A preparation system and method of an external preheating multi-stage adsorbent

Abstract

The application discloses a kind of external preheating multistage adsorbent preparation system and method, belong to adsorbent synthesis and preparation technical field.The system uses multiple double-channel structure's exchange device, collocates valve group and pipeline, realizes the efficient mass transfer of solid phase particle and liquid phase exchange liquid, improves exchange degree, while reducing operating cost.In addition, combined with external preheating mode, effectively avoid the problem that adsorbent is due to its own adsorption exothermic, causes its surface structure to be destroyed, influences adsorption separation performance, reduces water consumption in wetting stage to some extent.At the same time, cooperate the system to propose a set of multistage exchange process method, can be compiled according to different working condition demand, different valve group timing is set, realizes multidimensional application, in different functional adsorbent synthesis and preparation industry field, with great applicability and practicality.

Description

TECHNICAL FIELD

[0001] The application belongs to the field of adsorbent synthesis and preparation, and particularly relates to a preparation system and method of externally preheated multi-stage adsorbent. BACKGROUND

[0002] Multi-stage rectification is a commonly used separation and purification method, but it is difficult to effectively separate some near-boiling homologues or isomers by conventional rectification method. The simulated moving bed technology imitates liquid chromatography technology and is applied in the fields of biological medicine synthesis, plant purification, etc. The technology generally uses resin filler as adsorbent, uses polystyrene and divinylbenzene copolymer as matrix, and is prepared by combining different length of chain segment alkane, such as C8 and C18 filler. When C5 sugar and C6 sugar are separated by chromatography, Ca 2+ Ion exchange resin after sulfonation is used as adsorbent, but metal ions in sugar mother liquor will replace the functional site ions of the filler resin in the separation process, thereby affecting the performance and service life of the resin, and the resin is generally difficult to regenerate. The resin filler has swelling problem in use, and generally uses dynamic axial compression column (DAC column), resulting in high cost. In addition, the above filler is not suitable for the separation of chemical products with high temperature demand, such as xylene homologues, methyl phenol homologues, dichlorobenzene homologues and other substances. Chinese patent document CN114008222A proposes a molecular sieve adsorption separation method, which realizes effective separation of xylose from a mixture containing C5 sugar and C6 sugar by adsorbing xylose with zeolite adsorbent.

[0003] As a new type of separation method, the molecular sieve adsorption method will be the mainstream separation and purification method in the future chemical industry. The method mainly uses molecular sieve as adsorbent and is filled in the corresponding adsorption device. Taking mixed cresol separation as an example, according to the molecular size of m-cresol and p-cresol, the corresponding molecular sieve adsorbent can be synthesized, the appropriate desorbent can be selected, and the corresponding process control can be carried out, so as to achieve the separation effect. Finally, the desorbent is removed, and the methyl phenol product with a purity of more than 99.5% is separated and refined from the mixed cresol. The desorbent can be recycled and reused, and the whole process has almost no environmental cost. At present, the synthesis and preparation of functional adsorbent is the main technical barrier of the method.

[0004] In the preparation process of molecular sieve adsorbent, ion exchange method is generally used to replace different ions to realize different adsorption functions and use scenarios. It is known that, compared with activated carbon, molecular sieve has not only developed voids, but also can realize adjustment of surface structure and pore size by changing the combined metal ions. This preparation process will release a large amount of adsorption heat when contacting with water vapor, which is easy to destroy the structure of the adsorbent. Compared with the kettle type exchange process, the column type exchange process is generally more thorough and easy to operate, so it is widely used. In the column type exchange process, the exchange column is first wetted with deionized water at a low air speed, and then contacted with the exchange liquid. The water consumption of this process is large. In addition, this process generally uses a jacket for heating, and the flange needs to be disassembled when loading and unloading the packing particles, which is extremely inconvenient, and the packing has poor flowability, which is time-consuming and labor-intensive. Therefore, it is urgent to develop a device and method to solve these problems. SUMMARY

[0005] In view of the existing technical deficiencies and equipment problems, the application discloses a kind of external preheating multistage adsorbent preparation system and method.

[0006] To achieve the above object, the technical scheme adopted by the application is as follows: a specially designed adsorbent preparation device is disclosed, which comprises a feed pipe and an exchange column. Inside the exchange column, from top to bottom, are sequentially arranged a guide plate, a distribution plate, a hopper, an inclined sieve plate and an isolation layer. The diffuser at one end of the feed pipe is inserted into the exchange column and sequentially penetrates the guide plate and the distribution plate. The bottom of the diffuser is concave and tapered. Elliptical holes are provided on the outer wall surface of the diffuser. The diameter or equivalent diameter of the guide plate is greater than the diameter or equivalent diameter of the feed pipe and less than the diameter or equivalent diameter of the distribution plate. The distribution plate and the inclined sieve plate each independently use a perforated plate with a pore size of 60-200 mesh. The inclination angle α of the inclined sieve plate is 10º-60º.

[0007] The application also discloses a preparation system for external preheating multistage adsorbent, which comprises n groups of ion exchange systems, a tail liquid tank, a recovery tank, a heat exchange tank and a control valve group. The ion exchange system comprises the ion exchange device and the heat exchange module.

[0008] The first main pipe is connected to the liquid inlet pipe of the ion exchange device. The liquid inlet pipe, the ion exchange device, the first liquid outlet pipe, the heat exchange module, the second liquid outlet pipe, the first circulating pump, the circulating pipe and the first branch pipe are sequentially connected to form a liquid circulation loop. The circulating pipe is connected to the recovery tank through the third branch pipe. The first liquid outlet pipe is connected to the tail liquid tank through the fourth branch pipe. The circulating pipe of the xth group of ion exchange systems is connected to the liquid inlet pipe of the x+1th group of ion exchange systems through the second branch pipe. The overflow port of the ion exchange device is connected to the tail liquid tank through the overflow pipe.

[0009] The second main pipe is connected to the inside of the heat exchange tank through the first heat exchange pipe, the first heat exchange branch pipe, the heat exchange module, the second heat exchange branch pipe and the second heat exchange pipe.

[0010] The heat exchange tank is connected to the liquid inlet pipe in sequence through the second circulating pump, the third heat exchange pipe and the fifth branch pipe, one branch of the third main pipe is connected to the heat exchange tank through the fourth heat exchange pipe, and the other branch is connected to the third heat exchange pipe.

[0011] The control valve group comprises valves arranged on the liquid inlet pipe, the first liquid outlet pipe, the second liquid outlet pipe, the circulating pipe, the first branch pipe, the second branch pipe, the third branch pipe, the fourth branch pipe, the first heat exchange pipe, the second heat exchange pipe, the third heat exchange pipe and the fourth heat exchange pipe.

[0012] Further, n is an integer not less than 4; the first heat exchange pipe is connected to the inner cavity of the heat exchange tank through the heat exchange pipe, the second heat exchange pipe and the fourth heat exchange pipe of the heat exchange tank.

[0013] Further, one end of the feed pipe extends into the exchange column through a feed cylinder at the top of the exchange column, the end position is a blind end, and a diffuser is designed, and the other end is an external filling port. The diffuser is suspended above the feed bin in sequence after penetrating the guide plate and the distribution plate, and the solid particles are sent to the feed bin.

[0014] Further, the diffuser adopts a cage structure, which is designed to enhance the smooth entry of particles through the feed pipe into the feed bin without affecting the uniform entry of exchange liquid into the feed bin.

[0015] Specifically, the diffuser is integrated with the feed pipe and adopts a cylindrical structure, and an oval opening is arranged on the outer wall, and a conical protrusion is formed in the bottom, which facilitates the dispersion of the particle materials to fly into the feed bin.

[0016] Specifically, the oval openings are evenly distributed in a ring shape on the outer wall of the diffuser, and the aperture size is 1.5-2.5 mm.

[0017] Further, the distribution plate is arranged above the feed bin, the side of the feed bin is provided with an overflow port, the lower part is provided with an inclined sieve plate, and a discharge port is arranged on the feed bin near the lower end of the inclined sieve plate. When filling, at least a certain height is required between the upper accumulation surface of the particle materials and the distribution plate. Specifically, the distance between the upper accumulation surface of the particle materials and the distribution plate is 5-20 mm.

[0018] Further, the feed cylinder at the top of the exchange column is provided with a liquid inlet, and the feed cylinder and the feed pipe form a liquid inlet cavity. The liquid flow enters through the liquid inlet, is distributed by the guide plate in the first stage and the distribution plate in the second stage, and then contacts the solid phase in the feed bin. The liquid flow passes through the isolation layer at the bottom of the exchange column and is discharged. The liquid flow in the exchange column is controlled by the valve group, and the process is completed by the circulating pump, and is divided into exchange tail liquid and recovered liquid.

[0019] Further, the heat exchange system comprises a preheating module, a heat exchange tank, a circulating pump, and a plurality of valve groups. In the preheating module, the liquid flow in the exchange column is heated through a water vapor pipeline. The water vapor condensate is sent to the heat exchange tank, which is used for heating the softened water pipeline and serving as a buffer temporary storage pool. Similarly, the water vapor condensate is sent to the heat exchange tank. The softened water with a certain temperature is sent to the inlet of each exchange column through the pump.

[0020] Further, the included angle between the inclined sieve plate and the horizontal plane is 25°-40°.

[0021] Further, the isolation layer is installed by using a movable clamp and comprises an upper sieve screen, a lower filter sieve screen, and a middle filler,

[0022] The filler is selected from one or more of glass balls, ceramic balls, alumina balls, and silicon carbide balls; the pore size of the filter sieve screen is greater than the diameter of the filler, and the diameter of the filler is 1.5-3 mm.

[0023] Further, the exchange column is installed in a circular cylinder or a square cylinder, and each exchange column is provided with a circulating pump, and the process conditions are realized through two groups of valve controls.

[0024] Further, the diameter of the guide plate is 1 / 3-3 / 4 of the diameter of the distribution plate; and the pore diameters of the guide plate and the distribution plate are independently 60-100 mesh.

[0025] Further, the water washing preheating temperature of the preheating module is 45-60℃, and the preheating temperature of the exchange liquid is 70-100℃.

[0026] Meanwhile, the application also provides a process method of a preparation system of an external preheating multi-stage adsorbent, which comprises the following steps:

[0027] Step 1, feeding, the adsorbent to be treated is loaded into a bin from the feeding pipe;

[0028] Step 2, wetting, the valve group on the liquid circulation loop is controlled, the exchange liquid is injected from the first main pipe, and the impurities are discharged from the overflow port;

[0029] Step 3, exchanging, the exchange liquid, steam, and softened water enter the system through the first main pipe, the second main pipe, and the third main pipe respectively, and multi-stage circulation exchange and multi-stage circulation heat exchange are realized in the system through different opening and closing states of the valve groups;

[0030] Step 4, discharging, the prepared adsorbent is discharged from the discharge port of the ion exchange device.

[0031] Further, the water washing preheating temperature of the preheating module is 45-60℃, and the preheating temperature of the exchange liquid is 70-100℃.

[0032] The application discloses an adsorbent preparation device, and has a unique structure of double channels inside and outside, a solid phase channel is provided with a diffuser, which is convenient to assemble and disassemble, does not affect the circulation of liquid phase materials in the system, ensures uniform material filling, a liquid phase channel is provided with two-stage distributors, exchange liquid uniformly enters the bin, fully exchanges mass transfer with solid phase particles, and the exchange efficiency and the quality of the adsorbent are improved. In addition, by arranging the inclined screen plate with a special inclined angle, the material can be discharged without disassembling the exchange column, a certain space is reserved between the inclined screen plate and the isolation layer, the exchange column can be recycled without disassembling.

[0033] The application provides a multi-stage adsorbent preparation system with external preheating, which effectively solves the problems of high local temperature, serious material caking and large water consumption in traditional column exchange. At the same time, a multi-stage process method with external preheating is proposed, which controls different process sections by compiling the switch state sequence of different program-controlled valves, realizes rapid material loading and unloading, has high degree of continuity, and greatly reduces the labor operation cost.

[0034] At the same time, a process method is also proposed, which can realize multi-dimensional application according to the working condition requirements, is suitable for synthesis of different functional adsorbents in industrial production, and has great applicability and practicability. BRIEF DESCRIPTION OF DRAWINGS

[0035] Figure 1 It is a structural schematic view of an adsorbent preparation device.

[0036] Figure 2 It is Figure 1 It is a partial structural schematic view of a feed pipe.

[0037] Figure 3 It is a process diagram of a multi-stage adsorbent preparation system with external preheating.

[0038] In the figure, 1 is an adsorbent preparation device, 2 is a heat exchange module, 3 is a first circulating pump, 4 is a second circulating pump, 5 is a heat exchange tank, 6 is a tail liquid tank, 7 is a recovery tank, 8 is a first main pipe, 9 is a second main pipe, 10 is a third main pipe, 11 is a liquid inlet pipe, 12 is a first liquid outlet pipe, 13 is a second liquid outlet pipe, 14 is a circulating pipe, 15 is a first branch pipe, 16 is a second branch pipe, 17 is a third branch pipe, 18 is a fourth branch pipe, 19 is a fifth branch pipe, 20 is a first heat exchange pipe, 21 is a first heat exchange branch pipe, 22 is a second heat exchange branch pipe, 23 is a second heat exchange pipe, 24 is a third heat exchange pipe, 25 is a fourth heat exchange pipe, 26-1 is a first valve, 26-2 is a second valve, 26-3 is a third valve, 26-4 is a fourth valve, and 27 is an overflow pipe.

[0039] a, first liquid discharge valve; b, first liquid inlet valve; c, second liquid inlet valve; d, third liquid inlet valve; e, fourth liquid inlet valve; f, second liquid discharge valve; h, circulation valve; i, first heat exchange valve; j, third liquid discharge valve.

[0040] 101, exchange column; 102, guide plate; 103, distribution plate; 104, bin; 105, inclined sieve plate; 106, isolation layer; 107, sieve; 108, filler; 109, movable clamp lock; 110, cylinder; 111, liquid inlet; 112, feed pipe; 113, diffuser; 114, oval hole; 115, conical protrusion; 116, overflow; 117, discharge port. DETAILED DESCRIPTION

[0041] The advantages and features of the present application will be further described in the preferred embodiments in conjunction with the accompanying drawings, so that the protection scope of the present application can be more clearly and definitely defined by those skilled in the art.

[0042] Figure 3 A structure diagram of a preparation system of an external preheating multi-stage adsorbent is shown. In the diagram, the preparation system of the external preheating multi-stage adsorbent includes four groups of ion exchange systems, a tail liquid tank 6, a recovery tank 7, a heat exchange tank 5 and a control valve group, and each ion exchange system includes an ion exchange device 1 and a heat exchange module 2.

[0043] A first main pipe 8 is connected to a liquid inlet pipe 11 of the ion exchange device 1, the liquid inlet pipe 11, the ion exchange device 1, a first liquid discharge pipe 12, the heat exchange module 2, a second liquid discharge pipe 13, a first circulation pump 3, a circulation pipe 14 and a first branch pipe 15 are sequentially connected to form a liquid circulation loop, the circulation pipe is connected to the recovery tank 7 through a third branch pipe 17, the first liquid discharge pipe 12 is connected to the tail liquid tank 6 through a fourth branch pipe 18, the circulation pipe 14 of the xth group of ion exchange systems is connected to the liquid inlet pipe 11 of the x+1th group of ion exchange systems through a second branch pipe 16, and the overflow port of the ion exchange device 1 is connected to the tail liquid tank 6 through an overflow pipe 27.

[0044] A second main pipe 9 is connected to the inside of the heat exchange tank 5 through a first heat exchange pipe 20 which is partially wound outside the heat exchange tank 5, connected to the inside of the heat exchange tank 5 through a first heat exchange branch pipe 21, the heat exchange module 2, a second heat exchange branch pipe 22 and a second heat exchange pipe 23.

[0045] The heat exchange tank 5 is sequentially connected to the liquid inlet pipe 11 through a second circulation pump 4, a third heat exchange pipe 24 and a fifth branch pipe 19, one branch of a third main pipe 10 is connected to the heat exchange tank 5 through a fourth heat exchange pipe 25, and the other branch is connected to the third heat exchange pipe 24.

[0046] The control valve group comprises a liquid inlet pipe 11, a first liquid outlet pipe 12, a circulation pipe 14, a first branch pipe 15, a second branch pipe 16, a third branch pipe 17, a fourth branch pipe 18, a fifth branch pipe 19, a first heat exchange pipe 20, a second heat exchange pipe 23, a third heat exchange pipe 24, a fourth heat exchange pipe 25, and valves arranged on the overflow pipe 27.

[0047] The first heat exchange pipe 20, the second heat exchange pipe 23, the third heat exchange pipe 24, and the fourth heat exchange pipe 25 are respectively provided with a first valve 26-1, a second valve 26-2, a third valve 26-3, and a fourth valve 26-4. The overflow pipe 27, the first branch pipe 15, the liquid inlet pipe 11, the fifth branch pipe 19, the second branch pipe 16, the third branch pipe 17, the circulation pipe 14, the first heat exchange branch pipe 21, the first liquid outlet pipe 12, and the fourth branch pipe 18 of each group of ion exchange systems are respectively provided with a first liquid outlet valve a, a first liquid inlet valve b, a second liquid inlet valve c, a third liquid inlet valve d, a fourth liquid inlet valve e, a second liquid outlet valve f, a circulation valve h, a first heat exchange valve i, and a third liquid outlet valve j. In order to distinguish the corresponding valves of the four groups of ion exchange systems, a1-j1, a2-j2, a3-j3, and a4-j4 are used as valve numbers of the first to fourth groups of ion exchange systems, respectively.

[0048] The adsorbent preparation device comprises a feed pipe 112 and an exchange column 101, the inside of the exchange column 101 is sequentially provided, from top to bottom, with a guide plate 102, a distribution plate 103, a bin 104, an inclined sieve plate 105, and an isolation layer 106; an expander 113 at one end of the feed pipe 112 extends into the exchange column through a feed cylinder 110 and sequentially penetrates the guide plate 102 and the distribution plate 103 to hang directly above the bin 104; the guide plate 102 is fixed on the feed pipe 112; the bottom of the expander 113 is concave and tapered to form a convex portion 115; and an oval hole 114 with a diameter of 2 mm is arranged on the outer wall surface of the expander 113; the diameter of the guide plate 102 is 1 / 2 of the diameter of the distribution plate 103; the distribution plate 103 and the inclined sieve plate 105 are both made of a 100-mesh hole plate; the inclination angle α of the inclined sieve plate 105 is 30°. 。 The feed cylinder 110 at the top of the exchange column is provided with a liquid inlet 111; the upper part of the bin 104 is provided with an overflow port 116; the lower part of the bin 104 is provided with the inclined sieve plate 105; and the bin is connected with the lower end of the inclined sieve plate to form a discharge port 117.

[0049] The isolation layer 106 comprises upper and lower screen meshes 107 and filler 108 in the middle part; the holes of the screen meshes 107 are smaller than the diameter of the filler; the filler 108 is made of alumina balls with a diameter of 1.5-3 mm; and the left and right sides of the isolation layer 106 are respectively installed at the bottom of the exchange column through live clamps 109. Example 1

[0050] As Figures 1-3Four ion exchange systems were used, with the exchange column having a specification of φ200x4000 mm; the feed inlet was φ60 mm; the adsorption packing material was NaY, the exchange solution was 0.65 mol / L KNO3 solution, and the preheating module temperature was 100±5 ℃; a 10 mm exchange solution layer was maintained between the adsorbent packing material and the distribution plate.

[0051] All valves are closed by default and are automatically controlled by a programmable controller. Two circulation pumps provide power. After the exchange column is humidified, valves h1-h4 and c1-c4 are opened, and steam is used to heat the exchange liquid in the preheating module to 100°C. Open valves g1-g4, b1-b4, and i1-i4 until they reach 5-10 times the bed volume (BV) of their own circulation. Then switch valves e1-e4 to the open state to achieve multi-stage series connection. Before this, control the on / off state of valves f1-f4 to discharge all into the recovery tank. Starting with the first set of separation columns, when 10-25 times BV is accumulated, switch valves i1-i4 to the closed state and valves j1-j4 to the open state to discharge all into the tail liquid tank. The tail liquid tank contains a high concentration of sodium ion solution. When 25-35 times BV is accumulated, close valves c1-c4 and switch valves d1-d4 to discharge 25-35 times BV from 40-50% of the heat exchange tank. The softened water completes the washing process, and all liquid is discharged into a recovery tank, which contains high-concentration potassium. + The solution is then discharged from the outlet. The exchanged adsorbent is discharged through the outlet. The exchange column is symmetrically arranged with all outlets facing each other, making operation easier.

[0052] The name of the product after the exchange is Adsorbent A;

[0053] Different control logics can be loaded according to process requirements. Typical valve group control methods are as follows:

[0054] Table 1 Valve manifold on / off status list

[0055]

[0056] Note: √ in the table represents the valve is open, and x represents the valve is closed.

[0057] The typical functionalities of each process are as follows:

[0058] Step 1 (Pre-wetting): This step mainly wets the solid adsorbent to be treated in each newly loaded exchange column to reduce the damage to the microstructure caused by the exothermic adsorption in the subsequent steps. At the same time, it pushes out the powdered impurities adsorbed by electrostatics through the overflow port. Therefore, it can also be called "top water".

[0059] Step sequence 2 (exchange): This section is mainly used for exchanging with the adsorbent in each exchange column by using the exchange solution, providing power through the pump body, and obtaining the required process temperature by external heating.

[0060] Step sequence 3 (series): This section mainly connects multiple exchange columns in series to use the tail liquid of the previous exchange column to improve the utilization rate of the exchange solution.

[0061] Step sequence 4 (cutting): This section continues step sequence 3 (series), and the concentration of metal ions in the tail liquid of each exchange column appears a gradient change, constantly enriches, and reaches a dynamic balance. In order to further improve the exchange degree, a part of the tail liquid of the exchange solution is "cut off" from the system, and the remaining part is exchanged for a period of time to achieve the best effect.

[0062] Step sequence 5 (washing): This section is a continuation of step sequence 4 (cutting), which washes the free metal ions of the pre-product, and finally collects the product from the discharge port in turn.

[0063] Softened water is directly connected to the exchange device for washing the adsorbent, and can also enter the heat exchange tank to exchange heat with condensed water and steam before entering the ion exchange device to wash the adsorbent. Example 2

[0064] The method of example 1 is repeated, the adsorption filler is 13X, and the exchange solution is 0.12 mol / L KCl, 0.43 mol / L BaCl2, and the preheating module temperature is 85±5 ℃; the product after exchange is named adsorbent B; Example 3

[0065] The method of example 1 is repeated, the adsorption filler is 13X, the exchange solution is 1.2 mol / L LiCl solution, and the preheating module temperature is 90±5 ℃; the product after exchange is named adsorbent C; Example 4

[0066] The method of example 1 is repeated, the adsorption filler is 13X, the exchange solution is 0.22 mol / L Ba(NO3)2 solution, and the preheating module temperature is 95±5 ℃; the product after exchange is named adsorbent D; Example 5

[0067] The exchange degree, adsorption capacity and specific surface area of the molecular sieves prepared in examples 1-4 are measured, and the specific test method is as follows:

[0068] The exchange degree a (%) of the molecular sieve adsorbents of examples 1-4 is analyzed by using the X Axios Max type X-ray fluorescence analyzer (XRF) of the Netherlands PANAnalytical company,

[0069] The following formula (1) is used for calculation:

[0070] (1) ;

[0071] Wherein, m1, the mass fraction of metal ion after exchange (%); m2, the mass fraction of metal ion before exchange (%);

[0072] Adsorption capacity τ (mg / g): 25 g of each of the adsorbents A, B, C and D prepared in Examples 1, 2, 3 and 4 was respectively taken into a 250 ml reaction kettle, then 200 ml of a mixture containing 5wt% of p-cresol and 5wt% of m-cresol was injected into the reaction kettle using n-heptane as a solvent, nitrogen was filled to 0.8-1.0 Mpa, and the reaction kettle was put into an oven for constant temperature at 150±5 ℃ for 1-2 h; the concentration of adsorbate cresol in the liquid phase before and after adsorption was analyzed by Agilent GC7820 gas chromatography area normalization method (area%).

[0073] The following formula (2) was used for calculation:

[0074] τ (mg / g) (2) ;

[0075] Wherein, C0, Ci, are the concentrations of the liquid phase before and after adsorption (%); ρ, the density of the adsorbate (g / cm 3 ); V, the volume of the liquid phase (ml); M, the adsorbent dosage (g)

[0076] Specific surface area S BET (m 2 / g): The specific surface area and pore size analyzer produced by Micromeritics Company was used to determine the specific surface area at 77.4 K by N2 adsorption method after degassing at 350 ℃ for 4 h.

[0077] Table 2: Example data table

[0078]

[0079] It can be known from the data in Table 2 that the functional adsorbent prepared by using the external preheating multi-stage adsorbent preparation system and the method thereof has good adsorption activity and adsorption capacity.

[0080] The above only describes the embodiments of the present application, and does not limit the patent scope of the present application, and any equivalent structure or equivalent process transformation using the content of the specification and drawings of the present application, or direct or indirect application in other related technical fields, are also included in the patent protection scope of the present application.

Claims

1. A preparation system of external preheating multistage adsorbent, comprising n sets of ion exchange system, tail liquid tank, recovery tank, heat exchange tank and control valve group, characterized in that, The ion exchange system comprises an ion exchange device and a heat exchange module; The first main pipe is connected with the liquid inlet pipe of the ion exchange device, the liquid inlet pipe, the ion exchange device, the first liquid outlet pipe, the heat exchange module, the second liquid outlet pipe, the first circulating pump, the circulating pipe, the first branch pipe are sequentially connected to form a liquid circulating loop, the circulating pipe is connected with the recovery tank through the third branch pipe, the first liquid outlet pipe is connected with the tail liquid tank through the fourth branch pipe, the circulating pipe of the xth ion exchange system is connected with the liquid inlet pipe of the x+1th ion exchange system through the second branch pipe, the overflow port of the ion exchange device is connected with the tail liquid tank through the overflow pipe; The second main pipe is connected with the inside of the heat exchange tank through the first heat exchange pipe, the first heat exchange branch pipe, the heat exchange module, the second heat exchange branch pipe and the second heat exchange pipe; The heat exchange tank is sequentially connected with the liquid inlet pipe through the second circulating pump, the third heat exchange pipe and the fifth branch pipe, one branch of the third main pipe is connected with the heat exchange tank through the fourth heat exchange pipe, and the other branch is connected with the third heat exchange pipe; The control valve group comprises valves arranged on the liquid inlet pipe, the first liquid outlet pipe, the second liquid outlet pipe, the circulating pipe, the first branch pipe, the second branch pipe, the third branch pipe, the fourth branch pipe, the first heat exchange pipe, the second heat exchange pipe, the third heat exchange pipe and the fourth heat exchange pipe; n is an integer not less than 4; The ion exchange device comprises a feed pipe and an exchange column, the inside of the exchange column is sequentially provided with a guide plate, a distribution plate, a bin, an inclined sieve plate and a separation layer from top to bottom; the diffuser at one end of the feed pipe is inserted into the exchange column and sequentially penetrates the guide plate and the distribution plate, the bottom of the diffuser is concave and forms a conical protrusion, and the outer wall surface is provided with elliptical holes with a pore size of 1.5-2.5 mm; the diameter or equivalent diameter of the guide plate is 1 / 3-3 / 4 of the diameter or equivalent diameter of the distribution plate; The distribution plate and the inclined sieve plate are independently provided with hole plates with a pore size of 60-200 mesh, and the inclined angle α of the inclined sieve plate is 25°-40°.

2. A system for the preparation of an externally preheated multistage adsorbent according to claim 1, characterized in that, The bin at the top of the exchange column is provided with a liquid inlet, the upper part of the bin is provided with an overflow port, the lower part of the bin is provided with the inclined sieve plate, and the bin is connected with the lower end of the inclined sieve plate and is provided with a discharge port.

3. The system for preparing an externally preheated multistage adsorbent according to claim 1, characterized in that, The separation layer comprises two sieve screens at the upper and lower parts and a filler at the middle part, and the separation layer is installed at the bottom of the exchange column through a live clamp lock; The filler is selected from at least one of glass balls, ceramic balls, alumina balls and silicon carbide balls with a diameter of 1.5-3 mm; The pore size of the sieve screen is smaller than the diameter of the filler.

4. The process for the preparation of an external preheating multistage adsorbent system according to any one of claims 1-3, characterized in that, The method comprises the following steps: Step 1, feeding, the adsorbent to be treated is loaded into the bin from the feed pipe; Step 2, wetting, the valve group on the liquid circulating loop is controlled, the exchange liquid is injected from the first main pipe, and the impurities are discharged from the overflow port; Step 3, exchange, the exchange liquid, steam and softened water are respectively introduced into the system through the first main pipe, the second main pipe and the third main pipe, and multi-stage circulating exchange and multi-stage circulating heat exchange are carried out in the system through different opening and closing states of the valve group; Step 4, discharging, the prepared adsorbent is discharged from the discharge port of the ion exchange device.

5. A process for the preparation of an externally preheated multi-stage adsorbent system as claimed in claim 4, wherein, Step 3 comprises: Exchange step: power is provided by the circulating pump, the exchange liquid enters the adsorbent in each ion exchange device through the liquid inlet pipe and is heated externally to obtain the required process temperature; Series step: control the valve group, connect multiple ion exchange devices in series, use the tail liquid of the previous ion exchange device, and improve the utilization rate of the exchange liquid; Cutting step: the concentration of metal ions in the exchange tail liquid of each ion exchange device shows a gradient change, constantly enriches, and reaches a dynamic balance. In order to improve the exchange degree, a part of the exchange tail liquid is "cut off" from the system, and the remaining part is repeatedly circulated and exchanged; Washing step: after washing the excess free metal ions, the finished product is discharged.

6. A process for the preparation of an externally preheated multi-stage adsorbent system according to claim 5, characterized in that, Through the valve group, the heating steam, the condensed water after heat exchange with the exchange liquid, and the softened water are integrated for heat exchange in the heat exchange tank, and then used for the washing step.

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