CN113559811A - Experimental device for anhydrous zinc acetate preparation and aftertreatment - Google Patents

Experimental device for anhydrous zinc acetate preparation and aftertreatment Download PDF

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Publication number
CN113559811A
CN113559811A CN202110959047.0A CN202110959047A CN113559811A CN 113559811 A CN113559811 A CN 113559811A CN 202110959047 A CN202110959047 A CN 202110959047A CN 113559811 A CN113559811 A CN 113559811A
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CN
China
Prior art keywords
post
zinc acetate
cavity
anhydrous zinc
preparing
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CN202110959047.0A
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Chinese (zh)
Inventor
周红艳
侯涛
仝庆
吴元明
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Sanmen Nuclear Power Co Ltd
Research Institute of Physical and Chemical Engineering of Nuclear Industry
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Sanmen Nuclear Power Co Ltd
Research Institute of Physical and Chemical Engineering of Nuclear Industry
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Application filed by Sanmen Nuclear Power Co Ltd, Research Institute of Physical and Chemical Engineering of Nuclear Industry filed Critical Sanmen Nuclear Power Co Ltd
Priority to CN202110959047.0A priority Critical patent/CN113559811A/en
Publication of CN113559811A publication Critical patent/CN113559811A/en
Pending legal-status Critical Current

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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
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D29/00—Filters with filtering elements stationary during filtration, e.g. pressure or suction filters, not covered by groups B01D24/00 - B01D27/00; Filtering elements therefor
    • B01D29/01—Filters with filtering elements stationary during filtration, e.g. pressure or suction filters, not covered by groups B01D24/00 - B01D27/00; Filtering elements therefor with flat filtering elements
    • B01D29/03—Filters with filtering elements stationary during filtration, e.g. pressure or suction filters, not covered by groups B01D24/00 - B01D27/00; Filtering elements therefor with flat filtering elements self-supporting
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
    • C07C51/41—Preparation of salts of carboxylic acids
    • C07C51/412—Preparation of salts of carboxylic acids by conversion of the acids, their salts, esters or anhydrides with the same carboxylic acid part
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
    • C07C51/42—Separation; Purification; Stabilisation; Use of additives
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F26—DRYING
    • F26B—DRYING SOLID MATERIALS OR OBJECTS BY REMOVING LIQUID THEREFROM
    • F26B11/00—Machines or apparatus for drying solid materials or objects with movement which is non-progressive
    • F26B11/12—Machines or apparatus for drying solid materials or objects with movement which is non-progressive in stationary drums or other mainly-closed receptacles with moving stirring devices
    • F26B11/14—Machines or apparatus for drying solid materials or objects with movement which is non-progressive in stationary drums or other mainly-closed receptacles with moving stirring devices the stirring device moving in a horizontal or slightly-inclined plane
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F26—DRYING
    • F26B—DRYING SOLID MATERIALS OR OBJECTS BY REMOVING LIQUID THEREFROM
    • F26B25/00—Details of general application not covered by group F26B21/00 or F26B23/00
    • F26B25/04—Agitating, stirring, or scraping devices

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Mechanical Engineering (AREA)
  • General Engineering & Computer Science (AREA)
  • Physical Or Chemical Processes And Apparatus (AREA)
  • Manufacture And Refinement Of Metals (AREA)

Abstract

The invention discloses an experimental device for preparing and post-treating anhydrous zinc acetate, which comprises a reaction device and a post-treatment device, wherein the reaction device and the post-treatment device are both provided with a stirring mechanism; the reaction device comprises a reaction cavity, a liquid inlet and a solid charging port are arranged at the upper part of the reaction cavity, a discharge port is arranged at the bottom of the reaction cavity, and a No. I jacket is arranged outside the reaction cavity; the post-treatment device comprises a post-treatment cavity, a condensing device, a heat exchanger and a collector which are connected in sequence; the upper portion of the post-treatment cavity is provided with a feed inlet communicated with the discharge outlet through a pipeline, the bottom of the post-treatment cavity is provided with a discharge outlet and a liquid discharge outlet, the bottom of the post-treatment cavity is provided with a filtering mechanism, and the outside of the post-treatment cavity is provided with a II-number jacket. The invention realizes solid-liquid separation through the pipeline and the device, can realize solid-liquid separation without transferring the feed liquid when the feed liquid is post-treated, can directly dry the separated solid, is hermetically operated in the whole process, does not need to transfer the feed liquid, and has simple operation and high working efficiency.

Description

Experimental device for anhydrous zinc acetate preparation and aftertreatment
Technical Field
The invention belongs to the technical field of chemical equipment, and particularly relates to an experimental device for preparation and post-treatment of anhydrous zinc acetate.
Background
The depleted zinc acetate dihydrate is an important nuclear power additive for adding zinc by nuclear power, the upstream product of the depleted zinc acetate is depleted anhydrous zinc acetate, the depleted anhydrous zinc acetate is prepared by taking depleted zinc oxide as a raw material, the preparation reaction is a solid-liquid reaction completed in multiple steps, after the reaction is finished, the solid product is required to be filtered, and after the filtration, the drying is carried out to obtain the anhydrous zinc acetate product, and the whole test operation process is relatively complex.
Disclosure of Invention
The invention is provided for overcoming the defects in the prior art, and aims to provide an experimental device for preparing and post-treating anhydrous zinc acetate.
The invention is realized by the following technical scheme:
an experimental device for preparing and post-treating anhydrous zinc acetate comprises a reaction device and a post-treatment device, wherein the reaction device and the post-treatment device are both provided with a stirring mechanism;
the reaction device comprises a reaction cavity, a liquid inlet and a solid charging port are arranged at the upper part of the reaction cavity, a discharge port is arranged at the bottom of the reaction cavity, and a No. I jacket is arranged outside the reaction cavity;
the post-treatment device comprises a post-treatment cavity, a condensing device, a heat exchanger and a collector which are connected in sequence; the upper portion of the post-treatment cavity is provided with a feed inlet communicated with the discharge outlet through a pipeline, the bottom of the post-treatment cavity is provided with a discharge outlet and a liquid discharge outlet, the bottom of the post-treatment cavity is provided with a filtering mechanism, and the outside of the post-treatment cavity is provided with a II-number jacket.
In the technical scheme, the bottom of the reaction cavity is also provided with a clean discharge port, and the clean discharge port is arranged at the lowest point of the bottom of the reaction cavity.
In the technical scheme, the No. I jacket is respectively provided with a heat conduction oil inlet and a heat conduction oil outlet.
In the above technical solution, the stirring form of the stirring paddle of the stirring mechanism of the reaction apparatus is a pitched blade paddle type.
In the above technical scheme, a valve is arranged on the pipeline.
In the technical scheme, the filtering mechanism comprises a filtering partition plate and side baffle plates arranged on two sides of the filtering partition plate, one end of each side baffle plate is connected with the filtering partition plate, and the other end of each side baffle plate is fixed on the inner wall of the aftertreatment cavity.
In the technical scheme, the longitudinal section of the filtering partition plate is V-shaped.
In the technical scheme, the No. II jacket is respectively provided with a heat exchange circulating inlet and a heat exchange circulating outlet.
In the technical scheme, the post-treatment cavity is internally provided with a scraper component, and the scraper component comprises at least one stirring scraper connected with a stirring shaft and at least one scraper arranged on the side part and/or the bottom part of the stirring scraper.
In the technical scheme, the stirring scraper is of a middle-included type and is arranged at intervals with the stirring blades.
In the technical scheme, the post-treatment cavity is provided with an evacuation port connected with the vacuum device, and the horizontal position of the evacuation port is arranged below the side baffle and above the filtering partition plate.
In the technical scheme, the discharging opening is provided with the discharging valve, and the discharging valve is a top plug type discharging valve.
In the technical scheme, the bottom of the post-treatment cavity is V-shaped or U-shaped.
In the technical scheme, the condensing device is connected with the top of the aftertreatment cavity.
In the technical scheme, the top of the collector is provided with a vacuum port, the bottom of the collector is provided with a liquid outlet, and the inside of the collector is provided with a liquid level meter.
The invention has the beneficial effects that:
the invention provides an experimental device for preparing and post-treating anhydrous zinc acetate, which realizes solid-liquid separation through a pipeline and a device, can realize solid-liquid separation without transferring feed liquid when the feed liquid is post-treated, can directly dry the separated solid, is sealed in the whole process, does not need to transfer the feed liquid, and has simple operation and high working efficiency.
Drawings
FIG. 1 is a schematic structural diagram of an experimental apparatus for preparing and post-treating anhydrous zinc acetate.
Wherein:
100 reaction device
101 liquid inlet of reaction chamber 102
103 solid feeding port 104 discharge port
105 put clean mouthful 106I jacket
107 heat transfer oil inlet and 108 heat transfer oil outlet
109 stirring paddle
200 post-processing device
201 post-treatment chamber 202 feed inlet
203 drain port 204 drain port
205 evacuation port 206 discharge valve
207 filtering baffle 208 side baffle
No. 209 II jacket 210 heat exchange circulation inlet
211 heat exchange circulation outlet 212 stirring shaft
213 stirring blade 214 stirring scraper
215 scraper 216 condensation device
217 heat exchanger 218 collector
219 vacuum port
300 line 301 valves.
For a person skilled in the art, other relevant figures can be obtained from the above figures without inventive effort.
Detailed Description
In order to make the technical scheme of the present invention better understood by those skilled in the art, the technical scheme of the experimental device for preparing and post-treating anhydrous zinc acetate of the present invention is further described below by the specific embodiments with reference to the drawings of the specification.
As shown in fig. 1, an experimental apparatus for preparing and post-treating anhydrous zinc acetate comprises a reaction apparatus 100 and a post-treatment apparatus 200 both having a stirring mechanism;
the reaction device comprises a reaction cavity 101, a liquid inlet 102 and a solid charging port 103 are arranged at the upper part of the reaction cavity 101, a discharge port 104 and a purge port 105 are arranged at the bottom of the reaction cavity, a No. I jacket 106 is arranged outside the reaction cavity 1, a heat conduction oil inlet 107 and a heat conduction oil outlet 108 are respectively arranged on the No. I jacket 106, and a stirring form of a stirring paddle 109 of the reaction device 100 is an inclined blade paddle type.
The post-treatment device 200 comprises a post-treatment cavity 201, a condensing device 216, a heat exchanger 217 and a collector 218 which are connected in sequence;
the upper part of the post-processing cavity 201 is provided with a feed inlet 202 communicated with a discharge outlet 104 through a pipeline 300, the bottom of the post-processing cavity is provided with a discharge outlet 203 and a liquid discharge outlet 204, and the pipeline 300 is provided with a valve 301; the bottom sets up filtering mechanism in the aftertreatment chamber 201, filtering mechanism is including filtering baffle 207 and setting up in the side shield 208 of its both sides, and side shield one end is connected with filtering baffle 207, and the other end is fixed in aftertreatment chamber 201 inner wall, it is the V type to filter baffle 207 longitudinal section, and aftertreatment chamber 201 outside sets up No. II and presss from both sides cover 209, sets up heat transfer circulation entry 210 and heat transfer circulation export 211 on No. II cover 209 respectively.
In this embodiment, in order to minimize the loss of solid wall build-up, a scraper assembly is disposed within the aftertreatment chamber 201, the scraper assembly comprising at least one bracketed stirring blade 214 connected to the stirring shaft 212, and at least one scraper 215 disposed at the side and/or bottom of the stirring blade 214. The stirring scraper 214 and the stirring blade 213 are arranged at intervals to ensure the normal rotation stirring of the stirring blade.
The condensing device 216 is connected with the top of the post-treatment cavity 201, the top of the collector 218 is provided with a vacuum port 219, the bottom of the collector 218 is provided with a liquid outlet, so that liquid can be transferred in time, and meanwhile, a liquid level meter is arranged inside the collector 218 for observing the liquid level height of the liquid in the collector 218.
In this embodiment, in order to further improve the filtering efficiency of the filtering mechanism, the post-processing chamber 201 is provided with an evacuation port 205 connected to the vacuum device, and the horizontal position of the evacuation port 205 is disposed below the side baffle 208 and above the filtering partition 207, so as to ensure that the filtering efficiency is improved and prevent the liquid from being sucked back during filtering.
In this embodiment, set up ejection of compact valve 206 on the drain hole 203, and ejection of compact valve 206 is the plug formula baiting valve, and the solid drops when effectively preventing to filter.
In this embodiment, in order to facilitate the discharge of the material, the bottom of the post-processing chamber 201 is V-shaped or U-shaped.
In the embodiment, in order to further improve the use convenience of the reaction device, the upper parts of the reaction chamber 101 and the post-treatment chamber 201 are respectively provided with a detachable upper seal head, and the upper seal head of the reaction chamber 101 is connected with an electric mechanism through a connecting piece, so that the mechanical opening of the upper seal head is realized, and the labor intensity is reduced; the reaction chamber 101 is convenient to be aligned due to the design of the detachable upper seal head. Thorough cleaning of the interior of the aftertreatment chamber 201, and maintenance or replacement of the paddles.
In this embodiment, reaction unit and aftertreatment device all set up on the dress frame, improve the compactedness of whole device design and to the rational utilization in place.
The working principle of the invention is as follows:
the reaction device part: liquid reagent in the reaction is added through the liquid inlet, solid reactant is added through the solid charging port, and the temperature control in the reaction process is realized through the heat conducting oil inlet and outlet of the No. I jacket. After the reaction in the reaction device is finished, materials containing anhydrous zinc acetate solids and the solvent are transferred into a post-treatment device together through a pipeline. The material transfer can be realized through positive pressure or negative pressure, the positive pressure is introduced into gas through a liquid upper gas inlet on the reaction device, and the negative pressure is realized through a liquid upper pumping pipeline on the post-treatment device.
A post-processing apparatus section: the filtering mechanism divides the post-treatment cavity into a solid part and a liquid part through a filtering clapboard capable of realizing solid-liquid separation and side baffles positioned at two sides of the clapboard. After the materials enter the post-treatment cavity, the materials are connected with a vacuum device through a vacuumizing opening, the materials are filtered in the post-treatment cavity through a filtering mechanism, and liquid is transferred in time through a liquid discharging opening. And after the filtration is finished, closing the valve of the evacuation port, and keeping solid materials in the solid part of the post-treatment cavity. The horizontal position of the evacuation port is arranged at the lower part of the side baffle and the upper part of the filtering baffle plate, so that the liquid is prevented from being sucked backwards during filtering.
The solid after filtering is stirred the stoving in the aftertreatment intracavity, and the rotatory stirring scraper blade that drives of (mixing) shaft is rotatory, and then realizes the scraper to the clearance on aftertreatment chamber wall, prevents the loss of material wall built-up. The heating medium is introduced into the jacket II to provide a heat source, the temperature of the heating medium is controlled by the heating device, the solid in the post-treatment cavity is dried, cold water is introduced into the jackets of the condenser and the heat exchanger, the condensing device takes away the solvent subjected to heating evaporation, and the solvent is collected by the collector to realize the collection of the evaporated solvent. The liquid level gauge in the collector realizes observing the liquid level height of liquid in the collector, and the collector can be provided with a liquid discharge port to transfer the liquid in time. The solid material that the drying was accomplished discharges through the drain hole of aftertreatment chamber bottom, simultaneously owing to set up the plug formula baiting valve, the solid dropped when can effectively preventing to filter.
According to the invention, the reaction device is connected with the post-treatment device through a pipeline, so that the closed conveying of fluid materials is realized, the filtering and drying of the materials are realized after the fluid enters the post-treatment device, and the dried anhydrous zinc acetate material can be directly obtained; the invention is suitable for solid-liquid reaction with various solid generation, finishes post-reaction treatment, does not need to discharge liquid for filtration and drying by a dryer, and has convenient operation; collecting vapor generated when the solid is dried by a collector, and volatilizing no solvent into air; the dried solid is discharged through the discharge hole, and the scraper can effectively avoid the loss of solid wall hanging and influence on the yield.
It should be noted that the embodiments and features of the embodiments may be combined with each other without conflict.
In the description of the present invention, it is to be understood that the terms "center", "longitudinal", "lateral", "up", "down", "front", "back", "left", "right", "vertical", "horizontal", "top", "bottom", "inner", "outer", and the like, indicate orientations or positional relationships based on those shown in the drawings, and are used only for convenience in describing the present invention and for simplicity in description, 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. Furthermore, the terms "first", "second", etc. are used for descriptive purposes only and are not to be construed as indicating or implying relative importance or implicitly indicating the number of technical features indicated. Thus, a feature defined as "first," "second," etc. may explicitly or implicitly include one or more of that feature. In the description of the present invention, "a plurality" means two or more unless otherwise specified.
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; they may be connected directly or indirectly through intervening media, or they may be interconnected between two elements. The specific meaning of the above terms in the present invention can be understood by those of ordinary skill in the art through specific situations.
The applicant declares that the above description is only a specific embodiment of the present invention, but the scope of the present invention is not limited thereto, and it should be understood by those skilled in the art that any changes or substitutions that can be easily conceived by those skilled in the art within the technical scope of the present invention are within the scope and disclosure of the present invention.

Claims (15)

1. The utility model provides an experimental apparatus of anhydrous zinc acetate preparation and aftertreatment which characterized in that: comprises a reaction device (100) and a post-treatment device (200) both provided with a stirring mechanism;
the reaction device comprises a reaction cavity (101), a liquid inlet (102) and a solid feeding port (103) are arranged at the upper part of the reaction cavity, a discharge port (104) is arranged at the bottom of the reaction cavity, and a No. I jacket (106) is arranged outside the reaction cavity (1);
the post-treatment device (200) comprises a post-treatment cavity (201), a condensing device (216), a heat exchanger (217) and a collector (218) which are connected in sequence; the upper portion of the post-processing cavity (201) is provided with a feed inlet (202) communicated with a discharge port (104) through a pipeline (300), the bottom of the post-processing cavity is provided with a discharge port (203) and a liquid discharge port (204), the bottom of the post-processing cavity (201) is provided with a filtering mechanism, and the outside of the post-processing cavity is provided with a No. II jacket (209).
2. The experimental facility for preparing and post-treating anhydrous zinc acetate according to claim 1, characterized in that: the bottom of the reaction cavity (101) is also provided with a clean discharge port (105), and the clean discharge port (105) is arranged at the lowest point position of the bottom of the reaction cavity (101).
3. The experimental facility for preparing and post-treating anhydrous zinc acetate according to claim 1, characterized in that: and the No. I jacket (106) is respectively provided with a heat conduction oil inlet (107) and a heat conduction oil outlet (108).
4. The experimental facility for preparing and post-treating anhydrous zinc acetate according to claim 1, characterized in that: the stirring form of the stirring paddle (109) of the stirring mechanism of the reaction device (100) is an inclined paddle type.
5. The experimental facility for preparing and post-treating anhydrous zinc acetate according to claim 1, characterized in that: a valve (301) is arranged on the pipeline (300).
6. The experimental facility for preparing and post-treating anhydrous zinc acetate according to claim 1, characterized in that: the filtering mechanism comprises a filtering partition plate (207) and side baffle plates (208) arranged on two sides of the filtering partition plate, one end of each side baffle plate is connected with the filtering partition plate (207), and the other end of each side baffle plate is fixed on the inner wall of the aftertreatment cavity (201).
7. The experimental facility for preparing and post-treating anhydrous zinc acetate according to claim 6, characterized in that: the longitudinal section of the filtering clapboard (207) is V-shaped.
8. The experimental facility for preparing and post-treating anhydrous zinc acetate according to claim 1, characterized in that: and the No. II jacket (209) is respectively provided with a heat exchange circulating inlet (210) and a heat exchange circulating outlet (211).
9. The experimental facility for preparing and post-treating anhydrous zinc acetate according to claim 1, characterized in that: a scraper component is arranged in the post-processing cavity (201), and comprises at least one stirring scraper (214) connected with the stirring shaft (212) and at least one scraper (215) arranged on the side and/or the bottom of the stirring scraper (214).
10. The experimental facility for preparing and post-treating anhydrous zinc acetate according to claim 9, characterized in that: the stirring scraper (214) is of a middle-included type and is arranged at intervals with the stirring blade (213).
11. The experimental facility for preparing and post-treating anhydrous zinc acetate according to claim 1, characterized in that: the post-treatment cavity (201) is provided with an evacuation port (205) connected with a vacuum device, and the horizontal position of the evacuation port (205) is arranged below the side baffle (208) and above the filtering partition plate (207).
12. The experimental facility for preparing and post-treating anhydrous zinc acetate according to claim 1, characterized in that: discharge gate (203) is last to set up discharge valve (206), and discharge valve (206) are top plug formula discharge valve.
13. The experimental facility for preparing and post-treating anhydrous zinc acetate according to claim 1, characterized in that: the bottom of the post-processing cavity (201) is V-shaped or U-shaped.
14. The experimental facility for preparing and post-treating anhydrous zinc acetate according to claim 1, characterized in that: the condensing device (216) is connected with the top of the post-processing cavity (201).
15. The experimental facility for preparing and post-treating anhydrous zinc acetate according to claim 1, characterized in that: the top of the collector (218) is provided with a vacuum port (219), the bottom of the collector is provided with a liquid outlet, and a liquid level meter is arranged in the collector (218).
CN202110959047.0A 2021-08-20 2021-08-20 Experimental device for anhydrous zinc acetate preparation and aftertreatment Pending CN113559811A (en)

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CN213132180U (en) * 2019-11-19 2021-05-07 哈尔滨圣泰生物制药有限公司 Biochemical filtration system that draws
CN213698951U (en) * 2020-06-23 2021-07-16 上海麦吉丽日用品有限公司 Liquid cosmetics impurity filter equipment
TWM615205U (en) * 2021-04-16 2021-08-01 增縉精機股份有限公司 Washing/filtering/drying machine
CN113230714A (en) * 2021-05-14 2021-08-10 开平市优洋化工有限公司 Paint filter
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CN1221727A (en) * 1997-12-30 1999-07-07 徐同香 Prepn. tech. of zinc acetate
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CN203829707U (en) * 2014-03-14 2014-09-17 山东瑞天化工有限公司 Resin solution mixed solvent separating device
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