있다. Patent Publication No. 10-0685535, "Method for preparing polyamide," accurately adjusts the molar balance between the diamine component and the dicarboxylic acid component in an appropriate balance in a batch-wise adjustment tank. And preparing a slurry liquid in which substantially no amidation reaction occurs, and the slurry liquid thus prepared is fed to a batch or continuous polymerization reactor, without causing problems such as foaming and solidification. A technique for advancing the amidation reaction to easily produce a polyamide having a desired diamine component and a dicarboxylic acid component is proposed.
이와 같은 종래기술에 따른 화학반응은 배치식 반응기, 연속식 반응기 및 반회분식 반응기 중 하나의 반응기를 이용하여 이루어지거나, 여러 종류의 반응기를 일렬로 연결시켜 순차적으로 반응공정이 이루어지도록 하여 생산성을 높이고자 하고 있다. 그러나, 이 경우 기존 설비의 사용이 어려워 설비 비용부담이 증가하고, 설비의 점유면적이 증가하여 설치 공간에서 제약되는 문제점이 있으며, 처리 속도를 증가시키는데 한계를 갖는 등의 문제점이 있다. Such a chemical reaction according to the prior art is performed using one reactor of a batch reactor, a continuous reactor and a semi-batch reactor, or by connecting several kinds of reactors in a row to increase the productivity by the reaction process sequentially I'm sleeping. However, in this case, it is difficult to use the existing equipment, and the cost of the equipment is increased, the occupancy area of the equipment is increased, there is a problem of being limited in the installation space, and there are problems such as a limitation in increasing the processing speed.
따라서, 본 발명은 이와 같은 종래기술의 문제점을 해결하기 위해 제안된 것으로, 서로 다른 액체를 반응시키거나 반응물에 수소 등의 기체를 첨가하여 생성물을 얻는 다양한 화학반응에 용이하게 적용할 수 있도록 하는 새로운 형태의 고효율 화학반응 방법 및 장치를 제공하는 것을 목적으로 한다. Accordingly, the present invention has been proposed to solve the problems of the prior art, and is a novel method that can be easily applied to various chemical reactions to obtain products by reacting different liquids or adding a gas such as hydrogen to the reactants. It is an object to provide a high efficiency chemical reaction method and apparatus in the form.
또한, 본 발명은 종래기술의 문제점을 개선하여 반응 속도를 증가시켜 불순물 형성의 감소와 함께 생산성을 향상시키고, 유지비용을 절감시킬 수 있으며, 필요시 반응 속도의 증가가 용이하도록 하는 새로운 형태의 고효율 화학반응 방법 및 장치를 제공하는 것을 목적으로 한다. In addition, the present invention improves the reaction speed of the prior art to increase the reaction rate to reduce the formation of impurities, improve productivity, reduce the maintenance cost, if necessary, a new form of high efficiency to facilitate the increase of the reaction rate It is an object to provide a chemical reaction method and apparatus.
특히, 본 발명은 종래기술에서 화학반응 설비에서 기존 설비의 사용이 어려워 설비 비용부담이 증가하고, 설비의 점유면적이 증가하여 설치 공간에서 제약되는 문제점이 있으며, 처리 용량을 증감시키는데 한계를 갖는 문제점을 해결할 수 있는 새로운 형태의 고효율 화학반응 방법 및 장치를 제공하는 것을 목적으로 한다. In particular, the present invention is difficult to use the existing equipment in the chemical reaction equipment in the prior art, the cost of the equipment is increased, the occupied area of the equipment is limited in the installation space, there is a problem that there is a limit to increase or decrease the treatment capacity It is an object of the present invention to provide a new type of high efficiency chemical reaction method and apparatus that can solve the problem.
상술한 목적을 달성하기 위한 본 발명의 특징에 따른 고효율 화학반응 방법은 배치형 반응 시스템(12)에 반응물을 넣고, 생성물을 얻기 위한 반응공정을 진행하는 배치 반응공정 단계와; 상기 배치형 반응 시스템(12)과 폐회로를 형성하도록 설치되는 순환형 반응 시스템(13)에 상기 배치형 반응 시스템(12)내에서 배치 반응공정이 진행되는 반응물을 순환시키면서 반응공정이 이루어지도록 하는 순환 반응공정 단계 및; 상기 순환형 반응 시스템(13)으로의 순환을 정지하고, 상기 배치형 반응 시스템(12)내의 생성물을 외부로 배출시키는 단계를 구비한다. The high-efficiency chemical reaction method according to the characteristics of the present invention for achieving the above object is a batch reaction process step of putting a reactant in the batch reaction system 12, and proceeds the reaction process to obtain a product; Circulation to make the reaction process while circulating the reactants in which the batch reaction process proceeds in the batch reaction system 12 to the circulating reaction system 13 installed to form a closed circuit with the batch reaction system 12 A reaction process step; Stopping circulation to the circulating reaction system 13 and discharging the product in the batch reaction system 12 to the outside.
이와 같은 본 발명에 따른 고효율 화학반응 방법에서 상기 배치 반응공정 단계는 상기 배치형 반응 시스템(12)에 반응물을 넣은 후, 첨가 반응물을 넣어 생성물을 얻기 위한 반응공정을 진행하고, 상기 순환 반응공정 단계는 상기 배치형 반응 시스템(12)로부터 공급되는 반응물에 상기 첨가 반응물을 넣어 반응공정이 이루어지도록 할 수 있다. In the high-efficiency chemical reaction method according to the present invention, the batch reaction step is carried out in the batch reaction system 12, and then the reaction step to obtain the product by adding the reactant, the cyclic reaction step The reaction may be performed by putting the additive reactant into the reactant supplied from the batch reaction system 12.
이와 같은 본 발명에 따른 고효율 화학반응 방법에서 상기 첨가 반응물은 기체일 수 있다. In the high-efficiency chemical reaction method according to the present invention, the additive reactant may be a gas.
이와 같은 본 발명에 따른 고효율 화학반응 방법에서 상기 순환 반응공정 단계는 상기 순환형 반응 시스템(13)의 내부 압력이 상기 배치형 반응 시스템(12)의 내부 압력보다 크게 작용되도록 하여 이루어질 수 있다. In the high-efficiency chemical reaction method according to the present invention, the circulating reaction step may be performed so that the internal pressure of the cyclic reaction system 13 is greater than the internal pressure of the batch reaction system 12.
이와 같은 본 발명에 따른 고효율 화학반응 방법에서 상기 반응물은 복수개 이상의 액상으로 이루어질 수 있다. In the high-efficiency chemical reaction method according to the present invention, the reactants may be formed in a plurality of liquid phases.
이와 같은 본 발명에 따른 고효율 화학반응 방법에서 상기 순환 반응공정 단계는 상기 배치형 반응 시스템(12)과 폐회로를 형성하도록 설치되는 연결 라인(15)상에 배치되는 연속식 반응기(14)를 통해 이루어지도록 할 수 있다. In the high-efficiency chemical reaction method according to the present invention, the circulating reaction process step is performed through a continuous reactor 14 disposed on the connection line 15 installed to form a closed circuit with the batch reaction system 12. Can be lost.
이와 같은 본 발명에 따른 고효율 화학반응 방법에서 상기 연속식 반응기(14)는 교반(mixing) 기능을 갖는 교반형 반응기(40)를 구비하고, 상기 순환 반응공정 단계는 반응물이 상기 교반형 반응기(40)를 통과중에 연속적인 교반이 이루어지도록 할 수 있다. In the high-efficiency chemical reaction method according to the present invention, the continuous reactor 14 is provided with a stirred reactor 40 having a mixing (mixing) function, the circulation reaction step is the reactant is the stirred reactor (40) Continuous stirring may be achieved during the passage.
이와 같은 본 발명에 따른 고효율 화학반응 방법에서 상기 연속식 반응기(14)는 분산(dispersion) 기능을 갖는 확산형 반응기(50)를 구비하고, 상기 순환 반응공정 단계는 상기 확산형 반응기(50)를 통해 반응물의 분산이 이루어지도록 할 수 있다. In the high-efficiency chemical reaction method according to the present invention, the continuous reactor 14 includes a diffusion reactor 50 having a dispersion function, and the circulation reaction step includes the diffusion reactor 50. Through the dispersion of the reactants can be made.
이와 같은 본 발명에 따른 고효율 화학반응 방법에서 상기 연속식 반응기(14)는 상기 연결 라인(15)상에 연이어 설치되는 복수개 이상의 반응기를 구비하고, 상기 순환 반응공정 단계는 상기 복수개 이상의 반응기를 순차적으로 통과하면서 이루어지도록 할 수 있다. In the high-efficiency chemical reaction method according to the present invention, the continuous reactor 14 includes a plurality of reactors installed in series on the connection line 15, and the circulation reaction step includes the plurality of reactors sequentially. You can make it through.
이와 같은 본 발명에 따른 고효율 화학반응 방법에서 상기 연속식 반응기(14)의 복수개 이상의 반응기는 교반(mixing) 기능을 갖는 교반형 반응기(40) 및, 분산(dispersion) 기능을 갖는 확산형 반응기(50)를 구비하여, 상기 순환 반응공정 단계는 상기 교반형 반응기(40)를 통해 반응물이 통과중에 연속적인 교반이 이루어진 후, 상기 확산형 반응기(50)를 통해 반응물의 분산이 이루어지도록 할 수 있다. In the high-efficiency chemical reaction method according to the present invention, the plurality of reactors of the continuous reactor 14 are agitated reactor 40 having a mixing function and a diffusion reactor 50 having a dispersion function. ), The circulating reaction step may be a continuous agitation while the reactant is passed through the stirred reactor 40, the dispersion of the reactant is made through the diffusion reactor (50).
상술한 목적을 달성하기 위한 본 발명의 특징에 의한 고효율 화학반응 장치는 반응물을 넣고 반응공정이 완료될 때까지 공정이 계속 진행되도록 하고, 반응공정이 완료된 생성물을 한꺼번에 배출시키도록 구성되는 배치형 반응 시스템(12) 및; 상기 배치형 반응 시스템(12)과 폐회로를 형성하도록 설치되고, 상기 배치형 반응 시스템(12)에 수용되어 반응공정이 진행되는 반응물을 순환시키면서 반응공정이 이루어지도록 하는 순환형 반응 시스템(13)를 구비할 수 있다. The high-efficiency chemical reaction device according to the features of the present invention for achieving the above object is a batch reaction that is configured to add a reactant and continue the process until the reaction process is completed, and to discharge the finished product at once System 12; The circulating reaction system 13 is installed to form a closed circuit with the batch reaction system 12, and is accommodated in the batch reaction system 12 to circulate the reactants through which the reaction process proceeds. It can be provided.
이와 같은 본 발명에 따른 고효율 화학반응 장치에서 상기 순환형 반응 시스템(13)은 상기 배치형 반응 시스템(12)과 폐회로를 형성하도록 설치되는 연결 라인(15) 및; 상기 연결 라인(15) 상에서 설치되는 연속식 반응기(14)를 구비할 수 있다. In the high-efficiency chemical reaction device according to the present invention, the circulation type reaction system 13 includes a connection line 15 installed to form a closed circuit with the batch type reaction system 12; It may be provided with a continuous reactor (14) installed on the connection line (15).
이와 같은 본 발명에 따른 고효율 화학반응 장치에서 상기 연속식 반응기(14)는 반응물이 통과중에 연속적인 교반이 이루어지도록 하는 교반(mixing) 기능을 갖는 교반형 반응기(40)를 구비할 수 있다. In the high-efficiency chemical reaction device according to the present invention, the continuous reactor 14 may include a stirred reactor 40 having a mixing function to allow continuous agitation while the reactants pass through.
이와 같은 본 발명에 따른 고효율 화학반응 장치에서 상기 연속식 반응기(14)는 반응물의 분산이 이루어지도록 하는 분산(dispersion) 기능을 갖는 확산형 반응기(50)를 구비할 수 있다. In the high-efficiency chemical reaction device according to the present invention, the continuous reactor 14 may be provided with a diffusion type reactor 50 having a dispersion function for dispersing the reactants.
이와 같은 본 발명에 따른 고효율 화학반응 장치에서 상기 연속식 반응기(14)는 상기 연결 라인(15)상에 연이어 설치되는 복수개 이상의 반응기를 구비할 수 있다. In the high-efficiency chemical reaction device according to the present invention, the continuous reactor 14 may include a plurality of reactors which are installed on the connection line 15 in series.
이와 같은 본 발명에 따른 고효율 화학반응 장치에서 상기 연속식 반응기(14)는 반응물이 통과중에 연속적인 교반이 이루어지도록 하는 교반(mixing) 기능을 갖는 교반형 반응기(40) 및, 상기 연속식 반응기(14)는 반응물의 분산이 이루어지도록 하는 분산(dispersion) 기능을 갖는 확산형 반응기(50)를 구비할 수 있다. In the high-efficiency chemical reaction device according to the present invention, the continuous reactor 14 is a stirred reactor (40) having a mixing (mixing) function to make a continuous stirring while the reactants pass, and the continuous reactor ( 14 may be equipped with a diffusion reactor 50 having a dispersion function to allow dispersion of the reactants.
이와 같은 본 발명에 따른 고효율 화학반응 장치에서 상기 배치형 반응 시스템(12) 및 순환형 반응 시스템(13)은 반응물을 넣은 후, 첨가 반응물을 공급시키기 위해 설치되는 첨가 반응물 공급 유니트(16)를 더 구비할 수 있다. In the high-efficiency chemical reaction device according to the present invention, the batch reaction system 12 and the circulation reaction system 13 further include an addition reactant supply unit 16 installed to supply the addition reactant after the addition of the reactant. It can be provided.
이와 같은 본 발명에 따른 고효율 화학반응 장치에서 상기 순환형 반응 시스템(13)은 상기 연결 라인(15)상에서 상기 연속 반응기(14)의 전단에 설치되는 펌프(30)와, 후단에 설치되는 액레벨 조정기(34)를 더 구비하여, 상기 순환형 반응 시스템(13)의 내부 압력이 상기 배치형 반응 시스템(12)의 내부 압력보다 높게 설정되도록 할 수 있다. In the high-efficiency chemical reaction device according to the present invention, the circulation type reaction system 13 includes a pump 30 installed at the front end of the continuous reactor 14 on the connection line 15 and a liquid level installed at the rear end. A regulator 34 may further be provided such that the internal pressure of the circulating reaction system 13 is set higher than the internal pressure of the batch reaction system 12.
이와 같은 본 발명에 따른 고효율 화학반응 장치에서 상기 연결 라인(15)은 상기 복수개 이상의 반응기 각각에 각 반응기의 전단과 후단을 연결함으로써, 상기 연결 라인(15)을 통해 흐르는 반응물이 각 반응기를 통과하여 흐르도록 하는 바이패스 라인을 더 구비할 수 있다. In the high-efficiency chemical reaction device according to the present invention, the connection line 15 connects the front end and the rear end of each reactor to each of the plurality of reactors, so that the reactants flowing through the connection line 15 pass through each reactor. It may further include a bypass line to flow.
본 발명에 의한 고효율 화학반응 방법 및 장치에 따르면, 배치형 반응 시스템(12)과 순환형 반응 시스템(13)을 조합하여 다양한 종류의 화학반응을 수행할 수 있도록 하고, 기존 배치식 반응기에 비해 반응 속도를 증가시킬 수 있어 용이하게 생산성을 향상시킬 수 있다. 특히, 기본적으로 배치식 반응기를 적용하는 배치형 반응 시스템(12)에 연속식 반응기(14)를 적용하는 순환형 반응 시스템(13)을 설치하여 이루어지므로, 기존 화학반응설비의 활용이 가능하고, 부가 유틸리티가 불필요하여 유지비용을 절감할 수 있으며, 반응속도의 상승으로 불순물의 형성이 감소된다. 또한, 순환형 반응 시스템(13)에서 연속 반응기(14)의 다단 설계가 가능하므로 반응 속도의 증대가 용이하여 서로 다른 액체를 반응시키거나 반응물에 수소 등의 기체를 첨가하여 생성물을 얻는 다양한 화학반응에 용이하게 적용할 수 있고, 반응 속도의 증가로 생산성이 향상되므로 전체적인 화학 반응장치(10)의 구성을 소규모로 하여 공간 제약을 줄이면서 설치가 간단해진다. According to the high-efficiency chemical reaction method and apparatus according to the present invention, by combining the batch reaction system 12 and the circulation reaction system 13 to perform a variety of chemical reactions, compared to the conventional batch reactor The speed can be increased, so productivity can be easily increased. In particular, it is basically made by installing a cyclic reaction system 13 applying the continuous reactor 14 to the batch reaction system 12 applying the batch reactor, it is possible to utilize the existing chemical reaction equipment, No additional utility is required to reduce maintenance costs, and the formation of impurities is reduced by increasing the reaction rate. In addition, since the multi-stage design of the continuous reactor 14 is possible in the cyclic reaction system 13, it is easy to increase the reaction rate, and various chemical reactions for reacting different liquids or adding a gas such as hydrogen to the reactants to obtain a product. It can be easily applied to, and the productivity is improved by increasing the reaction rate, so that the installation of the chemical reaction device 10 can be made small while reducing the space constraint.
도 1은 본 발명의 기술 사상에 따른 고효율 화학반응 방법 및 장치를 설명하기 위한 도면;1 is a view for explaining a high efficiency chemical reaction method and apparatus according to the technical idea of the present invention;
도 2는 본 발명의 바람직한 실시예에 따른 고효율 화학반응 방법 및 장치를 설명하기 위한 도면;2 is a view for explaining a high efficiency chemical reaction method and apparatus according to a preferred embodiment of the present invention;
도 3은 도 2에서 보인 본 발명의 바람직한 실시예에 따른 고효율 화학반응 방법 및 장치의 변형를 설명하기 위한 도면;3 is a view for explaining a modification of the high efficiency chemical reaction method and apparatus according to a preferred embodiment of the present invention shown in FIG.
도 4는 본 발명의 바람직한 다른 실시예에 따른 고효율 화학반응 방법 및 장치를 설명하기 위한 도면;4 is a view for explaining a high efficiency chemical reaction method and apparatus according to another embodiment of the present invention;
도 5는 본 발명의 바람직한 또 다른 실시예에 따른 고효율 화학반응 방법 및 장치를 설명하기 위한 도면;5 is a view for explaining a high efficiency chemical reaction method and apparatus according to another embodiment of the present invention;
도 6은 수소 첨가반응을 위해 구성되는 본 발명의 바람직한 실시예에 따른 고효율 화학반응 방법 및 장치를 설명하기 위한 도면이다.6 is a view for explaining a high efficiency chemical reaction method and apparatus according to a preferred embodiment of the present invention configured for the hydrogenation reaction.
이하, 본 발명의 바람직한 실시예를 첨부된 도면 도 2 내지 도 9에 의거하여 상세히 설명한다. 한편, 각 도면에서 종래기술로부터 용이하게 확인할 수 있는 연속식, 배치식 및 반배치식 반응공법과 시스템의 구성 및 공정 제어관련기술, 기체첨가반응이 적용되는 반응물 및 첨가 반응물의 종류 및 그에 따른 공정조건, 화학반응 시스템을 안전운영하기 위한 밸브, 센서, 제어장치 등 통상 본 발명에 적용되는 분야의 종사자들 및 그들이 관련분야의 종사자들을 통해 통상적으로 알 수 있는 부분들의 도시 및 상세한 설명은 생략하고, 본 발명과 관련된 부분들을 중심으로 도시 및 설명하였다.  Hereinafter, exemplary embodiments of the present invention will be described in detail with reference to FIGS. 2 to 9. On the other hand, the continuous, batch and semi-batch reaction method and system configuration and process control related technology, the kinds of reactants to which the gas addition reaction is applied, and the process accordingly, which can be easily identified from the prior art in each drawing. The illustration and detailed description of those skilled in the art and those commonly known by those skilled in the art, such as valves, sensors, and control devices for safe operation of conditions, chemical reaction systems, etc., will be omitted. The parts related to the present invention are illustrated and described.
도 2는 본 발명의 바람직한 실시예에 따른 고효율 화학반응 방법 및 장치를 설명하기 위한 도면이다. 2 is a view for explaining a high efficiency chemical reaction method and apparatus according to a preferred embodiment of the present invention.
도 2를 참조하면, 본 발명의 바람직한 실시예에 따른 고효율 화학반응 방법은 배치형 반응 시스템(12)에 반응물을 넣고, 생성물을 얻기 위한 반응공정을 진행하는 배치 반응공정 단계, 배치형 반응 시스템(12)과 폐회로를 형성하도록 설치되는 순환형 반응 시스템(13)에 배치형 반응 시스템(12)내에서 배치 반응공정이 진행되는 반응물을 순환시키면서 반응공정이 이루어지도록 하는 순환 반응공정 단계, 생성물이 형성되었을 때 순환형 반응 시스템(13)으로의 순환을 정지하고, 배치형 반응 시스템(12)내의 생성물을 외부로 배출시키는 단계로 이루어진다. 여기서, 반응물은 복수개 이상의 액상으로 이루어진다. Referring to Figure 2, the high-efficiency chemical reaction method according to a preferred embodiment of the present invention is to put the reactants in the batch reaction system 12, a batch reaction process step of proceeding the reaction process to obtain a product, batch reaction system ( 12) and a circulating reaction process step, the product is formed to circulate the reactants undergoing the batch reaction process in the batch reaction system 12 to the circulating reaction system 13 installed to form a closed circuit, the product is formed When it stops, the circulation to the circulating reaction system 13 is stopped, and the product in the batch reaction system 12 is discharged to the outside. Here, the reactants consist of a plurality of liquid phases.
또한, 본 실시예에 따른 고효율 화학반응 방법은 배치형 반응 시스템(12)과 폐회로를 형성하도록 설치되는 연결 라인(15)상에 배치되는 연속식 반응기(14)를 통해 순환 반응공정 단계가 이루어지도록 함으로써, 배치형 반응 시스템(12)으로부터 흐르는 반응물이 연결 라인(15)을 통해 흐르도록 하면서 반응효율을 높이는 다양한 반응공정을 실시할 수 있도록 한다. In addition, the high-efficiency chemical reaction method according to the present embodiment is such that the circulating reaction process step is made through the continuous reactor 14 disposed on the connection line 15 installed to form a closed circuit with the batch reaction system 12 By doing so, the reactants flowing from the batch reaction system 12 can be carried out through the connection line 15 to perform various reaction processes to increase the reaction efficiency.
본 실시예에서 순환 반응공정 단계는 연속 반응기(14)는 교반형 반응기(40)와 확산형 반응기(50)를 통해 수행된다. 이때, 교반형 반응기(40)는 교반(mixing) 기능을 갖는 반응기로서, 순환 반응공정 단계는 교반형 반응기(40)를 통해 층류의 유체를 난류유체로 변환시켜 주면서 통과중에 연속적인 교반이 이루어지도록 한다. 그리고, 확산형 반응기(50)는 분산(dispersion) 기능을 갖는 반응기로서, 순환 반응공정 단계는 확산형 반응기(50)를 통해 상이 다른 유체의 접촉을 용이하게 하는 반응물의 분산이 이루어지도록 한다. In the present embodiment, the cyclic reaction process step is performed through the continuous reactor 14 and the stirred reactor 40 and the diffusion reactor 50. At this time, the stirred reactor 40 is a reactor having a mixing (mixing) function, the circulating reaction step is to convert the laminar flow fluid into turbulent fluid through the stirred reactor 40 so that continuous stirring is performed during the passage. do. In addition, the diffusion reactor 50 is a reactor having a dispersion function, and the circulating reaction process step allows dispersion of reactants to facilitate contact of different fluids through the diffusion reactor 50.
한편, 이와 같은 본 발명의 바람직한 실시예의 고효율 화학반응 방법에서 순환 반응공정 단계는 단일의 연속 반응기(14)가 적용될 수도 있고, 연속식 반응기(14)가 연결 라인(15)상에 연이어 설치되는 복수개 이상의 반응기로 이루어지도록 하여, 복수개 이상의 반응기를 순차적으로 통과하면서 이루어지도록 할 수 있다. 즉, 전술한 교반(mixing) 기능을 갖는 교반형 반응기(40)와 분산(dispersion) 기능을 갖는 확산형 반응기(50)를 연결 라인(15)상에 연이어 설치되도록 하여 순환 반응공정 단계가 교반형 반응기(40)를 통해 층류의 유체를 난류유체로 변환시켜 주면서 통과중에 연속적인 교반이 이루어진 후, 확산형 반응기(50)를 통해 상이 다른 유체의 접촉을 용이하게 하는 반응물의 분산이 이루어지도록 함으로써, 반응속도를 더욱 높일 수 있도록 하는 것이다. 물론, 이와 같은 연속 반응기(14)를 이루는 반응기의 순서, 개수는 설비의 필요에 따라 다양하게 구성할 수 있는 것이다. On the other hand, in the high-efficiency chemical reaction method of the preferred embodiment of the present invention, the cyclic reaction step may be applied to a single continuous reactor 14, a plurality of continuous reactor 14 is installed in series on the connection line 15 It may be made of the above reactor, it may be made while sequentially passing through a plurality of reactors. That is, the cyclic reaction process step is agitated so that the above-mentioned stirring reactor 40 having the mixing function and the diffusion reactor 50 having the dispersion function are installed on the connection line 15 in succession. By converting the laminar flow fluid into the turbulent fluid through the reactor 40 while continuous stirring takes place during the passage, through the diffusion type reactor 50 to allow the dispersion of the reactants to facilitate the contact of the different fluids, It is to make the reaction rate higher. Of course, the order, number of reactors forming the continuous reactor 14 can be configured in various ways according to the needs of the installation.
다시, 도 2를 참조하면, 본 발명의 바람직한 실시예에 따른 고효율 화학반응 장치(10)는 전술한 바와 같은 화학반응 공정을 수행할 수 있도록 하기 위해 배치형 반응 시스템(12)과 순환형 반응 시스템(13)을 구비한다. 이때, 배치형 반응 시스템(12)은 반응물을 넣고 반응공정이 완료될 때까지 공정이 계속 진행되도록 하고, 반응공정이 완료된 생성물을 한꺼번에 배출시키도록 구성된다. 순환형 반응 시스템(13)은 배치형 반응 시스템(12)과 폐회로를 형성하도록 설치되고, 배치형 반응 시스템(12)에 수용되어 반응공정이 진행되는 반응물을 순환시키면서 반응공정이 이루어지도록 한다. Referring again to FIG. 2, the high efficiency chemical reaction device 10 according to a preferred embodiment of the present invention is a batch reaction system 12 and a circulating reaction system in order to be able to perform the chemical reaction process as described above. (13) is provided. At this time, the batch reaction system 12 is configured to put the reactants and to continue the process until the reaction process is completed, and to discharge the finished product at once. The circulating reaction system 13 is installed to form a closed circuit with the batch reaction system 12, and is accommodated in the batch reaction system 12 to circulate the reactants through which the reaction process proceeds.
본 실시예에 따른 고효율 화학반응 장치(10)에서 순환형 반응 시스템(13)은 연속식 반응기(14)와 연결 라인(15)을 구비하는데, 연결 라인(15)은 배치형 반응 시스템(12)과 폐회로를 형성하도록 설치되고, 연속식 반응기(14)는 연결 라인(15) 상에서 설치된다. 이와 같이 배치형 반응 시스템(12)과 폐회로를 형성하도록 설치되는 연결 라인(15)상에 연속식 반응기(14)를 배치하여 설치하도록 함으로써, 설계의 편의성을 높이고, 설계자 또는 사용자의 필요에 따라 더욱 다양한 설계 및 제작이 가능하도록 한다. In the high-efficiency chemical reaction device 10 according to the present embodiment, the circulating reaction system 13 includes a continuous reactor 14 and a connection line 15, and the connection line 15 is a batch reaction system 12. And to form a closed circuit, and a continuous reactor 14 is installed on the connecting line 15. By arranging and installing the continuous reactor 14 on the connection line 15 which is installed to form a closed circuit with the batch reaction system 12 in this way, it is possible to increase the convenience of the design, and according to the needs of the designer or user Various designs and manufacturing are possible.
한편, 본 실시예의 고효율 화학반응 장치(10)에서 연속식 반응기(14)는 대표적으로 교반형 반응기(40)와 확산형 반응기(50)가 적용될 수 있다. 이때, 교반형 반응기(40)는 층류의 유체를 난류의 유체로 변환시켜 주면서 통과중에 연속적인 교반이 이루어지도록 하는 교반(mixing) 기능을 갖고, 확산형 반응기(50)는 상이 다른 유체의 접촉을 용이하게 하는 반응물의 분산이 이루어지도록 하는 분산(dispersion) 기능을 갖는다. On the other hand, in the high-efficiency chemical reaction device 10 of the present embodiment, the continuous reactor 14 may typically be a stirred reactor 40 and a diffusion reactor 50. In this case, the stirred reactor 40 has a mixing function to convert the laminar fluid into a turbulent fluid while allowing continuous stirring to be performed during the passage, and the diffusion reactor 50 is capable of contacting different fluids. It has a dispersion function that facilitates dispersion of the reactants.
본 실시예에서 연속식 반응기(14)를 이루는 이들 반응기(40, 50)는 각각 별개로 사용되거나 연결 라인(15)상에 연이어 설치되어 복수개 이상이 사용될 수 있다. 예컨대, 본 실시예는 연속식 반응기(14)로 교반형 반응기(40)와 확산형 반응기(50)를 예로 보였는데, 이들은 각각이 복수개로 적용되거나 다른 종류의 연속식 반응기가 적용될 수 있는 것이다. In the present embodiment, the reactors 40 and 50 constituting the continuous reactor 14 may be used separately, or may be installed in series on the connection line 15, and a plurality or more thereof may be used. For example, the present embodiment showed the stirred reactor 40 and the diffused reactor 50 as an example of the continuous reactor 14, each of which may be applied in plural or different kinds of continuous reactors.
도 3은 도 2에서 보인 본 발명의 바람직한 실시예에 따른 고효율 화학반응 방법 및 장치의 변형예를 설명하기 위한 도면이다. 3 is a view for explaining a modification of the high efficiency chemical reaction method and apparatus according to a preferred embodiment of the present invention shown in FIG.
도 3을 참조하면, 본 실시예에 따른 고효율 화학반응 장치(10)는 도 2에서 보인 본 발명의 바람직한 실시예에 따른 고효율 화학반응 장치(10)의 연결 라인(15)에 바이패스 라인(15a, 15b)을 부가적으로 설치한 형태이다. 이때, 바이패스 라인(15a, 15b)은 복수개 이상의 반응기{본 실시예에서는 교반형 반응기(40)와 확산형 반응기(50)} 각각에 각 반응기의 전단과 후단을 연결함으로써, 연결 라인(15)을 통해 흐르는 반응물이 각 반응기를 통과하여 흐르도록 한다. 이와 같은 바이패스 라인(15a, 15b)은 두 반응기의 공정을 선택적으로 적용할 필요가 있는 경우 유용하게 적용할 수 있다. Referring to FIG. 3, the high efficiency chemical reaction device 10 according to the present embodiment may include a bypass line 15a on the connection line 15 of the high efficiency chemical reaction device 10 according to the preferred embodiment of the present invention shown in FIG. 2. , 15b) is additionally installed. In this case, the bypass lines 15a and 15b connect the front and rear ends of each reactor to each of a plurality of reactors (agitated reactor 40 and diffusion reactor 50 in this embodiment), thereby connecting the connection line 15. The reactant flowing through the flow through each reactor. Such bypass lines 15a and 15b may be usefully applied when it is necessary to selectively apply the processes of the two reactors.
도 4는 본 발명의 바람직한 다른 실시예에 따른 고효율 화학반응 방법 및 장치를 설명하기 위한 도면이다. 4 is a view for explaining a high efficiency chemical reaction method and apparatus according to another embodiment of the present invention.
도 4를 참조하면, 본 실시예에 따른 고효율 화학반응 방법은 배치 반응공정 단계에서 배치형 반응 시스템(12)에 반응물을 넣은 후, 첨가 반응물을 넣어 생성물을 얻기 위한 반응공정을 진행하고, 순환 반응공정 단계는 배치형 반응 시스템(12)로부터 공급되는 반응물에 첨가 반응물을 넣어 반응공정이 이루어지도록 한다. Referring to FIG. 4, in the high-efficiency chemical reaction method according to the present embodiment, after adding a reactant to the batch type reaction system 12 in a batch reaction process step, a reaction process for adding an added reactant to obtain a product and performing a cyclic reaction The process step involves adding reactants to the reactants supplied from the batch reaction system 12 so that the reaction process takes place.
이를 위해 본 실시예에 따른 고효율 화학반응 장치(10)는 배치형 반응 시스템(12) 및 순환형 반응 시스템(13)에는 반응물을 넣은 후, 첨가 반응물을 공급시키기 위해 설치되는 첨가 반응물 공급 유니트(16)가 설치된다. 이때, 순환형 반응 시스템(13)에서 첨가 반응물 공급 유니트(16)는 교반형 반응기(40)와 확산형 반응기(50) 각각에 첨가 반응물이 균일하게 공급될 수 있도록 다양한 형태로 구성될 수 있을 것이다. To this end, the high-efficiency chemical reaction device 10 according to the present embodiment includes an additive reactant supply unit 16 installed to supply an additive reactant after placing a reactant in the batch reaction system 12 and the circulating reaction system 13. ) Is installed. In this case, the additive reactant supply unit 16 in the circulating reaction system 13 may be configured in various forms so that the additive reactants may be uniformly supplied to each of the stirred reactor 40 and the diffusion reactor 50. .
이와 같은 본 실시예에 따른 고효율 화학반응 방법은 액상의 반응물을 2가지 이상 혼합시켜 이루어지는 액-액 반응, 액상의 반응물에 수소(H2), 이산화탄소(CO2), 메탄(CH4) 등의 기체를 첨가시키는 기-액 반응 등 다양한 첨가 반응공정을 진행할 수 있도록 한다. The high-efficiency chemical reaction method according to this embodiment is a liquid-liquid reaction by mixing two or more liquid reactants, such as hydrogen (H 2 ), carbon dioxide (CO 2 ), methane (CH 4 ) to the liquid reactants Various addition reaction processes, such as gas-liquid reaction to add gas, can be performed.
도 5는 본 발명의 바람직한 또 다른 실시예에 따른 고효율 화학반응 방법 및 장치를 설명하기 위한 도면이다. 5 is a view for explaining a high efficiency chemical reaction method and apparatus according to another embodiment of the present invention.
도 5를 참조하면, 본 실시예에 따른 고효율 화학반응 방법은 순환형 반응 시스템(13)의 내부 압력이 배치형 반응 시스템(12)의 내부 압력보다 크게 작용되도록 하여 순환 반응공정을 진행하도록 함으로써, 반응효율을 더욱 높이도록 한다. Referring to FIG. 5, the high-efficiency chemical reaction method according to the present embodiment allows the internal pressure of the circulating reaction system 13 to be greater than the internal pressure of the batch reaction system 12 so that the cyclic reaction process may be performed. Make the reaction more efficient.
이와 같은 고효율 화학반응 방법은 배치형 반응 시스템(12)에 비해 압력을 상대적으로 용이하게 높게 가져가도록 할 수 있는 순환형 반응 시스템(13)을 적용함으로써, 반응 장치의 제조비용 및 유지비용을 낮추면서도 더욱 높은 반응 효율을 기대할 수 있도록 한다. This high-efficiency chemical reaction method by applying a cyclic reaction system 13 that can make the pressure relatively easily compared to the batch reaction system 12, while reducing the manufacturing cost and maintenance cost of the reaction apparatus Higher reaction efficiency can be expected.
이를 위해 본 실시예에 따른 고효율 화학반응 장치(10)는 순환형 반응 시스템(13)에 펌프(30)와 액레벨 조정기(34)를 설치하여 이루어진다. 이때, 펌프(30)는 연결 라인(15)상에서 순환형 반응 시스템(13)의 연속 반응기(14)의 전단에 설치되어 배치형 반응 시스템(12)으로부터 반응물이 연결 라인(15)으로 흐르도록 한다. 이때, 펌프(30)의 후단에는 유량 및 압력을 제어가 위한 밸브(32)가 설치된다. 펌프(30)에 의해 연결 라인(15)을 통해 연속식 반응기(14)로 유입되는 반응물에는 첨가 반응물 공급 유니트(16)에 의해 수소 가스와 같은 첨가 반응물이 공급되어 순환형 반응 시스템(13)내의 압력을 고압으로 상승 및 유지하게 된다. 이와 같은 순환형 반응 시스템(13)내의 고압은 펌프(30) 후단의 밸브(32)부터 액레벨 조정기(34) 후단의 밸브(36)까지 걸리게 된다. 액레벨 조정기(34)는 연결 라인(15)상에서 연속 반응기(14)의 후단에 설치되어 순환형 반응 시스템(13)의 내부 압력이 유지되는 상태에서 유량과 압력을 조절하기 위한 ㅈ밸브(36)를 열어 반응물이 배치형 반응 시스템(12)으로 흐를 수 있도록 한다. To this end, the high-efficiency chemical reaction device 10 according to the present embodiment is formed by installing a pump 30 and a liquid level regulator 34 in a circulating reaction system 13. At this time, the pump 30 is installed at the front end of the continuous reactor 14 of the circulating reaction system 13 on the connection line 15 to allow the reactants to flow from the batch reaction system 12 to the connection line 15. . At this time, a valve 32 for controlling the flow rate and pressure is installed at the rear end of the pump 30. The reactants introduced into the continuous reactor 14 by the pump 30 through the connecting line 15 are supplied with an additive reactant such as hydrogen gas by the additive reactant supply unit 16 to supply the reactant in the circulating reaction system 13. The pressure is raised and maintained at high pressure. The high pressure in the circulating reaction system 13 is applied from the valve 32 at the rear end of the pump 30 to the valve 36 at the rear end of the liquid level regulator 34. The liquid level regulator 34 is installed at the rear end of the continuous reactor 14 on the connecting line 15 so as to adjust the flow rate and pressure while maintaining the internal pressure of the circulating reaction system 13. Open to allow reactants to flow into batch reaction system 12.
좀 더 구체적으로 보면, 본 실시예에 따른 고효율 화학반응 장치(10)는 배치형 반응 시스템(12)은 저압{순환형 반응 시스템(13)에 대한 상대적인 압}으로 반응공정이 진행되도록 하고, 순환형 반응 시스템(13)은 고압으로 반응공정이 진행되도록 하되, 순환형 반응 시스템(13)의 고압이 유지되도록 하기 위해{즉, 순환형 반응 시스템(13)에 공급되는 수고 가스와 같은 기체가 배치형 반응 시스템(12)으로 유입되는 것을 방지} 순환되어지는 반응액이 액레벨 조정기(34)에 모여지게 되는데, 이 액레벨 조정기(34)에 연동되어 있는 유량 및 압력 제어밸브(36)의 조절{물론, 이와 같은 유량 및 압력 제어밸브(36)는 반응장치(10)의 컨트롤러에 의해 이루어질 것이다}에 의해 액레벨 조정기(34)에 모이게 되는 반응액에 의해 유체의 흐름을 막고, 하나의 독립된 계로 만들게 된다. 그리고, 펌프(30)에서는 계속 반응물을 연속식 반응기(14) 방향으로 밀고 있기 때문에 순환형 반응 시스템(13)은 고압상태를 유지하고, 배치형 반응 시스템(12)은 저압상태를 유지하여 서로 독립된 공간으로 닫힌 계가 된다. 반응 압력은 각각의 반응기에 들어가는 수소압으로 조절하고, 각각의 독립된 계이기 때문에 압력을 따로 분리하여 사용할 수 있다. More specifically, the high-efficiency chemical reaction device 10 according to the present embodiment is a batch reaction system 12 allows the reaction process to proceed at low pressure (relative pressure relative to the cyclic reaction system 13), the circulation The type reaction system 13 allows the reaction process to proceed at a high pressure, but in order to maintain the high pressure of the circulating reaction system 13 (that is, a gas such as toil gas supplied to the circulating reaction system 13 is arranged. Prevent the flow into the type reaction system 12} circulating reaction liquid is collected in the liquid level regulator 34, the control of the flow rate and pressure control valve 36 that is linked to the liquid level regulator 34 The flow and pressure of the control valve 36, of course, will be made by the controller of the reactor 10, to prevent the flow of the fluid by the reaction liquid collected in the liquid level regulator 34, one independent Made into a system All. In addition, since the pump 30 continuously pushes the reactants in the direction of the continuous reactor 14, the circulation type reaction system 13 maintains a high pressure state, and the batch type reaction system 12 maintains a low pressure state and is independent of each other. It becomes a system closed to space. The reaction pressure is controlled by the hydrogen pressure entering each reactor, and the pressures can be used separately because they are independent systems.
따라서, 액레벨 조정기(34)에는 반응액의 높이를 조절하여야 하기 때문에 항상 일정한 높이 이상으로 반응액이 채워져 있도록 하고, 공정의 진행에 따라 반응액의 높이가 높아지면 액레벨 조정기(34)와 연동되어진 밸브(36)를 이용하여 일정한 액높이를 유지하게 된다. Therefore, the liquid level regulator 34 should always adjust the height of the reaction liquid, so that the reaction liquid is always filled to a predetermined height or more, and when the height of the reaction liquid increases as the process proceeds, the liquid level regulator 34 interworks with it. By using the valve 36 is maintained a constant liquid level.
도 6은 수소 첨가반응을 위해 구성되는 본 발명의 바람직한 실시예에 따른 고효율 화학반응 방법 및 장치를 설명하기 위한 도면이다. 6 is a view for explaining a high efficiency chemical reaction method and apparatus according to a preferred embodiment of the present invention configured for the hydrogenation reaction.
도 6을 참조하면, 본 발명의 바람직한 실시예에 따른 고효율 화학반응 방법은 액상의 반응물을 2가지 이상 혼합시켜 이루어지는 액-액 반응, 액상의 반응물에 수소(H2), 이산화탄소(CO2), 메탄(CH4) 등의 기체를 첨가시키는 기-액 반응 등 다양한 반응공정을 진행할 수 있도록 한다. Referring to FIG. 6, the high-efficiency chemical reaction method according to the preferred embodiment of the present invention is a liquid-liquid reaction made by mixing two or more liquid reactants, hydrogen (H 2 ), carbon dioxide (CO 2 ), Various reaction processes such as a gas-liquid reaction in which a gas such as methane (CH 4 ) is added may be performed.
이와 같은 본 실시예에 따른 고효율 화학반응 방법은 기본적으로 배치형 반응 시스템(12)에 반응물을 넣고, 생성물을 얻기 위한 반응공정을 진행하는 배치 반응공정 단계와, 배치형 반응 시스템(12)와 폐회로를 형성하도록 설치되는 순환형 반응 시스템(13)에 배치형 반응 시스템(12)내에서 배치 반응공정이 진행되는 반응물을 순환시키면서 반응공정이 이루어지도록 하는 순환 반응공정 단계 및, 생성물이 형성되었을 때 순환형 반응 시스템(13)로의 순환을 정지하고, 배치형 반응 시스템(12)내의 생성물을 외부로 배출시키는 단계로 이루어진다. Such a high-efficiency chemical reaction method according to the present embodiment is basically a batch reaction process step of putting the reactants in the batch reaction system 12, and proceeds with the reaction process to obtain a product, the batch reaction system 12 and the closed circuit A circulating reaction process step for circulating a reactant in which a batch reaction process proceeds in a batch reaction system 12 to a circulating reaction system 13 installed to form a reaction reaction step, and circulating when a product is formed. Stopping circulation to the type reaction system 13 and draining the product in the batch type reaction system 12 to the outside.
이때, 본 실시예에 따른 배치형 반응 시스템(12)으로부터 반응물이 유출되어 다시 유입되도록 폐회로를 형성하는 연결 라인(15)에는 교반형 반응기(40), 확산형 반응기(50)가 설치된다. 특히, 본 실시예는 두개의 교반형 분산 반응기(40a, 40b)가 연결 라인(15)상에서 연속적으로 설치된다. 교반형 반응기(40)의 전단의 연결 라인(15)에는 반응물을 순환형 반응 시스템(13)으로 흐르도록 하기 위한 펌프(30), 펌프(30) 전단에서 순환형 반응 시스템(13)내의 고압을 유지하도록 하면서 반응물의 흐름을 제어하기 위한 밸브(32), 반응물의 흐름상태를 확인하도록 하는 레벨 게이지(72), 교반형 반응기(40) 전단의 압력을 확인하도록 하는 압력 케이지(70)가 설치된다. 그리고, 확산형 반응기(50)의 후단의 연결 라인(15)에는 액레벨 조정기(34)와, 순환형 반응 시스템(13)내의 고압이 유지되도록 하면서 배치형 반응 시스템(12)으로의 반응물의 흐름을 제어하는 밸브(36)가 설치된다. At this time, the stirring line 40, the diffusion type reactor 50 is installed in the connection line 15 to form a closed circuit so that the reactant flows out from the batch reaction system 12 according to the present embodiment. In particular, in this embodiment, two stirred dispersion reactors 40a and 40b are installed continuously on the connecting line 15. The connecting line 15 at the front end of the stirred reactor 40 includes a pump 30 for flowing the reactants into the circulating reaction system 13, and a high pressure in the circulating reaction system 13 at the front of the pump 30. Valve 32 for controlling the flow of reactants while maintaining, level gauge 72 for checking the flow of reactants, and pressure cage 70 for checking the pressure in front of the stirred reactor 40 are installed. . Then, the connection line 15 at the rear end of the diffusion reactor 50 has a liquid level regulator 34 and a flow of reactants into the batch reaction system 12 while maintaining a high pressure in the circulation reaction system 13. The valve 36 to control the is installed.
또한, 본 실시예에 따른 고효율 화학반응 장치(10)는 교반형 반응기(40)와 확산형 반응기(50)에 바이패스라인(15a, 15b)를 설치하여 필요시 교반형 반응기(40)와 확산형 반응기(50)를 선택적으로 적용하여 반응공정을 진행할 수 있도록 한다. In addition, the high-efficiency chemical reaction device 10 according to the present embodiment is provided with bypass lines 15a and 15b in the stirred reactor 40 and the diffused reactor 50, and if necessary, diffused with the stirred reactor 40. Selective reactor 50 is selectively applied to allow the reaction process to proceed.
또한, 본 실시예에 따른 고효율 화학반응 장치(10)는 기체 첨가반응이 가능하도록 배치형 반응 시스템(12) 및 순환형 반응 시스템(13)은 반응물을 넣은 후, 첨가 반응물을 공급시키기 위해 첨가 반응물 공급 유니트(16)가 설치된다. 이때, 본 실시예에서는 수소 첨가반응을 위해 질소를 공급하기 위한 질소 공급 유니트(18)가 함께 구성된다. 첨가 반응물 공급 유니트(16)와 질소 반응물 공급 유니트(16)는 각각 배치식 반응 시스템(12)의 반응기(도시 않음), 교반형 반응기(40) 및 확산형 반응기(50)와 접속되어 수소와 질소를 각각 공급한다. 그리고, 수소와 같이 폭발성이 있는 첨가반응의 경우, 수소를 안전하게 배기하기 위해콘덴서(62), 포집기(64) 등을 구비하는 벤트 유니트(60)가 설치된다. In addition, the high-efficiency chemical reaction device 10 according to the present embodiment is a batch reaction system 12 and a circulating reaction system 13 to add a reactant after the addition of the reactant so as to enable a gas addition reaction The supply unit 16 is installed. At this time, in this embodiment, the nitrogen supply unit 18 for supplying nitrogen for the hydrogenation reaction is configured together. The additive reactant supply unit 16 and the nitrogen reactant supply unit 16 are connected to the reactor (not shown), the stirred reactor 40 and the diffusion reactor 50 of the batch reaction system 12, respectively, to form hydrogen and nitrogen. Supply each. In the case of an explosive addition reaction such as hydrogen, a vent unit 60 including a capacitor 62, a collector 64, and the like is installed to safely discharge hydrogen.
본 실시예에 따른 고효율 화학반응 방법은 순환 반응공정 단계가 연이어 설치되는 복수개 이상의 연속 반응기(14)를 통해 이루어지도록 한다. 즉, 전술한 교반형 반응기(40)와 확산형 반응기(50)를 연속적으로 배치하여 반응물의 스트림(stream)이 교반과 분산이 연이어 이루어지도록 함으로써, 반응시간을 단축시켜 생산효율을 높이도록 한다. The high-efficiency chemical reaction method according to the present embodiment is such that the cyclic reaction step is performed through a plurality of continuous reactors 14 installed in succession. That is, the above-described stirred reactor 40 and the diffusion reactor 50 are continuously arranged so that the stream of the reactant is continuously stirred and dispersed, thereby shortening the reaction time to increase production efficiency.
한편, 본 실시예에 따른 고효율 화학반응 방법은 수소 첨가반응과 같이 기체를 첨가시켜 이루어지는 반응공정을 진행할 수 있도록 한다. 이와 같은 첨가반응의 경우, 배치 반응공정 단계는 배치형 반응 시스템(12)에 반응물을 넣은 후, 첨가 반응물을 넣어 생성물을 얻기 위한 반응공정을 진행하고, 순환 반응공정 단계는 배치형 반응 시스템(12)로부터 공급되는 반응물에 첨가 반응물을 넣어 반응공정이 이루어지도록 한다. On the other hand, the high-efficiency chemical reaction method according to the present embodiment allows the reaction process made by adding a gas, such as hydrogenation reaction. In the case of such an addition reaction, the batch reaction step may include a reactant in a batch reaction system 12, and then proceed with a reaction step to obtain a product by adding an additional reactant, and the cyclic reaction step may include a batch reaction system 12. The reaction product is added to the reactant supplied from the reaction mixture.
그리고, 본 실시예에 따른 고효율 화학반응 방법에서 순환 반응공정 단계는 순환형 반응 시스템(13)의 내부 압력이 배치형 반응 시스템(12)의 내부 압력보다 크게 작용되도록 함으로써, 운용비용을 절감시키면서 반응 시간을 감소시켜 생산효율을 높이도록 한다. In the high-efficiency chemical reaction method according to the present embodiment, the cyclic reaction process step allows the internal pressure of the cyclic reaction system 13 to be greater than the internal pressure of the batch reaction system 12, thereby reducing the operating cost. Reduce time to increase production efficiency.
이하, 본 발명의 실험예 및 비교예를 통하여 보다 상세히 설명하기로 한다. Hereinafter, it will be described in more detail through the experimental and comparative examples of the present invention.
<실험예 1> 프로필렌글리콜의 제조Experimental Example 1 Preparation of Propylene Glycol
먼저, 본 발명의 바람직한 실시예에 따른 고효율 화학반응 장치의 배치형 반응 시스템에 글리세롤(glycerol) 78.4kg과 H2O 19.6kg을 투입하고, 배치형 반응 시스템의 온도를 60℃로 설정한 후, 100rpm으로 교반시키며 반응물을 완전히 용해시켰다. 다음으로, 반응물이 완전히 용해된 후, 배치형 반응 시스템의 온도를 70℃로 설정한 뒤, 70℃에 도달시 촉매(CuO/Cr2O4)를 3.9kg을 투입하고, 촉매 투입 후 배치형 반응 시스템을 완전히 밀폐하였다. 그리고, 상기 촉매를 반응물에 충분히 분산시킨 후, 배치형 반응 시스템의 밸브를 열어 펌프를 이용해 배치형 반응 시스템의 반응물을 순환형 반응 시스템의 교반형 반응기와 확산형 반응기로 순환시키는 데, 이 때 순환되는 반응물의 양을 유량계 밸브로 조절하여 10~15L/min으로 유지하였다. 용해된 반응물을 순환시키면서 배치형 및 순환형 반응 시스템 내부에 질소를 밀어 넣어 각 반응기 및 반응물에 잔존하는 산소를 제거한 후, 배치형 및 순환형 반응 시스템 내부를 수소 분위기로 만들기 위해 수소를 밀어 넣어 질소를 제거하였다. 이렇게 하여 반응기 내부가 수소 분위기가 된 후, 반응기 온도를 반응온도인 300℃로 설정한 뒤, 배치형 및 순환형 반응 시스템 내부 수소 압력을 5bar로 올려주고, 배치형 및 순환형 반응 시스템 내부 수소압력이 5bar에 도달한 뒤, 순환형 반응 시스템 내부의 수소 압력을 14bar로 올려주어, 300℃에서 반응기 내부 수소 압력을 배치형 반응 시스템 5bar, 순환형 반응 시스템 14bar로 유지하며 교반속도 300rpm 조건하에 글리세롤의 수소화 반응을 진행하였다.First, 78.4 kg of glycerol and 19.6 kg of H 2 O are added to a batch reaction system of a high-efficiency chemical reaction device according to a preferred embodiment of the present invention, and the temperature of the batch reaction system is set to 60 ° C. The reaction was completely dissolved by stirring at 100 rpm. Next, after the reactants are completely dissolved, the temperature of the batch reaction system is set to 70 ° C., and when the temperature reaches 70 ° C., 3.9 kg of the catalyst (CuO / Cr 2 O 4 ) is added thereto, and after the addition of the catalyst, the batch type The reaction system was completely sealed. After the catalyst is sufficiently dispersed in the reactant, the valve of the batch reaction system is opened and a pump is used to circulate the reactants of the batch reaction system to the stirred reactor and the diffusion reactor of the circulation reaction system, wherein the circulation The amount of reactant to be controlled was maintained at 10-15 L / min by flow meter valve. Nitrogen is pushed into the batch and circulating reaction system to circulate the dissolved reactants to remove oxygen remaining in each reactor and reactant, and then hydrogen is pushed into the nitrogen to make the inside of the batch and circulating reaction system into a hydrogen atmosphere. Was removed. After the reactor became a hydrogen atmosphere in this manner, the reactor temperature was set to 300 ° C., the reaction temperature, and then the hydrogen pressure in the batch and circulating reaction system was raised to 5 bar, and the hydrogen pressure in the batch and circulating reaction system. After reaching 5 bar, the hydrogen pressure in the circulating reaction system was raised to 14 bar. At 300 ° C., the hydrogen pressure in the reactor was maintained at 5 bar in the batch reaction system and 14 bar in the circulating reaction system. Hydrogenation reaction was performed.
반응 종료 후 순환형 반응 시스템 내부 반응물을 배치형 반응 시스템 내부로 배출(drain)하였다. 반응 후 생성된 생성물은 촉매와 혼합되어 있으며, 이 촉매의 분리를 위하여 생성물을 필터 베슬(도시 않음)로 이송하여 생성물과 촉매를 분리하였다. 이때, 배치형 반응 시스템 내부 생성물의 온도 및 필터 베슬 온도를 90℃로 유지하며 액체 상태로 필터 베슬로 이송하고 촉매분리 후, 필터 베슬에 얻어진 여과액에는 생성물인 프로필렌글리콜이 H2O에 용해되어진 상태로 존재한다. 이때 반응 종결시까지 걸리는 시간은 총 12시간이 소요되었다.After completion of the reaction, the reactants in the circulating reaction system were drained into the batch reaction system. The product produced after the reaction was mixed with the catalyst, and the product was transferred to a filter vessel (not shown) for separation of the catalyst to separate the product from the catalyst. At this time, the temperature of the product inside the batch reaction system and the filter vessel temperature is maintained at 90 ℃ and transferred to the filter vessel in a liquid state, after the catalyst separation, the propylene glycol product is dissolved in H 2 O in the filtrate obtained in the filter vessel. Exists in a state. At this time, the time required to complete the reaction was 12 hours in total.
<비교예 1> 프로필렌글리콜의 제조Comparative Example 1 Preparation of Propylene Glycol
종래 기술에 따른 배치형 반응시스템에 글리세롤(glycerol) 78.4kg과 H2O 19.6kg을 투입하고, 배치형 반응 시스템의 온도를 60℃로 설정한 후, 100rpm으로 교반시키며 반응물을 완전히 용해시켰다. 다음으로 반응물이 완전히 용해된 후 배치식 반응기의 온도를 70℃로 설정한 뒤, 70℃에 도달 시 촉매(CuO/Cr2O4)를 3.9kg을 투입하고, 촉매 투입 후 배치형 반응 시스템을 완전히 밀폐하였다. 상기 촉매를 반응물에 충분히 분산시킨 후, 배치형 반응 시스템 내부에 질소를 밀어 넣어 반응기 및 반응물에 잔존하는 산소를 제거하고, 배치형 반응 시스템 내부를 수소 분위기로 만들기 위해 수소를 밀어 넣어 질소를 제거하였다. 이렇게 하여 배치형 반응 시스템 내부가 수소 분위기가 된 후, 반응기 온도를 반응온도인 300℃로 설정한 뒤, 내부 수소 압력을 14bar로 올려주어 배치형 반응시스템을 14bar로 유지하며 교반속도 300rpm 조건하에 글리세롤의 수소화 반응을 진행하였다. 반응 후 생성된 생성물은 촉매와 혼합되어 있으며, 이 촉매의 분리를 위하여 생성물을 필터 베슬로 이송하여 생성물과 촉매를 분리하였다. 이때, 배치형 반응시스템 내부 생성물의 온도 및 필터 베슬 온도를 90℃로 유지하며 액체 상태로 필터 베슬로 이송한다. 그리고, 촉매분리 후, 필터 베슬에 얻어진 여과액에는 생성물인 프로필렌글리콜이 H2O에 용해되어진 상태로 존재한다. 이때 반응 종결시까지 걸리는 시간은 총 17시간이 소요되었다.78.4 kg of glycerol and 19.6 kg of H 2 O were added to a batch reaction system according to the prior art, and the temperature of the batch reaction system was set to 60 ° C., followed by stirring at 100 rpm to completely dissolve the reactants. Next, after completely dissolving the reactants, the temperature of the batch reactor was set to 70 ° C., and when the temperature reached 70 ° C., 3.9 kg of the catalyst (CuO / Cr 2 O 4 ) was added thereto. It was completely sealed. After the catalyst was sufficiently dispersed in the reactant, nitrogen was pushed into the batch reaction system to remove oxygen remaining in the reactor and reactants, and hydrogen was pushed to remove nitrogen to make the inside of the batch reaction system into a hydrogen atmosphere. . In this manner, after the inside of the batch reaction system became a hydrogen atmosphere, the reactor temperature was set to 300 ° C., the reaction temperature was raised, and the internal hydrogen pressure was raised to 14 bar to maintain the batch reaction system at 14 bar, and the glycerol was stirred under a stirring speed of 300 rpm. Hydrogenation reaction was carried out. The product produced after the reaction was mixed with the catalyst, and the product was transferred to a filter vessel to separate the catalyst and the product was separated from the catalyst. At this time, the temperature of the product inside the batch reaction system and the filter vessel temperature are maintained at 90 ° C. and transferred to the filter vessel in a liquid state. After the catalyst separation, propylene glycol as a product is present in a state where the product is dissolved in H 2 O in the filtrate obtained in the filter vessel. At this time, the time required to complete the reaction was 17 hours in total.
상기 실험예 1및 비교예 1에 따른 프로필렌글리콜의 합성 결과를 비교하여 하기 표 1에 나타내었다. The synthesis results of propylene glycol according to Experimental Example 1 and Comparative Example 1 are shown in Table 1 below.
표 1
전환율 선택도 수율 반응시간
실험예 1 80 % 88 % 70.4 % 12 시간
비교예 1 70 % 80 % 56 % 17 시간
Table 1
Conversion rate Selectivity yield Reaction time
Experimental Example 1 80% 88% 70.4% 12 hours
Comparative Example 1 70% 80% 56% 17 hours
상기 표 1에서 나타난 바와 같이, 글리세롤의 수소화반응에 의한 프로필렌글리콜의 합성시 본 발명에 다른 고효율 화학반응 방법 및 장치를 적용하는 경우, 기존 배치형 반응시스템에 순환형 반응시스템을 도입하여 순환반응을 추가시킴으로써, 압력 및 교반속도의 향상에 의하여 반응속도가 향상되고, 이에 따라 전환율 및 반응수율이 현저하게 향상됨을 나타내었고, 뿐만 아니라 선택도가 증가되어 불순물이 감소하여 고순도의 생성물을 얻을 수 있게 됨을 확인할 수 있었다. As shown in Table 1, in the case of applying another high-efficiency chemical reaction method and apparatus to the present invention when synthesizing propylene glycol by hydrogenation of glycerol, a circulating reaction is introduced by introducing a circulating reaction system into an existing batch reaction system. By the addition, the reaction rate is improved by the improvement of the pressure and the stirring speed, and thus, the conversion and the reaction yield are markedly improved, as well as the selectivity is increased, so that impurities can be reduced to obtain a high purity product. I could confirm it.
<실험예 2> 프로필렌 카보네이트의 제조Experimental Example 2 Preparation of Propylene Carbonate
본 발명의 바람직한 실시예에 따른 고효율 화학반응 장치의 배치형 반응 시스템에 플로필렌옥사이드(propylene oxide) 75kg을 투입하고, 배치형 반응 시스템의 온도를 110℃로 설정한 후, 300rpm으로 교반하였다. 상기 반응물을 교반하면서 촉매(ZnCl2)를 26.2kg을 투입하고, 촉매 투입 후 배치형 반응 시스템을 완전히 밀폐하였다. 상기 촉매를 반응물에 충분히 분산시킨 후, 배치형 반응 시스템의 밸브를 열어 펌프를 이용해 배치형 반응 시스템의 반응물을 순환형 반응 시스템의 교반형 반응기와 확산형 반응기로 순환시키고, 이때, 순환되는 반응물의 양을 유량계 밸브로 조절하여 10~15L/min으로 유지하였다. 상기 용해된 반응물을 순환시키면서 배치형 및 순환형 반응 시스템 내부에 질소를 밀어 넣어 각 반응기 및 반응물에 잔존하는 산소를 제거하고, 배치형 및 순환형 반응 시스템 내부를 CO2 분위기로 만들기 위해 CO2를 밀어 넣어 질소를 제거하였다. 이렇게하여 반응기 내부가 CO2 분위기가 된 후, 반응기 온도를 유지하면서, 배치형 및 순환형 반응 시스템 내부 CO2 압력을 5bar로 올려주어, 배치형 및 순환형 반응 시스템 내부 CO2 압력이 5bar에 도달한 뒤, 순환형 반응 시스템 내부의 수소 압력을 15bar로 올려주었다. 110℃에서 반응기 내부 수소 압력을 배치형 반응 시스템 5bar, 순환형 반응 시스템 15bar로 유지하며 교반속도 300rpm 조건하에 프로필렌옥사이의 CO2 첨가반응을 진행하였으며, 반응 종료 후 순환형 반응 시스템 내부 반응물을 배치형 반응 시스템 내부로 배출(drain)하였다. 반응 후 생성된 생성물은 촉매와 혼합되어 있으며, 이 촉매의 분리를 통하여 최종 생성물인 플로필렌 카보네이트(propylene carbonate)를 수득하였다. 이때 반응 종결시까지 걸리는 시간은 총 3시간이 소요되었다.75 kg of propylene oxide was added to a batch reaction system of a high-efficiency chemical reaction apparatus according to a preferred embodiment of the present invention, and the temperature of the batch reaction system was set to 110 ° C., followed by stirring at 300 rpm. While stirring the reaction, 26.2 kg of the catalyst (ZnCl 2 ) was added, and after the catalyst was added, the batch reaction system was completely sealed. After the catalyst is sufficiently dispersed in the reactant, the valve of the batch reaction system is opened and a pump is used to circulate the reactants of the batch reaction system into the stirred reactor and the diffusion reactor of the circulating reaction system, wherein The amount was controlled by a flow meter valve to maintain 10-15 L / min. Wherein while melting the circulation and the reaction of CO 2 to make the inside of batch type and circulation type reaction system into the internal slide nitrogen to remove the oxygen remaining in each reactor and the reaction product, batch type and circulation type reaction system with CO 2 atmosphere Push to remove nitrogen. In this manner inside the reactor is given up to, batch type and circulation type reaction system inside the CO 2 pressure while maintaining the reactor temperature after the CO 2 atmosphere at 5bar, batch type and circulation type reaction system inside the CO 2 pressure is reached 5bar Afterwards, the hydrogen pressure inside the circulating reaction system was raised to 15 bar. The hydrogen pressure inside the reactor was maintained at 5 bar in a reactor and 15 bar in a circulating reaction system at 110 ° C., and CO 2 addition reaction between propylene ox was carried out under a stirring speed of 300 rpm. Drained into the reaction system. The product produced after the reaction was mixed with the catalyst, and the catalyst was separated to obtain propylene carbonate, the final product. At this time, the time required to complete the reaction was 3 hours in total.
<비교예 1> 프로필렌 카보네이트의 제조Comparative Example 1 Preparation of Propylene Carbonate
종래 기술에 따른 배치형 반응시스템에 프로필렌 옥사이드(propylene oxide) 75kg을 투입하고, 배치형 반응시스템의 온도를 110℃로 설정한 후, 300rpm으로 교반하였다. 반응물을 교반하면서 촉매(ZnCl2)를 26.2kg을 투입하고, 상기 촉매 투입 후 반응기를 완전히 밀폐하였다. 상기 촉매를 반응물에 충분히 분산시킨 후, 반응기 내부에 질소를 밀어 넣어 반응기 및 반응물에 잔존하는 산소를 제거하였다. 그리고 반응기 내부를 CO2 분위기로 만들기 위해 CO2를 밀어 넣어 질소를 제거하여 반응기 내부가 CO2 분위기가 된 후, 반응기 온도를 유지하면서, 반응기 내부 CO2 압력을 15bar로 올려주었다. 이와 같이 110℃에서 반응기 내부 수소 압력을 15bar로 유지하며 교반속도 300rpm 조건하에 프로필렌 옥사이드의 CO2 첨가반응을 진행하였으며, 반응 종료 후 생성된 생성물은 촉매와 혼합되어 있으며, 이 촉매의 분리를 통하여 최종 생성물인 프로필렌 카보네이트를 수득하였다. 이때 반응 종결시까지 걸리는 시간은 총 6시간이 소요되었다.75 kg of propylene oxide was added to the batch reaction system according to the prior art, and the temperature of the batch reaction system was set to 110 ° C., followed by stirring at 300 rpm. While stirring the reaction, 26.2 kg of the catalyst (ZnCl 2) was added, and the reactor was completely sealed after the addition of the catalyst. After the catalyst was sufficiently dispersed in the reactant, nitrogen was pushed into the reactor to remove oxygen remaining in the reactor and the reactant. In addition, to make the inside of the reactor into a CO 2 atmosphere, CO 2 was pushed in to remove nitrogen to make the inside of the reactor become a CO 2 atmosphere, and while maintaining the reactor temperature, the CO 2 pressure inside the reactor was raised to 15 bar. As such, the hydrogen pressure inside the reactor was maintained at 15 bar at 110 ° C., and CO 2 addition reaction of propylene oxide was carried out under a stirring speed of 300 rpm. After the reaction was completed, the resulting product was mixed with the catalyst. The product propylene carbonate was obtained. At this time, the time required to complete the reaction was 6 hours in total.
상기 실험예 2및 비교예 2에 따른 프로필렌 카보네이트의 합성 결과를 비교하여 하기 표 2에 나타내었다.The synthesis results of propylene carbonates according to Experimental Example 2 and Comparative Example 2 are shown in Table 2 below.
표 2
수율 순도 반응시간
실험예 2 80 % 95 % 3 시간
비교예 2 70 % 87 % 6 시간
TABLE 2
yield water Reaction time
Experimental Example 2 80% 95% 3 hours
Comparative Example 2 70% 87% 6 hours
상기 표 2에서 나타난 바와 같이, 프로필렌 옥사이드의 이산화탄소 첨가반응에 의한 프로필렌 카보네이트의 합성에 있어서, 본 발명에 다른 고효율 화학반응 방법 및 장치를 적용하는 경우, 기존 배치형 반응시스템에 순환형 반응시스템을 도입하여 순환반응을 추가시킴으로써, 반응수율 및 반응속도가 현저하게 향상됨을 나타내었는 바, 특히 반응속도가 2배로 향상됨을 확인할 수 있었다. 뿐만 아니라 선택도가 증가되어 불순물이 감소하여 고순도의 생성물을 얻을 수 있게 됨을 확인할 수 있었다. As shown in Table 2, in the synthesis of propylene carbonate by the carbon dioxide addition reaction of propylene oxide, when another high efficiency chemical reaction method and apparatus is applied to the present invention, a cyclic reaction system is introduced into an existing batch reaction system. By adding a cyclic reaction, the reaction yield and the reaction rate were markedly improved, and in particular, the reaction rate was confirmed to be improved by 2 times. In addition, it was confirmed that the selectivity was increased to reduce impurities, thereby obtaining a high purity product.
<실험예 3> 1-니트로-2-부탄올의 제조Experimental Example 3 Preparation of 1-nitro-2-butanol
먼저, 본 발명의 바람직한 실시예에 따른 고효율 화학반응 장치의 배치형 반응 시스템에 니트로메탄(nitromethane) 71.7kg과 프로피온알데히드(propionaldehyde) 3.3kg을 투입하고, 배치형 반응 시스템의 온도를 25℃로 설정한 후, 100rpm으로 교반시키며 반응물을 완전히 섞은 다음, 반응물을 교반하면서 촉매(chloroaluminate ionic liquid)를 11.3kg을 투입하였다. 상기 촉매 투입 후 배치형 반응 시스템을 완전히 밀폐하고 촉매를 반응물에 충분히 분산시킨 다음, 배치형 반응 시스템의 밸브를 열어 펌프를 이용해 배치형 반응 시스템의 반응물을 순환형 반응 시스템의 교반형 반응기와 확산형 반응기로 순환시켰다. 이때, 순환되는 반응물의 양을 유량계 밸브로 조절하여 10~15L/min으로 유지하였다. 상기 용해된 반응물을 순환시키면서 배치형 및 순환형 반응 시스템 내부에 질소를 밀어 넣어 각 반응기 및 반응물에 잔존하는 산소를 제거한 후 상압 상태에서 반응을 진행하였다. 반응 종료 후 순환형 반응 시스템 내부 반응물을 배치형 반응 시스템 내부로 배출(drain)하였다. 반응 후 생성된 생성물은 1-니트로-2-부탄올(1-nitro-2-butanol)이며 이를 분리하기 위하여 물과 에틸 아세테이트(ethyl acetate)를 이용하여 상분리하여 에틸 아세테이트 층 위에서 순수한 1-니트로-2-부탄올을 얻었다. 이때 반응 종결시까지 걸리는 시간은 총 11시간이 소요되었다.First, 71.7 kg of nitromethane and 3.3 kg of propionaldehyde are added to a batch reaction system of a high-efficiency chemical reaction device according to a preferred embodiment of the present invention, and the temperature of the batch reaction system is set to 25 ° C. After stirring, the reaction mixture was thoroughly mixed with 100 rpm, and 11.3 kg of a catalyst (chloroaluminate ionic liquid) was added while stirring the reaction mixture. After the catalyst is added, the batch reaction system is completely sealed and the catalyst is sufficiently dispersed in the reactant, and then the valves of the batch reaction system are opened to pump the reactants of the batch reaction system using a pump. Circulated to the reactor. At this time, the amount of reactant circulated was controlled by a flow meter valve and maintained at 10-15 L / min. Nitrogen was pushed into the batch and circulating reaction systems while circulating the dissolved reactants to remove oxygen remaining in each reactor and reactants, and then the reaction was performed at atmospheric pressure. After completion of the reaction, the reactants in the circulating reaction system were drained into the batch reaction system. The product produced after the reaction was 1-nitro-2-butanol, and phase-separated with water and ethyl acetate to separate it, and purified pure 1-nitro-2 on the ethyl acetate layer. Butanol was obtained. At this time, the time required to complete the reaction was 11 hours in total.
<비교예 3> 1-니트로-2-부탄올의 제조Comparative Example 3 Preparation of 1-nitro-2-butanol
종래기술에 따른 배치형 반응시스템 니트로메탄 71.7kg과 프로피온알데히드 3.3kg을 투입하고, 배치형 반응시스템의 온도를 25℃로 설정한 후, 100rpm으로 교반시키며 반응물을 완전히 섞은 다음, 반응물을 교반하면서 촉매(chloroaluminate ionic liquid)를 11.3kg을 투입하였다. 상기 촉매 투입 후 배치형 반응 시스템을 완전히 밀폐하고 촉매를 반응물에 충분히 분산시킨 다음, 배치형 반응 시스템 내부에 질소를 밀어 넣어 각 반응기 및 반응물에 잔존하는 산소를 제거한 후 상압 상태에서 반응을 진행하였다. 반응 후 생성된 생성물은 1-니트로-2-부탄올이며 이를 분리하기 위하여 물과 에틸 아세테이트를 이용하여 상분리하여 에틸 아세테이트 층 위에서 순수한 1-니트로-2-부탄올을 수득하였다. 이때 반응 종결시까지 걸리는 시간은 총 16시간이 소요되었다.71.7 kg of the batch reaction system nitromethane and 3.3 kg of propionaldehyde according to the prior art were added, and the temperature of the batch reaction system was set to 25 ° C., followed by stirring at 100 rpm to completely mix the reactants, followed by stirring the catalyst while stirring the reactants. 11.3 kg of (chloroaluminate ionic liquid) was added. After the catalyst was added, the batch reaction system was completely enclosed and the catalyst was sufficiently dispersed in the reactant, and nitrogen was pushed into the batch reaction system to remove oxygen remaining in each reactor and the reactants, and the reaction was performed at atmospheric pressure. The product produced after the reaction was 1-nitro-2-butanol, and to separate it, phase separation was performed using water and ethyl acetate to obtain pure 1-nitro-2-butanol on an ethyl acetate layer. At this time, the time required to complete the reaction was 16 hours in total.
상기 실험예 3 및 비교예 3에 따른 1-니트로-2-부탄올의 합성 결과를 비교하여 하기 표 3에 나타내었다.The synthesis results of 1-nitro-2-butanol according to Experimental Example 3 and Comparative Example 3 are shown in Table 3 below.
표 3
수율 순도 반응시간
실험예 3 78 % 90 % 11 시간
비교예 3 69 % 81 % 16 시간
TABLE 3
yield water Reaction time
Experimental Example 3 78% 90% 11 hours
Comparative Example 3 69% 81% 16 hours
상기 표 3에서 나타난 바와 같이, 니트로메탄과 프로피온알데히드를 반응시켜 1-니트로-2-부탄올을 합성하는 액체-액체 반응에 있어서, 본 발명에 다른 고효율 화학반응 방법 및 장치를 적용하는 경우, 기존 배치형 반응시스템에 순환형 반응시스템을 도입하여 순환반응을 추가시킴으로써, 반응수율 및 반응속도가 현저하게 향상되는 것으로 나타났고, 뿐만 아니라 선택도가 증가되어 불순물이 감소하여 보다 고순도의 생성물을 얻을 수 있게 됨을 확인할 수 있었다. As shown in Table 3, in the liquid-liquid reaction of synthesizing 1-nitro-2-butanol by reacting nitromethane with propionaldehyde, when another high efficiency chemical reaction method and apparatus are applied to the present invention, the existing batch By introducing a circulating reaction system by adding a circulating reaction system to the type reaction system, the reaction yield and the reaction rate were found to be remarkably improved, as well as the selectivity was increased, so that impurities were reduced to obtain a higher purity product. It could be confirmed.
이와 같이, 본 발명에 따른 고효율 화학반응 방법 및 장치는 배치형 반응 시스템(12)을 통해 반응공정이 이루어지도록 하는 반응물을 순환형 반응 시스템(13)으로 순환시켜 추가적인 반응공정이 이루어지도록 함으로써, 반응 속도의 증가로 불순물의 형성을 감소시키면서 생산성을 현저하게 향상시킬 수 있게 된다. As described above, the method and apparatus for high-efficiency chemical reaction according to the present invention circulates the reactants for the reaction process through the batch reaction system 12 to the circulation type reaction system 13 so that an additional reaction process is performed. Increasing the rate can significantly improve productivity while reducing the formation of impurities.
뿐만 아니라, 본 발명에 따른 고효율 화학반응 방법 및 장치는 배치형 반응 시스템(12)을 통해 반응공정이 이루어지도록 하는 반응물을 순환형 반응 시스템(13)으로 순환시켜 추가적인 반응공정이 이루어지도록 함으로써, 반응 속도의 증가로 불순물의 형성을 감소시키면서 생산성을 향상시키고, 부가적인 유틸리티가 불필요하여 유지비용을 절감시키며, 처리효율을 높이면서도 반응설비의 규모를 작게 가져갈 수 있어 공간적 제약을 덜 받으면서 설치가 용이하도록 한다. 물론, 종래 배치식 반응 방법 및 반응기를 이용하여도 본 발명에 따른 고효율 화학반응 방법 및 장치와 동일한 효과를 볼 수 있으나, 종래 배치식 반응 방법 및 반응기로 본 발명에 따른 고효율 화학반응 방법 및 장치와 동일한 효율을 보기 위하여 부가되어져야 하는 설비의 비용과 공정비용이 높아지게 되는 것이다. In addition, the high-efficiency chemical reaction method and apparatus according to the present invention by circulating the reactant to the reaction process through the batch reaction system 12 to the circulating reaction system 13 to make an additional reaction process, reaction Increased speed improves productivity while reducing the formation of impurities, reduces maintenance costs by eliminating the need for additional utilities, and reduces the size of the reaction facility while improving processing efficiency, making it easier to install with less space constraints. do. Of course, using the conventional batch reaction method and reactor can see the same effect as the high efficiency chemical reaction method and apparatus according to the present invention, but with the high efficiency chemical reaction method and apparatus according to the present invention with the conventional batch reaction method and reactor In order to see the same efficiency, the cost of the equipment and the process cost to be added will be increased.
좀 더 구체적으로 보면, 반응 조건이 10bar일 경우, 종래기술은 배치식 반응기를 10bar로 설계하여야 하는 반면, 본 발명은 배치형 반응 시스템(12)의 반응기{일반적인 배치식 반응기와 대응}를 5bar로 설계를 하고, 순환형 반응 시스템(13)의 연속식 반응기(14) {즉, 교반형 반응기(40)와 확산형 반응기(50)}를 10bar로 설계를 하면 배치형 반응 시스템(12)의 반응기에 대하여 반응기에 소요되는 자재 및 설계 단가가 낮아지는 것이다. 즉, 배치형 반응 시스템(12)의 반응기를 전체 허용압력이 높은 압력으로 제작하는 것과, 배치형 반응 시스템(12)의 반응기는 낮은 압력으로 제작하고, 순환형 반응 시스템(13)의 연속식 반응기(14)만 높은 압력으로 제작하면 제작 단가면에서 많은 이점이 있는 것이다. More specifically, when the reaction conditions are 10 bar, the prior art should design a batch reactor of 10 bar, while the present invention is 5 bar to the reactor (corresponding to the general batch reactor) of the batch reaction system 12 After designing and designing the continuous reactor 14 (ie, stirred reactor 40 and diffusion reactor 50) of the circulating reaction system 13 to 10 bar, the reactor of the batch reaction system 12 is designed. The material and design costs for the reactor will be lowered. In other words, the reactor of the batch reaction system 12 is manufactured at a high allowable pressure, and the reactor of the batch reaction system 12 is manufactured at a low pressure, and the continuous reactor of the circulating reaction system 13 is manufactured. Producing only 14 at high pressure has many advantages in terms of manufacturing cost.
또한, 일반적으로 화학반응에서 반응성 향상의 핵심은 혼합되어지는 반응물의 접촉효율의 극대화로부터 오는 향상으로 볼 수 있는데, 이는 반응기의 교반속도를 향상시킴으로서 개선할 수 있다. 종래기술에 따른 배치식 반응기의 경우, 현재 산업적으로 적용할 수 있는 교반 속도는 최대 300rpm 정도로서, 300rpm보다 높게 가져갈 수 있으나, 그에 따른 제작비가 많이 상승하게 된다. 이에 반해 본 발명에 따른 고효율 화학반응 장치(10)는 배치형 반응 시스템(12)의 반응기를 300rpm으로 하고, 순환형 반응 시스템(13)의 연속식 반응기(14)로 순환을 시키면서 반응공정을 진행시키면 종래 배치식 반응기의 교반속도보다 훨씬 더 좋은 효과를 볼 수 있는 것이다. Also, in general, the key to improving the reactivity in the chemical reaction can be seen as an improvement that comes from maximizing the contact efficiency of the reactants to be mixed, which can be improved by improving the stirring speed of the reactor. In the case of a batch reactor according to the prior art, the current industrially applicable stirring speed is up to about 300rpm, but may be higher than 300rpm, but the production cost increases accordingly. On the contrary, the high-efficiency chemical reaction device 10 according to the present invention sets the reactor of the batch type reaction system 12 to 300 rpm and proceeds the reaction process while circulating to the continuous reactor 14 of the circulating type reaction system 13. The effect is much better than the stirring speed of the conventional batch reactor.
또한, 생산량이 10,000ton/yr 이라고 한다면, 종래 배치식 반응기는 10톤짜리 반응기 3대를 이용하여 하루에 1 ~ 1.5 batch를 생산하여야 하지만, 본 발명에 따른 고효율 화학반응 방법 및 장치를 이용하면 반응속도가 상승하기 때문에 10톤짜리 반응기 2대를 이용하여 하루에 2.5 ~ 3 batch를 생산하면 된다. 그러면 초기 설비 투자비용에 대하여 반응기 1대분만큼 제작비용을 절약할 수 있으며, 가동 중에도 반응기 1대분의 공정 운전 비용을 절약할 수 있는 것이다. 그리고, 전처리 장비 및 후처리 장비도 반응기 대수에 맞는 전처리 장비 및 후처리 장비를 구비하면 됨으로 전체적인 공정비용을 절약할 수 있어 최종 제품에 대한 가격 경쟁력의 우위를 점할 수 있는 것이다. In addition, if the production amount is 10,000ton / yr, the conventional batch reactor should produce 1 to 1.5 batches per day using three 10-ton reactors, but using the high-efficiency chemical reaction method and apparatus according to the present invention As the speed increases, 2.5 to 3 batches can be produced per day using two 10-ton reactors. Then, the production cost can be saved by one reactor for the initial equipment investment cost, and the operation cost of one reactor can be saved even during operation. In addition, the pretreatment equipment and the aftertreatment equipment may also be equipped with pretreatment equipment and post-treatment equipment suitable for the number of reactors, thereby reducing the overall process cost, and thus can obtain an advantage in price competitiveness for the final product.
또한, 본 발명에 따른 고효율 화학반응 장치(10)는 부가 유틸리티가 불필요하여 유지비용을 절감할 수 있다. 이때, 부가 유틸리티는 반응 장치를 운용하는데 있어 필요한 부수적인 장치를 지칭한다. 예컨대, 반응 조건을 유지하기 위하여, 대표적인 부가 유틸리티인 가열 및 냉각 시스템(Heat & Cooling system)이 있는데, 본 발명에 따른 고효율 화학반응 장치(10)의 경우 배치형 반응 시스템(12)의 반응기에 가열 및 냉각 시스템이 이루어져 있으므로, 순환형 반응 시스템(13)에 가열 및 냉각 시스템을 설치하지 않아도 되고, 순환형 반응 시스템(13)의 용량을 고려하여 액의 유속을 결정할수 있으므로 순환형 반응 시스템(13)에서는 따로 반응 조건을 조절할 수 있는 부가 유틸리티가 필요가 없다. 예컨대, 본 발명의 바람직한 실시예에 따른 고효율 화학반응 장치(10)의 실험결과 연속식 반응기(14)로 유입되는 액의 온도와 연속식 반응기(14)에서 나오는 부분의 액의 온도 편차가 없었다. In addition, the high-efficiency chemical reaction device 10 according to the present invention can reduce the maintenance cost because no additional utility. At this point, the additional utility refers to the additional equipment required for operating the reaction equipment. For example, in order to maintain the reaction conditions, there is a typical addition utility heating and cooling system (Heat & Cooling system), in the case of the high-efficiency chemical reaction device 10 according to the present invention is heated in the reactor of the batch reaction system 12 And a cooling system, it is not necessary to install a heating and cooling system in the circulating reaction system 13, and the flow rate of the liquid can be determined in consideration of the capacity of the circulating reaction system 13, so that the circulating reaction system 13 ) Eliminates the need for additional utilities to control reaction conditions. For example, as a result of the experiment of the high-efficiency chemical reaction device 10 according to the preferred embodiment of the present invention, there was no temperature difference between the temperature of the liquid flowing into the continuous reactor 14 and the portion of the liquid exiting the continuous reactor 14.
상술한 바와 같은, 본 발명의 바람직한 실시예에 따른 고효율 화학반응 방법및 장치를 상기한 설명 및 도면에 따라 도시하였지만, 이는 예를 들어 설명한 것에 불과하며 본 발명의 기술적 사상을 벗어나지 않는 범위 내에서 다양한 변화 및 변경가능하다는 것을 이 분야의 통상적인 기술자들은 잘 이해할 수 있을 것이다.As described above, the high-efficiency chemical reaction method and apparatus according to the preferred embodiment of the present invention are shown in accordance with the above description and drawings, but these are merely described for example and various within the scope without departing from the technical spirit of the present invention. It will be appreciated by those skilled in the art that changes and variations are possible.
도 1은 본 발명의 기술 사상에 따른 고효율 화학반응 방법 및 장치를 설명하기 위한 도면이다. 1 is a view for explaining a high efficiency chemical reaction method and apparatus according to the technical idea of the present invention.
도 1을 참조하면, 본 발명에 따른 고효율 화학반응 장치(10)는 배치형 반응 시스템(12)에 수용되는 반응물이 순환할 수 있도록 하는 순환형 반응 시스템(13)이 배치형 반응 시스템(12)과 폐회로를 형성하도록 설치되어 이루어진다. 여기서, 배치형 반응 시스템(12)은 반응물을 넣고 반응공정이 완료될 때까지 공정이 계속 진행되도록 하고, 반응공정이 완료된 생성물을 한꺼번에 배출시키도록 구성된다. 그리고, 순환형 반응 시스템(13)은 배치형 반응 시스템(12)과 폐회로를 형성하도록 설치되어 배치형 반응 시스템(12)에 수용되어 반응공정이 진행되는 반응물을 순환시키면서 반응공정이 이루어지도록 한다. Referring to FIG. 1, the high-efficiency chemical reaction device 10 according to the present invention includes a batch reaction system 12 that includes a circulating reaction system 13 for allowing a reactant contained in the batch reaction system 12 to circulate. And is formed to form a closed circuit. Here, the batch reaction system 12 is configured to contain the reactants and to allow the process to continue until the reaction process is completed, and to discharge the finished products at once. In addition, the circulation type reaction system 13 is installed to form a closed circuit with the batch type reaction system 12 so as to be accommodated in the batch type reaction system 12 to circulate the reactants through which the reaction process proceeds.
이때, 폐회로의 형성은 필요한 길이로 연장되어 배치형 반응 시스템(12)에 양단이 연결됨으로써 배치형 반응 시스템(12)으로부터 반응물이 유출되고 다시 유입되도록 하는 연결 라인(15)상에 연속식 반응기(14)를 설치하여 이루어질 수 있다. 물론, 이와 같은 연결 라인(15)은 순환형 반응 시스템(13)의 필요에 따라 다양한 경로와 길이로 설치될 수 있을 것이고, 액-액 화학반응, 기-액 화학반응 등 다양한 종류의 반응물을 순환시키고, 흐름을 제어하기 위한 다양한 밸브류, 계측기류, 센서류, 안전장치류 등이 설치될 것이다. At this time, the formation of the closed circuit extends to the required length so that both ends are connected to the batch reaction system 12 so that the reactant flows out from the batch reaction system 12 and flows back into the continuous line on the connecting line 15. 14) can be achieved by installing. Of course, such a connection line 15 may be installed in various paths and lengths according to the needs of the circulating reaction system 13, and circulates various kinds of reactants such as liquid-liquid chemical reactions and gas-liquid chemical reactions. And various valves, measuring instruments, sensors, safety devices, etc. will be installed to control the flow.
또한, 본 발명에 따른 고효율 화학반응 장치(10)는 일반적인 화학반응 장치와 같이 컨트롤러(제어부)를 통해 제어되도록 구성될 것이다. 특히, 반응 장치의 조작에 필요한 모든 사항에 대하여 한 곳에서 모두 모니터링하고 제어할 수 있도록 중앙제어하는 컨트롤러가 적용될 수 있을 것이다. 예컨대, 원료투입에 대한 밸브 on/off, 배치형 반응 시스템(12) 및 순환형 반응 시스템(13)에 대한 압력 조절, 순환형 반응 시스템(13)으로 반응물을 옮기기 위한 펌프(30; 도 5 및 도 6 참조)의 조절, 반응물이 순환되는데 있어서 유속의 조절, 배치형 반응 시스템(12) 및 순환형 반응 시스템(13)에서 수소 주입(도 6 참조)에 대한 on/off, 액레벨 조절기(34; 도 5 및 도 6 참조)의 액레벨 조절, 가스 방출(vent)에 대한 밸브 on/off 등에 대한 제어를 한 곳에서 모두 할 수 있도록 제어부를 구성하는 것이다. 이와 같은 제어부는 안전을 위해 일정 이상 압력이 되면 자동으로 가스 방출(gas vent) 밸브가 열림되도록 최대 압력치를 설정할 수 있고, 반응조건 설정을 위해 교반속도, 반응온도 설정 등을 할 수 있도록 한다.In addition, the high-efficiency chemical reaction device 10 according to the present invention will be configured to be controlled through a controller (control unit) like a general chemical reaction device. In particular, a centralized controller may be applied to monitor and control all the necessary things for the operation of the reaction apparatus in one place. For example, valve on / off for feed dosing, pressure regulation for batch reaction system 12 and circulating reaction system 13, pump 30 for transferring reactants to circulating reaction system 13 (FIG. 5 and FIG. 6), on / off of hydrogen injection (see FIG. 6) in the batch reaction system 12 and in the circulating reaction system 13, liquid level regulator 34. 5 and 6), the control unit is configured to control the liquid level control, the valve on / off for the gas vent, and the like in one place. Such a control unit may set the maximum pressure value so that the gas vent valve is automatically opened when the pressure exceeds a predetermined value for safety, and to set the stirring speed, reaction temperature, etc. to set the reaction conditions.
본 발명에서 배치형 반응 시스템(12)은 반응물을 넣고 반응공정이 완료될 때까지 공정이 계속 진행되도록 하고, 반응공정이 완료된 생성물을 한꺼번에 배출시키도록 구성된다. 순환형 반응 시스템(13)은 배치형 반응 시스템(12)과 폐회로를 형성하도록 설치되고, 배치형 반응 시스템(12)에 수용되어 반응공정이 진행되는 반응물을 순환시키면서 반응공정이 이루어지도록 한다. 즉, 순환형 반응 시스템(13)은 독립적으로 보았을 때, 계속해서 원료를 공급하고, 제품을 끌어내는 방식인 일반적인 연속식 반응기와 같은 개념을 갖는다. In the present invention, the batch reaction system 12 is configured to add a reactant and to continue the process until the reaction process is completed, and to discharge the finished products at once. The circulating reaction system 13 is installed to form a closed circuit with the batch reaction system 12, and is accommodated in the batch reaction system 12 to circulate the reactants through which the reaction process proceeds. In other words, the circulating reaction system 13 has a concept similar to that of a general continuous reactor, which is a method of continuously supplying raw materials and extracting products when viewed independently.
본 발명에 따른 고효율 화학반응 방법은 배치형 반응 시스템(12)에 반응물을 넣고, 생성물을 얻기 위한 반응공정을 진행하는 배치 반응공정 단계(①)와, 배치형 반응 시스템(12)과 폐회로를 형성하도록 설치되는 순환형 반응 시스템(13)에 배치형 반응 시스템(12)내에서 배치 반응공정이 진행되는 반응물을 순환시키면서 반응공정이 이루어지도록 하는 순환 반응공정 단계(②) 및, 생성물이 형성되었을 때 순환형 반응 시스템(13)로의 순환을 정지하고, 상기 배치형 반응 시스템(12)내의 생성물을 외부로 배출시키는 단계(③)를 구비하여 이루어진다. In the high-efficiency chemical reaction method according to the present invention, the reactant is placed in a batch reaction system 12, and a batch reaction step (①) of proceeding with a reaction process for obtaining a product, and a batch reaction system 12 and a closed circuit are formed. Circulating reaction process step (②) to circulate the reactants undergoing the batch reaction process in the batch reaction system 12 to the circulating reaction system 13 installed so as to perform the reaction process, and when the product is formed. Stopping circulation to the circulation reaction system 13 and discharging the product in the batch reaction system 12 to the outside.
이와 같은 본 발명에 따른 고효율 화학반응 방법은 액-액 반응은 물론, 본 발명의 바람직한 실시예와 같이 (기체; 특히, 수소) 첨가반응을 진행할 수 있도록 구성되고, 순환형 반응 시스템(13)에서 연속식 반응기(14)를 연결 라인(15)상에 순차적으로 다단으로 설치하여 다양한 순환 반응공정을 통해 반응 속도를 증가시켜 생산성을 향상시킬 수 있도록 한다. Such a high-efficiency chemical reaction method according to the present invention is configured to allow the addition of liquid-liquid reaction, as well as (gas; in particular, hydrogen) addition reaction as in the preferred embodiment of the present invention, and in the cyclic reaction system 13 The continuous reactor 14 is installed in multiple stages sequentially on the connection line 15 to increase the reaction rate through various circulation reaction processes to improve productivity.
한편, 본 발명에 따른 고효율 화학반응 장치(10)에서 순환형 반응 시스템(13)의 연속식 반응기(14)는 반응물을 스트림(stream) 상태로 반응공정을 진행할 수 있도록 하는 반응기로서, 다양한 형태가 적용될 수 있다. 예컨대, 본 발명의 바람직한 실시예에서 순환형 반응 시스템(13)의 연속식 반응기(14)에는 교반형 분산 반응기(40; 도 2 내지 도 4, 도 6 참조)와 타워형 분산 반응기(50; 도 2 내지 도 4, 도 6 참조)가 적용되는 예를 보이고 있는데, 본 발명의 고효율 화학반응 장치(10)의 순환형 반응 시스템(13)에는 반응물을 흐르도록 함으로써 반응물의 연속적인 스트림상태에서 반응공정이 진행되도록 하는 다양한 반응기가 적용될 수 있을 것이다. On the other hand, the continuous reactor 14 of the circulating reaction system 13 in the high-efficiency chemical reaction device 10 according to the present invention as a reactor to proceed the reaction process in the stream (stream), various forms are Can be applied. For example, in the preferred embodiment of the present invention, the continuous reactor 14 of the circulating reaction system 13 includes a stirred dispersion reactor 40 (see FIGS. 2 to 4 and 6) and a tower dispersion reactor 50 (FIG. 2). 4 to 6), the cyclic reaction system 13 of the high-efficiency chemical reaction device 10 of the present invention allows the reaction to flow in a continuous stream of reactants. Various reactors may be applied to allow the process to proceed.
여기서, 교반형 반응기(40)는 유체가 흐르는 관의 내부에 설치되어 액의 흐름에 방해를 주지 않으면서 액의 교반 효율을 높여주는 반응기로서, 반응물이 통과하며 반응물 사이의 접촉 효율을 높이고, 고속 교반을 통해 반응이 원활하게 일어나게 한다. 이와 같은 교반형 반응기(40)의 대표적인 구조는 관의 내부가 나선형(스크류형) 구조로 되어있고, 반응액이 나선형을 통과하면서 반응물이 섞이는 형태를 갖는데, 나선형은 액이 통과할 수 있는 폭 및 나선의 회전수에 따라 교반속도가 변하게 된다. 따라서, 본 발명에 따른 교반형 반응기(40)는 유체의 흐름에 방해를 주지 않으면서 반응액의 교반을 원활하게 하는 다양한 종류의 반응기가 적용될 수 있는 것이다. Here, the stirred reactor 40 is installed inside the pipe through which the fluid flows, and does not interfere with the flow of the liquid to increase the stirring efficiency of the liquid, the reactants pass through the reaction efficiency between the reactants, high speed, Stirring causes the reaction to occur smoothly. Representative structure of the stirred reactor 40 is a spiral (screw-type) structure of the inside of the tube, the reaction liquid has a form that the reactants are mixed while passing through the spiral, the spiral is the width that the liquid can pass and The stirring speed changes according to the rotation speed of the spiral. Therefore, the stirred reactor 40 according to the present invention can be applied to various kinds of reactors to smoothly stir the reaction liquid without disturbing the flow of the fluid.
또한, 확산형 반응기(50)는 충진물(Packing)과 같은 내부 구성(Column Internals)을 통해 순환되는 반응물의 머무름 시간(retention time)을 증가시키며, 액상의 반응물의 표면적을 확장시켜 반응물 분포를 용이하게 하고, 반응물 사이의 접촉면적을 넓혀 반응이 원활하게 일어날 수 있게 한다. 이와 같은 확산형 반응기(50)의 내부에는 액상 반응물의 액적을 늘릴 수 있는 액분산장치, 표면적 확장을 위한 장치, 머무름 시간(retention time)을 증가시킬 수 있는 장치 등을 포함하여 구성된다. In addition, the diffusion reactor 50 increases the retention time of the reactants circulated through the column internals such as packing, and expands the surface area of the reactants in the liquid phase to facilitate reactant distribution. In addition, the contact area between the reactants is increased to allow the reaction to occur smoothly. Inside the diffusion type reactor 50 is configured to include a liquid dispersing device that can increase the liquid droplets of the liquid reactant, a device for expanding the surface area, a device that can increase the retention time.
본 발명에 의한 고효율 화학반응 방법 및 장치에 따르면, 배치형 반응 시스템(12)과 순환형 반응 시스템(13)을 조합하여 다양한 종류의 화학반응을 수행할 수 있도록 하고, 기존 배치식 반응기에 비해 반응 속도를 증가시킬 수 있어 용이하게 생산성을 향상시킬 수 있다. 특히, 기본적으로 배치식 반응기를 적용하는 배치형 반응 시스템(12)에 연속식 반응기(14)를 적용하는 순환형 반응 시스템(13)을 설치하여 이루어지므로, 기존 화학반응설비의 활용이 가능하고, 부가 유틸리티가 불필요하여 유지비용을 절감할 수 있으며, 반응속도의 상승으로 불순물의 형성이 감소된다. 또한, 순환형 반응 시스템(13)에서 연속 반응기(14)의 다단 설계가 가능하므로 반응 속도의 증대가 용이하여 서로 다른 액체를 반응시키거나 반응물에 수소 등의 기체를 첨가하여 생성물을 얻는 다양한 화학반응에 용이하게 적용할 수 있고, 반응 속도의 증가로 생산성이 향상되므로 전체적인 화학 반응장치(10)의 구성을 소규모로 하여 공간 제약을 줄이면서 설치가 간단해진다. According to the high-efficiency chemical reaction method and apparatus according to the present invention, by combining the batch reaction system 12 and the circulation reaction system 13 to perform a variety of chemical reactions, compared to the conventional batch reactor The speed can be increased, so productivity can be easily increased. In particular, it is basically made by installing a cyclic reaction system 13 applying the continuous reactor 14 to the batch reaction system 12 applying the batch reactor, it is possible to utilize the existing chemical reaction equipment, No additional utility is required to reduce maintenance costs, and the formation of impurities is reduced by increasing the reaction rate. In addition, since the multi-stage design of the continuous reactor 14 is possible in the cyclic reaction system 13, it is easy to increase the reaction rate, and various chemical reactions for reacting different liquids or adding a gas such as hydrogen to the reactants to obtain a product. It can be easily applied to, and the productivity is improved by increasing the reaction rate, so that the installation of the chemical reaction device 10 can be made small while reducing the space constraint.

Claims (19)

  1. 배치형 반응 시스템(12)에 반응물을 넣고, 생성물을 얻기 위한 반응공정을 진행하는 배치 반응공정 단계와;Placing a reactant into the batch reaction system 12 and carrying out a reaction step to obtain a product;
    상기 배치형 반응 시스템(12)과 폐회로를 형성하도록 설치되는 순환형 반응 시스템(13)에 상기 배치형 반응 시스템(12)내에서 배치 반응공정이 진행되는 반응물을 순환시키면서 반응공정이 이루어지도록 하는 순환 반응공정 단계 및;Circulation to make the reaction process while circulating the reactants in which the batch reaction process proceeds in the batch reaction system 12 to the circulating reaction system 13 installed to form a closed circuit with the batch reaction system 12 A reaction process step;
    상기 순환형 반응 시스템(13)으로의 순환을 정지하고, 상기 배치형 반응 시스템(12)내의 생성물을 외부로 배출시키는 단계를 포함하는 것을 특징으로 하는 고효율 화학반응 방법.Stopping the circulation to the circulation reaction system (13) and discharging the product in the batch reaction system (12) to the outside.
  2. 제 1 항에 있어서, The method of claim 1,
    상기 배치 반응공정 단계는 상기 배치형 반응 시스템(12)에 반응물을 넣은 후, 첨가 반응물을 넣어 생성물을 얻기 위한 반응공정을 진행하고, 상기 순환 반응공정 단계는 상기 배치형 반응 시스템(12)로부터 공급되는 반응물에 상기 첨가 반응물을 넣어 반응공정이 이루어지도록 하는 것을 특징으로 하는 고효율 화학반응 방법.In the batch reaction process step, the reactant is added to the batch reaction system 12, and then the addition reaction is added to proceed with the reaction process to obtain a product, and the circulating reaction process step is supplied from the batch reaction system 12. High-efficiency chemical reaction method, characterized in that the reaction step is made by adding the addition reactant to the reactant.
  3. 제 2 항에서,In claim 2,
    상기 첨가 반응물은 기체인 것을 특징으로 하는 고효율 화학반응 방법. The addition reactant is a high efficiency chemical reaction method, characterized in that the gas.
  4. 제 3 항에 있어서, The method of claim 3, wherein
    상기 순환 반응공정 단계는 상기 순환형 반응 시스템(13)의 내부 압력이 상기 배치형 반응 시스템(12)의 내부 압력보다 크게 작용되도록 하여 이루어지는 것을 특징으로 하는 고효율 화학반응 방법.The circulation reaction process step is characterized in that the internal pressure of the circulating reaction system (13) is made to be greater than the internal pressure of the batch reaction system (12).
  5. 제 1 항에 있어서, The method of claim 1,
    상기 반응물은 복수개 이상의 액상으로 이루어지는 것을 특징으로 하는 고효율 화학반응 방법.The reactant is a high efficiency chemical reaction method, characterized in that consisting of a plurality of liquid phase.
  6. 제 1 항 내지 제 5 항 중 어느 한 항에 있어서, The method according to any one of claims 1 to 5,
    상기 순환 반응공정 단계는 상기 배치형 반응 시스템(12)과 폐회로를 형성하도록 설치되는 연결 라인(15)상에 배치되는 연속식 반응기(14)를 통해 이루어지도록 하는 것을 특징으로 하는 고효율 화학반응 방법.The cyclic reaction process step is to be carried out through a continuous reactor (14) disposed on a connection line (15) which is installed to form a closed circuit with the batch reaction system (12).
  7. 제 6 항에 있어서, The method of claim 6,
    상기 연속식 반응기(14)는 교반(mixing) 기능을 갖는 교반형 반응기(40)를 구비하고, 상기 순환 반응공정 단계는 반응물이 상기 교반형 반응기(40)를 통과중에 연속적인 교반이 이루어지도록 하는 것을 특징으로 하는 고효율 화학반응 방법.The continuous reactor 14 includes a stirred reactor 40 having a mixing function, and the circulating reaction step allows continuous stirring while reactants pass through the stirred reactor 40. High efficiency chemical reaction method, characterized in that.
  8. 제 6 항에 있어서, The method of claim 6,
    상기 연속식 반응기(14)는 분산(dispersion) 기능을 갖는 확산형 반응기(50)를 구비하고, 상기 순환 반응공정 단계는 상기 확산형 반응기(50)를 통해 반응물의 분산이 이루어지도록 하는 것을 특징으로 하는 고효율 화학반응 방법.The continuous reactor 14 includes a diffusion type reactor 50 having a dispersion function, and the circulating reaction step is characterized in that the dispersion of the reactants is made through the diffusion type reactor 50. High efficiency chemical reaction method.
  9. 제 6 항에 있어서, The method of claim 6,
    상기 연속식 반응기(14)는 상기 연결 라인(15)상에 연이어 설치되는 복수개 이상의 반응기를 구비하고, 상기 순환 반응공정 단계는 상기 복수개 이상의 반응기를 순차적으로 통과하면서 이루어지도록 하는 것을 특징으로 하는 고효율 화학반응 방법.The continuous reactor 14 has a plurality of reactors which are installed in series on the connection line 15, the circulating reaction process step is to be made while passing through the plurality of reactors in sequence Reaction method.
  10. 제 9 항에 있어서, The method of claim 9,
    상기 연속식 반응기(14)의 복수개 이상의 반응기는 교반(mixing) 기능을 갖는 교반형 반응기(40) 및, The plurality of reactors of the continuous reactor 14 is a stirred reactor (40) having a mixing (mixing) function, and
    분산(dispersion) 기능을 갖는 확산형 반응기(50)를 구비하여, With a diffusion reactor 50 having a dispersion function,
    상기 순환 반응공정 단계는 상기 교반형 반응기(40)를 통과중에 연속적인 교반이 이루어진 후, 상기 확산형 반응기(50)를 통해 반응물의 분산이 이루어지도록 하는 것을 특징으로 하는 고효율 화학반응 방법.The cyclic reaction step is a high-efficiency chemical reaction method, characterized in that the dispersion of the reactants through the diffusion reactor 50 after the continuous stirring is made while passing through the stirred reactor (40).
  11. 반응물을 넣고 반응공정이 완료될 때까지 공정이 계속 진행되도록 하고, 반응공정이 완료된 생성물을 한꺼번에 배출시키도록 구성되는 배치형 반응 시스템(12) 및;A batch reaction system 12 configured to add a reactant and allow the process to continue until the reaction process is completed and to discharge the finished products at once;
    상기 배치형 반응 시스템(12)과 폐회로를 형성하도록 설치되고, 상기 배치형 반응 시스템(12)에 수용되어 반응공정이 진행되는 반응물을 순환시키면서 반응공정이 이루어지도록 하는 순환형 반응 시스템(13)를 포함하는 것을 특징으로 하는 고효율 화학반응 장치.The circulating reaction system 13 is installed to form a closed circuit with the batch reaction system 12, and is accommodated in the batch reaction system 12 to circulate the reactants through which the reaction process proceeds. High efficiency chemical reaction device comprising a.
  12. 제 11 항에 있어서, The method of claim 11,
    상기 순환형 반응 시스템(13)은 상기 배치형 반응 시스템(12)과 폐회로를 형성하도록 설치되는 연결 라인(15) 및;The circulating reaction system (13) includes a connection line (15) installed to form a closed circuit with the batch reaction system (12);
    상기 연결 라인(15) 상에서 설치되는 연속식 반응기(14)를 구비하는 것을 특징으로 하는 고효율 화학반응 장치.High efficiency chemical reaction device characterized in that it comprises a continuous reactor (14) installed on the connection line (15).
  13. 제 12 항에 있어서, The method of claim 12,
    상기 연속식 반응기(14)는 반응물이 통과중에 연속적인 교반이 이루어지도록 하는 교반(mixing) 기능을 갖는 교반형 반응기(40)를 구비하는 것을 특징으로 하는 고효율 화학반응 장치.The continuous reactor (14) is a high-efficiency chemical reaction device, characterized in that it comprises a stirred reactor (40) having a mixing (mixing) function to enable continuous stirring while the reactants pass through.
  14. 제 12 항에 있어서, The method of claim 12,
    상기 연속식 반응기(14)는 반응물의 분산이 이루어지도록 하는 분산(dispersion) 기능을 갖는 확산형 반응기(50)를 구비하는 것을 특징으로 하는 고효율 화학반응 장치.The continuous reactor (14) is a high-efficiency chemical reaction device, characterized in that it comprises a diffusion reactor (50) having a dispersion (dispersion) function to make the dispersion of the reactants.
  15. 제 12 항에 있어서, The method of claim 12,
    상기 연속식 반응기(14)는 상기 연결 라인(15)상에 연이어 설치되는 복수개 이상의 반응기를 구비하는 것을 특징으로 하는 고효율 화학반응 장치.The continuous reactor (14) is a high-efficiency chemical reaction device, characterized in that it comprises a plurality of reactors are installed in series on the connecting line (15).
  16. 제 15 항에 있어서, The method of claim 15,
    상기 연속식 반응기(14)는 반응물이 통과중에 연속적인 교반이 이루어지도록 하는 교반(mixing) 기능을 갖는 교반형 반응기(40) 및, The continuous reactor 14 is a stirred reactor (40) having a mixing (mixing) function to make a continuous agitation during the reaction, and
    상기 연속식 반응기(14)는 반응물의 분산이 이루어지도록 하는 분산(dispersion) 기능을 갖는 확산형 반응기(50)를 구비하는 것을 특징으로 하는 고효율 화학반응 장치.The continuous reactor (14) is a high-efficiency chemical reaction device, characterized in that it comprises a diffusion reactor (50) having a dispersion (dispersion) function to make the dispersion of the reactants.
  17. 제 12 항 내지 제 16 항에 있어서, The method of claim 12, wherein
    상기 배치형 반응 시스템(12) 및 순환형 반응 시스템(13)은 반응물을 넣은 후, 첨가 반응물을 공급시키기 위해 설치되는 첨가 반응물 공급 유니트(16)를 더 구비하는 것을 특징으로 하는 고효율 화학반응 장치.The batch type reaction system (12) and the circulating type reaction system (13) further comprise an addition reactant supply unit (16) which is installed to supply the addition reactants after the addition of the reactants.
  18. 제 17 항에 있어서,The method of claim 17,
    상기 순환형 반응 시스템(13)은 상기 연결 라인(15)상에서 상기 연속 반응기(14)의 전단에 설치되는 펌프(30)와, 후단에 설치되는 액레벨 조정기(34)를 더 구비하여, 상기 순환형 반응 시스템(13)의 내부 압력이 상기 배치형 반응 시스템(12)의 내부 압력보다 높게 설정되도록 하는 것을 특징으로 하는 고효율 화학반응 장치.The circulation reaction system 13 further includes a pump 30 installed at the front end of the continuous reactor 14 on the connection line 15 and a liquid level regulator 34 installed at the rear end of the circulation line. High efficiency chemical reaction device, characterized in that the internal pressure of the type reaction system (13) is set higher than the internal pressure of the batch reaction system (12).
  19. 제 15 항에 있어서, The method of claim 15,
    상기 연결 라인(15)은 상기 복수개 이상의 반응기 각각에 각 반응기의 전단과 후단을 연결함으로써, 상기 연결 라인(15)을 통해 흐르는 반응물이 각 반응기를 통과하여 흐르도록 하는 바이패스 라인을 더 구비하는 것을 특징으로 하는 고효율 화학반응 장치.The connection line 15 further includes a bypass line for connecting the front and rear ends of each reactor to each of the plurality of reactors so that reactants flowing through the connection line 15 flow through each reactor. High efficiency chemical reaction device.
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Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2001121167A (en) * 1999-10-27 2001-05-08 Japan Organo Co Ltd Batchwise supercritical water reaction apparatus
US6426439B1 (en) * 1997-07-04 2002-07-30 Clariant Gmbh Continuous process for the preparation of pentafluoroethyl iodide
KR20020095206A (en) * 2000-04-04 2002-12-20 파니폴 오와이 A method and an apparatus for preparing polyaniline
JP2003286202A (en) * 2002-03-28 2003-10-10 Hokko Chem Ind Co Ltd Method for separating and recovering readily polymerizable substance from impurity-containing readily polymerizable substance containing high-boiling substance and apparatus therefor
JP2008069304A (en) * 2006-09-15 2008-03-27 Ricoh Co Ltd Method for dispersing pigment for inkjet ink, pigment dispersion and inkjet ink using the pigment dispersion

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US6426439B1 (en) * 1997-07-04 2002-07-30 Clariant Gmbh Continuous process for the preparation of pentafluoroethyl iodide
JP2001121167A (en) * 1999-10-27 2001-05-08 Japan Organo Co Ltd Batchwise supercritical water reaction apparatus
KR20020095206A (en) * 2000-04-04 2002-12-20 파니폴 오와이 A method and an apparatus for preparing polyaniline
JP2003286202A (en) * 2002-03-28 2003-10-10 Hokko Chem Ind Co Ltd Method for separating and recovering readily polymerizable substance from impurity-containing readily polymerizable substance containing high-boiling substance and apparatus therefor
JP2008069304A (en) * 2006-09-15 2008-03-27 Ricoh Co Ltd Method for dispersing pigment for inkjet ink, pigment dispersion and inkjet ink using the pigment dispersion

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