KR102313130B1 - organic-inorganic hybrid adsorbent and manufacturing method there of - Google Patents

Abstract

The present invention relates to an invention about a method for manufacturing a porous absorbent which is a combined material of an organic material and an inorganic material. Specifically, the present invention is based on a time sequential procedure comprising a mixing step (S200) of inputting a mixture (10) composed of an organic material (11), an inorganic material (12), and mixed water (13) in a reaction container (10); a reaction step (S400) of generating a reaction product (20) by conducting reaction of the mixture (10) after the mixing step; and a refining step (S500) of extracting impurities (22) and reaction water (23) contained in the reaction product (20) after the reaction step. According to the present invention, provided is an effect of maintaining the uniformity of quality.

Description

{organic-inorganic hybrid adsorbent and manufacturing method there of}

The present invention is a combination of an organic material and an inorganic material, and relates to a method for manufacturing a porous absorbent material.

Patent Inventions 001 to 004 suggest a patent for a method of manufacturing a material for moisture absorption using organic and inorganic materials.

In particular, Patent Invention 001 discloses that a porous molding agent is manufactured through a carbonization process of organic waste, and zeolite is coated on the surface of the porous molded body and then calcined at a high temperature to give adsorption properties of organic and inorganic substances. Waste carbonization and zeolite coating To an organic and inorganic adsorbent and a method for manufacturing the same, specifically, a first step of mixing organic waste and water to prepare a mixed raw material in a dough state having a moisture content; a second step of molding the mixed raw material into a predetermined shape and carbonizing the molded body; A third step of preparing a zeolite precursor coating solution; and a fourth step of coating and firing a zeolite coating solution on the carbonized molded body.

Patent Invention 002 relates to a method for producing a surface coating composition of an organic/inorganic nanoporous body for moisture adsorption, specifically dispersing the organic/inorganic nanoporous body in a solvent, and adding a silicone binder to the solution in which the organic/inorganic nanoporous body is dispersed. Steps including the step of adding are presented.

KR 10-1221658 B1 (Registration Date January 07, 2013) KR 10-2096333 B1 (Registration date March 27, 2020) KR 10-2018-0128383 A (published on December 03, 2018) KR 10-2145031 B1 (registration date August 10, 2020)

The present invention is a combined material of an organic material and an inorganic material, and an object of the present invention is to provide a method for manufacturing a porous absorbent material.

The present invention relates to a method for manufacturing an organic-inorganic porous adsorbent, specifically, a mixing step of introducing a mixture (10) consisting of an organic material (11), an inorganic material (12), and mixed water (13) into the reaction vessel (201) (S200); After the mixing step, a reaction step (S400) of reacting the mixture (10) to produce a reactant (20); After the reaction step, a purification step (S500) of extracting the impurities 22 and the reaction water 23 accommodated in the reactant 20; consists of a time series procedure.

The present invention relates to a method for manufacturing an organic-inorganic porous adsorbent, and in the invention presented above, before the mixing step, a supply step (S100) of supplying the organic material 11, the inorganic material 12, and the mixed water 13, respectively ); further includes the procedure of

The present invention relates to a method for manufacturing an organic-inorganic porous adsorbent, and in the invention presented above, the reaction step (S400) includes a constant temperature maintenance step (S410) of maintaining the temperature of the reaction vessel 201 at a constant temperature; Among the constant temperature maintaining step, the stirring step (S420) of stirring the mixture 10 by the stirring means 400; further includes the procedure.

The present invention relates to a method for producing an organic-inorganic porous adsorbent, and in the invention presented above, after the reaction step, a cooling step 300 of cooling the reactant 20 produced is further included.

The present invention relates to a method for manufacturing an organic-inorganic porous adsorbent, and in the invention presented above, the purification step includes a purification supply step (S510) of supplying the reactant 20 to the filter 501; Separation step (S520) of separating the compound (21), impurities (22) and reaction water (23) contained in the reactant (20) after the purification supply step; After the separation step, the purification and discharging step (S550) of separating and discharging the compound (21), the impurities (22), and the reaction water (23);

The present invention relates to a method for producing an organic-inorganic porous adsorbent, and in the invention presented above, after the purification step, a pulverizing step (S600) of pulverizing the produced compound (21); further comprising a procedure. The present invention relates to an organic-inorganic porous adsorbent, and provides an organic-inorganic porous adsorbent produced by the manufacturing method presented above.

The present invention is an invention for a mass production process of an organic-inorganic porous adsorbent (MOF), and has the effect of maintaining the homogeneity of quality.

1 and 2 are flowcharts of a method for manufacturing a porous adsorbent of the present invention.
3 is a conceptual diagram of the apparatus of the supply step, mixing step, and reaction step of the present invention.
Figure 4 is a conceptual diagram of various embodiments of the stirring step of the present invention.
5 is a conceptual diagram of temperature adjustment of the reaction step of the present invention.
6 is a conceptual diagram of the manufacturing method of the present invention.
7 is a conceptual diagram of a refining step and a refining step.

Hereinafter, the most preferred embodiment of the present invention will be described in detail in order to describe in detail enough that a person of ordinary skill in the art to which the present invention pertains can easily carry out the present invention.

The numbers cited in the examples below are not limited only to the objects of reference, and may be applied to all examples. Objects exhibiting the same purpose and effect as the configuration presented in the examples correspond to equivalent replacement objects. The higher-level concept presented in the examples includes sub-concept objects that are not described.

[Example 1-1] The present invention relates to a method for manufacturing an organic-inorganic porous adsorbent, specifically, in a reaction vessel ( 201) a mixing step (S200) for inputting the inside; After the mixing step, a reaction step (S400) of reacting the mixture (10) to produce a reactant (20); After the reaction step, a purification step (S500) of extracting the impurities 22 and the reaction water 23 contained in the reactant 20;

[Example 1-2] The present invention relates to a method for manufacturing an organic-inorganic porous adsorbent, and in Example 1-1, the mixed water is distilled water.

[Example 1-3] The present invention relates to a method for manufacturing an organic/inorganic porous adsorbent, and in Example 1-1, the inorganic material is formed of metal ion clusters; includes.

[Example 1-4] The present invention relates to a method for manufacturing an organic-inorganic porous adsorbent, and in Example 1-3, the metal ion is formed of ferric nitrate [Fe(NO3)39H2O]; include

[Example 1-5] The present invention relates to a method for manufacturing an organic-inorganic porous adsorbent, and in Example 1-3, the metal ion cluster is formed in a liquid form or a powder form; includes. The metal ions of the organic-inorganic porous adsorbent are Li+, Na+, K+, Rb+, Be2+, Mg2+, Ca2+, Sr2+, Ba2+, Sc3+, Y3+, Ti4+, Zr4+, Hf+, V4+, V3+, V2+, Nb3+, Ta3+, Cr3+ , Mo3+, W3+, Mn3+, Mn2+, Re3+, Re2+, Fe3+, Fe2+, Ru3+, Ru2+, Os3+, Os2+, Co3+, Co2+, Rh2+, Rh+, Ir2+, Ir+, Ni2+, Ni+, Pd2+, Pd+, Cu2+, Pd+, Pt2+, Pt+, Pt2+ , Cu+, Ag+, Au+, Zn2+, Cd2+, Hg2+, Al3+, Ga3+, In3+, Tl3+, Si4+, SI2+, Ge4+, Ge2+, Sn4+, Sn2+, Pb4+, Pb2+, As5+, As3+, As+, Sb3+, Bi3+, Sb3+, Bi3+ And Bi + may be selected from the group consisting of, but is not limited thereto.

[Example 1-6] The present invention relates to a method for manufacturing an organic-inorganic porous adsorbent, and in Example 1-1, the organic material may be any organic compound having a functional group capable of coordinating as an organic ligand. For example, the organic ligand is a carboxyl group (-COOH), a carboxylic acid anion group (COO-), an amine group (-NH2) and an amino group (-NH), a nitro group (-NO2), a hydroxyl group (-OH), A compound having at least one functional group selected from the group consisting of a halogen group (-X) and a sulfonic acid group (-SO3H), a sulfonic acid anion group (-SO3-), a methanedithioic acid group (-CS2H), a pyridine group, and a pyrazine group, or a compound thereof Mixtures may be used. The MOF may have a dicarboxylic acid anion of a heterocyclic ring as a ligand. Preferably, the ligand may be at least one selected from the group consisting of a terephthalate anion and a pyrazoledicarboxylic acid anion, but is not limited thereto.

The present invention (refer to Examples 1-1 to 1-6, and FIGS. 1 and 3) is an invention for a method for manufacturing an organic-inorganic porous adsorbent. Specifically, the invention relates to a method for manufacturing a metal organic framework (MOF).

The adsorbent obtained by this preparation method is obtained by (a) mixing a plurality of mixtures, (b) reacting the plurality of mixtures chemically to obtain a reactant 20, (c) unreacted substances (impurities 22) in the reactants ) and the reaction water (23) is made in the order of the purification step for separating from the compound (21).

The mixture 10 includes an organic material 11 , an inorganic material 22 , and mixed water 23 . The reactant 20 is composed of a completely chemically reacted compound 21 , an impurity 22 made of unreacted material, and reaction water 23 remaining after the reaction. The mixture may include an additive 14 having a functionality as needed.

The inorganic material is formed of a metal cluster, and ferric nitrate is preferably employed. In addition, it can be substituted with other substances that exhibit the same purpose and effect as ferric nitrate. The organic material has a molecular structure of an organic ligand.

Distilled water is used as the mixed water to prevent the formation of foreign substances due to impurities contained in the mixed water during the reaction process.

Mixed water is in liquid form, and inorganic substances are in liquid or powder form. The organic and inorganic materials combined with the mixed water have fluidity, which is to ensure smooth mobility of the process to be described later and to facilitate heat treatment.

[Example 2-1] The present invention relates to a method for producing an organic-inorganic porous adsorbent, and in Example 1-1, before the mixing step, the organic material 11, the inorganic material 12, and the mixed water 13 ) of supplying each of the supply step (S100); consists of a step including.

[Example 2-2] The present invention is an invention for a method for producing an organic-inorganic porous adsorbent, and in Example 2-1, the supplying step includes a metering step (S110) of measuring the supply amount.

[Example 2-3] The present invention relates to a method for manufacturing an organic-inorganic porous adsorbent, and in Example 2-2, the metering step includes a continuous metering step (S121) made continuously.

[Example 2-4] The present invention is an invention for a method for manufacturing an organic-inorganic porous adsorbent, and in Example 2-2, the metering step includes a unit metering step (S122) performed for each unit.

The present invention (see Examples 2-1 to 2-4, see Figs. 1 and 3) specifies the mixture supply before the mixing step. The supply step may be divided into a continuous supply step and a unit supply step.

The continuous supply step aims at mass production of the organic-inorganic porous adsorbent, and the mixtures are continuously fed in an accurate ratio. The mixtures are accommodated in each individual vessel 111 , and the individual vessel communicates with the reaction vessel through an individual communication pipe 112 . A fixed quantity feeder 113 is mounted on the individual communication pipe, and the input amount is controlled by the feed controller 114 to be input.

The quantitative feeder controls the liquid material by the flow control valve 113a, and the powdery material is controlled by the powder supply feeder 113b having a spiral screw. Since the continuous supply step enables continuous production, it has the advantage of improving productivity.

The unit supply stage aims at step-by-step production in units of lots. Specifically, it consists of the following configuration. A plurality of mixtures (organic material, inorganic material, distilled water) are accommodated in each individual container 121, and the material supplied from the individual container is filled in the measuring container 122, and the input amount is accurately measured by filling the material of the individual container. The metered material is introduced into the reaction vessel 201 through the individual communication pipe 123 .

The measuring container detects the capacity based on volume or weight. The unit supply step has the advantage of producing an adsorbent by measuring an accurate amount.

[Example 3-1] The present invention relates to a method for producing an organic-inorganic porous adsorbent, and in Example 1-1, the reaction step (S400) is a constant temperature for maintaining the temperature of the reaction vessel 201 at a constant temperature. maintaining step (S410); Among the constant temperature maintaining step, a stirring step (S420) of stirring the mixture 10 by the stirring means 400; consists of a step including.

[Example 3-2] The present invention is an invention for a method for producing an organic-inorganic porous adsorbent, and in Example 3-1, the temperature is 90 ° C to 120 ° C, preferably formed at 100 ° C; include

[Example 3-3] The present invention relates to a method for producing an organic-inorganic porous adsorbent, and in Example 3-1, the reaction step includes maintaining 12 to 24 hours.

[Example 3-4] The present invention relates to a method for manufacturing an organic-inorganic porous adsorbent, and in Example 3-1, after the reaction step, a gas discharge step of discharging the reaction gas 26 inside the reaction vessel (S430); includes. In addition, during the reaction step, the steam discharge step (S451); Condensing step of condensing the discharged steam (S452); Resupplying the condensed steam into the reaction vessel (S453).

[Example 3-5] The present invention relates to a method for producing an organic-inorganic porous adsorbent, and in Example 3-1, after the reaction step, a temporary storage step of storing the compound (21) in a temporary storage container (S440) ); includes.

[Example 3-6] The present invention relates to a method for manufacturing an organic-inorganic porous adsorbent. In Example 3-1, the stirring means 400 is a stirring motor 411 located inside or outside the reaction vessel. includes ;

It is located inside the container for half, and the stirring blade 412 to which the rotational force of the stirring motor is transmitted; includes.

[Example 3-7] The present invention relates to a method for manufacturing an organic-inorganic porous adsorbent. In Example 3-1, the stirring means 400 is a stirring pump 421 located inside or outside the reaction vessel. ; One side communicates with the upper layer of the half container, the other side communicates with the lower part of the stirring vessel, and the stirring tube 422 in which the stirring pump is formed in the middle side; includes.

[Example 3-8] The present invention relates to a method for manufacturing an organic-inorganic porous adsorbent. In Example 3-1, the stirring means 400 is a reaction vessel, which is formed in the form of a cylindrical flow tube, and a reaction tube 431 through which the mixture flows; a plurality of stirring blades 432 formed on the inner periphery of the reaction tube and fixed or rotated; and a flow pump 433 communicating with the reaction tube and flowing the mixture into the reaction tube.

[Example 3-9] The present invention relates to a method for manufacturing an organic-inorganic porous adsorbent, and in Example 3-1, the constant temperature maintenance step includes a temperature sensor 451 located inside and/or outside the reaction vessel. ; a heat generator 452 located inside or outside the reaction vessel and maintaining a set temperature; and a temperature controller 453 that detects the signal of the temperature sensor and controls the operation of the heat generator.

The present invention (see 3-1 to 3-9, see Fig. 1) specifies the reaction step. The reaction step is carried out inside the reaction vessel. The reaction vessel may be selected from a closed vessel or a tubular vessel. Reactions in closed containers are used in lot-unit production, while tubular containers are used in continuous production. That is, the sealed container reacts the mixture 10 in a stagnant space, and the tubular container reacts the mixture 10 in the flow process.

The temperature of the reaction vessel is maintained in the range of 90°C to 120°C, preferably at 100°C. The reaction time lasts from 12 hours to 24 hours. In addition, during the reaction process, the stirring process is performed simultaneously. This is to obtain a stable and homogeneous chemical change of the mixture 10 through the stirring process.

The stirrer of Example 3-6 is provided with a rotating blade inside the reaction vessel, and the blade rotates inside the liquid-mixed mixture 10 . The rotational power of the blade is driven by a stirring motor outside the reaction vessel. The rotation speed of the stirring blade is controlled according to the temperature, and since the stirring blade forms different torsional angles for each section, it is possible to implement a constant flow condition inside the reaction vessel.

The stirrer of embodiment 3-7 is formed with two stirring tubes coupled with a stirring pump, one side of the stirring tube is located inside the liquid mixture 10, and the other side is located in the gaseous space. That is, it may have an effect of supplying bubbles to the liquid phase by driving the stirring pump or spraying the liquid phase into the gas portion. The bubble-forming and liquid-phase spraying may interact with each other. This is to obtain a complete stirring effect.

The stirrer of Example 3-8 is formed as a reaction tube. The reaction tube is formed long to transport the mixture therein. During the transfer process, the mixture is stirred by the twisted blade inside the reaction tube, and when the mixture exits the reaction tube, the finished material is produced by chemical change. The blade forms a vortex in the flowing mixture, and the efficiency of stirring can be increased by the vortex. By substituting the blades, an orifice may be formed, or baffles or through plates of different sizes may be combined.

In Examples 3-6 to 3-8, a temperature sensor is mounted inside the reaction vessel, the measured value of the temperature sensor is transmitted to the temperature controller, and the temperature controller operates the heat generator to set the reaction vessel temperature to the set temperature. keep In order to cut off the temperature from the outside, a thermal insulation device is installed on the outside of the reaction vessel.

In the temperature control of Example 3-8, the outside of the reaction tube is accommodated by the chamber, and a heat generator and a temperature sensor are mounted inside the chamber. Accordingly, it is possible to control the temperature of the flowing mixture to the set temperature in real time.

Example 3-5 implements the temporary storage step of the reactant 20 in which the reaction is completed. The temporary storage step is a step of temporarily storing the reactants 20 produced in LOT units in the mass production process, and the reactants 20 are stored in the storage container 301 under a uniform temperature condition.

[Example 4-1] The present invention is an invention for a method for producing an organic-inorganic porous adsorbent, and in Example 1-1, after the reaction step, a cooling step 300 of cooling the generated reactant 20; It consists of steps including

[Example 4-2] The present invention is an invention for a method for manufacturing an organic-inorganic porous adsorbent. In Example 4-1, the cooling step includes a first cooling step (S310) of cooling to a first temperature section; After the first cooling step, a second cooling step (S320) of cooling to a second temperature section; includes.

[Example 4-3] The present invention is an invention for a method for manufacturing an organic-inorganic porous adsorbent, and in Example 4-2, the first cooling step is formed by any one selected from water cooling, air cooling, and forced cooling; include

[Example 4-4] The present invention is an invention for a method for manufacturing an organic-inorganic porous adsorbent, and in Example 4-2, the second cooling step is formed by any one selected from water cooling, air cooling, and forced cooling; include

[Example 4-5] The present invention relates to a method for producing an organic-inorganic porous adsorbent, and in Example 4-1, the cooling step is performed inside the reaction vessel.

[Example 4-6] The present invention is an invention for a method for producing an organic-inorganic porous adsorbent, and in Example 4-1, the cooling step is made in a cooling vessel 400 in communication with the reaction vessel; including; do.

The present invention (see Example 4-1 to Example 4-6, see FIG. 1) specifies the step of cooling the reactant 20 in which the reaction is completed.

The cooling step is divided into a first cooling step and a second cooling step. The first cooling step maintains a set temperature of 90°C to 95°C for a certain period of time. Preferably, it is maintained at 90°C. The second cooling step is a step of cooling from the temperature of the first cooling step to a temperature range of 4°C to 60°C.

The reason for forming the cooling step in multiple stages is to maintain the chemical stability of the reacting compound. Specifically, after the reaction step, the rapid temperature change causes a secondary reaction of the reactant 20 or. The agglomeration effect of the impurities 22 is generated. To prevent this, it is necessary to implement a cooling step that maintains the set temperature for a set time.

The first cooling step and/or the second cooling step may implement cooling conditions by any one method selected from air cooling, water cooling, and forced cooling.

In the case of air cooling, the reaction vessel is brought into contact with external air to cool the reactant, or external air is introduced into the reactant to cool the reaction vessel. When external air is introduced, only air with foreign substances prepared by the filter is introduced.

The water cooling type is cooled by introducing cooling water 51 into the reaction vessel. During the cooling process, a plurality of stirring processes may be involved, thereby improving cooling efficiency. At this time, the cooling temperature should be maintained at the temperature set by the temperature control. As the cooling water uses distilled water, there is no chemical change. The inputted coolant forms a section in a plurality of steps, and the temperature of the inputted coolant can be implemented differently for each section.

The forced cooling method is a method of cooling a mixture by using a refrigerant to realize heat transfer by non-contact with the refrigerant. The refrigerant temperature sets a multi-stage section, and the differential temperature flows for each section. The refrigerant presented above is implemented as a refrigeration cycle, and as another embodiment, it enables temperature control by using a teltier element or the like.

The cooling process presented above may be performed inside the reaction vessel or may be implemented in a separate cooling vessel.

[Example 5-1] The present invention is an invention for a method for producing an organic-inorganic porous adsorbent, and in Example 1-1, the purification step is a purification supply step of supplying the reactant 20 to the filter 501 ( S510); Separation step (S520) of separating the compound (21), impurities (22) and reaction water (23) contained in the reactant (20) after the purification supply step; After the separation step, the purification and discharging step (S550) of separately discharging the compound (21), the impurities (22), and the reaction water (23);

[Example 5-2] The present invention relates to a method for manufacturing an organic-inorganic porous adsorbent, and in Example 5-1, the filter is formed of any one selected from a press filter, a centrifugal filter, and an osmotic filter; do.

The present invention (see Example 5-1 to Example 5-2, see Figure 2, Figure 4) secures the pure compound (21) from the reactant (20), and separates the impurities (22) and the reaction water (23) purpose is to Therefore, it is to secure the cake compound 30 in a complete form.

The reactant 20 obtained through the cooling process is supplied to the filter, and is divided into compounds, impurities, and reaction water through the filter. The compound is commercialized through a post-treatment process, and impurities and water are reused in the previous process.

The separation step presented above is performed by a filter, and the filter may be formed by any one process selected from a centrifugal filter, an osmotic filter, and a press filter.

[Example 5-3] The present invention relates to a method for manufacturing an organic/inorganic porous adsorbent, and in Example 5-1, the separation step is a process of liquid reaction water 23 and powder into the press filter 511. A filter internal supply step of supplying the compound (21) and the impurities (22) together (S521); After the step of supplying the filter inside, the liquid phase discharging step (S522) of first discharging the reaction water 23 by pressing the press 512; After the liquid phase discharging step, the remaining liquid phase discharging step (S523) of injecting discharged air 31 to secondarily separate the remaining reaction water 23 and impurities 22; After the residual liquid discharge step, the cake discharge step (S524) of discharging the solidified cake-like compound 30 to the exhaust air 31; includes.

In the present invention (refer to Example 5-3, see Figs. 2 and 4), a pressurized press filter method is used. The press filter method is advantageous in forming a cake, and in particular, there is an easy specificity for releasing small-sized impurities contained together with water. In addition, since the remaining water is discharged by high-pressure air, it is easy to discharge impurities by the circulation system in the forward and reverse directions.

[Example 5-4] The present invention relates to a method for manufacturing an organic-inorganic porous adsorbent, and in Example 5-1, the separation step is in the filter for supplying the reactant 20 into the rotary cylindrical filter 521 supply step (S541); a discharging step (S542) of discharging the reaction water 23 and impurities 22 by rotation of the rotary cylindrical filter after the in-filter supply step; In the discharging step, the compound 21 is transferred in the axial direction inside the cylindrical filter (S543); includes a.

[Example 5-5] The present invention is an invention for a method for manufacturing an organic-inorganic porous adsorbent, and in Example 5-4, additional purified water supply step in which additional purified water 32 is additionally supplied during the intra-filter transfer step (S544); includes.

The present invention (see Examples 5-4 to 5-5, see Figs. 2 and 4) uses a pressurized press filter method. The press filter method is advantageous in forming a cake, and in particular, there is an easy specificity for releasing small-sized impurities contained together with water. In addition, since the remaining water is discharged by high-pressure air, it is easy to discharge impurities by the circulation system in the forward and reverse directions.

One example (5-4) uses a centrifugal press filter method. The centrifugal filter puts reaction compounds (compounds, impurities, water) inside the rotating cylinder formed in the form of a mesh, and discharges the reaction water and impurities by centrifugal force by the high-speed rotating cylinder. The network is formed to a size for discharging impurities and reaction water. The discharged impurities and reaction water are again divided into water and impurities through a secondary network, and the water is again put into the rotating cylinder of the centrifugal filter and used as additional purified water 32 . The additional purified water has the effect of removing the remaining impurities again. This can be repeated several times.

Since the rotating cylinder has an eccentric protrusion in the form of a plate eccentric inside, the material inside is moved in one direction during the cylinder rotation process. At the end of the transfer process, compound (21) in a complete form can be obtained.

[Example 5-6] The present invention is an invention for a method for producing an organic-inorganic porous adsorbent, and in Example 5-1, after the purification and discharging step, a repurification step (S560) of repurifying the compound (21); include

[Example 5-7] The present invention is an invention for a method for producing an organic-inorganic porous adsorbent, and in Example 5-4, the re-refining step pulverizes the cake-like compound 30 to produce the pulverized compound 40 a purification and grinding step (561); After the refining and pulverizing step, a residual material dissolving step of dissolving the remaining impurities 22 by mixing the mixed solvent 41 and the pulverized compound 40 in the mixing tank 530 (S562); After the step of dissolving the residual material, the re-separation step (S563) of re-entering the filter 501 to separate it; includes.

[Example 5-8] The present invention relates to a method for manufacturing an organic-inorganic porous adsorbent, and in Example 5-5, the mixed solvent is distilled water (41a) and/or ethanol (41b);

[Example 5-9] The present invention is an invention for a method for producing an organic-inorganic porous adsorbent, and in Example 5-6, the residual material dissolving step is a first dissolving step ( S542a); A second dissolution step (S542b) of dissolving the remaining inorganic material by the neutral water; is formed.

The present invention (see Examples 5-6, to Examples 5-9, see FIGS. 1 and 5) specifies the step of repurifying the purified cake compound 30 again. This step corresponds to a two-step purification step, and the second step purification step involves a chemical purification process, unlike the first step purification step.

In the first purification step, a small amount of micro-compounds was size-selected through a filter network formed of a mesh network. The secondary purification step has the purpose of dissolving and separating unreacted organic and inorganic substances using ethanol and distilled water.

The first dissolution step and the second dissolution step are sequentially performed, and may be performed through a process repeated several times. However, the final step is finished with the second dissolution step, which is to completely remove the remaining ethanol with distilled water.

[Example 6-1] The present invention is an invention for a method for producing an organic-inorganic porous adsorbent, and in Example 1-1, after the purification step, a pulverizing step (S600) of pulverizing the produced compound (21); It consists of steps including

[Example 6-2] The present invention is an invention for a method for producing an organic-inorganic porous adsorbent, and in Example 6-1, after the pulverization step, a fractionation step of classifying the produced compound 21 into size (S700) includes ;

[Example 6-3] The present invention is an invention for a method for producing an organic-inorganic porous adsorbent, and in Example 6-2, before the fractionation step, a drying step (S820) of drying the compound (21); includes; .

[Example 6-4] The present invention relates to a method for manufacturing an organic-inorganic porous adsorbent, and in Example 6-3, the drying step is performed by heating drying method using a dryer 810 or blowing method with a blower 820. What is formed; includes.

The present invention (see Example 6-1, to Example 6-4, see FIG. 1) suggests a process of pulverizing the resulting compound after the purification step. The pulverization step consists of a mill crusher, a jaw crusher, and the like, and the pulverized compound is subjected to a fractionation step in which it is selected by size. Before the fractionation step, a drying step is performed to remove moisture, etc. contained in the pulverized compound.

The drying step consists of a heating drying method in which air is dried at a set temperature and a blow drying method in which air at room temperature is blown to dry.

During the blowing process, only completely dehumidified air is used. This is to prevent chemical change due to moisture during the drying process.

[Example 7-1] The present invention relates to an organic/inorganic porous adsorbent, and presents an organic/inorganic porous adsorbent prepared by the manufacturing method of the above-mentioned Example.

The present invention is specific to the article obtained by the manufacturing method of the embodiment presented above, and as a result, it is possible to secure a porous adsorbent synthesized from organic and inorganic substances. The porous adsorbent may form a coating solution or an aqueous solution of a cake as an aqueous solution, and may be formed in a cake-shaped block or powder form.

10: mixture 11: organic substance
12: inorganic substance 13: mixed water
14: additive 20: reactant
21: compound 22: impurity
23: reaction water 26: reaction gas
30: cake-like compound 31: exhaust air
32: additional purified water 40: pulverized compound
41: mixed solvent 41a: distilled water
41b: ethanol 51: cooling water
111: individual container 112: individual communication pipe
113: quantitative supply 113a: flow control valve
113b: powder supply feeder 114: supply controller
121: individual container 122: measuring container
123: individual communication pipe 201: reaction vessel
301: storage container 400: stirring means
411: stirring motor 412: stirring blade
421: stirring pump 422: stirring tube
431: reaction tube 432: stirring blade
433: flow pump 451: temperature sensor
452: heat generator 453: temperature controller
511: press filter 512: press
521: rotary cylindrical filter 530: mixing tank
810: dryer 820: blower

Claims (7)

In the organic-inorganic porous adsorbent manufacturing method,
A mixing step (S200) of introducing a mixture (10) comprising an organic material (11), an inorganic material (12), and mixed water (13) into the reaction vessel (201);
After the mixing step, a reaction step (S400) of reacting the mixture (10) to produce a reactant (20);
After the reaction step, a purification step of extracting the impurities 22 and the reaction water 23 contained in the reactant 20 (S500); including,
The purification step may include a purification supply step (S510) of supplying the reactant 20 to the filter 501;
Separation step (S520) of separating the compound (21), impurities (22), and reaction water (23) contained in the reactant (20) after the purification and supply step;
After the separation step, a purification and discharge step (S550) of separating and discharging the compound (21), the impurities (22), and the reaction water (23) (S550);
After the purification and discharging step, a repurification step (S560) of repurifying the compound again;
The re-refining step is a refining and pulverizing step (561) of pulverizing the cake-like compound (30) to produce a pulverized compound (40);
After the refining and pulverizing step, a residual material dissolving step of dissolving the remaining impurities 22 by mixing the mixed solvent 41 and the pulverized compound 40 in the mixing tank 530 (S562);
After the step of dissolving the residual material, the re-separation step (S563) of separating by putting it back into the filter 501;
The residual material dissolving step may include a first dissolving step of dissolving the remaining organic material (S542a); and
A method of manufacturing an organic-inorganic porous adsorbent comprising a; a second dissolving step (S542b) of dissolving the remaining inorganic material.
The method according to claim 1,
Before the mixing step, a supply step (S100) of supplying the organic material 11, the inorganic material 12, and the mixed water 13, respectively;
A method for producing an organic-inorganic porous adsorbent comprising a.
The method according to claim 1,
The reaction step (S400) includes a constant temperature maintenance step (S410) of maintaining the temperature of the reaction vessel 201 at a constant temperature;
A stirring step (S420) of stirring the mixture (10) by means of a stirring means (400) during the constant temperature maintenance step (S420);
A method for producing an organic-inorganic porous adsorbent comprising a.
The method according to claim 1,
After the reaction step, a cooling step (300) of cooling the produced reactant (20);
A method for producing an organic-inorganic porous adsorbent comprising a.
delete The method according to claim 1,
After the purification step, a pulverizing step of pulverizing the produced compound (21) (S600);
A method for producing an organic-inorganic porous adsorbent comprising a.
In the organic-inorganic porous adsorbent,
An organic-inorganic porous adsorbent prepared by the manufacturing method of any one of claims 1 to 4 and 6.

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