CN112939071A - Preparation and storage method of titanium tetrachloride crystal seed - Google Patents
Preparation and storage method of titanium tetrachloride crystal seed Download PDFInfo
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- CN112939071A CN112939071A CN202110199235.8A CN202110199235A CN112939071A CN 112939071 A CN112939071 A CN 112939071A CN 202110199235 A CN202110199235 A CN 202110199235A CN 112939071 A CN112939071 A CN 112939071A
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- 239000013078 crystal Substances 0.000 title claims abstract description 80
- XJDNKRIXUMDJCW-UHFFFAOYSA-J titanium tetrachloride Chemical compound Cl[Ti](Cl)(Cl)Cl XJDNKRIXUMDJCW-UHFFFAOYSA-J 0.000 title claims abstract description 54
- 238000000034 method Methods 0.000 title claims abstract description 42
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- 238000003860 storage Methods 0.000 title claims abstract description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 46
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 28
- 239000000243 solution Substances 0.000 claims abstract description 22
- 239000003513 alkali Substances 0.000 claims abstract description 20
- 239000007864 aqueous solution Substances 0.000 claims abstract description 17
- 238000002156 mixing Methods 0.000 claims abstract description 14
- 238000006386 neutralization reaction Methods 0.000 claims abstract description 14
- 239000000725 suspension Substances 0.000 claims abstract description 14
- 238000010790 dilution Methods 0.000 claims abstract description 12
- 239000012895 dilution Substances 0.000 claims abstract description 12
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims abstract description 7
- 229910052719 titanium Inorganic materials 0.000 claims abstract description 7
- 239000010936 titanium Substances 0.000 claims abstract description 7
- 239000002253 acid Substances 0.000 claims abstract description 4
- 239000008367 deionised water Substances 0.000 claims abstract description 4
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 4
- 238000005070 sampling Methods 0.000 claims description 27
- 239000007788 liquid Substances 0.000 claims description 22
- 238000003756 stirring Methods 0.000 claims description 21
- 239000007921 spray Substances 0.000 claims description 18
- 239000006228 supernatant Substances 0.000 claims description 13
- 238000005406 washing Methods 0.000 claims description 13
- 239000000463 material Substances 0.000 claims description 12
- 239000004408 titanium dioxide Substances 0.000 claims description 10
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 9
- 230000007246 mechanism Effects 0.000 claims description 8
- 229910000831 Steel Inorganic materials 0.000 claims description 5
- 238000007599 discharging Methods 0.000 claims description 5
- 239000010959 steel Substances 0.000 claims description 5
- 229920001971 elastomer Polymers 0.000 claims description 4
- 230000003014 reinforcing effect Effects 0.000 claims description 4
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 3
- 238000006243 chemical reaction Methods 0.000 claims description 3
- 238000011010 flushing procedure Methods 0.000 claims description 3
- 230000035484 reaction time Effects 0.000 claims description 3
- 150000003839 salts Chemical class 0.000 claims description 3
- 238000007789 sealing Methods 0.000 claims description 3
- 230000008878 coupling Effects 0.000 claims description 2
- 238000010168 coupling process Methods 0.000 claims description 2
- 238000005859 coupling reaction Methods 0.000 claims description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-N ammonia Natural products N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims 1
- 230000008569 process Effects 0.000 abstract description 14
- 235000010215 titanium dioxide Nutrition 0.000 abstract description 11
- 239000000049 pigment Substances 0.000 abstract description 2
- 230000007062 hydrolysis Effects 0.000 description 14
- 238000006460 hydrolysis reaction Methods 0.000 description 14
- 238000004062 sedimentation Methods 0.000 description 12
- 239000003351 stiffener Substances 0.000 description 5
- 229910003074 TiCl4 Inorganic materials 0.000 description 4
- 239000000047 product Substances 0.000 description 4
- 239000000919 ceramic Substances 0.000 description 3
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 2
- 230000009471 action Effects 0.000 description 2
- 235000011114 ammonium hydroxide Nutrition 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- 238000009434 installation Methods 0.000 description 2
- 238000010030 laminating Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 238000007790 scraping Methods 0.000 description 2
- 238000009283 thermal hydrolysis Methods 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 1
- 238000003556 assay Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229920005549 butyl rubber Polymers 0.000 description 1
- 210000002421 cell wall Anatomy 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 230000003472 neutralizing effect Effects 0.000 description 1
- 238000005728 strengthening Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000012808 vapor phase Substances 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G23/00—Compounds of titanium
- C01G23/04—Oxides; Hydroxides
- C01G23/047—Titanium dioxide
- C01G23/053—Producing by wet processes, e.g. hydrolysing titanium salts
- C01G23/0536—Producing by wet processes, e.g. hydrolysing titanium salts by hydrolysing chloride-containing salts
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D9/00—Crystallisation
- B01D9/0036—Crystallisation on to a bed of product crystals; Seeding
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D9/00—Crystallisation
- B01D2009/0086—Processes or apparatus therefor
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Crystallography & Structural Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Life Sciences & Earth Sciences (AREA)
- Environmental & Geological Engineering (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Inorganic Chemistry (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
The invention discloses a preparation and storage method of titanium tetrachloride seed crystals, which comprises the following steps: firstly, titanium tetrachloride to be diluted passes through a heat exchanger, then the titanium tetrachloride is input into a dilution tank and added with deionized water for dilution, the dilution temperature is controlled to be below 40 ℃, the diluted titanium tetrachloride aqueous solution is used for storage, and the titanium tetrachloride aqueous solution is fed into a seed crystal preparation tank in batches; feeding the alkali liquor into a seed crystal preparation tank, reacting the diluted titanium tetrachloride solution with the alkali liquor, and quickly mixing the titanium tetrachloride solution with a preset alkali liquor amount and water amount to realize partial neutralization to meet the requirement of an acid/titanium target ratio; in step S2, the alkali solution is added again to complete the neutralization reaction, and the pH is controlled to 7.5-10.5 to prepare a seed crystal suspension. The invention has the advantages of simple process, easy control, high rutile content of the seed crystal and stable quality, and the obtained rutile seed crystal can be used for producing common pigment titanium white on a large scale.
Description
Technical Field
The invention relates to the technical field of titanium tetrachloride production and processing, in particular to a preparation and storage method of titanium tetrachloride crystal seeds.
Background
At present, most of titanium dioxide manufacturers in China adopt a sulfate process titanium dioxide process, and for the sulfate process titanium dioxide process, the selection of a titanium liquid hydrolysis process is one of key factors influencing the quality of a titanium dioxide product. Typically, hydrolysis includes an autoseeded atmospheric thermal hydrolysis process and an external seeded atmospheric thermal hydrolysis process. Compared with the autogenous seed crystal hydrolysis process, the additional seed crystal hydrolysis process has the advantages of simple hydrolysis operation, stable seed crystal quality, small fluctuation of the quality among product batches, low requirement on the concentration of the titanium solution to be hydrolyzed and the like, so the additional seed crystal hydrolysis process is a more advanced hydrolysis process compared with the autogenous seed crystal hydrolysis.
For the external seed hydrolysis process, the key point is to prepare the seed suitable for the hydrolysis of the titanium liquid. The summary of the current situation for the preparation of hydrolysis plus seed crystals starting from an aqueous TiCl4 solution is as follows:
chinese patent application publication No. CN 101863510a discloses a method for preparing titanium white seed crystal with added hydrolysis by using aqueous TiCl4 solution as raw material, the seed crystal produced by the method is a substance obtained by heating and peptizing the material after neutralizing the aqueous TiCl4 solution with alkali solution, and directly cooling.
U.S. patent application publication No. US4021533A discloses a method for preparing hydrolysis addition seed crystal from TiCl4 as raw material by a vapor phase method, and the method for preparing the addition seed crystal has the advantages of continuity, stability and the like, but the method has high requirements on the corrosion resistance and automation control of equipment.
Therefore, the inventor aims to provide a method for preparing and storing titanium tetrachloride seed crystals by taking the experience of abundant design development and actual manufacturing of the related industry for years as a basis and researching and improving the existing structure and deficiency so as to achieve the aim of higher practical value.
Disclosure of Invention
In order to solve the problems mentioned in the background art, the invention provides a preparation and storage method of titanium tetrachloride seed crystals.
In order to achieve the purpose, the invention adopts the following technical scheme:
a preparation and storage method of titanium tetrachloride seed crystals comprises the following steps:
s1: firstly, titanium tetrachloride to be diluted passes through a heat exchanger, then the titanium tetrachloride is input into a dilution tank and added with deionized water for dilution, the dilution temperature is controlled to be below 40 ℃, the diluted titanium tetrachloride aqueous solution is used for storage, and the titanium tetrachloride aqueous solution is fed into a seed crystal preparation tank in batches;
s2: feeding the alkali liquor into a seed crystal preparation tank, reacting the diluted titanium tetrachloride solution with the alkali liquor, and quickly mixing the titanium tetrachloride solution with a preset alkali liquor amount and water amount to realize partial neutralization to meet the requirement of an acid/titanium target ratio;
s3: adding alkali liquor again in the step S2 to complete the neutralization reaction, and controlling the pH value to be 7.5-10.5 to prepare and form a seed crystal suspension;
s4: feeding the prepared seed crystal suspension into a seed crystal settling tank, washing with hot water, fully stirring and mixing, settling after the seed crystal is separated out, controlling the concentration of the settled solution to be 40 g/L, and discharging supernatant containing a large amount of soluble salts generated by neutralization after the settlement;
s5: after the supernatant is discharged, the settled seed crystals need to be stirred, and then pumped to a storage tank for storage.
Preferably, the alkali liquor is NaOH aqueous solution, KOH aqueous solution or ammonia water.
Preferably, the concentration of the titanium tetrachloride aqueous solution in the step S1 is 2.5 to 4.2mol/L based on the titanium dioxide therein.
Preferably, the concentration of the seed crystal suspension in the step S3 is 25-30 g/L in terms of titanium dioxide, and the neutralization reaction time is 10-20 minutes.
Preferably, the method adopts the following system reaction, the system comprises a settling tank body, a bottom plate, an emptying port, a hot water inlet, a liquid level meter port, a material inlet and a quick-opening manhole, the emptying port, the hot water inlet, the liquid level meter port, the material inlet and the quick-opening manhole are arranged on the upper end surface of the settling tank body, the turbidity meter port, a sampling mechanism and a liquid collecting pipe are sequentially arranged on one side of the outer wall of the settling tank body from top to bottom, the thermometer port, the manhole and a discharge port are sequentially arranged on the other side of the outer wall of the settling tank body from top to bottom, a slope is arranged at the bottom of the inner side of the settling tank body, a tile lining is laid at the upper end of the slope, a driving shaft is vertically arranged at the center of the upper end of the settling tank body, the lower end of the driving shaft is connected with a stirring, first drive wheel is connected with the second drive wheel through the drive belt transmission, the second drive wheel is connected with driving motor through the pivot, the circumference lateral wall of (mixing) shaft evenly encircles and is equipped with a plurality of stiffener, the one end that the (mixing) shaft was kept away from to the stiffener is fixed with the baffle, the baffle is equipped with a plurality of groups of scraper blades towards one side equidistance of subsider body inner wall, the inner wall laminating of scraper blade and subsider body.
Preferably, the sampling mechanism comprises sampling tube, closing cap, flange and sample connection, and the sampling tube level sets up in the lateral wall of subsider body, and closing cap and flange pass through bolted connection, and the sample connection extends to this internal extension of subsider, and the opening of sample connection is the inclined plane opening, and the last incision and the lower incision one-tenth angle of sample connection.
Preferably, a turbidimeter is installed in the turbidimeter port, and the installation position of the turbidimeter port is higher than the upper opening of the liquid collecting pipe.
Preferably, the inner wall of the settling tank body is provided with a layer of rubber lining, the bottom of the settling tank body is provided with a bottom plate, and tank bottom I-shaped steel is arranged at the bottom of the bottom plate at equal intervals.
Preferably, the inner wall of driving shaft is equipped with water pipeline perpendicularly, and water pipeline's bottom even intercommunication has a plurality of communicating pipe, the tip intercommunication of communicating pipe has the spray tube, and the spray tube extends to the baffle in, the outer wall one side evenly distributed of spray tube has a plurality of washing terminals, and washing terminals distributes along the spray tube is perpendicular.
Preferably, the upper port of the water pipeline is vertically inserted with a water inlet pipe, and the outer wall of the joint of the water inlet pipe and the water pipeline is sleeved with a bearing.
Compared with the prior art, the invention has the beneficial effects that: the seed crystal produced by the method for preparing and storing the titanium tetrachloride seed crystal has high rutile content and good stability, and can be still used as a hydrolysis seed crystal after being placed for more than 15 days at least. The invention has the advantages of simple process, easy control, high rutile content of the seed crystal and stable quality, and the obtained rutile seed crystal can be used for producing common pigment titanium white on a large scale.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the drawings without creative efforts.
FIG. 1 is a schematic structural view of the present invention;
FIG. 2 is a schematic cross-sectional view of the structure A-A of the present invention;
FIG. 3 is an enlarged view of the structure B of the present invention;
FIG. 4 is a schematic structural diagram of a sampling mechanism according to the present invention.
In the figure: the device comprises a settling tank body 1, a rubber lining 2, a bottom plate 3, tank bottom I-steel 4, a slope 5, a tile lining 6, a vent 7, a hot water inlet 8, a liquid level meter port 9, a material inlet 10, a quick-opening manhole 11, a thermometer port 12, a manhole 13, a discharge port 14, a turbidimeter port 15, a sampling mechanism 16, a sampling pipe 161, a sealing cover 162, a flange 163, a sampling port 164, a liquid collecting pipe 17, a stirring shaft 18, a stirring wheel 19, a coupling 20, a driving shaft 21, a water pipeline 22, a first driving wheel 23, a driving belt 24, a second driving wheel 25, a driving motor 26, a water inlet pipe 27, a bearing 28, a baffle 29, a scraper 30, a flushing nozzle 31, a spray pipe 32, a communicating pipe 33 and a reinforcing.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, 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 some, but not all, embodiments of the present invention. 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.
Example 1
Referring to fig. 1 to 3, a method for preparing and storing titanium tetrachloride seed crystals is characterized by comprising the following steps:
s1: firstly, titanium tetrachloride to be diluted passes through a heat exchanger, then the titanium tetrachloride is input into a dilution tank and added with deionized water for dilution, the dilution temperature is controlled to be below 40 ℃, the diluted titanium tetrachloride aqueous solution is used for storage, and the titanium tetrachloride aqueous solution is fed into a seed crystal preparation tank in batches;
s2: feeding the alkali liquor into a seed crystal preparation tank, reacting the diluted titanium tetrachloride solution with the alkali liquor, and quickly mixing the titanium tetrachloride solution with a preset alkali liquor amount and water amount to realize partial neutralization to meet the requirement of an acid/titanium target ratio;
s3: adding alkali liquor again in the step S2 to complete the neutralization reaction, and controlling the pH value to be 7.5-10.5 to prepare and form a seed crystal suspension;
s4: feeding the prepared seed crystal suspension into a seed crystal settling tank, washing with hot water, fully stirring and mixing, settling after the seed crystal is separated out, controlling the concentration of the settled solution to be 40 g/L, and discharging supernatant containing a large amount of soluble salts generated by neutralization after the settlement;
s5: after the supernatant is discharged, the settled seed crystals need to be stirred, and then pumped to a storage tank for storage.
Wherein the alkali liquor is NaOH aqueous solution, KOH aqueous solution or ammonia water.
Wherein the concentration of the titanium tetrachloride aqueous solution in the step S1 is 2.5-4.2 mol/L based on the titanium dioxide therein.
Wherein the concentration of the seed crystal suspension in the step S3 is 25-30 g/L in terms of titanium dioxide, and the neutralization reaction time is 10-20 minutes.
Wherein, the preparation sedimentation method adopts the following sedimentation reaction of a crystal seed sedimentation tank, comprising a sedimentation tank body 1, a bottom plate 3, an emptying port 7, a hot water inlet 8, a liquid level meter port 9, a material inlet 10 and a quick-opening manhole 11, wherein the emptying port 7, the hot water inlet 8, the liquid level meter port 9, the material inlet 10 and the quick-opening manhole 11 are arranged on the upper end surface of the sedimentation tank body 1, one side of the outer wall of the sedimentation tank body 1 is sequentially provided with a turbidity meter port 15, a sampling mechanism 16 and a liquid collecting pipe 17 from top to bottom, the lower port of the liquid collecting pipe 17 is provided with a valve, the other side of the outer wall of the sedimentation tank body 1 is sequentially provided with a thermometer port 12, a manhole 13 and a discharge port 14 from top to bottom, the bottom of the inner side of the sedimentation tank body 1 is provided with a slope 5, the upper end of the slope 5 is paved with a ceramic tile, the bottom of (mixing) shaft 18 is equipped with stirring wheel 19, the upper end outer wall of driving shaft 21 has cup jointed first drive wheel 23, first drive wheel 23 is connected with second drive wheel 25 through the transmission of driving belt 24, second drive wheel 25 is connected with driving motor 26 through the pivot, the circumference lateral wall of (mixing) shaft 18 evenly encircles and is equipped with a plurality of stiffener 34, the one end that (mixing) shaft 18 was kept away from to stiffener 34 is fixed with baffle 29, baffle 29 is equipped with a plurality of groups scraper blade 30 towards one side equidistance of subsider body 1 inner wall, scraper blade 30 and the laminating of the inner wall of subsider body 1, carry out the scraper blade cleanness to the seed crystal of attaching to at subsider body 1 inner wall through scraper blade 30, the inner wall of subsider body 1 is equipped with one deck rubber lining 2, butyl rubber is chooseed.
Wherein, install the turbidimeter in the turbidimeter mouth 15, the turbidimeter chooses JI-0101 model, and the installation position of turbidimeter mouth 15 is higher than the upper opening of collector tube 17, and when the reading of turbidimeter had obvious decline, it indicates that the light that comes from the turbidimeter can pass the supernatant, and the settlement is accomplished.
Wherein, the bottom of subsider body 1 is equipped with bottom plate 3, and the bottom equidistance of bottom plate 3 is provided with tank bottom I-steel 4, plays the fixed support effect of strengthening through setting up bottom plate 3 and tank bottom I-steel 4.
Wherein, the inner wall of driving shaft 21 is equipped with water pipeline 22 perpendicularly, and the even intercommunication in bottom of water pipeline 22 has a plurality of communicating pipe 33, the tip intercommunication of communicating pipe 33 has spray tube 32, spray tube 32 extends to baffle 29 in, outer wall one side evenly distributed of spray tube 32 has a plurality of washing terminals 31, and washing terminals 31 distributes along spray tube 32 is perpendicular, hot water gets into water pipeline 22 through inlet tube 27, get into washing terminals 31 through communicating pipe 33 and spray tube 32 again, spray through washing terminals 31 to the cell wall of subsider body 1 at last and wash, thereby realize the automatically cleaning, the cost of labor has been greatly reduced.
Wherein, the perpendicular grafting of last port of water pipeline 22 has inlet tube 27, and the outer wall of inlet tube 27 and water pipeline 22 junction has cup jointed bearing 28, does not influence inlet tube 27's fixed when making driving shaft 21 rotate through setting up bearing 28.
Wherein, baffle 29 is the arc structure, and baffle 29, spray tube 32, communicating pipe 33 and stiffener 34 set up the quantity the same, can effectively reduce seed crystal and the contact of subsider body 1 inner wall through setting up baffle 29, avoids the seed crystal to adhere to in a large number in the unable clearance of inner wall.
The working principle is as follows: when the device is used, a seed crystal suspension enters the settling tank body 1 through the material inlet 10, hot pure water is added through the hot water inlet 8 for washing, at the moment, the driving motor 26 is started, the driving motor 26 drives the second driving wheel 25 to rotate through the rotating shaft, the second driving wheel 25 drives the first driving wheel 23 to rotate through the driving belt 24, the first driving wheel 23 drives the driving shaft 21 to rotate, the driving shaft 21 drives the stirring shaft 18 to rotate under the action of the coupler 20, so that the stirring wheel 19 fully mixes and stirs the seed crystal suspension, meanwhile, the side wall of the stirring shaft 18 is fixedly connected with the baffle 29 through the reinforcing rod 34, the baffle 29 can effectively reduce the adhesion amount of the seed crystal on the inner wall of the settling tank body 1, and after full mixing and stirring, standing and settling are;
the turbidity meter is used for determining the sedimentation endpoint, when the reading of the turbidity meter is obviously reduced, the light from the turbidity meter can pass through the supernatant, and the sedimentation is finished; at this time, a valve at the lower port of the liquid collecting pipe 17 is opened, and the supernatant is discharged outwards through the liquid collecting pipe 17;
after the supernatant is discharged, opening the discharge hole 14, discharging the titanium tetrachloride crystal seeds outwards along the slope 5, wherein the angle between the slope 5 and the horizontal plane is 35-45 degrees, and the ceramic tile lining 6 is paved at the upper end of the slope 5, so that the finished product materials cannot be accumulated in the settling tank body 1;
thereafter, the wash water gets into water pipeline 22 through inlet tube 27, passes through communicating pipe 33, spray tube 32 and washing nozzle 31 outward blowout again, and washes under the scraping off of scraper blade 30 to improved greatly and washed quality and efficiency, reduced the adhering to of seed crystal, reduced artifical abluent cost simultaneously.
Example 2
Referring to fig. 4, the present embodiment is different from embodiment 1 in that the sampling mechanism 16 is composed of a sampling tube 161, a cover 162, a flange 163 and a sampling port 164, the sampling tube 161 is horizontally disposed on the sidewall of the settling tank body 1, the cover 162 and the flange 163 are connected by a bolt, the sampling port 164 extends into the settling tank body 1, the opening of the sampling port 164 is a bevel opening, and an upper notch and a lower notch of the sampling port 164 form an angle of 45 degrees, so that the contact area of the sampling port 164 and the liquid is enlarged, thereby facilitating sampling.
Other undescribed structures refer to example 1.
The working principle is as follows: when the device is used, a seed crystal suspension enters the settling tank body 1 through the material inlet 10, hot pure water is added through the hot water inlet 8 for washing, at the moment, the driving motor 26 is started, the driving motor 26 drives the second driving wheel 25 to rotate through the rotating shaft, the second driving wheel 25 drives the first driving wheel 23 to rotate through the driving belt 24, the first driving wheel 23 drives the driving shaft 21 to rotate, the driving shaft 21 drives the stirring shaft 18 to rotate under the action of the coupler 20, so that the stirring wheel 19 fully mixes and stirs the seed crystal suspension, meanwhile, the side wall of the stirring shaft 18 is fixedly connected with the baffle 29 through the reinforcing rod 34, the baffle 29 can effectively reduce the adhesion amount of the seed crystal on the inner wall of the settling tank body 1, and after full mixing and stirring, standing and settling are;
the turbidity meter is used for determining the sedimentation endpoint, when the reading of the turbidity meter is obviously reduced, the light from the turbidity meter can pass through the supernatant, and the sedimentation is finished; at this time, a valve at the lower port of the liquid collecting pipe 17 is opened, and the supernatant is discharged outwards through the liquid collecting pipe 17;
after the supernatant liquid is discharged, manually sampling, and carrying out assay analysis on whether the seed crystal is qualified or not; if not, continuing to settle; if the titanium tetrachloride crystal seed is qualified, opening the discharge hole 14, discharging the titanium tetrachloride crystal seed outwards along the slope 5, wherein the angle between the slope 5 and the horizontal plane is 35-45 degrees, and the ceramic tile lining 6 is laid at the upper end of the slope 5, so that the finished product material cannot be accumulated in the settling tank body 1;
thereafter, the wash water gets into water pipeline 22 through inlet tube 27, passes through communicating pipe 33, spray tube 32 and washing nozzle 31 outward blowout again, and washes under the scraping off of scraper blade 30 to improved greatly and washed quality and efficiency, reduced the adhering to of seed crystal, reduced artifical abluent cost simultaneously.
In the description of the present invention, it is to be understood that the terms "central," "longitudinal," "lateral," "length," "width," "thickness," "upper," "lower," "front," "rear," "left," "right," "vertical," "horizontal," "top," "bottom," "inner," "outer," "clockwise," "counterclockwise," "axial," "radial," "circumferential," and the like are used in the orientations and positional relationships indicated in the drawings for convenience in describing the invention and to simplify the description, and are not intended to indicate or imply that the referenced devices or elements must have a particular orientation, be constructed and operated in a particular orientation, and are therefore not to be considered limiting of the invention.
In the present invention, unless otherwise expressly stated or limited, the terms "disposed," "mounted," "connected," "secured," and the like are to be construed broadly and can, for example, be fixedly connected, detachably connected, or integrally formed; they may be mechanically coupled, directly coupled, or indirectly coupled through intervening agents, both internally and/or in any other manner known to those skilled in the art. The specific meanings of the above terms in the present invention can be understood by those skilled in the art according to specific situations.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered to be within the technical scope of the present invention, and the technical solutions and the inventive concepts thereof according to the present invention should be equivalent or changed within the scope of the present invention.
Claims (10)
1. A preparation and storage method of titanium tetrachloride seed crystals is characterized by comprising the following steps:
s1: firstly, titanium tetrachloride to be diluted passes through a heat exchanger, then the titanium tetrachloride is input into a dilution tank and added with deionized water for dilution, the dilution temperature is controlled to be below 40 ℃, the diluted titanium tetrachloride aqueous solution is used for storage, and the titanium tetrachloride aqueous solution is fed into a seed crystal preparation tank in batches;
s2: feeding the alkali liquor into a seed crystal preparation tank, reacting the diluted titanium tetrachloride solution with the alkali liquor, and quickly mixing the titanium tetrachloride solution with a preset alkali liquor amount and water amount to realize partial neutralization to meet the requirement of an acid/titanium target ratio;
s3: adding alkali liquor again in the step S2 to complete the neutralization reaction, and controlling the pH value to be 7.5-10.5 to prepare and form a seed crystal suspension;
s4: feeding the prepared seed crystal suspension into a seed crystal settling tank, washing with hot water, fully stirring and mixing, settling after the seed crystal is separated out, controlling the concentration of the settled solution to be 40 g/L, and discharging supernatant containing a large amount of soluble salts generated by neutralization after the settlement;
s5: after the supernatant is discharged, the settled seed crystals need to be stirred, and then pumped to a storage tank for storage.
2. The method for preparing and storing titanium tetrachloride seed crystals as claimed in claim 1, wherein the alkali solution is an aqueous solution of NaOH, an aqueous solution of KOH or aqueous ammonia.
3. The method for preparing and storing titanium tetrachloride seed crystals according to claim 1, wherein the concentration of the titanium tetrachloride aqueous solution in step S1 is 2.5 to 4.2mol/L in terms of titanium dioxide.
4. The method for preparing and storing titanium tetrachloride seed crystals as claimed in claim 1, wherein the concentration of the seed crystal suspension in step S3 is 25 to 30g/L in terms of titanium dioxide, and the neutralization reaction time is 10 to 20 minutes.
5. The preparation and storage method of the titanium tetrachloride seed crystal according to claim 1, characterized in that the method adopts a seed crystal settling tank settling reaction, the seed crystal settling tank comprises a settling tank body (1), a bottom plate (3), a vent (7), a hot water inlet (8), a liquid level meter port (9), a material inlet (10) and a quick-opening manhole (11), the vent (7), the hot water inlet (8), the liquid level meter port (9), the material inlet (10) and the quick-opening manhole (11) are arranged on the upper end surface of the settling tank body (1), a turbidity meter port (15), a sampling mechanism (16) and a liquid collecting pipe (17) are sequentially arranged on one side of the outer wall of the settling tank body (1) from top to bottom, and a thermometer port (12), a manhole (13) and a discharge port (14) are sequentially arranged on the other side of the outer wall of the settling tank body (1) from top to, the improved settling tank is characterized in that a slope (5) is arranged at the bottom of the inner side of the settling tank body (1), a tile lining (6) is laid at the upper end of the slope (5), a driving shaft (21) is vertically arranged at the center of the upper end of the settling tank body (1), the lower end of the driving shaft (21) is connected with a stirring shaft (18) through a coupling (20), a stirring wheel (19) is arranged at the bottom of the stirring shaft (18), a first driving wheel (23) is sleeved on the outer wall of the upper end of the driving shaft (21), the first driving wheel (23) is connected with a second driving wheel (25) through a driving belt (24), the second driving wheel (25) is connected with a driving motor (26) through a rotating shaft, a plurality of reinforcing rods (34) are uniformly arranged on the circumferential side wall of the stirring shaft (18) in a surrounding manner, and a baffle, one side of the baffle (29) facing the inner wall of the settling tank body (1) is provided with a plurality of groups of scrapers (30) at equal intervals, and the scrapers (30) are attached to the inner wall of the settling tank body (1).
6. The method for preparing and storing the titanium tetrachloride seed crystal according to claim 5, wherein the sampling mechanism (16) comprises a sampling tube (161), a sealing cover (162), a flange (163) and a sampling port (164), the sampling tube (161) is horizontally arranged on the side wall of the settling tank body (1), the sealing cover (162) and the flange (163) are connected through bolts, the sampling port (164) extends into the settling tank body (1), the opening of the sampling port (164) is a bevel opening, and an upper opening and a lower opening of the sampling port (164) form an angle of 45 degrees.
7. The method for preparing and storing titanium tetrachloride seed crystals as claimed in claim 5, wherein a turbidimeter is installed in the turbidimeter port (15), and the turbidimeter port (15) is installed at a position higher than the upper opening of the liquid collecting pipe (17).
8. The method for preparing and storing the titanium tetrachloride seed crystal according to claim 5, wherein the inner wall of the settling tank body (1) is provided with a layer of rubber lining (2), the bottom of the settling tank body (1) is provided with a bottom plate (3), and the bottoms of the bottom plate (3) are provided with tank bottom I-shaped steels (4) at equal intervals.
9. The method for preparing and storing the titanium tetrachloride seed crystal according to claim 5, wherein a water pipeline (22) is vertically arranged on the inner wall of the driving shaft (21), a plurality of communicating pipes (33) are uniformly communicated with the bottom of the water pipeline (22), a spray pipe (32) is communicated with the end part of each communicating pipe (33), the spray pipe (32) extends into the baffle plate (29), a plurality of flushing nozzles (31) are uniformly distributed on one side of the outer wall of each spray pipe (32), and the flushing nozzles (31) are vertically distributed along the spray pipes (32).
10. The method for preparing and storing the titanium tetrachloride seed crystal according to claim 9, wherein a water inlet pipe (27) is vertically inserted into an upper port of the water pipeline (22), and a bearing (28) is sleeved on an outer wall of a joint of the water inlet pipe (27) and the water pipeline (22).
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Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB554683A (en) * | 1941-10-13 | 1943-07-15 | Cornelis Joannes Hugo Penning | Improvements in or relating to apparatus for the removal of matter in suspension from liquids by settlement or subsidence |
| DE1467319A1 (en) * | 1963-05-20 | 1969-05-08 | Dow Chemical Co | Titanium dioxide pigment and process for its manufacture |
| GB9512960D0 (en) * | 1994-07-13 | 1995-08-30 | Tioxide Group Services Ltd | Production of rutile titanium dioxide |
| CN101698505A (en) * | 2009-11-06 | 2010-04-28 | 攀钢集团研究院有限公司 | Method for preparing additional hydrolyzing seed crystal |
| CN101863510A (en) * | 2010-06-18 | 2010-10-20 | 攀钢集团钢铁钒钛股份有限公司 | Method for preparing titanium dioxide hydrolysis crystal seed |
| CN102432066A (en) * | 2011-09-29 | 2012-05-02 | 攀钢集团攀枝花钢铁研究院有限公司 | Method for preparing titanium tetrachloride hydrolyzed crystal seed |
| CN104129813A (en) * | 2014-07-31 | 2014-11-05 | 四川龙蟒钛业股份有限公司 | Method of using TiCl4 to prepare high-activity double-effect crystal seed and control titanium dioxide particle size |
| CN206103432U (en) * | 2016-08-11 | 2017-04-19 | 贵州开磷集团股份有限公司 | Degradable hangs down device that subsides of phosphoric acid by wet process solid content |
| CN206632051U (en) * | 2017-02-13 | 2017-11-14 | 人良生物科技（上海）有限公司 | A kind of polydextrose agitator tank with automatically and manually cleaning function |
-
2021
- 2021-02-22 CN CN202110199235.8A patent/CN112939071A/en active Pending
Patent Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB554683A (en) * | 1941-10-13 | 1943-07-15 | Cornelis Joannes Hugo Penning | Improvements in or relating to apparatus for the removal of matter in suspension from liquids by settlement or subsidence |
| DE1467319A1 (en) * | 1963-05-20 | 1969-05-08 | Dow Chemical Co | Titanium dioxide pigment and process for its manufacture |
| GB9512960D0 (en) * | 1994-07-13 | 1995-08-30 | Tioxide Group Services Ltd | Production of rutile titanium dioxide |
| CN101698505A (en) * | 2009-11-06 | 2010-04-28 | 攀钢集团研究院有限公司 | Method for preparing additional hydrolyzing seed crystal |
| CN101863510A (en) * | 2010-06-18 | 2010-10-20 | 攀钢集团钢铁钒钛股份有限公司 | Method for preparing titanium dioxide hydrolysis crystal seed |
| CN102432066A (en) * | 2011-09-29 | 2012-05-02 | 攀钢集团攀枝花钢铁研究院有限公司 | Method for preparing titanium tetrachloride hydrolyzed crystal seed |
| CN104129813A (en) * | 2014-07-31 | 2014-11-05 | 四川龙蟒钛业股份有限公司 | Method of using TiCl4 to prepare high-activity double-effect crystal seed and control titanium dioxide particle size |
| CN206103432U (en) * | 2016-08-11 | 2017-04-19 | 贵州开磷集团股份有限公司 | Degradable hangs down device that subsides of phosphoric acid by wet process solid content |
| CN206632051U (en) * | 2017-02-13 | 2017-11-14 | 人良生物科技（上海）有限公司 | A kind of polydextrose agitator tank with automatically and manually cleaning function |
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Application publication date: 20210611 |