A reaction apparatus and a reaction method for preparing a low-sodium aluminum sol

By combining the design of the reaction vessel and the ion exchange column, continuous preparation of aluminum sol and removal of sodium ions were achieved, solving the problem of difficult sodium ion removal in the preparation of aluminum sol in the existing technology, improving the yield and removal effect of aluminum sol, and reducing the cost.

CN120860968BActive Publication Date: 2025-12-23SHANDONG ZHANCHI NEW MATERIALS CO LTD +1
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Patent Information

Application Number
CN202511379999.X
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2025-09-25
Publication Date
2025-12-23
Estimated Expiration
2045-09-25

AI Technical Summary

Technical Problem

In the preparation of aluminum sol, existing technologies have difficulty in effectively removing sodium ions, leading to performance degradation. Furthermore, traditional removal methods are costly or prone to clogging of ion exchange columns.

Method used

Design a reaction apparatus including a reaction vessel, a fixed hood, and an annular hood, to continuously remove sodium ions through an ion exchange column, and combine a cooling jacket to control temperature and impurity separation, thereby realizing the continuous preparation of aluminum sol and the removal of sodium ions.

Benefits of technology

This method enables efficient and continuous preparation of aluminum sol, reduces costs, avoids clogging of ion exchange columns, improves aluminum sol yield and sodium ion removal efficiency, and features a high degree of device integration.

✦ Generated by Eureka AI based on patent content.

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Abstract

The application discloses a reaction equipment for preparing low-sodium aluminum sol and relates to the technical field of chemical equipment. The reaction equipment comprises a reaction kettle, and an inner cavity for aluminum sol preparation reaction is arranged in the reaction kettle. The application further discloses a reaction method of the reaction equipment for preparing low-sodium aluminum sol, which comprises the following steps: aluminum sol generation, aluminum sol transfer, product discharge and back flushing. The reaction kettle, the fixing cover and the annular cover are arranged, the aluminum and the hydrochloric acid are reacted in the reaction kettle to generate the colloidal solution of the aluminum sol, the aluminum sol colloid is in the nano-particle state after being generated, the colloidal solution of the aluminum sol colloid is directly transferred into the annular cover, the colloidal solution of the aluminum sol colloid in the nano-particle state passes through the ion exchange column in the annular cover, the sodium ions in the colloidal solution of the aluminum sol colloid are adsorbed and separated by the strong-acid cation exchange resin in the ion exchange column, and thus the low-sodium aluminum sol can be obtained.
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Description

TECHNICAL FIELD

[0001] The present application relates to the technical field of chemical equipment, in particular to a reaction device and a reaction method for preparing low-sodium aluminum sol. BACKGROUND

[0002] Aluminum sol is an important inorganic colloidal material, which is widely used in catalyst carrier, ceramic binder, refractory binder, paper sizing agent, textile aid and other fields. The core is to convert aluminum compounds into stable and dispersed nano or sub-micron hydrated aluminum oxide colloidal particles.

[0003] In the prior art, aluminum sol is prepared by continuous reaction of hydrochloric acid and metal aluminum. Aluminum chloride is generated by acidolysis reaction of metal aluminum and hydrochloric acid, and then aluminum sol colloid is generated by hydrolysis and polymerization of aluminum chloride. However, in the process of preparing aluminum sol by reaction of hydrochloric acid and metal aluminum, sodium ions are carried by sodium impurities in raw aluminum, sodium hydroxide for acid-base adjustment, and sodium salt in process water. When the aluminum sol colloid is formed, the sodium ions will be mixed with the aluminum sol colloid under the action of charge adsorption. For the use in electronic packaging and high-temperature bonding, the migration of sodium ions in the aluminum sol will cause its performance degradation. Therefore, how to remove the sodium ions in the aluminum sol is particularly important when the aluminum sol is prepared by hydrochloric acid and metal aluminum.

[0004] In the prior art, the sodium ions in the aluminum sol are generally removed by electrodialysis or resin adsorption. However, the cost of removing the sodium ions in the aluminum sol by electrodialysis is high, and the electrodialysis membrane needs to be cleaned regularly, which has high maintenance cost. When the sodium ions in the aluminum sol are removed by resin adsorption, the aluminum sol needs to be transported separately to the ion exchange column storing the resin after being formed. During the transportation process, the aluminum sol colloid is aggregated due to aging, and the colloid of the aluminum sol is easy to block the resin in the ion exchange column after aggregation, which causes irreversible damage to the ion exchange column.

[0005] Therefore, it is necessary to invent a reaction device and a reaction method for preparing low-sodium aluminum sol to solve the above problems. SUMMARY

[0006] The purpose of the present application is to provide a reaction device and a reaction method for preparing low-sodium aluminum sol to solve the problems raised in the background.

[0007] To achieve the above purpose, the present application provides the following technical scheme: a reaction device for preparing low-sodium aluminum sol, comprising:

[0008] A reaction kettle is arranged inside the reaction kettle and is used for aluminum sol preparation reaction.

[0009] The fixed cover is arranged at the top end of the reaction kettle and communicates with the inner cavity of the reaction kettle, a middle part of the fixed cover is fixedly provided with an annular cover, a plurality of treatment grooves are arranged around the inner part of the annular cover, circular through grooves are arranged at both ends of the treatment grooves, ion exchange columns are arranged in the inner part of the treatment grooves, both ends of the ion exchange columns respectively communicate with the two circular through grooves, a transition cavity is arranged at the top end of the annular cover, the circular through grooves at the top end of the plurality of treatment grooves communicate with the transition cavity, a plurality of material extraction pipes are arranged around the inner part of the annular cover, and the bottom end of the material extraction pipe is located in the inner part of the reaction kettle, a material return pipe is fixedly arranged outside the annular cover, one end of the material return pipe communicates with the material extraction pipe, and the other end of the material return pipe communicates with the transition cavity, and the aluminum sol colloidal solution generated by the reaction in the inner part of the reaction kettle is introduced into the ion exchange column through the material extraction pipe and the material return pipe to complete the adsorption and separation of sodium ions.

[0010] Preferably, a material pump is fixedly arranged at the top end of the outer wall of the fixed cover, an input end of the material pump is fixedly provided with a connecting pipe, the plurality of material extraction pipes communicate with the connecting pipe, and an output end of the material pump communicates with the material return pipe.

[0011] Preferably, a stirring rod is rotatably arranged at the middle part of the top end of the fixed cover, a positive and negative motor is arranged at the top end of the stirring rod, the positive and negative motor is used to drive the stirring rod to rotate forward to complete solution stirring in the early stage of the reaction, the positive and negative motor is used to drive the stirring rod to rotate reversely to complete colloidal aggregation in the late stage of the reaction, a stirring blade is fixedly arranged at the bottom end of the stirring rod, the stirring blade is provided with two groups of upper and lower stirring blades, and the two groups of stirring blades are provided in an inclined structure.

[0012] A material guide plate is provided with a plurality of groups and is arranged around the inner part of the reaction kettle, and the material guide plate is used to cooperate with the stirring rod to collect and gather aluminum sol colloidal particles.

[0013] Preferably, an extension plate is fixedly arranged on the side of the material guide plate away from the inner wall of the reaction kettle, an inclination angle is arranged between the extension plate and the material guide plate, an ear plate is fixedly arranged on the side of the extension plate away from the material guide plate, an inclination angle is arranged between the ear plate and the extension plate, and a plurality of material passing grooves are sequentially arranged from bottom to top in the middle part of the extension plate.

[0014] Preferably, a support rod is fixedly arranged on the side of the material guide plate close to the reaction kettle, positioning rings are sleeved and arranged at both ends of the support rod, and the positioning rings are fixedly arranged on the inner wall of the reaction kettle, a plurality of support blocks are fixedly arranged on the side of the material guide plate close to the reaction kettle, the support blocks are provided in an arc-shaped structure, and the support blocks are located on the side of the material guide plate away from the extension plate.

[0015] Preferably, a cooling jacket is fixedly arranged on the inner side of the annular cover, the cooling jacket communicates with the inner part of the annular cover, the plurality of material extraction pipes are arranged in the inner part of the cooling jacket, and second jacket nozzles are fixedly arranged at both sides of the top end of the cooling jacket.

[0016] Preferably, the middle part of the extraction pipe is fixedly provided with a plurality of heat-conducting fins, the plurality of heat-conducting fins are in a spiral structure, and the plurality of heat-conducting fins are arranged in the interior of the cooling jacket.

[0017] Preferably, the temperature control jacket is arranged on the outer side of the reaction kettle, is used for controlling the reaction temperature in the reaction kettle, and is fixedly provided with first jacket nozzles on both sides.

[0018] Preferably, a fixing seat is detachably connected to the slot of the treatment tank, a circular insertion groove is arranged in the middle part of the fixing seat, the ion exchange column is detachably inserted into the circular insertion groove, an observation window is arranged on the outer side of the fixing seat, and the fixing seat is used for mounting and fixing the ion exchange column in the treatment tank.

[0019] The bottom end of the annular cover is fixedly provided with a storage cavity, the bottom end of the storage cavity is fixedly provided with a discharge valve and a backflush valve, and the outer side wall of the transition cavity is fixedly provided with a waste discharge valve.

[0020] A reaction method of a reaction device for preparing low-sodium aluminum sol, comprising the following steps:

[0021] Step one, aluminum sol generation, raw aluminum and hydrochloric acid are injected into a reaction kettle, the raw aluminum is dissolved in the hydrochloric acid to form aluminum chloride, water is injected into the reaction kettle, and the aluminum chloride undergoes hydrolysis and polymerization to generate aluminum sol colloid; sodium ion salt is mixed in the generated aluminum sol colloid in this process; in this process, sodium hydroxide is added to the mixed solution to control the pH value to be between 2 and 3.

[0022] Step two, aluminum sol transfer, the initially formed aluminum sol colloid is transported to a transition cavity through an extraction pipe and a return pipe, the aluminum sol colloid mixed solution in the transition cavity passes through a plurality of ion exchange columns, and sodium ion salt in the aluminum sol colloid solution is adsorbed by strong acidic cation exchange resin in the ion exchange columns, so that the aluminum sol colloid solution is converted into a low-sodium aluminum sol colloid solution.

[0023] Step three, product discharge, the low-sodium aluminum sol colloid solution is discharged and guided to an aging tank for aging treatment.

[0024] Step four, backflush, the ion exchange column is backflushed by using dilute hydrochloric acid to regenerate the strong acidic cation exchange resin, and thus one preparation cycle of the low-sodium aluminum sol is completed.

[0025] Technical effects and advantages of the present application:

[0026] 1. The present application is provided with a reaction kettle, a fixed cover and an annular cover, aluminum and hydrochloric acid react in the reaction kettle to form an aluminum sol colloid solution, the aluminum sol colloid is in a nanoparticle state after formation, at this time the aluminum sol colloid solution is directly transferred to the annular cover, the aluminum sol colloid solution in the nanoparticle state passes through the ion exchange column in the annular cover, the sodium ions in the aluminum sol colloid solution are adsorbed and separated by the strong acid cation exchange resin in the ion exchange column, so that low-sodium aluminum sol can be obtained, compared with the prior art, the present application realizes continuous preparation of aluminum sol and removal of sodium ions, avoids resin blockage in the ion exchange column caused by aging and convergence of the aluminum sol colloid during the conveying process, improves the yield of the aluminum sol colloid while ensuring the removal effect of sodium ions, and the device has high integration degree and low cost;

[0027] 2. The present application is provided with a cooling jacket, the aluminum sol colloid solution passes through the cooling jacket during the transfer process, the coolant injected into the cooling jacket can realize rapid cooling of the aluminum sol colloid solution, so as to achieve the effect of inhibiting the aging of the aluminum sol colloid, at the same time, the coolant jacket can also control the temperature of the environment where the ion exchange column is located, so as to ensure the working environment of the strong acid cation exchange resin when adsorbing sodium ions, and thus ensure the removal effect of sodium ions in the aluminum sol colloid solution;

[0028] 3. The present application is provided with an annular cover, a transition cavity and a storage cavity, the annular cover, the transition cavity and the storage cavity together form a conveying channel for the aluminum sol colloid, and when the aluminum sol colloid is transferred after being generated, part of the undissolved impurities are extracted into the transition cavity under the action of centrifugal force along with the aluminum sol colloid, the undissolved impurities stay in the transition cavity because they cannot pass through the ion exchange column, and after the aluminum sol colloid removes the sodium ions, dilute hydrochloric acid can be injected through the storage cavity to realize backflushing and regeneration of the ion exchange column, in this process, the undissolved impurities remaining in the transition cavity can be discharged along with the backflushing solution, so as to realize synchronous cleaning of the residual impurities in the reaction process, so as to facilitate continuous operation and production of the device. BRIEF DESCRIPTION OF DRAWINGS

[0029] Figure 1 It is a schematic diagram of the overall structure of the present application.

[0030] Figure 2 It is a schematic diagram of the overall structure of the present application.

[0031] Figure 3 It is a schematic diagram of the motion trajectory of the aluminum sol colloid solution of the present application.

[0032] Figure 4 It is a schematic diagram of the internal structure of the fixed cover of the present application.

[0033] Figure 5 It is a schematic diagram of the internal structure of the fixed cover of the present application.

[0034] Figure 6 This is a schematic diagram of the internal structure of the reactor of the present invention.

[0035] Figure 7 For the present invention Figure 6 Enlarged schematic diagram of the structure at point A in the middle.

[0036] Figure 8 This is a schematic diagram of the guide plate structure of the present invention.

[0037] Figure 9 This is a schematic diagram of the ion exchange column and fixture structure of the present invention.

[0038] In the diagram: 1. Reactor; 2. Fixed cover; 3. Annular cover; 31. Processing tank; 32. Circular through-slot; 33. Ion exchange column; 3301. Fixed base; 3302. Circular slot; 3303. Observation window; 34. Transition chamber; 341. Waste discharge valve; 35. Feed pipe; 3501. Heat-conducting fins; 351. Connecting pipe; 352. Material pump; 36. Return pipe; 37. Storage chamber; 371. Discharge valve; 372. Backflush valve; 4. Cooling jacket; 41. Second jacket nozzle; 5. Stirring rod; 51. Forward and reverse motor; 52. Stirring blade; 6. Guide plate; 601. Support rod; 602. Positioning ring; 61. Extension plate; 611. Feed trough; 62. Ear plate; 63. Support block; 7. Temperature control jacket; 71. First jacket nozzle. Detailed Implementation

[0039] The technical solutions of the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings. Obviously, the described embodiments are only some embodiments of the present invention, and not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those skilled in the art without creative effort are within the scope of protection of the present invention. Example 1

[0040] like Figures 1 to 3 As shown, the reaction apparatus for preparing low-sodium aluminum sol provided by the present invention is essentially a reaction apparatus that can continuously carry out the preparation of aluminum sol colloid and the removal of sodium ion salt. By setting up a reaction vessel 1, a fixed cover 2 and an annular cover 3, metallic aluminum and hydrochloric acid react in the reaction vessel 1 to generate a colloidal solution of aluminum sol. After the aluminum sol colloid is generated, it is in a nanoparticle state. At this time, the aluminum sol colloidal solution is directly transferred into the annular cover 3. The aluminum sol colloidal solution in the nanoparticle state passes through the ion exchange column 33 in the annular cover 3. The sodium ions in the aluminum sol colloidal solution are adsorbed and separated by the strong acid cation exchange resin in the ion exchange column 33, thereby obtaining low-sodium aluminum sol.

[0041] In the specific structural installation, the structural body can be constructed according to the inventive concept of the embodiment, and in the embodiment, no specific limitation is made.

[0042] In the embodiment, a reaction device for preparing low-sodium aluminum sol includes:

[0043] The reaction kettle 1 is internally provided with an inner cavity for an aluminum sol preparation reaction;

[0044] The fixed cover 2 is arranged at the top end of the reaction kettle 1 and communicates with the inner cavity of the reaction kettle 1. The middle part of the fixed cover 2 is fixedly provided with an annular cover 3. A plurality of treatment tanks 31 are arranged around the inside of the annular cover 3. Circular through grooves 32 are arranged at both ends of the treatment tanks 31. Ion exchange columns 33 are arranged in the treatment tanks 31. The two ends of the ion exchange columns 33 respectively communicate with the two circular through grooves 32. A transition cavity 34 is arranged at the top end of the annular cover 3. The circular through grooves 32 at the top ends of the plurality of treatment tanks 31 all communicate with the transition cavity 34. A plurality of material extraction pipes 35 are arranged around the inside of the annular cover 3, and the bottom ends of the material extraction pipes 35 are located in the inside of the reaction kettle 1. A material return pipe 36 is fixedly arranged at the outside of the annular cover 3. One end of the material return pipe 36 communicates with the material extraction pipe 35, and the other end of the material return pipe 36 communicates with the transition cavity 34. The aluminum sol colloidal solution generated by the reaction in the inside of the reaction kettle 1 enters the ion exchange columns 33 through the material extraction pipe 35 and the material return pipe 36 to complete the adsorption and separation of sodium ions;

[0045] The bottom end of the annular cover 3 is fixedly provided with a material storage cavity 37. The bottom end of the material storage cavity 37 is fixedly provided with a material discharge valve 371 and a backflush valve 372. The bottom end of the outer side wall of the transition cavity 34 is fixedly provided with a waste discharge valve 341. The waste discharge valve 341 is used to discharge the solution backflushed from the ion exchange columns 33;

[0046] The top end of the outer side wall of the fixed cover 2 is fixedly provided with a material pump 352. The input end of the material pump 352 is fixedly provided with a connecting pipe 351. The plurality of material extraction pipes 35 all communicate with the connecting pipe 351. The output end of the material pump 352 communicates with the material return pipe 36. The material pump 352 is used to realize the transfer of the aluminum sol colloidal solution;

[0047] The treatment tank 31 is provided with a fixed seat 3301 at the tank opening. A circular insertion groove 3302 is arranged at the middle part of the fixed seat 3301. The ion exchange column 33 is detachably inserted into the circular insertion groove 3302. An observation window 3303 is arranged at the outside of the fixed seat 3301. The fixed seat 3301 is used to realize the installation and fixation of the ion exchange column 33 in the treatment tank 31;

[0048] The temperature control jacket 7 is arranged at the outside of the reaction kettle 1. The temperature control jacket 7 is used to control the reaction temperature in the inside of the reaction kettle 1. First jacket nozzles 71 are fixedly arranged at both sides of the temperature control jacket 7. The first jacket nozzles 71 are used to connect the heat medium pipeline to realize the control of the temperature in the inside of the reaction kettle 1.

[0049] The embodiment also provides a reaction method of a reaction device for preparing low-sodium aluminum sol, comprising the following steps:

[0050] Step one, aluminum sol generation, raw aluminum and hydrochloric acid are injected into the reaction kettle 1, the raw aluminum is dissolved in the hydrochloric acid to form aluminum chloride, water is injected into the reaction kettle 1, and the aluminum chloride undergoes hydrolysis reaction and polymerization reaction to generate aluminum sol colloid, sodium ion salt is mixed in the aluminum sol colloid generated in the process, and in the process, sodium hydroxide is added to the mixed solution to control the pH value to be between 2 and 3;

[0051] In the process, the heat medium is delivered to the temperature control jacket 7 through the first jacket nozzle 71, so that the temperature inside the reaction kettle 1 is kept between 85-95℃, to ensure the normal progress of the reaction, and the aluminum sol colloid particles generated in the reaction are suspended in the solution;

[0052] Step two, aluminum sol transfer, the initially formed aluminum sol colloid is delivered to the transition cavity 34 through the material extraction pipe 35 and the material return pipe 36, the aluminum sol colloid mixed solution in the transition cavity 34 passes through multiple ion exchange columns 33 respectively, the sodium ion salt in the aluminum sol colloid solution is adsorbed by the strong acid cation exchange resin in the ion exchange column 33, so that the aluminum sol colloid solution is converted into low-sodium aluminum sol colloid solution;

[0053] After the aluminum sol colloid particles are generated, the aluminum sol colloid solution generated in the reaction kettle 1 is extracted through the material pump 352, the connecting pipe 351 and the material extraction pipe 35, the aluminum sol colloid solution is injected into the transition cavity 34 through the material pump 352 and the material return pipe 36, and then is uniformly dispersed into the multiple ion exchange columns 33 in the transition cavity 34, the strong acid cation exchange resin in the ion exchange column 33 exchanges with the sodium ions to remove the sodium ions, in the process, the aluminum sol colloid moves downward through the ion exchange column 33 and enters the storage cavity 37;

[0054] In the process of exchange reaction between the strong acid cation exchange resin and the sodium ions, the hydrogen ions displaced by the exchange reaction cause the local pH value to rise, and when the aluminum sol colloid solution is extracted from the reaction kettle 1, the sodium hydroxide originally added in the reaction kettle 1 is extracted together with the aluminum sol colloid solution into the transition cavity 34, and the sodium hydroxide solution can undergo acid-base neutralization reaction with the hydrogen ions displaced by the exchange reaction to generate water, in the process, the unreacted sodium hydroxide solution in the reaction kettle 1 can be treated, and the unreacted sodium hydroxide solution can be used to control the pH value of the aluminum sol colloid solution in the exchange reaction process, to ensure the stability of the aluminum sol colloid solution;

[0055] It should be noted that when the aluminum sol colloidal solution and the sodium hydroxide solution are not extracted in the reaction kettle 1, in order to ensure that the pH value during the preparation of the aluminum sol colloidal solution is maintained between 2 and 3, and the acidification reaction continuously generates dilute hydrochloric acid during the preparation of the aluminum sol colloidal solution, the addition of the sodium hydroxide solution is in a continuous state, and after the preparation of the aluminum sol colloidal solution is completed, the sodium hydroxide solution is left over because it is not added in time, at this time the aluminum sol colloidal solution and the sodium hydroxide solution are quickly extracted into the transition chamber 34 for the removal of sodium ions, and the excess sodium hydroxide solution can be reused;

[0056] It should be further noted that the transfer of the aluminum sol colloidal solution should be carried out within 10 minutes after the generation of the aluminum sol colloidal solution, at this time the aluminum sol colloidal solution is in a nanoparticle state, and the aluminum sol colloidal solution in the nanoparticle state will not cause the strong acid cation exchange resin to be blocked, and for the generation of the aluminum sol colloidal solution, the change of the pH value in the reaction kettle 1 can be detected, when the pH value in the reaction kettle 1 increases, it indicates that the reaction stops generating hydrogen ions insufficient to react with the continuously added sodium hydroxide solution, then it indicates that the reaction of the raw material aluminum and hydrochloric acid stops, at this time the aluminum sol colloidal solution is generated, and the aluminum sol colloidal solution can pass through the ion exchange column 33 under normal pressure, if the sodium ion content in the aluminum sol colloidal solution is required to be relatively high, a air compressor can be used to pressurize the transition chamber 34, so that the aluminum sol colloidal solution passes through the ion exchange column 33 under pressure, and the aluminum sol colloidal solution under pressure can pass through the ion exchange column faster, thereby the preparation efficiency of the aluminum sol colloidal solution can be improved, accordingly the sodium ion content in the aluminum sol colloidal solution will increase, and for the selection of normal pressure and pressure, the sodium ion content in the aluminum sol colloidal solution can be selected according to the standard;

[0057] Step three, product discharge, discharging the low-sodium aluminum sol colloidal solution, and guiding the low-sodium aluminum sol colloidal solution to the aging tank for aging treatment;

[0058] The low-sodium aluminum sol colloidal solution can be discharged through the discharge valve 371 and guided to the aging tank for aging treatment to complete the preparation of the low-sodium aluminum sol;

[0059] Step four, backflush, using dilute hydrochloric acid to backflush the ion exchange column 33 to regenerate the strong acid cation exchange resin, and thus a preparation cycle of the low-sodium aluminum sol is completed;

[0060] After the low-sodium aluminum sol colloidal solution is completely discharged, the discharge valve 371 is closed. Then, dilute hydrochloric acid is injected into the storage chamber 37 through the backflushing valve 372. The dilute hydrochloric acid then passes through the ion exchange column 33 under pressure. The dilute hydrochloric acid reacts with the strongly acidic cation exchange resin that has undergone an exchange reaction in the ion exchange column 33 to regenerate the exchange resin. After passing through the ion exchange column 33, the dilute hydrochloric acid enters the transition chamber 34 and is then discharged through the waste discharge valve 341. During this process, the regeneration effect of the exchange resin is judged by measuring the pH value of the discharged solution at the waste discharge valve 341. When the pH value of the discharged solution is 2.5, the injection of dilute hydrochloric acid is stopped, and the excess dilute hydrochloric acid is discharged from the discharge valve 371. Example 2

[0061] This embodiment is a supplement to Embodiment 1. It takes into account that the reaction temperature is high during the preparation of aluminum sol colloid, while the temperature required for the aluminum sol colloid solution to remove sodium ions is low when passing through ion exchange column 33.

[0062] like Figures 4 to 5 As shown, the reaction apparatus for preparing low-sodium aluminum sol provided by the present invention is essentially a reaction apparatus that can control the temperature of the aluminum sol colloidal solution during the transfer process. By setting a cooling jacket 4, the aluminum sol colloidal solution passes through the cooling jacket 4 during the transfer process. The refrigerant injected into the cooling jacket 4 can achieve rapid cooling of the aluminum sol colloidal solution, thereby achieving the effect of inhibiting the aging of the aluminum sol colloid. At the same time, the cooling jacket 4 can also control the temperature of the environment where the ion exchange column 33 is located, so as to ensure the working environment when the strongly acidic cation exchange resin adsorbs sodium ions, thereby ensuring the removal effect of sodium ions in the aluminum sol colloidal solution.

[0063] In terms of specific structural installation, the structural body can be constructed according to the inventive concept of this embodiment. In this embodiment, no special limitations are imposed.

[0064] In this embodiment, a reaction apparatus for preparing low-sodium aluminum sol includes:

[0065] Cooling jacket 4 is fixedly installed inside the annular cover 3 and is connected to the interior of the annular cover 3. Multiple material extraction pipes 35 are installed through the interior of the cooling jacket 4. Second jacket nozzles 41 are fixedly installed on both sides of the top of the cooling jacket 4. The second jacket nozzles 41 are used to connect to the refrigerant inlet.

[0066] Multiple heat-conducting fins 3501 are fixedly provided in the middle of the feed tube 35. The multiple heat-conducting fins 3501 have a spiral structure and are all located inside the cooling jacket 4. The spiral structure of the heat-conducting fins 3501 can guide the flow of refrigerant to improve the heat exchange efficiency between the refrigerant and the feed tube 35.

[0067] When using the reaction apparatus for preparing low-sodium aluminum sol in this embodiment, the refrigerant is injected into the cooling jacket 4 through the second jacket nozzle 41, and the interior of the cooling jacket 4 is filled with refrigerant. At this time, the refrigerant is in contact with the interior of the heat-conducting fins 3501 and the annular cover 3. When the aluminum sol colloidal solution is drawn through the extraction pipe 35, the extraction pipe 35 exchanges heat with the refrigerant through the heat-conducting fins 3501, thereby achieving the cooling treatment of the aluminum sol colloidal solution. At the same time, the refrigerant exchanges heat with the annular cover 3, so that the temperature of the environment where the ion exchange column 33 is located is controlled. The aluminum sol colloidal solution after the temperature is reduced enters the ion exchange column 33 through the transition chamber 34 and removes sodium ions. Example 3

[0068] This embodiment is a supplement to Embodiment 1 and Embodiment 2. Considering that the aluminum sol colloid is suspended in the mixed solution after it is generated, the extraction tube 35 may easily extract the remaining solution at the same time when extracting the aluminum sol colloid, which will waste the raw materials and affect the removal of sodium ions by the ion exchange column 33. In addition, some undissolved impurities remain in the mixed solution during the reaction, which will affect the subsequent reaction.

[0069] like Figures 6 to 8 As shown, the reaction apparatus for preparing low-sodium aluminum sol according to the present invention is essentially a reaction apparatus that can guide the separation of aluminum sol colloid from the mixed solution to reduce the waste of raw material solution. When the aluminum sol colloid is transferred after its formation, some undissolved impurities are drawn into the transition chamber 34 under the action of centrifugal force. The undissolved impurities remain in the transition chamber 34 because they cannot pass through the ion exchange column 33. After the aluminum sol colloid removes sodium ions, dilute hydrochloric acid can be injected through the storage chamber 37 to achieve backflushing regeneration of the ion exchange column 33. During this process, the undissolved impurities remaining in the transition chamber 34 can be discharged together with the backflushing solution, thereby achieving synchronous cleaning of residual impurities during the reaction process, so as to facilitate continuous operation and production of the apparatus.

[0070] In terms of specific structural installation, the structural body can be constructed according to the inventive concept of this embodiment. In this embodiment, no special limitations are imposed.

[0071] In this embodiment, a reaction apparatus for preparing low-sodium aluminum sol includes:

[0072] A stirring rod 5 is rotatably mounted at the top center of the fixed cover 2. A forward and reverse motor 51 is mounted at the top of the stirring rod 5. The forward and reverse motor 51 is used to drive the stirring rod 5 to rotate forward in the early stage of the reaction to complete the solution stirring. The forward and reverse motor 51 is used to drive the stirring rod 5 to rotate in reverse in the later stage of the reaction to complete the colloid aggregation. A stirring blade 52 is fixedly mounted at the bottom of the stirring rod 5. The stirring blade 52 has two sets, upper and lower, and both sets of stirring blades 52 are inclined.

[0073] The guide plate 6 is provided with a plurality of groups and is arranged around the inside of the reaction kettle 1, and the guide plate 6 is used in cooperation with the stirring rod 5 to collect and gather the aluminum sol colloidal particles;

[0074] The side of the guide plate 6 away from the inner wall of the reaction kettle 1 is fixedly provided with an extension plate 61, and an inclination angle is arranged between the extension plate 61 and the guide plate 6. The side of the extension plate 61 away from the guide plate 6 is fixedly provided with an ear plate 62, and an inclination angle is arranged between the ear plate 62 and the extension plate 61. A plurality of material passing grooves 611 are sequentially and penetratingly arranged in the middle part of the extension plate 61 from bottom to top. Since the ear plate 62 and the extension plate 61 have inclination angles relative to the guide plate 6, when the guide plate 6 and the extension plate 61 are attached to the inner wall of the reaction kettle 1, there is an inclination angle between the ear plate 62 and the inner wall of the reaction kettle 1. In this state, the reversed solution can push the guide plate 6 to rotate through the ear plate 62.

[0075] The side of the guide plate 6 close to the reaction kettle 1 is fixedly provided with a support rod 601, and the both ends of the support rod 601 are sleeved with positioning rings 602, and the positioning rings 602 are fixedly arranged on the inner wall of the reaction kettle 1. The side of the guide plate 6 close to the reaction kettle 1 is fixedly provided with a plurality of support blocks 63, and the support blocks 63 are arranged in an arc structure, and the support blocks 63 are located on the side of the guide plate 6 away from the extension plate 61.

[0076] When the reaction equipment for preparing low-sodium aluminum sol is used, in the process of the aluminum sol colloidal generation reaction, the forward and reverse motor 51 drives the stirring rod 5 to rotate forward, and the stirring rod 5 drives the stirring blade 52 to rotate counterclockwise. At this time, the mixed solution is counterclockwise under the push of the stirring blade 52, and the mixed solution counterclockwise pushes the guide plate 6 and the extension plate 61, so that the guide plate 6 is flipped relative to the reaction kettle 1, until the guide plate 6, the extension plate 61 and the ear plate 62 are attached to the inner wall of the reaction kettle 1. In this process, the mixed solution between the guide plate 6 and the inner wall of the reaction kettle 1 is discharged through the material passing grooves 611, so as to ensure the reaction effect of the mixed solution.

[0077] After the aluminum sol colloidal generation reaction stops, the forward and reverse motor 51 drives the stirring rod 5 to reverse, and the stirring rod 5 drives the stirring blade 52 to rotate clockwise. At this time, the ear plate 62 is flipped by the push of the mixed solution, and the ear plate 62 drives the extension plate 61 and the guide plate 6 to flip, until the support blocks 63 on the outside of the guide plate 6 are attached to the inner wall of the reaction kettle 1. At this time, a storage space is formed between the guide plate 6 and the inner wall of the reaction kettle 1. In this process, the aluminum sol colloidal particles and the undissolved impurities gradually approach the inner wall of the reaction kettle 1 under the action of centrifugal force, and stay between the guide plate 6 and the reaction kettle 1. At this time, the material extraction pipe 35 can extract the aluminum sol colloidal particles and the undissolved impurities between the guide plate 6 and the reaction kettle 1, so as to avoid the effect of extracting the raw material solution.

[0078] Finally, it should be noted that the above only describes the preferred embodiments of the present application and is not intended to limit the present application. Although the present application has been described in detail with reference to the foregoing embodiments, those skilled in the art will appreciate that the technical solutions described in the foregoing embodiments can be modified or some technical features thereof can be replaced by equivalent features, and any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present application shall be included in the protection scope of the present application.

Claims

1. A reaction apparatus for preparing a low-sodium alumina sol, characterized by comprising: Include: The reactor (1) is internally provided with an inner cavity for aluminum sol preparation reaction; The fixed cover (2) is provided at the top end of the reactor (1) and communicates with the inner cavity of the reactor (1), the middle part of the fixed cover (2) is fixedly provided with an annular cover (3), a plurality of treatment tanks (31) are annularly arranged in the inner part of the annular cover (3), circular through grooves (32) are penetratingly arranged at both ends of the treatment tank (31), an ion exchange column (33) is arranged in the inner part of the treatment tank (31), both ends of the ion exchange column (33) respectively communicate with the two circular through grooves (32), a transition cavity (34) is arranged at the top end of the annular cover (3), the circular through grooves (32) at the top end of the plurality of treatment tanks (31) all communicate with the transition cavity (34), a plurality of material extraction pipes (35) are annularly arranged in the inner part of the annular cover (3), and the bottom ends of the material extraction pipes (35) are located in the inner part of the reactor (1), a material return pipe (36) is fixedly arranged outside the annular cover (3), one end of the material return pipe (36) communicates with the material extraction pipe (35), and the other end of the material return pipe (36) communicates with the transition cavity (34), the aluminum sol colloidal solution generated by the reaction in the inner part of the reactor (1) enters the ion exchange column (33) through the material extraction pipe (35) and the material return pipe (36) to complete the adsorption and separation of sodium ions; The outer wall of the fixed cover (2) is fixedly provided with a material pump (352) at the top end, the input end of the material pump (352) is fixedly provided with a connecting pipe (351), the plurality of material extraction pipes (35) all communicate with the connecting pipe (351), and the output end of the material pump (352) communicates with the material return pipe (36).

2. The reaction apparatus for preparing a low-sodium alumina sol according to claim 1, wherein Also include: The stirring rod (5) is rotatably arranged at the middle part of the top end of the fixed cover (2), and the top end of the stirring rod (5) is provided with a forward and reverse motor (51), which is used to drive the stirring rod (5) to rotate forward to complete solution stirring in the early stage of reaction, and is used to drive the stirring rod (5) to rotate reversely to complete colloid gathering in the later stage of reaction, the bottom end of the stirring rod (5) is fixedly provided with stirring blades (52), the stirring blades (52) are provided with two groups of upper and lower groups, and the two groups of stirring blades (52) are all provided in an inclined structure; The material guide plate (6) is provided with a plurality of groups and is annularly arranged in the inner part of the reactor (1), and the material guide plate (6) is used to collect and gather the aluminum sol colloidal particles in cooperation with the stirring rod (5).

3. The reaction apparatus for preparing a low-sodium alumina sol according to claim 2, wherein Also include: The side of the extension plate (61) away from the material guide plate (6) is fixedly provided with an ear plate (62), and an inclination angle is arranged between the extension plate (61) and the material guide plate (6), the side of the extension plate (61) away from the material guide plate (6) is fixedly provided with an ear plate (62), and an inclination angle is arranged between the extension plate (61) and the material guide plate (6), and a plurality of material passing grooves (611) are sequentially penetratingly arranged in the middle part of the extension plate (61) from bottom to top.

4. The reaction apparatus for preparing a low-sodium alumina sol according to claim 3, wherein Also include: The material guide plate (6) is fixed with a support rod (601) on one side close to the reactor (1), both ends of the support rod (601) are sleeved with a positioning ring (602), and the positioning ring (602) is fixed on the inner wall of the reactor (1), a plurality of support blocks (63) are fixed on one side of the material guide plate (6) close to the reactor (1), the support blocks (63) are arc-shaped structures, and the support blocks (63) are located on the side of the material guide plate (6) away from the extension plate (61).

5. The reaction apparatus for preparing a low-sodium alumina sol according to claim 1, wherein Also includes: The cooling jacket (4) is fixed on the inner side of the annular cover (3), and the cooling jacket (4) is communicated with the inside of the annular cover (3), a plurality of the material extraction pipes (35) are arranged in the inside of the cooling jacket (4), and the top of the cooling jacket (4) is fixed with a second jacket nozzle (41) on both sides.

6. The reaction apparatus for preparing a low-sodium alumina sol according to claim 1, wherein Also includes: The middle of the material extraction pipe (35) is fixed with a plurality of heat conduction fins (3501), the plurality of heat conduction fins (3501) are spiral structures, and the plurality of heat conduction fins (3501) are arranged in the inside of the cooling jacket (4).

7. The reaction apparatus for preparing a low-sodium alumina sol according to claim 1, wherein Also includes: The temperature control jacket (7) is located on the outside of the reactor (1), the temperature control jacket (7) is used for controlling the reaction temperature in the reactor (1), and the temperature control jacket (7) is fixed with a first jacket nozzle (71) on both sides.

8. The reaction apparatus for preparing a low-sodium alumina sol according to claim 1, wherein Also includes: The slot of the treatment tank (31) is inserted with a fixed seat (3301), the middle of the fixed seat (3301) is penetrated with a circular insertion slot (3302), the ion exchange column (33) is detachably inserted into the circular insertion slot (3302), the outside of the fixed seat (3301) is penetrated with an observation window (3303), and the fixed seat (3301) is used for installing and fixing the ion exchange column (33) in the treatment tank (31). The bottom of the annular cover (3) is fixed with a storage cavity (37), the bottom of the storage cavity (37) is fixed with a discharge valve (371) and a backflush valve (372), and the bottom of the outer wall of the transition cavity (34) is fixed with a waste discharge valve (341).

9. The reaction method of claim any one of claims 1 to 8, wherein the reaction method is characterized by, The steps include: Step one, aluminum sol generation, raw aluminum and hydrochloric acid are injected into the reactor (1), the raw aluminum is dissolved in the hydrochloric acid to form aluminum chloride, water is injected into the reactor (1), the aluminum chloride undergoes hydrolysis reaction and polymerization reaction to generate aluminum sol colloid, and sodium ion salt is mixed in the generated aluminum sol colloid in this process, in this process, sodium hydroxide is added to the mixed solution to control the pH value to be between 2-3; Step two, aluminum sol transfer, the initially formed aluminum sol colloid is transported into the transition cavity (34) through the material extraction pipe (35) and the material return pipe (36), the aluminum sol colloid mixed solution in the transition cavity (34) passes through a plurality of ion exchange columns (33) respectively, and the sodium ion salt in the aluminum sol colloid solution is adsorbed by the strong acid cation exchange resin in the ion exchange column (33), so that the aluminum sol colloid solution is converted into a low-sodium aluminum sol colloid solution; Step three, product discharge, the low-sodium aluminum sol colloidal solution is discharged and guided to an aging tank for aging treatment; Step four, back flushing, the ion exchange column (33) is back flushed using dilute hydrochloric acid to regenerate the strong acidic cation exchange resin, thus completing a preparation cycle of the low-sodium aluminum sol.

Citation Information

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