CN112495333A - Macroporous ion exchange resin processing device and processing technology - Google Patents
Macroporous ion exchange resin processing device and processing technology Download PDFInfo
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- CN112495333A CN112495333A CN202011230610.2A CN202011230610A CN112495333A CN 112495333 A CN112495333 A CN 112495333A CN 202011230610 A CN202011230610 A CN 202011230610A CN 112495333 A CN112495333 A CN 112495333A
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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
- B01J19/20—Stationary reactors having moving elements inside in the form of helices, e.g. screw reactors
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D33/00—Filters with filtering elements which move during the filtering operation
- B01D33/27—Filters with filtering elements which move during the filtering operation with rotary filtering surfaces, which are neither cylindrical nor planar, e.g. helical surfaces
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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
- B01J19/0006—Controlling or regulating processes
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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
- B01J19/0053—Details of the reactor
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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
- B01J4/00—Feed or outlet devices; Feed or outlet control devices
- B01J4/001—Feed or outlet devices as such, e.g. feeding tubes
- B01J4/007—Feed or outlet devices as such, e.g. feeding tubes provided with moving parts
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F8/00—Chemical modification by after-treatment
- C08F8/30—Introducing nitrogen atoms or nitrogen-containing groups
- C08F8/32—Introducing nitrogen atoms or nitrogen-containing groups by reaction with amines
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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
- B01J2204/00—Aspects relating to feed or outlet devices; Regulating devices for feed or outlet devices
- B01J2204/005—Aspects relating to feed or outlet devices; Regulating devices for feed or outlet devices the outlet side being of particular interest
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Abstract
The invention discloses a processing device and a processing technology of macroporous ion exchange resin, the processing device comprises a reaction kettle, a first feeding pipe and a second feeding pipe are arranged on the left side of the reaction kettle, a stirring device is also arranged in the reaction kettle, the stirring device is arranged on the right part of the reaction kettle, a filtering device is also connected on the reaction kettle on the right side of the stirring device, the filtering device is communicated with the reaction kettle, heating devices are wrapped outside the filtering device and the reaction kettle, and the heating devices are powered by an external power supply.
Description
Technical Field
The invention relates to the technical field of processing of macroporous ion exchange resin, and particularly belongs to a processing device and a processing technology of macroporous ion exchange resin.
Background
The macroporous ion exchange resin refers to an insoluble infusible polymer having a macroporous structure and a network structure with functional groups. The macroporous resin generally has a pore diameter of 10nm or more. Surface area of 5m2The difference between the true density and the apparent density is not less than 0.059/mL resin, the size and the shape of the pores are not changed along with the environmental condition, the resin is opaque and milk white in a wet state, and the resin is easy to permeate a solvent and is less swelled. During polymerization, pore-foaming agent (solvent, non-solvent, salt or soluble high polymer) is added to prepare ion exchange resin. For example, divinylbenzene, styrene and inert filler calcium carbonate are polymerized to prepare resin, and the filler is extracted to form a macroporous structure. The organic polymer compound can be adsorbed and eluted during regeneration due to the large pore diameter, porosity and surface area. It also has good wear resistance, oxidation resistance and organic pollution resistance, and can be used for separation and purification. The existing macroporous ion exchange resin production process mainly adopts an intermittent production method, mainly because the white balls need enough reaction time in the production process to form macroporous white balls with uniform particles, and meanwhile, the existing reaction system has slow reaction process, so that the production period is longer.
Disclosure of Invention
The invention aims to provide a processing device and a processing technology of macroporous ion exchange resin, which overcome the problems that the production period of white balls of macroporous ion exchange resin raw materials in the prior art is long and continuous production cannot be realized.
In order to solve the problems, the technical scheme adopted by the invention is as follows:
the utility model provides a macroporous ion exchange resin's processingequipment, includes reation kettle, reation kettle left side be equipped with first inlet pipe and second inlet pipe, reation kettle in still be equipped with agitating unit, agitating unit install in reation kettle's right part, and still be connected with filter equipment on the reation kettle on agitating unit right side, filter equipment communicates with each other with reation kettle, filter equipment and reation kettle's outside parcel have heating device, heating device supplied power by external power source.
Wherein, agitating unit include motor, first belt pulley, stirring rake and agitator, the agitator install in reation kettle's top, and the bottom opening of agitator, agitator bottom not contact with reation kettle, the motor is located the top of agitator, the stirring rake comprises puddler and the paddle of installing on the puddler, the paddle adopts helical blade, the puddler install in the pivot of motor, and the paddle is located inside the agitator, puddler and agitator between be connected through the bearing, the agitator of paddle top on still be equipped with the bin outlet, the bin outlet with filter equipment and agitator intercommunication, first belt pulley install on the puddler of stirring rake top, first belt pulley is connected through belt drive with filter equipment, the motor supplied power by external power source.
The stirring barrel is internally provided with a first partition plate and a second partition plate, the first partition plate and the second partition plate are arranged on the stirring barrel between the first belt pulley and the discharge port, a heat insulation cavity is formed between the first partition plate and the second partition plate, the first partition plate and the stirring rod are connected through a bearing, and the second partition plate and the stirring rod are connected through a rubber ring.
Wherein, the filtering device comprises a filtering barrel, a mounting plate, a filtering paddle and a second belt pulley, the filtering barrel is arranged on the right side of the reaction kettle, the bottom of the filtering barrel is communicated with the reaction kettle, the mounting plate is fixedly arranged on the upper part of the filtering barrel, the filtering paddle is arranged on the mounting plate through a bearing, the second belt pulley is arranged on the filtering paddle above the mounting plate, the second belt pulley is connected with the first belt pulley through a belt transmission, the filtering paddle comprises a rotary rod and a spiral filter screen arranged on the rotary rod, the spiral filter screen is arranged below the mounting plate, a drain pipe and a discharge pipe are arranged on the right side of the filtering barrel, the drain pipe is positioned at the bottom of the filtering barrel and is arranged on a stop valve, the discharge pipe is positioned on the upper part of the filtering barrel below the mounting plate and is positioned on the filtering barrel on the right side of the top of the spiral filter screen, the discharge port is positioned in the middle of the spiral filter screen and communicates the middle of the reaction kettle with the filter vat.
The process of processing macroporous ion exchange resin with the processing device of macroporous ion exchange resin includes the following steps:
s1, vacuumizing the reaction kettle, and then filling nitrogen;
s2, adding an aqueous solution containing Arabic gum and aluminum chloride into the reaction kettle through a first feeding pipe, stirring and heating;
s3, continuously adding a mixed solution containing styrene, benzoyl peroxide, a pore-forming agent, divinylbenzene and ferrocene into the reaction kettle through the second feeding pipe, simultaneously adding an aqueous solution containing Arabic gum and aluminum chloride into the reaction kettle through the first feeding pipe, stirring for reaction, and obtaining a macroporous white ball through the discharging pipe;
s4, chloromethylating the macroporous white spheres with chloromethyl ether under the catalysis of ferric trichloride, and then filtering and washing to obtain chlorine spheres;
s5, placing the chlorine ball in isobutanol to swell, then adding trioctyl decyl tertiary amine to carry out amination reaction under the condition of condensation reflux, and obtaining the macroporous ion exchange resin after the amination reaction is finished.
Wherein the volume flow ratio of the mixed solution to the aqueous solution is 12-15: 1.
Compared with the prior art, the invention has the following implementation effects:
1. the processing device of the invention enables the reaction liquid at the lower part of the reaction kettle to be extracted to the upper part of the stirring barrel through the stirring and drawing effects generated by the stirring paddle of the stirring device, and then the reaction liquid enters the stirring barrel from the discharge port and then flows back into the reaction kettle, so that the reaction liquid in the reaction kettle is always in the stirring reaction process, and the white balls prepared in the reaction kettle are prevented from being adhered.
2. The filter vat of the processing device of the invention is internally provided with the spiral filter screen and the rotary rod, so that the large-pore white balls with the particle size meeting the requirement in the reaction liquid entering the filter vat from the discharge port are filtered by the spiral filter screen, and are continuously discharged from the discharge pipe under the rotary conveying action of the spiral filter screen.
3. The processing device provided by the invention has the advantages that through the matching of the stirring device and the filtering device, the solution in the reaction kettle is stirred and mixed, and the macroporous white ball products meeting the particle size requirement can be continuously discharged from the discharge pipe through continuous filtering and conveying, so that the processing device can be used for continuous white ball production to meet the production of macroporous ion exchange resin.
4. The aluminum chloride and the Arabic gum are used in a matching manner, and the electron transfer effect of iron ions in ferrocene is utilized, so that the synthesis efficiency of the macroporous white ball is improved, the synthesis time is shortened, the macroporous white ball can be continuously produced, and the continuous preparation of the macroporous ion exchange resin is guaranteed.
Drawings
FIG. 1 is a top view of the present invention;
FIG. 2 is a schematic view of the structure of the present invention.
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 the description of the present invention, it should be noted that the terms "upper", "lower", "front", "rear", "left", "right", "vertical", "inner", "outer", etc., indicate orientations or positional relationships based on the orientations or positional relationships shown in the drawings, and are only for convenience of description and simplicity of description, but do not indicate or imply that the device or element being referred to must have a particular orientation to be constructed and operated in a particular orientation, and thus, should not be construed as limiting the present invention.
In the description of the present invention, it should be noted that, unless otherwise explicitly specified or limited, the terms "mounted," "connected," and "connected" are to be construed broadly, e.g., as meaning either a fixed connection, a removable connection, or an integral connection; can be mechanically or electrically connected; may be directly connected or indirectly connected through an intermediate. The specific meanings of the above terms in the present invention can be understood in specific cases to those skilled in the art.
The processing device for continuously producing the macroporous ion exchange resin comprises a reaction kettle 1, wherein a first feeding pipe 11 and a second feeding pipe 12 are arranged on the left side of the reaction kettle 1, a stirring device is also arranged in the reaction kettle 1 and comprises a motor 4, a first belt pulley 5, a stirring paddle and a stirring barrel 2, the stirring barrel 2 is arranged at the top of the reaction kettle 1 and is positioned at the right part of the reaction kettle 1, the bottom of the stirring barrel 2 is opened, the bottom of the stirring barrel 2 is not contacted with the reaction kettle 1, the stirring paddle is arranged on a rotating shaft of the motor 4 and is positioned inside the stirring barrel 2, the motor 4 is positioned at the top of the stirring barrel 2, the stirring paddle consists of a stirring rod 3 and a paddle 31 arranged on the stirring rod 3, the paddle 31 adopts a spiral paddle blade 31, the stirring rod 3 is connected with the stirring barrel 2 through a bearing 23, a discharge hole 15 is also arranged on the stirring barrel 2 above the paddle 31, and the reaction kettle 1 on the right side of, discharge gate 15 communicates filter equipment and agitator 2, and first belt pulley 5 is installed on the puddler 3 of stirring rake top, and first belt pulley 5 passes through belt 6 drive with filter equipment to be connected, and motor 4 is supplied power by external power source.
Still be equipped with first baffle 21 and second baffle 22 in agitator 2, first baffle 21 and second baffle 22 set up on agitator 2 between first belt pulley 5 and bin outlet 15, and form thermal-insulated chamber between first baffle 21 and the second baffle 22, be connected through bearing 23 between first baffle 21 and the puddler 3, be connected through rubber circle 24 between second baffle 22 and the puddler 3, the thermal-insulated chamber between first baffle 21 and the second baffle 22 makes to keep apart between motor 4 and the reaction liquid in the reation kettle 1, avoid motor 4 temperature to rise, lead to motor 4 to damage easily, avoid volatilizing of the organic solvent in the reaction liquid to produce the corruption to motor 4 simultaneously.
The filtering device comprises a filtering barrel 9, a mounting plate 8, a filtering paddle and a second belt pulley 72, the filtering barrel 9 is arranged at the right side of the reaction kettle 1, the bottom of the filter barrel 9 is communicated with the reaction kettle 1, the mounting plate 8 is fixedly arranged at the upper part of the filter barrel 9, the filter paddle is arranged on the mounting plate 8 through a bearing 23, the second belt pulley 72 is arranged on the filter paddle above the mounting plate 8, the second belt pulley 72 is in transmission connection with the first belt pulley 5 through a belt 6, the filter paddle comprises a rotating rod 7 and a spiral filter screen 71 arranged on the rotating rod 7, the spiral filter screen 71 is positioned below the mounting plate 8, a liquid discharge pipe 13 and a discharge pipe 14 are arranged on the right side of the filtering barrel 9, the liquid discharge pipe 13 is positioned at the bottom of the filtering barrel 9, and a stop valve is arranged on the liquid discharge pipe 13, and the discharge pipe 14 is positioned at the upper part of the filter barrel 9 below the mounting plate 8 and is positioned on the filter barrel 9 at the right side of the top of the spiral filter screen 71.
The heating sleeve 10 is wrapped outside the filtering device and the reaction kettle 1 and is powered by an external power supply.
When the device is used for preparing the macroporous ion exchange resin, the reaction kettle 1 is firstly vacuumized, then nitrogen is filled, and the process is repeated for three times; subsequently, 5kg of an aqueous solution containing 1.6 wt% of gum arabic and 4 wt% of aluminum chloride was added to the reaction tank 1 through the first feed tube 11, followed by stirring and heating to 73 ℃.
Then, a mixed solution containing styrene, benzoyl peroxide, a porogen, divinylbenzene and ferrocene was continuously fed into the reaction vessel 1 through the second feed pipe 12, and the flow rate was controlled at 2L/min. The mass ratio of styrene to benzoyl peroxide to pore-forming agent to divinylbenzene to ferrocene is 1.1:0.032:3.1:1.4:0.008, meanwhile, an aqueous solution containing 8.6 wt% of Arabic gum and 17.6 wt% of aluminum chloride is continuously added into a reaction kettle 1 through a first feeding pipe 11, the volume flow ratio of the mixed solution to the aqueous solution is 12:1, stirring reaction is carried out, a discharging pipe 14 obtains macroporous white balls, a spiral filter screen 71 used in the method is 20 meshes, the particle size of the macroporous white balls obtained at the discharging pipe 14 is 0.9-1.1mm, and after the reaction is carried out for 3 hours, 1.3kg of macroporous white balls can be obtained at the discharging pipe 14 per hour.
Then, chloromethylating the macroporous white spheres with chloromethyl ether under the catalysis of ferric trichloride, wherein the mass ratio of the macroporous white spheres to the ferric trichloride and the chloromethyl ether is 1:3.2:0.06, and then filtering and washing to obtain the chlorine spheres; and then placing the chlorine balls in isobutanol with the mass 5 times that of the chlorine balls for swelling for 12 hours, adding trioctyl decyl tertiary amine with the mass 0.3 times that of the chlorine balls for amination under the condition of condensation reflux, wherein the amination temperature is 70 ℃, and the amination time is 16 hours, so as to obtain the macroporous ion exchange resin.
If aluminum chloride and ferrocene are not added in the reaction process, only 0.6kg of macroporous white balls can be obtained in the discharge pipe 14 of the reaction kettle 1 per hour.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (6)
1. A processing device of macroporous ion exchange resin is characterized in that: including reation kettle, reation kettle left side be equipped with first inlet pipe and second inlet pipe, reation kettle in still be equipped with agitating unit, agitating unit install in reation kettle's right part, and still be connected with filter equipment on the reation kettle on agitating unit right side, filter equipment communicates with each other with reation kettle, filter equipment and reation kettle's outside parcel have heating device, heating device supplied power by external power source.
2. The apparatus for processing macroporous ion exchange resin as claimed in claim 1, wherein: agitating unit include motor, first belt pulley, stirring rake and agitator, the agitator install in reation kettle's top, and the bottom opening of agitator, agitator bottom not contact with reation kettle, the motor is located the top of agitator, the stirring rake comprises puddler and the paddle of installing on the puddler, the paddle adopts screw propeller blade, the puddler install in the pivot of motor, and the paddle is located inside the agitator, puddler and agitator between be connected through the bearing, the agitator of paddle top on still be equipped with the bin outlet, the bin outlet with filter equipment and agitator intercommunication, first belt pulley install on the puddler of stirring rake top, first belt pulley passes through belt drive with filter equipment and is connected, the motor supplied power by external power source.
3. The apparatus for processing macroporous ion exchange resin as claimed in claim 2, wherein: the agitator in still be equipped with first baffle and second baffle, first baffle and second baffle set up on the agitator between first belt pulley and bin outlet, and form thermal-insulated chamber between first baffle and the second baffle, first baffle and puddler between be connected through the bearing, second baffle and puddler between be connected through the rubber circle.
4. The apparatus for processing macroporous ion exchange resin as claimed in claim 2, wherein: the filtering device comprises a filtering barrel, a mounting plate, a filtering paddle and a second belt pulley, the filtering barrel is arranged on the right side of the reaction kettle, the bottom of the filtering barrel is communicated with the reaction kettle, the mounting plate is fixedly arranged on the upper part of the filtering barrel, the filtering paddle is arranged on the mounting plate through a bearing, the second belt pulley is arranged on the filtering paddle above the mounting plate, the second belt pulley is connected with the first belt pulley through a belt transmission, the filtering paddle comprises a rotary rod and a spiral filter screen arranged on the rotary rod, the spiral filter screen is arranged below the mounting plate, a liquid discharge pipe and a discharge pipe are arranged on the right side of the filtering barrel, the liquid discharge pipe is positioned at the bottom of the filtering barrel, a stop valve is arranged on the liquid discharge pipe, the discharge pipe is positioned on the upper part of the filtering barrel below the mounting plate and is positioned on the filtering barrel on the right side of the, the discharge gate be located the middle part of spiral filter screen, the discharge gate is with reation kettle's middle part and filter vat intercommunication.
5. The process for processing macroporous ion exchange resin by using the apparatus for processing macroporous ion exchange resin as claimed in any one of claims 1 to 4, wherein: the method comprises the following steps:
s1, vacuumizing the reaction kettle, and then filling nitrogen;
s2, adding an aqueous solution containing Arabic gum and aluminum chloride into the reaction kettle through a first feeding pipe, stirring and heating;
s3, continuously adding a mixed solution containing styrene, benzoyl peroxide, a pore-forming agent, divinylbenzene and ferrocene into the reaction kettle through the second feeding pipe, simultaneously adding an aqueous solution containing Arabic gum and aluminum chloride into the reaction kettle through the first feeding pipe, stirring for reaction, and obtaining a macroporous white ball through the discharging pipe;
s4, chloromethylating the macroporous white spheres with chloromethyl ether under the catalysis of ferric trichloride, and then filtering and washing to obtain chlorine spheres;
s5, placing the chlorine ball in isobutanol to swell, then adding trioctyl decyl tertiary amine to carry out amination reaction under the condition of condensation reflux, and obtaining the macroporous ion exchange resin after the amination reaction is finished.
6. The process for processing macroporous ion exchange resins of claim 5, wherein: the volume flow ratio of the mixed solution to the aqueous solution is 12-15: 1.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011230610.2A CN112495333A (en) | 2020-11-06 | 2020-11-06 | Macroporous ion exchange resin processing device and processing technology |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011230610.2A CN112495333A (en) | 2020-11-06 | 2020-11-06 | Macroporous ion exchange resin processing device and processing technology |
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| CN112495333A true CN112495333A (en) | 2021-03-16 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN202011230610.2A Pending CN112495333A (en) | 2020-11-06 | 2020-11-06 | Macroporous ion exchange resin processing device and processing technology |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO1992004114A1 (en) * | 1990-09-04 | 1992-03-19 | Reanal Finomvegyszergyár | Apparatus for creating intensive contact between a liquid and a particulate solid |
| CN1103812A (en) * | 1993-05-26 | 1995-06-21 | 威勒·杜兰建筑设备公司 | Filter device |
| CN1122582A (en) * | 1993-05-05 | 1996-05-15 | 海瑞·尼尔森 | Rotating filter |
| CN108164622A (en) * | 2018-02-28 | 2018-06-15 | 江苏苏青水处理工程集团有限公司 | A kind of preparation method of Thermal Stable Anion Exchange Resin |
| CN208757598U (en) * | 2018-08-20 | 2019-04-19 | 江苏苏青水处理工程集团有限公司 | Ion exchange resin continuous reacting device |
-
2020
- 2020-11-06 CN CN202011230610.2A patent/CN112495333A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO1992004114A1 (en) * | 1990-09-04 | 1992-03-19 | Reanal Finomvegyszergyár | Apparatus for creating intensive contact between a liquid and a particulate solid |
| CN1122582A (en) * | 1993-05-05 | 1996-05-15 | 海瑞·尼尔森 | Rotating filter |
| CN1103812A (en) * | 1993-05-26 | 1995-06-21 | 威勒·杜兰建筑设备公司 | Filter device |
| CN108164622A (en) * | 2018-02-28 | 2018-06-15 | 江苏苏青水处理工程集团有限公司 | A kind of preparation method of Thermal Stable Anion Exchange Resin |
| CN208757598U (en) * | 2018-08-20 | 2019-04-19 | 江苏苏青水处理工程集团有限公司 | Ion exchange resin continuous reacting device |
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Application publication date: 20210316 |
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