CN114247411A - Device and method for preparing hydrotalcite-like compound by continuous flow coprecipitation - Google Patents

Device and method for preparing hydrotalcite-like compound by continuous flow coprecipitation Download PDF

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CN114247411A
CN114247411A CN202111586766.9A CN202111586766A CN114247411A CN 114247411 A CN114247411 A CN 114247411A CN 202111586766 A CN202111586766 A CN 202111586766A CN 114247411 A CN114247411 A CN 114247411A
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metal ion
compartment
solution
reaction kettle
ion solution
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CN114247411B (en
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刘晓
孟益名
陈艳华
钟卉元
王昊
杨永
袁跃
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North China University of Science and Technology
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North China University of Science and Technology
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/18—Stationary reactors having moving elements inside
    • B01J19/1862—Stationary reactors having moving elements inside placed in series
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/0006—Controlling or regulating processes
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/0053—Details of the reactor
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/0086—Processes carried out with a view to control or to change the pH-value; Applications of buffer salts; Neutralisation reactions
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J4/00—Feed or outlet devices; Feed or outlet control devices
    • B01J4/001—Feed or outlet devices as such, e.g. feeding tubes
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J4/00—Feed or outlet devices; Feed or outlet control devices
    • B01J4/008—Feed or outlet control devices
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J4/00—Feed or outlet devices; Feed or outlet control devices
    • B01J4/02—Feed or outlet devices; Feed or outlet control devices for feeding measured, i.e. prescribed quantities of reagents
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2204/00—Aspects relating to feed or outlet devices; Regulating devices for feed or outlet devices
    • B01J2204/002—Aspects relating to feed or outlet devices; Regulating devices for feed or outlet devices the feeding side being of particular interest
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2208/00—Processes carried out in the presence of solid particles; Reactors therefor
    • B01J2208/00008—Controlling the process
    • B01J2208/00592—Controlling the pH
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P20/00—Technologies relating to chemical industry
    • Y02P20/50—Improvements relating to the production of bulk chemicals
    • Y02P20/52—Improvements relating to the production of bulk chemicals using catalysts, e.g. selective catalysts

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
  • Physical Or Chemical Processes And Apparatus (AREA)

Abstract

The invention discloses a device and a method for preparing hydrotalcite-like compound by continuous flow coprecipitation, which comprises a coprecipitation reaction kettle, a multipoint dripping shower nozzle, a second stirring kettle, a metal ion solution storage tank and an alkali solution storage tank; a pH meter is arranged in the coprecipitation reaction kettle; the multipoint dripping shower head comprises an alkaline solution compartment and a metal ion solution compartment, dripping micropores are formed in the bottoms of the alkaline solution compartment and the metal ion solution compartment, and sleeves are fixedly connected to the bottoms of the side walls of the metal ion solution compartment; the second stirring kettle is communicated with the first discharge hole; the metal ion solution storage tank is communicated with the metal ion solution compartment, and the alkaline solution storage tank is communicated with the alkaline solution compartment; constant temperature stirrers are arranged at the bottoms of the coprecipitation reaction kettle and the second stirring kettle. The invention can effectively shorten the synthetic period of the hydrotalcite-like compound, and the prepared hydrotalcite-like compound has good crystallization, narrow size distribution range, large specific surface area and high reaction activity.

Description

Device and method for preparing hydrotalcite-like compound by continuous flow coprecipitation
Technical Field
The invention relates to the technical field of hydrotalcite-like compound preparation, in particular to a device and a method for preparing hydrotalcite-like compound by continuous flow coprecipitation.
Background
Hydrotalcite-like compounds, also known as layered double-hydroxy metal oxides, are supramolecular materials formed by self-assembly of sheets with positive charges and interlayer anions through electrostatic forces or hydrogen bonds. Because of the strong interlayer anion exchange capacity, the method has great application potential in various fields such as high-performance adsorption, catalysis, biomedicine, additives and the like. The synthetic method of the hydrotalcite-like compound comprises a direct coprecipitation method, a homogeneous coprecipitation method, a template method and the like, which are all intermittent synthesis, and the basic principle of the method is that metal cations (M)2 +/M3+) Solution with base (OH)-) The solution undergoes a coprecipitation reaction. Among the prior reports on hydrotalcite-like synthesis, the coprecipitation method has been most frequently used. Mainly comprises a metal ion solution and alkali solution opposite spraying method (comprising a spraying reaction method and a micro-channel reaction method), a metal ion solution dropping method to alkali solution, and a metal ion solution and alkali solution dropping method to water with constant pH.
Patent CN205616580U and patent CN207891059U adopt a jet reaction kettle to spray metal ion solution and alkali solution in an atomized form, so as to strengthen the material contact and homogenize the nucleation environment, although the method can control the concentration of the metal solution and alkali solution to be uniform, the primary nucleated hydrotalcite-like precursor slurry is discharged after each jet reaction by the jet device, so as to perform the next jet reaction; the nucleation process of the precursor slurry is mainly completed in the crystallization kettle, and precursors generated in different batches continuously enter the crystallization kettle, so that the size distribution range of crystal grains is inevitably enlarged. Therefore, the process is complicated to operate and it is difficult to control the grain size distribution range. Yaseneva P et al use a T/Y type microchannel reactor with an inner diameter of 2mm as a coprecipitation nucleation site, inject a metal solution and an alkali solution into the microchannel from two ends of the microchannel in opposite directions at a flow rate of 4mL/min, vigorously mix and react at the junction of the two liquid flows to generate a hydrotalcite-like precursor, flow the precursor material out of the converging channel, and age for a certain period of time to form nanocrystals. It is noteworthy that neither jet reactors nor microchannel reactors allow precise control of the pH of the mixture and the reaction site, which is determined by the pH, concentration and reaction rate of the influent, which makes the operation extremely complicated.
In contrast, the addition method allows the reaction to be carried out under constant pH conditions with relatively simple operation. In the existing dropping method, the dropping mode of each solution is single-point dropping. Under the influence of diffusion mass transfer, single large liquid drop generates concentration polarization locally, a large amount of hydrotalcite-like precursors are generated at the contact part of the metal solution and the alkali solution instantly, and the whole solution is in an uneven state. This local over-concentration results in a large impurity doping of the grain precipitates, and the nucleation reaction continues to occur as the reaction time is extended. Precipitates which are precipitated at different moments and have different thermodynamic states are inevitably mixed together, and after the aging of tens of hours, crystal grains are further aggregated, recrystallized and grown up, so that a product with less impurities can be obtained. The product plies obtained under such conditions are tightly stacked; the horizontal size of the lamellar is from nano-scale to micron-scale, the distribution range of the length-diameter ratio of crystal grains is large, and the quality and the performance of the product are very unstable. The homogeneous coprecipitation method utilizes OH generated by urea slow-release alkaline water thermal decomposition-And M2+/M3+The grain size of the product is relatively uniform, but the method takes a long time and cannot be used for synthesizing Ca-containing hydrotalcite. The template method is to introduce a template agent into a direct coprecipitation method and a homogeneous coprecipitation method and deposit the template agent as hydrotalcite-like layer sheetsA core and a support.
The synthesis methods are all intermittent synthesis, and generally have the problems of complicated steps, discontinuous operation, harsh reaction conditions, long synthesis period and low productivity; the products synthesized under different conditions have larger difference in structural morphology and reactivity. These have greatly hindered the further popularization and application of hydrotalcite-like compounds in the production field. Therefore, how to obtain a product with ideal aggregation form, stable yield and high reactivity in a simple process is still a great challenge in hydrotalcite-like synthesis technology. Therefore, the device and the method for preparing the hydrotalcite-like compound by continuous flow coprecipitation are provided.
Disclosure of Invention
The present invention aims to provide an apparatus and a method for preparing hydrotalcite-like compounds by continuous flow co-precipitation, which aim to solve or improve at least one of the above technical problems.
In order to achieve the purpose, the invention provides the following scheme: the invention provides a device for preparing hydrotalcite-like compound by continuous flow coprecipitation, which comprises a coprecipitation reaction kettle, a multipoint dripping shower nozzle, a second stirring kettle, a metal ion solution storage tank and an alkali solution storage tank;
a pH meter is arranged in the coprecipitation reaction kettle, and a plurality of first discharge ports are formed in the side wall of the coprecipitation reaction kettle;
the multipoint dripping shower head comprises an alkaline solution compartment fixedly arranged on the top surface of an inner cavity of the coprecipitation reaction kettle and a metal ion solution compartment sleeved outside the alkaline solution compartment, dripping micropores are formed in the bottoms of the alkaline solution compartment and the metal ion solution compartment, and a sleeve is fixedly connected to the bottom of the side wall of the metal ion solution compartment;
the second stirring kettle is communicated with the first discharge hole, and a plurality of second discharge holes are formed in the side wall of the second stirring kettle;
the metal ion solution storage tank is communicated with the metal ion solution compartment through a feeding and discharging mechanism, and the alkali solution storage tank is communicated with the alkali solution compartment through another feeding and discharging mechanism;
wherein, the bottom of coprecipitation reation kettle with the second stirred tank all installs the constant temperature agitator, and is a plurality of first discharge gate and a plurality of all install the outflow valve in the second discharge gate.
Preferably, the feeding and discharging mechanism comprises a charging barrel, an upper opening one-way valve, a lower opening one-way valve, a push-pull piston arranged in the charging barrel, and a controller fixedly connected to the top of the push-pull piston;
a liquid inlet and a liquid outlet are formed in the end face of the bottom of the charging barrel, the upper opening one-way valve is fixedly mounted in the liquid inlet, and the lower opening one-way valve is fixedly mounted in the liquid outlet;
the charging barrels of the two feeding and discharging mechanisms are respectively set as a first charging barrel and a second charging barrel;
the liquid inlet of the first material cylinder is communicated with the metal ion solution storage tank through a first inlet pipe, and the liquid outlet of the first material cylinder is communicated with the metal ion solution compartment through a first outlet pipe;
the liquid inlet of the second material cylinder is communicated with the alkali solution storage tank through a second inlet pipe, and the liquid outlet of the second material cylinder is communicated with the alkali solution compartment through a second outlet pipe.
Preferably, the detection end of the pH meter is positioned between the outer wall of the sleeve and the inner wall of the coprecipitation reaction kettle.
Preferably, the top of the coprecipitation reaction kettle and the top of the second stirring kettle are both provided with sealing covers, the sealing covers are provided with hole pipes, and the metal ion solution compartment is fixedly arranged on the bottom surfaces of the sealing covers of the coprecipitation reaction kettle.
Preferably, the ratio of the area of the bottom end face of the metal ion solution compartment to the area of the bottom end face of the caustic solution compartment is 1: 8.
Preferably, the number ratio of the dropping pores of the metal ion solution compartment to the dropping pores of the alkali solution compartment is 1: 8.
Preferably, the first discharge ports are respectively arranged at different heights of the side wall of the coprecipitation reaction kettle; and the plurality of second discharge ports are respectively arranged at different heights of the side wall of the second stirring kettle.
Preferably, the side walls of the first material cylinder and the second material cylinder are provided with scales.
The invention also provides a method for preparing hydrotalcite-like compound by continuous flow coprecipitation, which comprises the following steps:
step one, filling a solution A into a metal ion solution storage tank;
secondly, adding an alkali solution B into an alkali solution storage tank;
step three, respectively filling distilled water into the coprecipitation reaction kettle and the second stirring kettle, adjusting the pH value by using NaOH, and adding polyethylene glycol;
step four, respectively storing the solution A and the alkali solution B in two feeding and discharging mechanisms;
step five, starting the two constant-temperature stirrers, and setting the required stirring speed and temperature;
sixthly, adding the solution A into a metal ion solution compartment and adding the alkali solution B into an alkali solution compartment, and dropwise adding the solution A and the alkali solution B into a coprecipitation reaction kettle;
step seven, after the liquid level of the mixed liquid in the coprecipitation reaction kettle is higher than the first discharge hole, the mixed liquid enters a second stirring kettle, and materials can be collected when the liquid level in the second stirring kettle is higher than the second discharge hole;
step eight, ageing the materials at constant temperature, and centrifugally dewatering or filtering and dewatering the materials into cakes;
and step nine, uniformly mixing the cake-shaped material with a displacement solvent, removing water, and finally drying to remove the displacement solvent, thereby obtaining the hydrotalcite-like product.
Preferably, in the first step, the solution a is a solution containing divalent metal ions and trivalent metal ions, and the divalent metal includes Ca2+、Mg2+、Fe2+、Zn2+、Ni2+、Co2+、Cu2+、Ti2+Either one or both of; the trivalent metal comprises Al3+、Fe3+Either one or both of;
in the second step, the base isThe solution B is NaOH solution, NaOH and NaCO3Any one of the mixed solutions;
in the ninth step, the displacement solvent is any one of methanol, ethanol, propanol, acetone, n-butanol, hexane and cyclohexane.
The invention discloses the following technical effects:
1. compared with the existing batch synthesis method, the method can realize the continuous preparation of the hydrotalcite-like compound, has simple device, large or small scale and is easy to operate.
2. The invention can ensure that the pH value in the whole reaction process is in a relatively constant state, optimizes the crystal generation environment and is beneficial to forming hydrotalcite-like compounds with uniform quality.
3. The metal ion solution in the metal ion solution storage tank and the alkali solution in the alkali solution storage tank are respectively converted into dispersed micro-droplets through the dripping micropores and enter the coprecipitation reaction kettle, and the dispersed micro-droplets are used for replacing the traditional dripped single-droplet and large-droplet, so that the contact area of two reaction liquids can be increased, the concentration polarization effect is reduced, the mass transfer effect is enhanced, and the precipitation reaction can be rapidly and uniformly carried out.
4. According to the invention, the metal ion solution and the alkali solution respectively enter the metal ion solution compartment and the alkali solution compartment, and the metal ion solution compartment and the alkali solution compartment adopt a separation arrangement mode of an inner ring and an outer ring, so that the problems of uneven products and blockage caused by the advanced reaction of the two solutions are effectively avoided, and the coprecipitation reaction is effectively controlled to occur in the solution of the coprecipitation reaction kettle.
5. The invention can operate continuously, make the products produced at different moments in relatively balanced dwell time, avoid the tiny crystalline grain produced in short time and coarse crystalline grain produced in long time to mix each other, thus the particle size distribution range of the effective control product, the invention can regulate the appropriate material dwell time according to the particle size requirement of the desired product, under the condition of equal output, coprecipitation reaction time and aging time are both greatly shortened, the overall synthesis cycle is shortened by more than half compared with batch synthesis, and the product property is more stable.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings needed in the embodiments will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art to obtain other drawings without creative efforts.
FIG. 1 is a schematic structural diagram of an apparatus and a method for preparing hydrotalcite-like compound by continuous flow co-precipitation according to the present invention;
FIG. 2 is a schematic structural view of a charging and discharging device according to the present invention;
FIG. 3 is a schematic view of a multi-point drop shower head according to the present invention;
FIG. 4 is a cross-sectional view A-A of FIG. 3;
wherein, 1, a metal ion solution storage tank; 2. an alkali solution storage tank; 3. a feeding and discharging mechanism; 41. a first inlet pipe; 42. a second inflow pipe; 51. a first outlet pipe; 52. a second outlet pipe; 6. a pH meter; 7. a multipoint dripping shower nozzle; 8. a coprecipitation reaction kettle; 9. a constant temperature stirrer; 10. a sleeve; 11. a second stirred tank; 12. a first discharge port; 13. an outlet valve; 14. a second discharge port; 301. a controller; 302. pushing and pulling the piston; 303. a charging barrel; 304. a check valve is opened upwards; 305. a check valve is opened at the lower part; 701. a metal ion solution compartment; 702. a caustic solution compartment.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
In order to make the aforementioned objects, features and advantages of the present invention comprehensible, embodiments accompanied with figures are described in further detail below.
Referring to fig. 1-4, the invention provides a device for preparing hydrotalcite-like compound by continuous flow coprecipitation, comprising a coprecipitation reaction kettle 8, a multipoint dripping shower nozzle 7, a second stirring kettle 11, a metal ion solution storage tank 1 and an alkali solution storage tank 2;
a pH meter 6 is arranged in the coprecipitation reaction kettle 8, and a plurality of first discharge ports 12 are formed in the side wall of the coprecipitation reaction kettle 8; the pH meter 6 is used for monitoring the pH of the mixed solution on line so as to adjust the concentration or the dropping speed of the alkali solution;
the multipoint dripping shower nozzle 7 comprises an alkali solution compartment 702 fixedly installed on the top surface of an inner cavity of the coprecipitation reaction kettle 8 and a metal ion solution compartment 701 sleeved outside the alkali solution compartment 702, dripping micropores are formed at the bottoms of the alkali solution compartment 702 and the metal ion solution compartment 701 respectively, a sleeve 10 is fixedly connected to the bottom of the side wall of the metal ion solution compartment 701, the alkali solution compartment 702 and the metal ion solution compartment 701 are fixedly installed on the top surface of the inner cavity of the coprecipitation reaction kettle 8, the metal ion solution compartment 701 is located at the center of the top wall of the inner cavity of the coprecipitation reaction kettle 8, and the metal ion solution compartment 701 is fixedly sleeved on the outer side wall of the alkali solution compartment 702; the aperture of the dripping micropores is preferably 0.12mm, the open pores of the alkali solution compartment 702 and the metal ion solution compartment 701 are distributed at the positions R/5 and 4R/5 away from the circle center, and the average open pore number is 1500-2500 pores/m2The number of the holes and the area of the bottom end faces of the metal ion solution compartment 701 and the alkali solution compartment 702 can be designed according to actual requirements;
with the arrangement, the metal ion solution and the alkali solution respectively enter the metal ion solution compartment 701 and the alkali solution compartment 702, the metal ion solution compartment 701 and the alkali solution compartment 702 adopt a separation arrangement mode of an inner ring and an outer ring, the problems of product unevenness and blockage caused by advanced reaction of the two solutions are effectively avoided, and the coprecipitation reaction is effectively controlled to occur in the solution of the coprecipitation reaction kettle 8; the metal ion solution in the metal ion solution storage tank 1 and the alkali solution in the alkali solution storage tank 2 are respectively converted into dispersed micro-droplets through the dropping micropores and enter the coprecipitation reaction kettle 8, the dispersed micro-droplets are used for replacing the traditional dropping single-droplets and large-droplets, the contact area of the two reaction liquids can be increased, the concentration polarization effect is reduced, the mass transfer effect is strengthened, and the precipitation reaction can be rapidly and uniformly carried out; the sleeve 10 can effectively avoid generating short flow of sediment, so that products generated at different moments are in relatively balanced residence time in the solution in the coprecipitation reaction kettle 8, and the mutual mixing of fine grains generated in short time and coarse grains generated in long time is avoided, thereby effectively controlling the grain size distribution range of the products,
the second stirring kettle 11 is communicated with the first discharge hole 12, and the side wall of the second stirring kettle 11 is provided with a plurality of second discharge holes 14; discharging the material stirred by the second stirring kettle 11 through a second discharge port 14, and performing constant-temperature aging and solvent replacement drying to obtain a final hydrotalcite-like product;
the metal ion solution storage tank 1 is communicated with the metal ion solution compartment 701 through a feeding and discharging mechanism, and the alkali solution storage tank 2 is communicated with the alkali solution compartment 702 through another feeding and discharging mechanism;
wherein, the bottoms of the coprecipitation reaction kettle 8 and the second stirring kettle 11 are both provided with a constant temperature stirrer 9, and a plurality of first discharge ports 12 and a plurality of second discharge ports 14 are both provided with an outflow valve 13; the first discharge ports 12 and the second discharge ports 14 are both inclined downward by 45 degrees, and the type of the constant-temperature stirrer 9 may be set according to a specific use environment, for example, a constant-temperature magnetic stirrer, a constant-temperature mechanical stirrer, and the like, which is not specifically limited in this embodiment;
the invention can operate continuously, make the products produced at different moments in the relatively balanced dwell time, avoid the tiny crystalline grain produced in short time and coarse crystalline grain produced in long time to mix each other, thus the particle size distribution range of the effective control product, the invention can regulate the appropriate material dwell time according to the particle size requirement of the desired product, under the condition of the equal output, coprecipitation reaction time and aging time are greatly shortened, the overall synthetic cycle is shortened by more than half compared with batch synthesis, and the product property is more stable; compared with the existing batch synthesis method, the method can realize the continuous preparation of the hydrotalcite-like compound, has simple device, large or small scale and is easy to operate; the invention can ensure that the pH value in the whole reaction process is in a relatively constant state, optimizes the crystal generation environment and is beneficial to forming hydrotalcite-like compounds with uniform quality.
In a further optimized scheme, the feeding and discharging mechanism comprises a charging barrel 303, an upper opening one-way valve 304, a lower opening one-way valve 305, a push-pull piston 302 arranged in the charging barrel 303, and a controller 301 fixedly connected to the top of the push-pull piston 302; with such arrangement, the controller 301 controls the push-pull piston 302 to control upward rotation or downward pressing, so that liquid inlet and liquid outlet in the charging barrel 303 are realized; during normal dripping reaction, the push-pull pistons 302 of the two feeding and discharging mechanisms 3 move downwards at the same speed, the dripping speed of a single micropore is controlled to be 30-120 drops/min, and the releasing flow of the single micropore is 0.4-1.6 mL/min.
A liquid inlet and a liquid outlet are formed in the end face of the bottom of the charging barrel 303, an upper opening one-way valve 304 is fixedly mounted in the liquid inlet, and a lower opening one-way valve 305 is fixedly mounted in the liquid outlet; the upper opening one-way valve 304 can only be opened upwards, the lower opening one-way valve 305 can only be opened downwards, liquid is fed into the charging barrel 303 through the upper opening one-way valve 304, and liquid is discharged from the charging barrel 303 through the lower opening one-way valve 305; the controller 301 is operated to lift and push the piston 302 to reduce the internal pressure of the charging barrel 303, the upper opening one-way valve 304 is opened, the lower opening one-way valve 305 is closed, and the feed liquid is sucked into the charging barrel 303 from the metal ion solution storage tank 1 and the alkali solution storage tank 2 along the first inflow pipe 41 and the second inflow pipe 42 respectively; the push-pull piston 302 is pressed downwards, the upper opening one-way valve 304 is closed and the lower opening one-way valve 305 is opened under the action of the pressure of the solution in the charging barrel 303, the feed liquid is sent to the multipoint dripping shower nozzle 7 from the outlet pipe 5, and the inlet and outlet speeds of the feed liquid are controlled by the upward or downward pressing speed of the piston;
the material cylinders 303 of the two feeding and discharging mechanisms are respectively set as a first material cylinder and a second material cylinder;
the liquid inlet of the first material cylinder is communicated with the metal ion solution storage tank 1 through a first inlet pipe 41, and the liquid outlet of the first material cylinder is communicated with the metal ion solution compartment 701 through a first outlet pipe 51;
the inlet of the second cartridge is connected to the alkaline solution reservoir 2 via a second inlet conduit 42 and the outlet of the second cartridge is connected to the alkaline solution compartment 702 via a second outlet conduit 52.
In a further optimized scheme, the detection end of the pH meter 6 is positioned between the outer wall of the sleeve 10 and the inner wall of the coprecipitation reaction kettle 8; the lower edge of the outer edge sleeve 10 is arranged between the first discharge hole 12 in the middle and the first discharge hole 12 in the bottom, so that short flow of sediment can be effectively avoided.
According to a further optimized scheme, sealing covers are mounted at the tops of the coprecipitation reaction kettle 8 and the second stirring kettle 11, a hole pipe is formed in each sealing cover, and the metal ion solution compartment 701 is fixedly mounted on the bottom surface of each sealing cover of the coprecipitation reaction kettle 8; the material of the sealing cover can be set according to the specific use environment, the material of the sealing cover in the embodiment is silica gel, and the arrangement is such that when the reaction is carried out in the air atmosphere, each hole pipe is opened, and the balance of the internal and external air pressures of the device coprecipitation reaction kettle 8 and the second stirring kettle 11 is kept; when the reaction is carried out under anaerobic conditions, the perforated pipe is used for the intake or exhaust of inert gas stripping.
In a further optimized scheme, the ratio of the area of the bottom end face of the metal ion solution compartment 701 to the area of the bottom end face of the alkali solution compartment 702 is 1: 8.
In a further optimized scheme, the number ratio of the dropping micropores of the metal ion solution compartment 701 to the dropping micropores of the alkali solution compartment 702 is 1: 8.
According to a further optimized scheme, a plurality of first discharge ports 12 are respectively arranged at different heights on the side wall of the coprecipitation reaction kettle 8; a plurality of second discharge ports 14 are respectively arranged at different heights on the side wall of the second stirring kettle 11; the number of the first discharge ports 12 and the number of the second discharge ports 14 can be set according to a specific use environment, in the embodiment, the number of the first discharge ports 12 and the number of the second discharge ports 14 are 3, and the 3 first discharge ports 12 and the 3 second discharge ports 14 are fixedly provided with the outflow valves 13;
the second stirring kettle 11 is communicated with two first discharge ports 12 positioned at the middle upper part; the first discharge port 12 positioned at the bottommost part and the second discharge port 14 positioned at the bottommost part are both provided with sampling ports, so that sampling analysis at different moments is facilitated, and the concentration and component change of materials in the coprecipitation reaction kettle 8 and the second stirring kettle 11 are monitored; the other two first discharge ports 12 can be switched for use, and the other two second discharge ports 14 can also be switched for use; so set up, when opening the play of flowing out valve 13 ejection of compact from one of them, the other closes play of flowing out valve 13, and the effective cauldron capacity that two ejection of compact positions correspond is different, and corresponding material average residence time is also different.
According to a further optimization scheme, scales are arranged on the side walls of the first charging barrel and the second charging barrel.
The invention also provides a method for preparing hydrotalcite-like compound by continuous flow coprecipitation, which comprises the following steps:
step one, a solution A containing divalent metal ions and trivalent metal ions is filled in a metal ion solution storage tank 1;
secondly, adding an alkali solution B into an alkali solution storage tank 2;
step three, respectively filling distilled water with a certain volume into the coprecipitation reaction kettle 8 and the second stirring kettle 11, adjusting the pH value by using NaOH, and adding 2% V/V polyethylene glycol;
operating the two feeding and discharging mechanisms to respectively store a solution A and an alkali solution B with preset volumes in the two feeding and discharging mechanisms;
step five, starting the two constant-temperature stirrers 9, and setting the required stirring speed and temperature;
sixthly, operating the two feeding and discharging mechanisms to enable the solution A to enter a metal ion solution compartment 701 and the alkali solution B to enter an alkali solution compartment 702, and dropwise adding the solution A and the alkali solution B into the coprecipitation reaction kettle 8;
step seven, opening an outflow valve 13 of each first discharge port 12, enabling the mixed liquor in the coprecipitation reaction kettle 8 to enter a second stirring kettle 11 after the liquid level of the mixed liquor is higher than that of the first discharge port 12, and collecting materials when the liquid level in the second stirring kettle 11 is higher than that of a second discharge port 14;
step eight, performing constant-temperature aging on the collected materials for a certain time, and performing centrifugal dehydration or filtration dehydration on the aged materials to form cakes;
and step nine, uniformly mixing the cake-shaped material with a certain amount of displacement solvent, removing water, and finally drying to remove the displacement solvent, thereby obtaining the hydrotalcite-like product with uniform particle size and good dispersibility.
In a further preferred embodiment, in step one, the divalent metal comprises Ca2+、Mg2+、Fe2+、Zn2+、Ni2+、Co2+、Cu2+、Ti2 +Either one or both of; the trivalent metal includes Al3+、Fe3+Either one or both of;
in the second step, the alkali solution B is NaOH solution, NaOH and NaCO3Any one of the mixed solutions;
in the ninth step, the displacing solvent is any one of methanol, ethanol, propanol, acetone, n-butanol, hexane and cyclohexane.
Example 1
Referring to fig. 1 to 4, in the present embodiment, the charging barrel 303 of the charging and discharging mechanism 3 has an inner diameter of 12cm and a height of 20 cm; the inner diameter of the coprecipitation reaction kettle 8 is 12cm, the height of the coprecipitation reaction kettle is 14cm, and a first discharge port 12 is arranged at the position 6cm, 8cm and 10cm high of the kettle; the outer diameter of the metal ion solution compartment 701 is 10cm, the outer diameter of the alkali solution compartment 702 is 3.3cm, 2 holes are formed in the bottom of the alkali solution compartment 702, and 16 holes are formed in the bottom of the metal ion solution compartment 701; the inner diameter of the second stirring kettle 11 is 12cm, the height of the second stirring kettle is 14cm, the height of an inlet connected with the coprecipitation reaction kettle 8 is 4cm, and a second discharge hole 14 is arranged at the position 6cm, 8cm and 12cm higher than the opposite side of the second stirring kettle.
In a further optimized scheme, MgCl with the concentration of 0.5mol/L is contained in the metal ion solution storage tank 12And 0.25mol/L AlCl3The solution of (1); NaOH solution with the concentration of 2mol/L is contained in the alkali solution storage tank 2; adding 250mL of distilled water into a coprecipitation reaction kettle 8, adjusting the pH to 11.8 by using 0.1mol/L NaOH solution, and then adding 5mL of polyethylene glycol; adding 150mL of distilled water into the second stirring kettle 11, adjusting the pH to 11.8, and adding 3mL of polyethylene glycol;
starting the controller 301, rapidly lifting the push-pull piston 302, opening the upper open one-way valve 304, closing the lower open one-way valve 305, sucking the metal ion solution and the alkali solution into the first charging barrel and the second charging barrel through the first inflow pipe 41 and the second inflow pipe 42 respectively, and keeping the liquid level of the metal ion solution and the liquid level of the alkali solution to be 2000mL and 1000mL scribed lines respectively; starting the constant temperature stirrer 9, setting the magnetic stirring speed to be 600r/min and the temperature to be 40 ℃; the push-pull piston 302 is pressed downwards, the upward opening one-way valve 304 is closed, the downward opening one-way valve 305 is opened, the metal ion solution and the alkali solution respectively enter a metal ion solution compartment 701 and an alkali solution compartment 702 of the multipoint dripping shower head 7 through the first outflow pipe 51 and the second outflow pipe 52, and dripping to the coprecipitation reaction kettle 8 is started;
setting the propelling speed of the metal ion solution to be 120 drops/hole/min (the total flow of the acid solution is about 25mL/min) and the liquid inlet speed of the alkali solution to be 120 drops/hole (the total flow of the alkali solution is about 3mL/min), starting an outflow valve 13 of the coprecipitation reaction kettle 8 and a second stirring kettle 11 at the position of 8cm, wherein the retention time of coprecipitation and continuous stirring are both 0.54h, the coprecipitation mixed liquid reaches a first discharge port 12 and enters the second stirring kettle 11, and the mixed liquid in the second stirring kettle 11 reaches a second discharge port 14 to start collecting materials; aging the collected materials for 12h, filtering into cake, replacing with sufficient ethanol to remove water, and drying at 85 deg.C to remove ethanol.
Example 2
Referring to FIGS. 1 to 4, this example is different from example 1 in that MgCl having a concentration of 0.25mol/L is contained in a metal ion solution tank 12，0.25mol/L CaCl2And 0.25mol/L AlCl3The solution of (1); NaOH solution with the concentration of 2mol/L is contained in the alkali solution storage tank 2; adding 250mL of distilled water into a coprecipitation reaction kettle 8, adjusting the pH to 11.8 by using 0.1mol/L NaOH solution, and then adding 5mL of polyethylene glycol; adding 150mL of distilled water into the second stirring kettle 11, adjusting the pH to 11.8, and adding 3mL of polyethylene glycol;
starting the controller 301, rapidly lifting the push-pull piston 302, opening the upper open one-way valve 304, closing the lower open one-way valve 305, sucking the metal ion solution and the alkali solution into the first charging barrel and the second charging barrel through the first inflow pipe 41 and the second inflow pipe 42 respectively, and keeping the liquid level of the metal ion solution and the liquid level of the alkali solution to be 2000mL and 500mL reticle respectively; starting the constant temperature stirrer 9, setting the magnetic stirring speed to be 600r/min and the temperature to be 40 ℃; the push-pull piston 302 is pressed downwards, the upward opening one-way valve 304 is closed, the downward opening one-way valve 305 is opened, the metal ion solution and the alkali solution respectively enter a metal ion solution compartment 701 and an alkali solution compartment 702 of the multipoint dripping shower head 7 through the first outflow pipe 51 and the second outflow pipe 52, and dripping to the coprecipitation reaction kettle 8 is started;
setting the propulsion speed of the metal ion solution at 75 drops/hole/min (the total flow of the acid solution is about 16mL/min) and the liquid inlet speed of the alkali solution at 75 drops/hole/min (the total flow of the alkali solution is about 2mL/min), starting an outflow valve 13 of a coprecipitation reaction kettle 8 at the position of 10cm and a second stirring kettle 11 at the position of 12cm, wherein the coprecipitation retention time is 1h, and the continuous stirring is 1.3 h; the coprecipitation mixed liquid reaches a first discharge port 12 and enters a second stirring kettle 11, and the mixed liquid in the second stirring kettle 11 reaches a second discharge port 14 to begin to collect materials; aging the collected materials for 6h, filtering into cake, removing water by using sufficient n-butanol, and finally drying at 120 ℃ to remove the n-butanol.
In the description of the present invention, it is to be understood that the terms "longitudinal", "lateral", "upper", "lower", "front", "rear", "left", "right", "vertical", "horizontal", "top", "bottom", "inner", "outer", and the like, indicate orientations or positional relationships based on those shown in the drawings, are merely for convenience of description of the present invention, and do not indicate or imply that the referenced devices or elements must have a particular orientation, be constructed and operated in a particular orientation, and thus, are not to be construed as limiting the present invention.
The above-described embodiments are merely illustrative of the preferred embodiments of the present invention, and do not limit the scope of the present invention, and various modifications and improvements of the technical solutions of the present invention can be made by those skilled in the art without departing from the spirit of the present invention, and the technical solutions of the present invention are within the scope of the present invention defined by the claims.

Claims (10)

1. The device for preparing hydrotalcite-like compound by continuous flow coprecipitation is characterized by comprising:
the device comprises a coprecipitation reaction kettle (8), wherein a pH meter (6) is arranged in the coprecipitation reaction kettle (8), and a plurality of first discharge holes (12) are formed in the side wall of the coprecipitation reaction kettle (8);
the multipoint dripping shower head (7) comprises an alkaline solution compartment (702) fixedly mounted on the top surface of the inner cavity of the coprecipitation reaction kettle (8) and a metal ion solution compartment (701) sleeved outside the alkaline solution compartment (702), dripping micropores are formed in the bottoms of the alkaline solution compartment (702) and the metal ion solution compartment (701), and a sleeve (10) is fixedly connected to the bottom of the side wall of the metal ion solution compartment (701);
the second stirring kettle (11), the second stirring kettle (11) is communicated with the first discharge hole (12), and a plurality of second discharge holes (14) are formed in the side wall of the second stirring kettle (11);
a metal ion solution storage tank (1) and an alkaline solution storage tank (2), wherein the metal ion solution storage tank (1) is communicated with the metal ion solution compartment (701) through a feeding and discharging mechanism, and the alkaline solution storage tank (2) is communicated with the alkaline solution compartment (702) through another feeding and discharging mechanism;
the bottom of the coprecipitation reaction kettle (8) and the bottom of the second stirring kettle (11) are both provided with a constant temperature stirrer (9), and the first discharge hole (12) and the second discharge hole (14) are both provided with an outflow valve (13).
2. The apparatus for preparing hydrotalcite-like compound by continuous flow co-precipitation according to claim 1, wherein: the feeding and discharging mechanism comprises a charging barrel (303), an upper opening one-way valve (304), a lower opening one-way valve (305), a push-pull piston (302) arranged in the charging barrel (303), and a controller (301) fixedly connected to the top of the push-pull piston (302);
a liquid inlet and a liquid outlet are formed in the end face of the bottom of the charging barrel (303), the upper opening check valve (304) is fixedly mounted in the liquid inlet, and the lower opening check valve (305) is fixedly mounted in the liquid outlet;
the charging barrels (303) of the two feeding and discharging mechanisms are respectively set as a first charging barrel and a second charging barrel;
the liquid inlet of the first material cylinder is communicated with the metal ion solution storage tank (1) through a first inlet flow pipe (41), and the liquid outlet of the first material cylinder is communicated with the metal ion solution compartment (701) through a first outlet flow pipe (51);
the liquid inlet of the second cartridge is in communication with the alkaline solution storage tank (2) via a second inlet pipe (42), and the liquid outlet of the second cartridge is in communication with the alkaline solution compartment (702) via a second outlet pipe (52).
3. The apparatus for preparing hydrotalcite-like compound by continuous flow co-precipitation according to claim 1, wherein: and the detection end of the pH meter (6) is positioned between the outer wall of the sleeve (10) and the inner wall of the coprecipitation reaction kettle (8).
4. The apparatus for preparing hydrotalcite-like compound by continuous flow co-precipitation according to claim 1, wherein: sealing covers are mounted at the tops of the coprecipitation reaction kettle (8) and the second stirring kettle (11), a hole pipe is formed in each sealing cover, and the metal ion solution compartment (701) is fixedly mounted on the bottom surface of each sealing cover of the coprecipitation reaction kettle (8).
5. The apparatus for preparing hydrotalcite-like compound by continuous flow co-precipitation according to claim 1, wherein: the ratio of the area of the bottom end face of the metal ion solution compartment (701) to the area of the bottom end face of the caustic solution compartment (702) is 1: 8.
6. The apparatus for preparing hydrotalcite-like compound by continuous flow co-precipitation according to claim 1, wherein: the number ratio of the dropping pores of the metal ion solution compartment (701) to the dropping pores of the alkali solution compartment (702) is 1: 8.
7. The apparatus for preparing hydrotalcite-like compound by continuous flow co-precipitation according to claim 1, wherein: the first discharge ports (12) are respectively arranged at different heights on the side wall of the coprecipitation reaction kettle (8); the plurality of second discharge holes (14) are respectively arranged at different heights on the side wall of the second stirring kettle (11).
8. The apparatus for preparing hydrotalcite-like compound by continuous flow co-precipitation according to claim 2, wherein: the side walls of the first material cylinder and the second material cylinder are provided with scales.
9. A method for preparing hydrotalcite-like compound by continuous flow co-precipitation, based on the device for preparing hydrotalcite-like compound by continuous flow co-precipitation according to any one of claims 1 to 8, characterized by comprising the following steps:
step one, a solution A is contained in a metal ion solution storage tank (1);
secondly, filling an alkali solution B into an alkali solution storage tank (2);
step three, respectively filling distilled water into the coprecipitation reaction kettle (8) and the second stirring kettle (11), adjusting the pH value by using NaOH, and adding polyethylene glycol;
step four, respectively storing the solution A and the alkali solution B in two feeding and discharging mechanisms;
step five, starting the two constant-temperature stirrers (9) and setting the required stirring speed and temperature;
sixthly, adding the solution A into a metal ion solution compartment (701), adding the alkali solution B into an alkali solution compartment (702), and dropwise adding the solution A and the alkali solution B into a coprecipitation reaction kettle (8);
seventhly, after the liquid level of the mixed liquid in the coprecipitation reaction kettle (8) is higher than the first discharge hole (12), the mixed liquid enters a second stirring kettle (11), and the materials can be collected when the liquid level in the second stirring kettle (11) is higher than the second discharge hole (14);
step eight, ageing the materials at constant temperature, and centrifugally dewatering or filtering and dewatering the materials into cakes;
and step nine, uniformly mixing the cake-shaped material with a displacement solvent, removing water, and finally drying to remove the displacement solvent, thereby obtaining the hydrotalcite-like product.
10. The apparatus and method for preparing hydrotalcite-like compound by continuous flow co-precipitation according to claim 9, wherein: in the first step, the solution A is a solution containing divalent metal ions and trivalent metal ions, and the divalent metal includes Ca2+、Mg2+、Fe2+、Zn2+、Ni2+、Co2+、Cu2+、Ti2+Either one or both of; the trivalent metal comprises Al3+、Fe3+Either one or both of;
in the second stepThe alkali solution B is NaOH solution, NaOH and NaCO3Any one of the mixed solutions;
in the ninth step, the displacement solvent is any one of methanol, ethanol, propanol, acetone, n-butanol, hexane and cyclohexane.
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Citations (24)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
FR2601937A1 (en) * 1986-07-23 1988-01-29 Commissariat Energie Atomique PROCESS FOR THE PREPARATION OF METAL FLUOROS FOR USE IN THE MANUFACTURE OF FLUORESCENT GLASSES
CN1231266A (en) * 1998-04-03 1999-10-13 深圳广远实业发展有限公司 Method and apparatus for making spherical nickel hydroxide with surface defect
JP2001342233A (en) * 2000-06-01 2001-12-11 Asahi Kasei Corp Method for polymerizing gaseous monomer and polymerization apparatus
JP2003229406A (en) * 2002-02-04 2003-08-15 Matsushita Environment Airconditioning Eng Co Ltd Preparing device for liquid medicine and preparing method thereof
CN101381094A (en) * 2007-09-03 2009-03-11 襄樊市油建化工有限公司 Method for preparing nano magnalium hydrotalcite and equipment thereof
CN101735109A (en) * 2009-12-04 2010-06-16 赛鼎工程有限公司 Method for continuously producing organic isocyanate
US20110300470A1 (en) * 2006-03-31 2011-12-08 H.C. Starck Gmbh Device and method for the production of compounds by precipitation
CN202170627U (en) * 2011-06-08 2012-03-21 牛智勇 Composite spraying device for wall heat-preservation decoration plates
CN103014846A (en) * 2013-01-14 2013-04-03 东莞市中镓半导体科技有限公司 Concentric-ring sprayer structure for material vapor phase epitaxy
US20130194723A1 (en) * 2010-07-21 2013-08-01 Cleanvolt Energy, Inc. Use of organic and organometallic high dielectric constant material for improved energy storage devices and associated methods
CN104418388A (en) * 2013-08-26 2015-03-18 荆门市格林美新材料有限公司 Process and device for continuous production of superfine cobalt carbonate powder
CN105289346A (en) * 2015-11-27 2016-02-03 安徽理工大学 Jet medicament disperse system and fine coal particle pulp mixing modification equipment applying same
CN205340797U (en) * 2015-12-19 2016-06-29 张嘉强 But high security chemical reaction cauldron of automatic blending
CN205761191U (en) * 2016-05-25 2016-12-07 湖州创能新材料科技有限公司 A kind of continuous way multicomponent coprecipitation reaction device
CN106241856A (en) * 2016-01-13 2016-12-21 四川理工学院 A kind of preparation method of zinc-magnesium aluminum houghite
CN106512466A (en) * 2016-12-29 2017-03-22 天津中医药大学 Alcohol precipitation apparatus and method combining high-speed centrifugal atomization with continuous alcohol precipitation
CN106943907A (en) * 2017-04-14 2017-07-14 西南化工研究设计院有限公司 A kind of coprecipitation prepares the device and method of copper-based catalysts
CN107651712A (en) * 2017-09-13 2018-02-02 太原理工大学 It is co-precipitated the method that a step prepares nitrate anion intercalation NiAl-HTLcs
CN207121470U (en) * 2017-07-18 2018-03-20 成都浩宇思源环境科技有限公司 A kind of telescopic reactor realized biogas residue and biogas liquid and efficiently separated
CN207769802U (en) * 2017-12-29 2018-08-28 重庆华森制药股份有限公司 A kind of novel device producing Hydrotalcite
CN108644085A (en) * 2018-03-26 2018-10-12 徐志富 A kind of disinfectant is blended device
CN109483770A (en) * 2018-12-20 2019-03-19 中绿新材料（江苏）有限公司 A kind of discarded recycling processing unit (plant) of butyl rubber
CN109514858A (en) * 2018-11-02 2019-03-26 四川大学华西医院 Multi-channel 3D printing nozzle and method for manufacturing pipeline by adopting same
CN209188548U (en) * 2018-08-31 2019-08-02 大连固瑞聚氨酯股份有限公司 A kind of bi-component group angle glue mixing head connector

Patent Citations (24)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
FR2601937A1 (en) * 1986-07-23 1988-01-29 Commissariat Energie Atomique PROCESS FOR THE PREPARATION OF METAL FLUOROS FOR USE IN THE MANUFACTURE OF FLUORESCENT GLASSES
CN1231266A (en) * 1998-04-03 1999-10-13 深圳广远实业发展有限公司 Method and apparatus for making spherical nickel hydroxide with surface defect
JP2001342233A (en) * 2000-06-01 2001-12-11 Asahi Kasei Corp Method for polymerizing gaseous monomer and polymerization apparatus
JP2003229406A (en) * 2002-02-04 2003-08-15 Matsushita Environment Airconditioning Eng Co Ltd Preparing device for liquid medicine and preparing method thereof
US20110300470A1 (en) * 2006-03-31 2011-12-08 H.C. Starck Gmbh Device and method for the production of compounds by precipitation
CN101381094A (en) * 2007-09-03 2009-03-11 襄樊市油建化工有限公司 Method for preparing nano magnalium hydrotalcite and equipment thereof
CN101735109A (en) * 2009-12-04 2010-06-16 赛鼎工程有限公司 Method for continuously producing organic isocyanate
US20130194723A1 (en) * 2010-07-21 2013-08-01 Cleanvolt Energy, Inc. Use of organic and organometallic high dielectric constant material for improved energy storage devices and associated methods
CN202170627U (en) * 2011-06-08 2012-03-21 牛智勇 Composite spraying device for wall heat-preservation decoration plates
CN103014846A (en) * 2013-01-14 2013-04-03 东莞市中镓半导体科技有限公司 Concentric-ring sprayer structure for material vapor phase epitaxy
CN104418388A (en) * 2013-08-26 2015-03-18 荆门市格林美新材料有限公司 Process and device for continuous production of superfine cobalt carbonate powder
CN105289346A (en) * 2015-11-27 2016-02-03 安徽理工大学 Jet medicament disperse system and fine coal particle pulp mixing modification equipment applying same
CN205340797U (en) * 2015-12-19 2016-06-29 张嘉强 But high security chemical reaction cauldron of automatic blending
CN106241856A (en) * 2016-01-13 2016-12-21 四川理工学院 A kind of preparation method of zinc-magnesium aluminum houghite
CN205761191U (en) * 2016-05-25 2016-12-07 湖州创能新材料科技有限公司 A kind of continuous way multicomponent coprecipitation reaction device
CN106512466A (en) * 2016-12-29 2017-03-22 天津中医药大学 Alcohol precipitation apparatus and method combining high-speed centrifugal atomization with continuous alcohol precipitation
CN106943907A (en) * 2017-04-14 2017-07-14 西南化工研究设计院有限公司 A kind of coprecipitation prepares the device and method of copper-based catalysts
CN207121470U (en) * 2017-07-18 2018-03-20 成都浩宇思源环境科技有限公司 A kind of telescopic reactor realized biogas residue and biogas liquid and efficiently separated
CN107651712A (en) * 2017-09-13 2018-02-02 太原理工大学 It is co-precipitated the method that a step prepares nitrate anion intercalation NiAl-HTLcs
CN207769802U (en) * 2017-12-29 2018-08-28 重庆华森制药股份有限公司 A kind of novel device producing Hydrotalcite
CN108644085A (en) * 2018-03-26 2018-10-12 徐志富 A kind of disinfectant is blended device
CN209188548U (en) * 2018-08-31 2019-08-02 大连固瑞聚氨酯股份有限公司 A kind of bi-component group angle glue mixing head connector
CN109514858A (en) * 2018-11-02 2019-03-26 四川大学华西医院 Multi-channel 3D printing nozzle and method for manufacturing pipeline by adopting same
CN109483770A (en) * 2018-12-20 2019-03-19 中绿新材料（江苏）有限公司 A kind of discarded recycling processing unit (plant) of butyl rubber

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
SALWA BOUGACHA GHORBEL等: "Phosphoric acid intercalated Mg–Al hydrotalcite-like compounds for catalytic carboxylation reaction of methanol in a continuous system" *

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