CN115317952B - Titanium dioxide separation production auxiliary device - Google Patents

Titanium dioxide separation production auxiliary device Download PDF

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Publication number
CN115317952B
CN115317952B CN202211238420.4A CN202211238420A CN115317952B CN 115317952 B CN115317952 B CN 115317952B CN 202211238420 A CN202211238420 A CN 202211238420A CN 115317952 B CN115317952 B CN 115317952B
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China
Prior art keywords
sleeve
kettle body
driving piece
pipe
piece
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CN202211238420.4A
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Chinese (zh)
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CN115317952A (en
Inventor
周兰英
岳南平
谢求清
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Jiangsu Hushen Titanium White Technology Co ltd
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Jiangsu Hushen Titanium White Technology Co ltd
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D9/00Crystallisation
    • B01D9/0018Evaporation of components of the mixture to be separated
    • B01D9/0031Evaporation of components of the mixture to be separated by heating
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D33/00Filters with filtering elements which move during the filtering operation
    • B01D33/58Handling the filter cake in the filter for purposes other than for regenerating the filter cake remaining on the filtering element
    • B01D33/60Handling the filter cake in the filter for purposes other than for regenerating the filter cake remaining on the filtering element for washing
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D9/00Crystallisation
    • B01D9/02Crystallisation from solutions
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/0053Details of the reactor
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/18Stationary reactors having moving elements inside
    • B08B1/165
    • B08B1/20
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B08CLEANING
    • B08BCLEANING IN GENERAL; PREVENTION OF FOULING IN GENERAL
    • B08B9/00Cleaning hollow articles by methods or apparatus specially adapted thereto 
    • B08B9/08Cleaning containers, e.g. tanks
    • B08B9/0804Cleaning containers having tubular shape, e.g. casks, barrels, drums
    • B08B9/0808Cleaning containers having tubular shape, e.g. casks, barrels, drums by methods involving the use of tools, e.g. by brushes, scrapers
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D9/00Crystallisation
    • B01D2009/0086Processes or apparatus therefor
    • YGENERAL 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
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P10/00Technologies related to metal processing
    • Y02P10/20Recycling

Abstract

The invention relates to the technical field of titanium dioxide production, in particular to an auxiliary device for titanium dioxide separation production; comprises a kettle body for hydrolysis reaction; the rotary driving piece is used as a rotary driving source in the titanium liquid mass transfer process and is arranged at the upper end of the kettle body; the upper end of the telescopic driving piece is connected with the lower end of the rotary driving piece; the scraping plate is connected with the lower end of the telescopic driving piece; the heating rods uniformly arranged in the kettle body penetrate through the scraping plate and are in sliding connection with the scraping plate; the scraper can scrape the crystallization on the inner wall surface of the heating rod and the kettle body; the method solves the problems of low hydrolysis efficiency in the whole process of titanium liquid hydrolysis and low content of titanium dioxide and separation efficiency caused by low content of the metatitanic acid crystals obtained after the hydrolysis.

Description

Titanium dioxide separation production auxiliary device
Technical Field
The invention relates to the technical field of titanium dioxide production, in particular to an auxiliary device for titanium dioxide separation production.
Background
The production method of the titanium dioxide comprises the relatively common process steps of producing the titanium dioxide by a sulfuric acid method, wherein the process steps of producing the titanium dioxide by the sulfuric acid method comprise: (1) acidolysis, namely acidolysis of a titanium dioxide raw material by sulfuric acid; (2) settling, and separating soluble titanyl sulfate from solid impurities; (3) hydrolyzing, namely mixing soluble titanyl sulfate with water to form a titanium solution, and hydrolyzing the titanyl sulfate to form insoluble hydrolysate or metatitanic acid; (4) washing, namely washing the obtained metatitanic acid to remove a large amount of impurities such as free sulfuric acid, ferrous sulfate and the like attached to the surface of the metatitanic acid so as to obtain pure metatitanic acid; (5) calcining the pure meta-titanic acid to remove water and generate dry pure titanium dioxide; (6) grinding; (7) coating, namely coating rutile type titanium dioxide; in the hydrolysis process of the titanium liquid formed by mixing soluble titanyl sulfate and water, fine crystal nucleus is separated out firstly, in the continuous process of hydrolysis, metatitanic acid solid precipitation occurs on the surface of the crystal nucleus, the crystal nucleus is promoted to grow up and finally precipitate, and then the crystal nucleus continues to grow up and aggregate, and the crystal nucleus precipitates and precipitates from the solution after aggregation to a certain degree.
The patent application number 2021222385168 discloses a Chinese patent publication, which comprises a sealing cover and a motor, wherein a motor is arranged above the middle part of the sealing cover, a feeding port is arranged above the left end of the sealing cover, an observation port is arranged above the right end of the sealing cover, a machine body is arranged at the lower end of the sealing cover, a discharging port is arranged in the middle of the lower end of the machine body, a supporting leg is arranged below the right end of the machine body, a connecting pipe is arranged at the left side of the upper end of the machine body, a stop valve is arranged in the middle of the right end of the connecting pipe, a pump is arranged at the lower end of the connecting pipe, a water storage barrel is arranged at the lower end of the pump, a switch is arranged in the middle of the front end of the water storage barrel, the machine body comprises a reaction barrel, a stirring rod, a heat insulation layer and stirring blades, the stirring rod is arranged inside the reaction barrel, and the stirring blades are arranged at the lower end of the stirring rod;
according to the scheme, although the hydrolysis of the titanium liquid can be realized, the applicant researches show that the metatitanic acid obtained by filtering the stirred titanium liquid after the long-time full hydrolysis is completed is lower than the metatitanic acid obtained by filtering the titanium liquid which is not stirred under the same condition, and the applicant researches further find that in the hydrolysis stirring process of the titanium liquid, stirring only plays a certain role in promoting the mass transfer process in the hydrolysis process of the titanium liquid, and in the subsequent real hydrolysis chemical reaction process, stirring does not have a significant influence on the hydrolysis reaction speed, but can reduce the particle size of the metatitanic acid crystals generated by hydrolysis, so that part of the metatitanic acid crystals have too small particle size, and in the subsequent solid-liquid separation process, the too small metatitanic acid crystals are lost along with waste liquid, so that the content of the metatitanic acid obtained by hydrolysis is too small, and the content of the titanium dioxide separated later is low.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides an auxiliary device for titanium dioxide separation production, which improves mass transfer and uniform heating efficiency by stirring titanium liquid only in the mass transfer process in the titanium liquid through the mutual cooperation of a rotary driving piece, a telescopic driving piece, a heating rod and a scraping plate, avoids the problems that the acquisition rate of the meta-titanic acid is low and the separation efficiency is low due to the fact that the solid-liquid separation is caused by stirring and crushing of the meta-titanic acid crystal granularity in the hydrolysis chemical reaction process, the attachment area of the meta-titanic acid crystal is increased by adding a plurality of heating rods, the telescopic driving piece drives the heating rod and the ascending part distance of the meta-titanic acid crystal on the heating rod to reduce the concentration of the meta-titanic acid crystal in the titanium liquid, and the forward reaction is accelerated, and after the reaction is finished, the telescopic driving piece drives the scraping plate to downwards scrape the crystals attached on the heating rod and the inner wall of a kettle body, so that the problems of low hydrolysis efficiency and low acquisition rate and low separation efficiency of the follow-up titanium dioxide are comprehensively solved;
in order to achieve the above purpose, the present invention provides the following technical solutions: a titanium dioxide separation production auxiliary device, comprising:
a kettle body for hydrolysis reaction;
the rotary driving piece is used as a rotary driving source in the titanium liquid mass transfer process and is arranged at the upper end of the kettle body;
the upper end of the telescopic driving piece is connected with the lower end of the rotary driving piece;
the scraping plate is connected with the lower end of the telescopic driving piece;
the heating rods uniformly arranged in the kettle body penetrate through the scraping plate and are in sliding connection with the scraping plate; and the scraper can scrape the crystallization on the inner wall surface of the heating rod and the kettle body.
As an improvement, the kettle body is also provided with a first feeding pipe and an exhaust pipe.
As an improvement, the kettle body comprises a kettle bottom and a kettle cover, and spiral holes for introducing gas or liquid into the kettle body are formed in the periphery of the kettle bottom.
As an improvement, the upper layer of the scraper is made of glass, and fine glass particles are generated by friction between the glass and the heating rod in the downward moving process of the scraper, so that the glass particles serve as crystal nuclei to promote the improvement of crystallization rate;
as an improvement, the heating rod includes:
the heating part comprises a first section, a second section and a third section which are sequentially connected and can be independently controlled to be heated;
and the upper end of the installation part is larger than the lower end of the installation part, and the upper end of the installation part is positioned at the upper end of the scraping plate.
As an improvement, a second feeding pipe communicated with all the spiral holes is arranged on the kettle body, and the upper end of the second feeding pipe is also communicated with an air blowing component; the air blowing component is connected with an air source and a water source, and a heater is arranged on a flow path of the water source.
As an improvement, the air blowing component is a water-air dual-purpose pump, an air valve is arranged at the connecting end of the water-air dual-purpose pump and an air source, and a water valve is arranged at the connecting end of the water-air dual-purpose pump and a water source;
as an improvement, the kettle bottom is also provided with a discharge hole; the discharging hole is internally provided with a cylindrical filter screen assembly capable of sliding relative to the discharging hole, and the upper part of the cylindrical filter screen assembly is provided with a sealing cover.
As an improvement, the cylindrical screen assembly includes:
one end of the rotating shaft is vertically and rotatably connected to the sealing cover;
the rotating plates are connected with the rotating shaft and uniformly encircle a plurality of rotating plates into a circle;
the first sleeve is sleeved on the outer side of the rotating plate which is enclosed into a circle, and the upper end of the first sleeve is communicated with the discharge hole;
the upper end of the second sleeve is in sliding communication with the inner wall of the first sleeve, and the inner diameter of the second sleeve is smaller than the inner diameter of a minimum circle formed by a plurality of rotating shafts; the lower end of the rotating shaft extends into the second sleeve and is rotationally connected with the second sleeve;
the discharging pipe is arranged at the lower end of the second sleeve and communicated with the second sleeve;
the plate driving assembly is used for simultaneously driving all the rotating shafts to rotate so as to realize synchronous adjustment of gaps between all the adjacent rotating plates, and is arranged at the lower end of the second sleeve;
the lifting piece is used for driving the second sleeve to lift relative to the first sleeve, and is connected with the lower end of the second sleeve.
As an improvement, the gap between two adjacent shafts is larger than the maximum width of the largest crystal of the crystals.
As an improvement, the plate driving assembly includes:
the first transmission piece is respectively connected with each rotating shaft;
the second transmission parts are in transmission connection with all the first transmission parts;
the first driving piece is used for driving the first driving piece driven by the second transmission piece to be connected with the second sleeve;
as an improvement, the first transmission part is a first gear, and the second transmission part is a gear ring meshed with the first transmission part; the first driving piece is a first servo motor with a gear arranged at the end part and in transmission engagement with the second transmission piece;
as an improvement, the first driving part is a chain wheel, the second driving part is a chain meshed with the first driving part, the chain driving path is limited to be meshed with all the first driving parts, and the first driving part is a first servo motor with a gear at the end part and meshed with the second driving part.
As an improvement, the upper end of the lifting piece is provided with a rotary driving piece; a transmission assembly which is in transmission connection with the rotation driving piece and the discharging pipe is arranged between the rotation driving piece and the discharging pipe; and the lifting piece is rotationally connected with the discharging pipe.
As an improvement, the bottom surface of the kettle body is a concave cambered surface, the bottom surface of the scraping plate is matched with the bottom surface of the kettle body, and a scraping knife is arranged on the bottom surface of the scraping plate.
As an improvement, the outer part of the discharging pipe is rotationally connected with an air slip ring communicated with the inside of the discharging pipe; the side of the cauldron body is provided with circulation subassembly, circulation subassembly includes:
the first waste water tank is used for storing waste titanium liquid, is communicated with the inside of the gas slip ring through a first pipe, and a first valve and a first pump are arranged on the first pipe;
the second wastewater tank is used for storing washing liquid, is communicated with the inside of the gas slip ring through a second pipe, and a second valve is arranged on the second pipe;
the storage tank, the storage tank can be dismantled with the lower extreme of discharging pipe and the junction of storage tank and discharging pipe is provided with the third valve.
As improvement, the filtering gap A between two adjacent rotating plates is larger than the filtering gap B between two adjacent rotating plates when the metatitanic acid crystals are washed when the waste titanium liquid is discharged; the filtering gap C between two adjacent rotating plates discharged by the recrystallized titanium liquid flowing back into the kettle body of the first wastewater tank is far smaller than the filtering gap A.
The invention has the beneficial effects that:
1. according to the invention, the scraper is driven by the rotary driving piece and the telescopic driving piece to move downwards and drive the heating rod to rotate so as to heat and boil titanium liquid in the kettle body, so that soluble titanyl sulfate is fully dissolved in water to finish the mass transfer process, stirring is stopped, the difficulty of increasing subsequent solid-liquid separation caused by crushing meta-titanic acid generated by subsequent hydrolysis reaction is avoided, the area of crystal adhesion precipitation is increased by a plurality of heating rods, the efficiency of crystal precipitation is improved, the telescopic driving piece drives the heating rod to move upwards for a part of distance so that part of crystals adhered to the heating rod are separated from titanium liquid, the content of meta-titanic acid in the titanium liquid is reduced, the forward direction of reaction is accelerated, after titanium liquid in the kettle body is crystallized, the telescopic driving piece drives the heating rod to move downwards, the lower end of the heating rod is abutted to the bottom of the kettle and the scraper is continuously moved downwards, the crystals adhered to the heating rod are scraped by the scraping plate, and the crystals adhered to the inner wall of the kettle body are scraped, and the loss of the crystals collected later is reduced; through the mutual matching work of the rotary driving piece, the telescopic driving piece, the heating rod and the scraping plate, the hydrolysis efficiency of the titanium liquid and the crystallization rate of the meta-titanic acid are improved in various forms, and the separation efficiency and the yield of the subsequent titanium dioxide are further improved;
2. according to the invention, inert gas or air is introduced into the kettle body through the spiral holes, so that the fluidity of titanium liquid in the kettle body is promoted, the temperature uniformity of the titanium liquid in the kettle body and the dispersity of the metatitanic acid generated by reaction are improved, the difficulty of the subsequent crushing process is increased due to the fact that excessive metatitanic acid is coagulated into larger-particle metatitanic acid, meanwhile, the problem that the particle size of crystal particles generated by hydrolysis is too small to increase the difficulty of subsequent solid-liquid separation due to the fact that the crystal particles generated by stirring the titanium liquid directly through the stirring component is avoided, the stability of the particle size of the separated metatitanic acid crystal particles is not too large or too small, and the stability of the particle size of titanium dioxide separated by subsequent calcination is improved;
3. according to the invention, the cylindrical filter screen assembly is arranged at the liquid outlet of the kettle bottom, so that after the hydrolysis reaction of the titanium liquid is finished, the kettle body is spirally filled with ionized water or clean water through the spiral hole, and then the cylindrical filter screen assembly is controlled to move upwards, so that the metatitanic acid in the kettle body can be washed and decontaminated, the two-in-one use of the hydrolysis of the titanium liquid and the washing and decontaminating of the metatitanic acid crystal is realized, and the practicability of the auxiliary device is improved;
4. according to the invention, the edges of the upper end and the lower end of the counter-rotating plates of the first sleeve and the second sleeve are plugged, so that the washed wastewater can only flow down from a gap between the side surfaces of two adjacent rotating plates and flow out through the discharging pipe; all rotating plates are driven to synchronously rotate through the plate driving assembly so as to change gaps between adjacent rotating plates, so that the screening and discharging of crystals with different particle sizes and the filtering gaps required by actual filtering can be realized, and the flushing and filtering of the metatitanic acid crystals in the kettle body can be realized; after the crystal is washed, the rotating plates are driven to rotate through the plate driving assembly, so that the gap between the adjacent rotating plates is increased, the crystals are discharged conveniently, and the auxiliary device is simple in structure and high in practicability;
5. according to the invention, the filtering gap A between two adjacent rotating plates is larger than the filtering gap B between two adjacent rotating plates when the meta-titanic acid crystal is washed when the waste titanium liquid is discharged; the filtering clearance C between two adjacent rotating plates discharged by the titanium liquid which flows back into the kettle body again from the first wastewater tank is far smaller than the filtering clearance A, so that the washing efficiency of the metatitanic acid and the acquisition amount of the metatitanic acid crystal are improved;
in conclusion, the invention has the advantages of simple structure, strong practicability, more separated metatitanic acid crystal grains, uniform particles and the like.
Drawings
FIG. 1 is a schematic diagram of the overall structure of the present invention;
FIG. 2 is a schematic diagram showing the overall structural connection of the kettle body, the cylindrical filter screen assembly and the circulating assembly according to the invention;
FIG. 3 is a schematic diagram showing the connection of the kettle body and the rotary driving member and the second feeding pipe;
FIG. 4 is a schematic diagram of the internal structure of the kettle body of the present invention;
FIG. 5 is a schematic diagram of the structure of the partial tank bottom, the scraping plate and the heating rod of the invention;
FIG. 6 is a structural view of the cylindrical screen assembly of the present invention extending out of the bottom of the tank;
FIG. 7 is a schematic view of the overall structure of a cylindrical screen assembly of the present invention;
FIG. 8 is a schematic view of the internal structure of a cylindrical screen assembly of the present invention;
FIG. 9 is a schematic illustration of a partial structural attachment of a cylindrical screen assembly according to the present invention;
FIG. 10 is an enlarged view at A of FIG. 9;
FIG. 11 is a schematic view of a rotary driving member according to the present invention;
reference numerals: 1. a kettle body; 11. a kettle bottom; 111. a spiral hole; 112. a discharge hole; 12. a kettle cover; 13. a first feed tube; 14. an exhaust pipe; 15. a high temperature resistant battery; 16. a first frame; 17. a second frame; 2. a rotary driving member; 21. a telescopic driving member; 22. a heating rod; 221. a heating section; 222. a mounting part; 23. a scraper; 231. a scraper; 3. a second feed tube; 31. a gas blowing assembly; 32. a gas source; 33. a water source; 34. a heater; 4. a cylindrical screen assembly; 41. sealing cover; 42. a rotating shaft; 43. a rotating plate; 44. a first sleeve; 45. a second sleeve; 46. a discharge pipe; 47. a board driving assembly; 471. a first transmission member; 472. a second transmission member; 473. a first driving member; 48. a lifting member; 49. a rotary driving member; 491. a transmission assembly; 5. a circulation assembly; 51. a first wastewater tank; 511. a first tube; 512. a first valve; 513. a first pump; 52. a second wastewater tank; 521. a second tube; 522. a second valve; 53. a storage tank; 531. a third valve; 54. an air slip ring.
Detailed Description
The following description of the embodiments of the present invention will be made clearly and completely with reference to the accompanying drawings, in which it is apparent that the embodiments described are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
In the description of the present invention, it should be understood that the terms "center", "longitudinal", "lateral", "length", "width", "thickness", "upper", "lower", "front", "rear", "left", "right", "vertical", "horizontal", "top", "bottom", "inner", "outer", "clockwise", "counterclockwise", etc. indicate orientations or positional relationships based on the orientations or positional relationships shown in the drawings are merely for convenience in describing the present invention and simplifying the description, and do not indicate or imply that the apparatus or elements referred to must have a specific orientation, be configured and operated in a specific orientation, and thus should not be construed as limiting the present invention.
Furthermore, the terms "first," "second," and the like, are used for descriptive purposes only and are not to be construed as indicating or implying a relative importance or implicitly indicating the number of technical features indicated. Thus, a feature defining "a first" or "a second" may explicitly or implicitly include one or more such feature. In the description of the present invention, the meaning of "a plurality" is two or more, unless explicitly defined otherwise.
Example 1
As shown in FIGS. 3-6, the embodiment provides an auxiliary device for separating and producing titanium dioxide, comprising
A kettle body 1 for hydrolysis reaction;
the rotary driving piece 2 is only used as a rotary driving source in the titanium liquid mass transfer process, and the rotary driving piece 2 which is not used as a rotary driving source in the hydrolysis chemical reaction process is arranged at the upper end of the kettle body 1;
a telescopic driving member 21;
a plurality of heating rods 22;
the upper end of the telescopic driving piece 21 is connected with the lower end of the rotary driving piece 2, and the lower end of the telescopic driving piece 21 is connected with the scraper 23; the heating rods 22 uniformly arranged in the kettle body 1 pass through the scraping plate 23 and are in sliding connection with the scraping plate 23; and the scraping plate 23 can scrape off the crystallization on the inner wall surfaces of the heating rod 22 and the kettle body 1.
Further, the kettle body 1 is further provided with a first feeding pipe 13 and an exhaust pipe 14.
Further, the telescopic driving piece 21 is a telescopic cylinder or a telescopic hydraulic cylinder or an electric telescopic rod;
further, the rotary driving piece 2 is a servo motor;
it should be further noted that, water or ionized water is put into the kettle body 1, the telescopic driving piece 21 drives the scraping plate 23 to move downwards for a certain distance, so that the heating rod 22 stretches into the water in the kettle body 1 to heat the water to boil, and the rotary driving piece 2 drives the telescopic driving piece 21 to rotate and drives the heating rod 22 to rotate, so that the heating speed can be increased; the soluble titanyl sulfate prepared by the sulfuric acid method is then put into the kettle body 1 through the first feeding pipe 13 to be mixed with water
And forming titanium liquid, driving the heating rod 22 to continue rotating through the rotary driving piece 2 to heat the titanium liquid, keeping the temperature of the titanium liquid to 90-100 ℃ and continuing stirring for 0-15 minutes to ensure that the soluble titanyl sulfate is fully dissolved in water to finish the mass transfer process, and stopping stirring, if continuing stirring for 3 minutes, heating the titanium liquid to 95 ℃ to avoid crushing the meta-titanic acid generated by the subsequent hydrolysis reaction; wherein, the titanium liquid hydrolysis process comprises a mass transfer process and a hydrolysis chemical reaction process; the subsequent hydrolysis chemical reaction process mainly comprises the steps that as the plurality of heating rods 22 are arranged, in the hydrolysis process, the heating speed and the heating uniformity of the uniformly distributed heating rods 22 are improved when the titanium liquid is initially mixed, and on the other hand, the surface area of the heating rods 22 is large, adhesion can be provided for precipitation of crystals, and the surface of the heating rods 22 can serve as crystal nuclei so as to facilitate precipitation of crystal grains, so that the crystallization efficiency is improved; after the titanium liquid is fully crystallized, the heating rod 22 is driven to move upwards by a part of distance through the telescopic driving piece 21, so that part of crystals attached to the heating rod 22 are separated from the titanium liquid, the content of metatitanic acid in the titanium liquid is reduced, the forward direction of the reaction is accelerated, and the crystallization rate in the titanium liquid is further improved; after the titanium liquid in the kettle body 1 is crystallized, the heating rod 22 is driven to move downwards through the telescopic driving piece 21, so that the lower end of the heating rod 22 is abutted against the kettle bottom 11, meanwhile, the scraping plate 23 continues to move downwards, the scraping plate 23 scrapes off crystals attached to the heating rod 22 and the crystals attached to the inner wall of the kettle body 1, and the loss of the crystals collected later is reduced.
Further, as shown in fig. 4, a high temperature resistant battery 15 is disposed below the kettle cover 12, the high temperature resistant battery 15 rotates along with the scraper 23, and the high temperature resistant battery 15 supplies power to the plurality of heating rods 22 for heating; the high temperature resistant battery 15 is externally provided with a protective housing.
Further, as shown in fig. 4-6, the kettle body 1 includes a kettle bottom 11 and a kettle cover 12, and spiral holes 111 for introducing gas or liquid into the kettle body 1 are formed around the kettle bottom 11.
After stirring is stopped, inert gas or air is introduced into the kettle body 1 through the spiral hole 111 so as to promote the fluidity of titanium liquid in the kettle body 1, improve the temperature uniformity of the titanium liquid in the kettle body 1, improve the dispersibility of the metatitanic acid generated by the reaction, avoid the difficulty of the subsequent crushing process caused by the fact that excessive metatitanic acid is coagulated into metatitanic acid with larger particles, and simultaneously avoid the problems that the generated crystal grains are crushed by directly stirring the titanium liquid through a stirring part, and the subsequent solid-liquid separation difficulty is increased due to the fact that the particle size of the crystal grains generated by hydrolysis is too small, so that the generated metatitanic acid is not too large or too small, and the generated metatitanic acid particle size is stabilized within a reasonable particle size range.
Further, the upper layer of the scraper 23 is made of glass, and fine glass particles are generated by friction between the glass and the heating rod 22 in the downward moving process of the scraper 23, so that the glass particles serve as crystal nuclei to promote the improvement of crystallization rate;
further, as shown in fig. 4 to 6, the heating rod 22 includes a heating part 221 and a mounting part 222 connected to the heating part 221, the upper end of the mounting part 222 is larger than the lower end of the mounting part 222, and the upper end of the mounting part 222 is located at the upper end of the scraper 23; the installation part 222 is always positioned above the liquid level in the kettle body 1, and the heating part 221 comprises a first section, a second section and a third section which are sequentially connected and can be independently controlled to be heated.
It should be noted that, in the process that the telescopic driving member 21 drives the heating rod 22 to move up by a part of distance to separate part of the crystal on the heating rod 22 from the titanium liquid, when the two-stage and three-stage heating rods 22 separate from the titanium liquid, the two-stage and three-stage heating rods 22 stop heating to reduce the waste of electric energy; the present case is not limited to heating by the heating rod 22, but the hydrolyzed titanium liquid may be heated by steam heating in a conventional technique.
Further, as shown in fig. 1-6, the kettle body 1 is provided with a second feeding pipe 3 communicated with all the spiral holes 111, and the upper end of the second feeding pipe 3 is also communicated with an air blowing component 31; the air blowing component 31 is connected with an air source 32 and a water source 33, and a heater 34 is arranged on the flow path of the water source 33.
When the kettle body 1 needs to be inflated, the air blowing component 31 is used as power, the kettle body 1 is inflated, when the boiling water needs to be added into the kettle body 1, the air blowing component 31 is used for pumping water from the water source 33 and heating and boiling the water by the heater 34, and then the water is flushed into the kettle body 1, and when the water needs to be filled into the kettle body 1 for washing, the heater 34 is turned off, so that the water is filled into the kettle body 1 for washing.
Further, the air blowing component 31 is a water-air dual-purpose pump, an air valve is arranged at the connection end of the water-air dual-purpose pump and the air source 32, a water valve is arranged at the connection end of the water-air dual-purpose pump and the water source 33, and the water-air dual-purpose pump is in the prior art, so that not only can water be conveyed, but also air can be conveyed;
further, the water source 33 is an oxalic acid solution with a reducing effect, and the oxalic acid solution can reduce ferric iron to ferrous iron to inhibit the hydrolysis of the ferric iron in the washing process, so that the purity of the metatitanic acid is improved; meanwhile, the titanium oxalate complex formed in the hydrolysis can promote the hydrolysis reaction, and the titanium oxalate complex is thermally decomposed to generate rutile titanium dioxide and volatilize carbon dioxide.
Further, as shown in fig. 4-6, the bottom 11 is further provided with a discharge hole 112;
a cylindrical filter screen assembly 4 capable of sliding relative to the discharge hole 112 is arranged in the discharge hole 112, and a sealing cover 41 is arranged on the upper part of the cylindrical filter screen assembly 4.
Through arranging the cylindrical filter screen assembly 4, after the titanium liquid hydrolysis reaction is finished, the kettle body 1 is filled with ionized water or clean water through the spiral hole 111 in a spiral manner, then the cylindrical filter screen assembly 4 is controlled to move upwards, so that the washed clean water flows away through the cylindrical filter screen assembly 4, and impurities on the surface of crystals are washed cleanly through multiple times of washing, so that the hydrolysis reaction and washing are combined into a whole, and the practicability of the auxiliary device is improved; at the same time, the higher the cylindrical screen assembly 4 is raised below the wastewater level, the larger the filtration area.
Further, as shown in fig. 6-11, the cylindrical screen assembly 4 includes:
a rotating shaft 42, one end of which is vertically rotatably connected to the sealing cover 41;
a rotating plate 43 connected to the rotating shaft 42 and uniformly surrounded by a plurality of rotating plates 43;
the first sleeve 44 is sleeved outside the rotating plate 43 which is enclosed into a circle, and the upper end of the first sleeve 44 is communicated with the discharge hole 112;
the upper end of the second sleeve 45 is in sliding communication with the inner wall of the first sleeve 44, and the inner diameter of the second sleeve 45 is smaller than the inner diameter of the smallest circle surrounded by the plurality of rotating shafts 42; the lower end of the rotating shaft 42 extends into the second sleeve 45 and is rotationally connected with the second sleeve 45;
the discharging pipe 46 is arranged at the lower end of the second sleeve 45 and is communicated with the second sleeve 45;
the plate driving assembly 47 is used for simultaneously driving all the rotating shafts 42 to rotate so as to realize synchronous adjustment of gaps between all the adjacent rotating plates 43, and the plate driving assembly 47 is arranged at the lower end of the second sleeve 45;
the lifting member 48 for driving the second sleeve 45 to lift relative to the first sleeve 44, the lifting member 48 being connected to the lower end of the second sleeve 45.
Further, the gap between adjacent two of the shafts 42 is larger than the maximum width of the largest crystal of the crystals.
By arranging the first sleeve 44 and the second sleeve 45, the upper end and the lower end of the counter-rotating plate 43 are plugged, so that the washed wastewater can only flow down from the gap between the side surfaces of two adjacent rotating plates 43 and flow out through the discharging pipe 46; all rotating plates 43 are driven to synchronously rotate through a plate driving assembly 47 so as to change the gaps between adjacent rotating plates 43 to achieve the gaps required by actual filtration, thereby realizing the flushing filtration of crystals in the kettle body 1; when the crystal flushing is completed, the rotating plates 43 are driven to rotate by the plate driving assembly 47, so that the gap between the adjacent rotating plates 43 is increased, and the crystals are discharged conveniently;
meanwhile, the clearance between two adjacent rotating plates 43 is controlled by the driving of the plate driving assembly 47, and the heating rod 22 which rotates slowly is matched, so that the screening and discharging of crystals with different particle sizes can be realized.
As a modification, the lifting member 48 is a telescopic cylinder or a telescopic hydraulic cylinder or an electric telescopic rod;
further, as shown in fig. 6 to 11, the plate driving assembly 47 includes:
a first driving member 471 connected to each of the rotary shafts 42;
a second transmission member 472 in transmission connection with all the first transmission members 471;
a first driving member 473 for driving the second driving member 472 to drive the first driving member 473 to be connected with the second sleeve 45;
further, the first transmission member 471 is a first gear, and the second transmission member 472 is a gear ring meshed with the first transmission member 471; the first driving member 473 is a first servo motor with a gear at its end and in driving engagement with the second driving member 472;
further, the first driving member 471 is a sprocket, the second driving member 472 is a chain meshed with the first driving member 471, the chain driving path is limited to be meshed with all the first driving members 471, and the first driving member 473 is a first servo motor with a gear at an end portion and meshed with the second driving member 472.
Further, a rotation driving member 49 is disposed at the upper end of the lifting member 48; a transmission assembly 491 which is in transmission connection with the rotation driving piece 49 and the discharging pipe 46 is arranged between the rotation driving piece 49 and the discharging pipe 46; and the lifting piece 48 is rotatably connected with the discharging pipe 46.
The rotation driving member 49 drives the transmission assembly 491 to rotate the discharge pipe 46, so that the second sleeve rotating shaft and the integral rotating plate rotate around the second sleeve rotating center, and the problem of blockage of the filtering gap between the adjacent rotating plates during the filtration of the metatitanic acid can be reduced.
Further, the rotation driving member 49 is a servo motor, and the transmission assembly 491 is a gear set;
further, the bottom surface of the kettle body 1 is a concave cambered surface, the bottom surface of the scraper 23 is matched with the bottom surface of the kettle body 1, and the bottom surface of the scraper 23 is provided with a scraper 231.
It should be noted that, setting the bottom surface of the kettle body 1 as a concave cambered surface is favorable to the discharge of waste liquid and the discharge of crystal, and through setting up scraper 231, is favorable to scraping the crystal of kettle body 1 bottom to promote the crystal discharge cleaner.
Example two
As shown in fig. 1 to 11, wherein the same or corresponding parts as those in the first embodiment are denoted by the same reference numerals as those in the first embodiment, only the points of distinction from the first embodiment will be described below for the sake of brevity. The second embodiment is different from the first embodiment in that: as shown in fig. 1-3 and 7-8, the gas slip ring 54 communicated with the inside of the discharging pipe 46 is rotatably connected to the outside of the discharging pipe 46; the side of the kettle body 1 is provided with a circulating assembly 5, and the circulating assembly 5 comprises:
a first waste water tank 51 for storing waste titanium liquid, the first waste water tank 51 being communicated with the inside of the gas slip ring 54 through a first pipe 511 provided with a first valve 512 and a first pump 513 provided on the first pipe 511;
a second wastewater tank 52, wherein the second wastewater tank 52 for storing the washing liquid is communicated with the inside of the gas slip ring 54 through a second pipe 521, and a second valve 522 is arranged on the second pipe 521;
the storage tank 53, the lower extreme of storage tank 53 and discharging pipe 46 can be dismantled and be connected and the junction of storage tank 53 and discharging pipe 46 is provided with the third valve 531.
The gas slip ring 54 can only rotate relative to the discharging pipe 46 and cannot slide along the axial direction of the discharging pipe 46, and the gas slip ring 54 is used for realizing the communication between the rotating discharging pipe 46 and the first pipe 511 and the second pipe 521 which do not rotate; the first pipe 511 and the second pipe 521 are both hoses or metal hoses;
further, the filtering gap A between two adjacent rotating plates 43 is larger than the filtering gap B between two adjacent rotating plates 43 when the metatitanic acid crystals are washed during the discharge of the waste titanium liquid; the filtering gap C between two adjacent rotating plates 43 discharged by the recrystallized titanium liquid flowing back into the kettle body 1 from the first wastewater tank 51 is far smaller than the filtering gap A.
After the titanium solution is hydrolyzed, the plate driving assembly 47 drives the rotating shaft 42 to rotate so that the gap between two adjacent rotating plates 43 is adjusted to be a required filtering gap A, meanwhile, the second valve 522 and the third valve 531 are closed so as to open the first valve 512, then the lifting piece 48 drives the second sleeve 45 to move upwards so as to open the sealing cover 41, the second sleeve 45 is stopped when the lifting piece cannot lift, so that the filtering area is enlarged, the waste titanium solution flows into the first waste water tank 51, then the first spiral filling of clean water into the kettle body 1 is performed through the spiral hole 111, and the waste water after the first washing enters the first waste water tank 51; then the first valve 512 is closed, the second valve 522 is opened, clean water is filled into the kettle body 1 for the second time in a spiral manner through the spiral hole 111, meanwhile, the rotary driving piece 2 is controlled to drive the heating rod 22 to stir washing liquid at a low speed, the cleaning effect is improved, as crystals are not heated any more during the cleaning process and are less separated out, at this time, the influence of the low-speed stirring of the heating rod 22 on the washing liquid on the metatitanic acid crystals is small, the effect is neglected, after the cleaning is finished, the second sleeve 45 is driven to move upwards through the lifting piece 48, the rotating plates 43 are moved to the position above the liquid outlet holes, and at this time, the filtering gap B < filtering gap A between two adjacent rotating plates 43 is formed, wherein the filtering gap A allows crystals with the particle size of M to pass through, the filtering gap B does not allow crystals with the particle size of M to pass through, most of crystals with the particle size of less than M fall into the first waste water tank 52, and the waste water from the second cleaning process enters the second waste water tank 52, so that the content of crystals with the particle size of less than M in the second waste water tank 52 is reduced; and similarly, the crystals in the kettle body 1 are the same as the crystals in the second washing for several times, and are discharged into a second wastewater tank 52 after being stirred and washed at a low speed; then closing the second valve 522 and opening the third valve 531, and opening the gap between the adjacent rotating plates 43 to the maximum, so that the washed metatitanic acid crystals in the kettle body 1 fall into the storage tank 53, then driving the scraper 23 to move downwards by the telescopic driving piece 21 to enable the heating rod 22 to abut against the kettle bottom 11, and continuing to move downwards by the scraper 23 to scrape the metatitanic acid crystals condensed on the heating rod 22 and the inner wall of the kettle body 1 and the bottom of the kettle body 1 and fall into the kettle bottom 11, wherein the reason that the metatitanic acid crystals in the kettle body 1 fall into the storage tank 53 and then are scraped by the scraper 23 is that if the metatitanic acid crystals condensed on the heating rod 22 and the inner wall of the kettle body 1 are scraped beforehand, on the one hand, metatitanic acid crystal powder is easily washed off to generate waste, and on the other hand, the scraper 23 cannot be scraped to the lower end of the heating rod 22 and the lower end of the kettle body 1 and the lower end of the bottom of the kettle body 1 are blocked by a large amount of metatitanic acid crystals, so that the metatitanic acid crystals condensed on the lower end of the heating rod 22 and the bottom of the kettle body 1 are scraped off cleanly and fall into the kettle bottom 11, and then the metatitanic acid crystals fall into the storage tank 53 after the kettle body 1 is scraped by the next time, and the metatitanic acid crystals fall into the storage tank 53 is selected;
when all the metatitanic acid crystals in the kettle body 1 fall into the storage pipe, the third valve 531 is closed, the first valve 512 is opened, the waste water in the first waste water tank 51 flows back to the kettle body 1 through the first pump 513 to be concentrated or diluted as titanium liquid until the concentration reaches 160g/L, 160g/L of titanium liquid has high crystallization efficiency and good crystallization quality, if the titanium liquid is diluted, boiling water is added into the kettle body 1 through the spiral hole 111 to dilute the titanium liquid, after the titanium liquid is recrystallized, the plate driving assembly 47 drives the rotating shaft 42 to rotate, the filter gap C between two adjacent rotating plates 43 is several times smaller than the filter gap A, the gap blockage between the two adjacent rotating plates 43 is reduced because of few metatitanic acid crystals generated by the recrystallization at this time, the waste water after the recrystallization can be rapidly discharged, the recovery of the metatitanic acid crystals left in the waste titanium liquid can be realized, the yield of the metatitanic acid crystals is improved, the quantity of the added washed is reduced accordingly, and the waste water is discharged into the second waste water tank 52 because the recovered from the titanium crystals is greatly blocked, and the waste water is rapidly discharged into the waste water tank 52; the wastewater in the second wastewater tank 52 is filtered by precipitation to remove impurities and then is reused as hydrolyzed boiling water; meanwhile, by making the filter gap a several times larger than the filter gap C, the metatitanic acid crystal grains with smaller particle size enter the first waste water tank 51 for temporary storage, so that the waste titanium liquid is discharged rapidly and the metatitanic acid crystals with larger particles are washed rapidly for multiple times, thereby improving the washing efficiency of the overall metatitanic acid.
The foregoing description of the preferred embodiments of the invention is not intended to be limiting, but rather is intended to cover all modifications, equivalents, and alternatives falling within the spirit and principles of the invention.

Claims (6)

1. A titanium dioxide separation production auxiliary device which is characterized in that: comprising
A kettle body for hydrolysis reaction;
the rotary driving piece is used as a rotary driving source in the titanium liquid mass transfer process and is arranged at the upper end of the kettle body;
the upper end of the telescopic driving piece is connected with the lower end of the rotary driving piece;
the scraping plate is connected with the lower end of the telescopic driving piece; the upper layer of the scraping plate is made of glass;
the heating rods uniformly arranged in the kettle body penetrate through the scraping plate and are in sliding connection with the scraping plate; the scraper can scrape the crystallization on the inner wall surface of the heating rod and the kettle body;
the kettle body comprises a kettle bottom and a kettle cover, and spiral holes for introducing gas or liquid into the kettle body are formed in the periphery of the kettle bottom;
the heating rod includes:
the heating part comprises a first section, a second section and a third section which are sequentially connected and can be independently controlled to be heated;
the upper end of the installation part is larger than the lower end of the installation part, and the upper end of the installation part is positioned at the upper end of the scraping plate;
the kettle body is provided with a second feeding pipe communicated with all the spiral holes, and the upper end of the second feeding pipe is also communicated with an air blowing component; the air blowing component is connected with an air source and a water source, and a heater is arranged on a flow path of the water source;
the kettle bottom is also provided with a discharge hole;
a cylindrical filter screen assembly capable of sliding relative to the discharge hole is arranged in the discharge hole, and a sealing cover is arranged on the upper portion of the cylindrical filter screen assembly.
2. The titanium dioxide separation and production auxiliary device according to claim 1, wherein: the cylindrical screen assembly includes:
one end of the rotating shaft is vertically and rotatably connected to the sealing cover;
the rotating plates are connected with the rotating shaft and uniformly encircle a plurality of rotating plates into a circle;
the first sleeve is sleeved on the outer side of the rotating plate which is enclosed into a circle, and the upper end of the first sleeve is communicated with the discharge hole;
the upper end of the second sleeve is in sliding communication with the inner wall of the first sleeve, and the inner diameter of the second sleeve is smaller than the inner diameter of a minimum circle formed by a plurality of rotating shafts; the lower end of the rotating shaft extends into the second sleeve and is rotationally connected with the second sleeve;
the discharging pipe is arranged at the lower end of the second sleeve and communicated with the second sleeve;
the plate driving assembly is used for simultaneously driving all the rotating shafts to rotate so as to realize synchronous adjustment of gaps between all the adjacent rotating plates, and is arranged at the lower end of the second sleeve;
the lifting piece is used for driving the second sleeve to lift relative to the first sleeve, and is connected with the lower end of the second sleeve.
3. The titanium dioxide separation and production auxiliary device according to claim 2, wherein: the board driving assembly includes:
the first transmission piece is respectively connected with each rotating shaft;
the second rotating piece is in transmission connection with all the first transmission pieces;
the first driving piece is used for driving the second rotating piece to drive the first driving piece to be connected with the second sleeve.
4. The titanium dioxide separation and production auxiliary device according to claim 2, wherein:
the upper end of the lifting piece is provided with a rotary driving piece; a transmission assembly which is in transmission connection with the rotation driving piece and the discharging pipe is arranged between the rotation driving piece and the discharging pipe; and the lifting piece is rotationally connected with the discharging pipe.
5. The apparatus according to any one of claims 2 to 4, wherein: the gas slip ring is rotationally connected with the outside of the discharge pipe and is communicated with the inside of the discharge pipe; the side of the cauldron body is provided with circulation subassembly, circulation subassembly includes:
the first waste water tank is used for storing waste titanium liquid, is communicated with the inside of the gas slip ring through a first pipe, and a first valve and a first pump are arranged on the first pipe;
the second wastewater tank is used for storing washing liquid, is communicated with the inside of the gas slip ring through a second pipe, and a second valve is arranged on the second pipe;
the storage tank, the storage tank can be dismantled with the lower extreme of discharging pipe and the junction of storage tank and discharging pipe is provided with the third valve.
6. The titanium dioxide separation and production auxiliary device according to claim 5, wherein: the filtering gap A between two adjacent rotating plates is larger than the filtering gap B between two adjacent rotating plates when the metatitanic acid crystals are washed when the waste titanium liquid is discharged;
the filtering gap C between two adjacent rotating plates discharged by the recrystallized titanium liquid flowing back into the kettle body of the first wastewater tank is far smaller than the filtering gap A.
CN202211238420.4A 2022-10-11 2022-10-11 Titanium dioxide separation production auxiliary device Active CN115317952B (en)

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CN211097623U (en) * 2019-11-12 2020-07-28 湖北澳格森化工有限公司 Crystallization kettle capable of effectively avoiding influence of stirring on crystal precipitation
CN213942128U (en) * 2020-12-04 2021-08-13 云南丁氏蜂业工贸有限公司 Energy-saving vacuum concentration device for honey production
CN113769687A (en) * 2021-09-10 2021-12-10 河北化工医药职业技术学院 Method for producing chiral drug
CN217265811U (en) * 2022-03-03 2022-08-23 漳州山峰食品有限公司 Special-shaped crystallization device of rock sugar
CN114989231A (en) * 2022-06-20 2022-09-02 新琪安科技股份有限公司 Crystallization method of sucralose
CN115069204A (en) * 2022-08-23 2022-09-20 山东彩客新材料有限公司 Continuous production device and method for synthesizing iron phosphate from mixed phosphoric and phosphoric acid
CN115069123A (en) * 2022-05-21 2022-09-20 明光市昊昊蜂业有限公司 A head tank for honey processing

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN211097623U (en) * 2019-11-12 2020-07-28 湖北澳格森化工有限公司 Crystallization kettle capable of effectively avoiding influence of stirring on crystal precipitation
CN213942128U (en) * 2020-12-04 2021-08-13 云南丁氏蜂业工贸有限公司 Energy-saving vacuum concentration device for honey production
CN113769687A (en) * 2021-09-10 2021-12-10 河北化工医药职业技术学院 Method for producing chiral drug
CN217265811U (en) * 2022-03-03 2022-08-23 漳州山峰食品有限公司 Special-shaped crystallization device of rock sugar
CN115069123A (en) * 2022-05-21 2022-09-20 明光市昊昊蜂业有限公司 A head tank for honey processing
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