CN107935038A - The preparation process of plastic color master grain special titanium pigment - Google Patents
The preparation process of plastic color master grain special titanium pigment Download PDFInfo
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Abstract
A kind of preparation process of Masterbatch special titanium pigment, has following characteristics：1st, raw ore crushes, 2, acidolysis, 3, leaching, 4, reduction, 5, sedimentation, 6, the concentration of titanium liquid, 7, hydrolysis, 8, washing and bleaching, 9, salt treatment, 10, filtering, calcining, surface treatment, 11, dry, dedusting.
Description
Technical field
The invention belongs to field of titanium dioxide production, and in particular to manufacture the preparation work of the Masterbatch special titanium pigment of plastics
Skill.
Background technology
Titanium dioxide scientific name titanium dioxide (TiO2), mainly there are two kinds of crystal forms of rutile-type and anatase titanium dioxide.Since it is with excellent
The advantages that whiteness more, tinting strength, tinting power, covering power, the refraction index highest in all Chinese whites, it is considered to be best one kind
Chinese white, therefore it is widely used in the industries such as coating, plastics, printing and rubber.Second large user of the plastics as titanium dioxide,
In addition to using its high covering power, high coloring power and other pigment performances, it can also improve the heat-resisting, resistance to of plastic products
Light, weatherability.Titanium dioxide for producing color master batch is located at the core layer of Masterbatch, therefore to whiteness, dispersiveness, covering power, processes moment of torsion
The requirements such as energy are higher, and the titanium dioxide that traditional handicraft obtains often is difficult to reach above-mentioned requirements, therefore how to improve existing process
Asked with obtaining more preferable whiteness higher, dispersiveness, covering power, processing the stronger titanium dioxide product of moment of torsion as the technology for being badly in need of solving
Topic.
The content of the invention
For above-mentioned technical problem of the prior art, the present invention provides a kind of work of modified method for producing gtitanium dioxide with sulphuric acid
Skill, and more preferable a kind of whiteness higher, dispersiveness, covering power, the processing stronger titanium dioxide product of moment of torsion are provided, it can expire well
Particular/special requirement of the sufficient plastic industry particularly ABS plastic to titanium dioxide performance.
The processing step that it is prepared is specific as follows：1st, raw ore crushes, and 2, acidolysis, 3, leaching, 4, reduction, 5, sedimentation, 6, titanium
The concentration of liquid, 7, hydrolysis, 8, washing and bleaching, 9, salt treatment, 10, filtering, calcining, surface treatment, 11, dry, dedusting.
1) raw ore crushes：
Raw ore selection needs to meet certain Ti content, and preferably (all mass percents are with TiO for Ti contents2Meter) 40
~50%, it is desirable to which titanium component is acid-soluble to get well, i.e., rutile content is low in ilmenite, preferably≤3%, while requires ilmenite
In ferrous iron meet >=94% with high Fe content, high Fe content should be less than 13%, and Cr, Co isocolloid property impurity content are low,
It is preferred that≤3%.It is relatively crude and uneven by the selected general particle of menaccanite, it is not easy to react and react with sulfuric acid
Completely, in order to improve acidolysis rate, it is necessary to be crushed to it, preferable raw ore is crushed to fineness by horizontal ball mill is
320 mesh, and residue on sieve≤3.5%, then the miberal powder crushed is sent to acidolysis pot in batches with impulse pneumatic conveying pump.
2) acidolysis：
In acidolysis pot, under strong compression air stirring, the sulfuric acid that concentration is 93~95% is first put into, is then put into again
Miberal powder, controls sour ore deposit than 1.52~1.55, after miberal powder adds, the stronger compressed air of use, and mixing homogenizing 8~15 minutes, preferably
10~12 minutes, miberal powder is sufficiently mixed with sulfuric acid, after stirring homogenizing, acidolysis pot lid closing and fixation, prevent
Only pot cover is dug in main reaction, and dilution water is added into acidolysis pot, and the addition time does not exceed 5 minutes generally, and preferably more than 3
Minute, about stirring 5~trigger main reaction after ten minutes, while main reaction warning lamp is opened, acid hydrolysis tail gas spray pump is opened, it is main
After reaction, tail gas spray pump is closed, compressed air is turned down and is cured, the curing time was controlled at 20~45 minutes, preferably
25~35 minutes, while be passed through steam and be directly warmed to 80 DEG C~100 DEG C, it is smoothed out acidolysis reaction.
3) leach
After curing, big compressed air valve is opened, logical compressed air helps cold for 25~30 minutes, adds about 3000ml and gives up
Acid, adds thereafter enough water, controls addition speed, and it is 30~40 minutes to make whole process, titanium liquid temperature after leaching
Spend for 60~75 DEG C, when leaching need to control leaching volume, and add water once to fill up, generally should not moisturizing among leaching.
After leaching water adds, compressed air stirring is continuing with, solid formation is constantly dissolved, with the continuous dissolving of solid formation, operation
Personnel will be every 20 minutes proportions for surveying a solution, temperature, and the temperature for keeping solution is 65~75 DEG C, about adds water 60 and divides
Zhong Hou, solution temperature in increase, do not illustrate that solid formation dissolves completely substantially, the ultimate density of solution should generally contain at this time
TiO2120~135g/l, gravity are about 48~51, and F values (ratio of effective acid and total Ti content) control of leachate exists
1.85~2.05, leaching time be generally 5~12 it is small when.
4) reduce
When carrying out restoring operation, solution temperature is necessary≤65 DEG C just allow to add iron powder, when reduced iron powder should control addition
Between at 25 minutes or so, first 15 minutes are quicker, and latter 10 minutes are slow, and solution reaction maximum temperature does not exceed 75 DEG C, together
When, starting reduction phase, compressed air require control 0.8NM3/ minute, so as to prevent titanous oxidation soon and emit a pot phenomenon
Occur, it is 1.5~3.0g/l that trivalent Ti content should be kept in reducing solution.
5) settle
Insoluble impurities in titanium liquid, particularly colloid are removed in the purpose of sedimentation.When detecting in above-mentioned reduction liquid
Titanous can add to dissolve and measure sedimentation agent in 3g/l or so, and the sedimentation agent is the Sb of 1~1.5kg/L2O3Hydrochloric acid
Solution, adds 1~2kg/L ferrous sulfides, adds the time control of sedimentation agent at 5~8 minutes, compression is opened in adition process
Air, makes configuration solution, ferrous sulfide uniformly be mixed with titanium liquid, and settlement treatment ensures at 2 more than hour.
Lower workshop section's vacuum crystallization is pumped through settling obtained clear liquid, lower sections of residue also contains a certain amount of titanium liquid,
Filtered with filter press, filtrate recycling, (butt contains TiO to residue240~50%, containing Fe10~25%) general discarded, also can reuse
Part.6) concentration of titanium liquid
In order to which the particle of the hydrated titanium dioxide obtained after hydrolyzing is thin and uniformly needs the concentration by titanium liquid to bring up to dioxy
Change Ti content in more than 190g/l, the concentration of titanium liquid use vacuum film inspissator continuous concentration, controls vacuum in 0.09MPa,
50~55 DEG C of titanium liquid temperature degree.
7) hydrolyze
The purpose of hydrolysis is to obtain metatitanic acid, its basic process includes forming nucleus of crystal, and the growth of nucleus is with sinking
The change of the formation in shallow lake, metatitanic acid particle coacervation precipitation and solution composition.Need to add anatase titanium dioxide crystal seed in hydrolytic process.
It is as follows to hydrolyze concrete technology：
7.1) the titanium liquid prepared by technological requirement is measured and squeezes into hydrolysis foreheater and crystal seed titanium liquid bath respectively, work as liquid level
When reaching agitating paddle, that is, foreheater stirring is opened, the ammonium hydroxide for preparing concentration is measured to throw crystal seed ammonia vessel into spare；
7.2) after having broken material, crystal seed to be added is waited.Start crystal seed and make groove stirring, open ammonia vessel baiting valve ammonium hydroxide is quick
Put crystal seed into and make groove, and, used during then opening crystal seed titanium liquid bath baiting valve makes crystal seed titanium liquid and ammonium hydroxide in crystal seed making groove
The ammonium hydroxide that mass percent concentration is 18~20% neutralizes, to pH value 9~10, when N-process holding 1 is small, and side stirring, Bian Zhong
With.Material is warming up to 90 DEG C after the completion of neutralization, 1 DEG C/min of heating rate, when insulation 1 is small.75 DEG C are subsequently cooled to, quick inspection
Its stability is surveyed, crystal seed is quickly opened when stability is in 90ml and makes groove outlet valve, the crystal seed made quickly is put into pre-
Heat is in 96 DEG C of foreheater titanium liquid；Have to allow the titanium liquid of foreheater to be warming up to 96 DEG C waits crystal seed to carry out again, must not allow crystalline substance
Kind make and to wait titanium liquid to heat up, otherwise crystal seed stability can drastically decline, and influence whole pot quality.
7.3) stirred 10 minutes after adding crystal seed, open hydrolyzer inlet valve, foreheater baiting valve is opened, foreheater
Titanium liquid is put into hydrolyzer, while starts hydrolyzer stirring.
7.4) after foreheater titanium liquid is put into hydrolyzer, hydrolyzer live (open) steam inlet valve is opened, starts hydrolysis heating.
7.5) after Hydrolysis of Titanium liquid once seethes with excitement, from time requirement≤28 minute for being warming up to boiling, turn steam down, prevented
Cross boiling；When hydrolysis, which reaches 1: 1, turns white, stop steam, stop stirring insulation 30 minutes.
7.6) insulation terminates, then opens stirring and steam progress secondary temperature elevation, and allows Hydrolysis of Titanium liquid to reach two in 20 minutes
Secondary boiling.
7.7) rinse the foreheater of titanium liquid well and crystal seed makes pot, its flushing liquor is discharged into hydrolyzer when dilution water use, punching
Wash to finish and close valve.
7.8) turn down live (open) steam valve and keep slight boiling condition, keep pot inner pressure in 90~120mmH2O, 150 minutes.
7.9) pressurize terminates, and opens the exhaust-valve of hydrolyzer, adds quantitative dilution water, concentration is reduced to 140~
Between 155g/l, add volume 13.5m after water3, it is continuously heating to seethe with excitement, keeps slightly boiling 50 minutes.
7.10) hydrolysis terminates, steam off valve.
7.11) quantitative lignocellulosic is added toward the metatitanic acid after hydrolysis, and stirring 10 minutes can blowing.
7.12) open the bottom of a pan baiting valve and metatitanic acid after hydrolysis is sent to cooling system.
7.13) after blowing, rinse hydrolyzer inner wall to no plain boiled water well and flow out.
8) wash and bleach
The hydrated titanium dioxide slurry that titanium sulfate solution hydrolyzes contains the impurity such as a large amount of free sulfuric acids and ferrous sulfate,
The height of these impurity ion contents directly affects the form and aspect of finished titanium dioxide.Therefore need to its further washing and drift
In vain.
9) salt treatment
Salt treatment process step is specific as follows：1st step, meta-titanium acid solution after bleaching adds 3~6%, preferably 4~
5% calcining rutilization nuclei；2nd step, adds ZnO, addition 0.05~0.25%, preferably 0.10%, are stirred after addition
30 minutes.Add NH4H2PO4Powder 0.5~0.7%, preferably 0.55~0.65%, after stirring 10~15 minutes, preferably 12 points
Clock, adds KOH solution 0.85~1.1%, preferably 0.9~1.0%, is eventually adding Al2(SO4)3Powder 0.1~0.8%, it is excellent
0.2~0.5% is selected, is then stirred for 100~160 minutes, preferably 150 minutes.With being pumped into kiln tail storage tank.
But above-mentioned five classes material additional proportion needs stringent control, rutilization nuclei and zinc salt, ammonium salt, sylvite and
Mass ratio between aluminium salt needs to meet following relation, wherein each salt is all with oxidation material gauge, crystal seeds of rutile：ZnO∶
P2O5∶K2O∶Al2O3Mass percent should control in (9~18): 1: (1~2): (1.3~2.5): (1~8).
Wherein, the above-mentioned specific preparation method of salt treatment rutilization nuclei is as follows：
A. the preparation of positive sodium titanate：TiO of the filter press filtration washing qualification iron content less than 50ppm is washed through two2Hydrate,
Be pumped into metatitanic acid heating measuring tank, NaOH through alkali heating measuring tank metering after be heated separately to 60 DEG C and 90 DEG C after, will
TiO2Hydrate NaOH and being put into alkali fusion tank carries out reaction and 50%NaOH solution reactions, generates positive sodium titanate.After cooling
With pump squeeze into filter press by upper piece, washing, discharging, filter cake mashing, positive sodium titanate from containing a large amount of free NaOH solution
Separated in filtrate, 15%NaOH filtrates flow into ammonium hydroxide collecting tank, then are used as tail gas with pumping external system and spray.Use filter press
The NaOH in positive sodium titanate filter cake is washed, after measurement filtrate NaOH content is less than 1500ppm, discharging enters hollander tub, Ran Houzai
Be neutralized to pH value in 3.5~4.0 scopes with 10% hydrochloric acid, with pump squeeze into filter press again by upper piece, washing, until washing filtrate
When pH value is more than 7, discharging, filter cake mashing, are made TiO2Concentration control is in 200~220g/l, the positive metatitanic acid prepared for crystal seed
Intermediate products.B. prepared by crystal seed：The positive sodium titanate of step A and 30% hydrochloric acid reaction generation rutile type calcining seeds, system
The crystal seed performed is squeezed into storage tank with pump.
10) filter, calcine, surface treatment
Metatitanic acid mixture after salt treatment passes through filtration treatment, is then fed into calcined by rotary kiln, calcining heat control
System is at 800~980 DEG C, preferably 850~900 DEG C.Add the kaolin powder and Al that particle diameter is 1.5~2.5 μm2O3Powder one
Rise and carry out general inorganic clad surface processing.
11) dry, dedusting
11.1) washed again, when wash time holding 1 is small, washing terminal ensures that filter cake sulfur content is less than 0.3%.
11.2) filter cake by washing after qualified, is beaten, it is 300g/ to control concentration of slurry with 300,000 Ω cm deionized waters
L, then press dry through filter press, controls cake moisture up to 50%.
11.3) after taking off cake, filter cake is delivered to expansion drying host, while hot-air is inputted into expansion drying host,
Filter cake is kept to reach 95 DEG C with temperature after hot air.High speed agitator is set in expansion drying machine host bottom, by filter cake
Break up rapidly, under stream of hot air and air-introduced machine collective effect, material was risen very rapidly up to do in 3~5 seconds by drier bottom
It is oven-dried during at the top of dry device.Top sets cyclone classifier, and unqualified material is returned expansion drying motor spindle again
Drying；Qualified material drying is pumped into pulse dust collector by air-introduced machine and is attached to filter bag of dust collector surface, is shaken by electromagnetism
The impact of device and compressed air stream is played, material is fallen into pulse dust collector bottom, passes through auger conveyor and star discharge valve
Storage bin is collected into, up to high-specific surface area titanium dioxide product after micron disintegrator crushes.
Technique effect：
1. above-mentioned preparation method is by the stringent control of each step parameter to whole titanium white powder preparation technique, so as to have
Effect improves titanium dioxide performance：
2nd, the present invention adds the new salt treatment agent for being mixed with crystal seed, and the colour killing of product can be improved by adding rutilization nuclei
Power, when improving calcining titanium dioxide primary particle shape, make particle is round and smooth regular, soft to be easy to crush；Zinc salt is very strong
Rutile-type accelerating agent.Addition zinc salt can improve the weatherability and anti-grinded hardness index of product, sylvite be rutile type titanium white not
The crystal stabilization that can or lack.It can suppress the conversion rate of rutile-type using sylvite, desulfurization temperature is calcined in reduction, avoids grain
Son sintering grows up, improves pigment performance, improves reducing power.It can also be neutralized during salt treatment using ammonium dihydrogen phosphate in metatitanic acid
Free acid, makes product reach neutral in calcining, reacts the CO of generation2And H2O can make product loose when volatilizing, and can improve product
Whiteness.And add aluminum sulfate and be then conducive to the decomposition of sulfide and the reduction of rutile crystal type conversion origin temp.
3rd, the salt treatment agent used in the present invention is the compound prescription of a variety of different type inorganic agents, therefore its proportioning is main
Key technology, if for example, individually add zinc salt, since grain growth is too fast, be easy to cause sintering and reduces the pigment of product
Performance, causes that the phase yellowing of product bottom, particle are hardened, dispersion performance declines.Excessive aluminum sulfate is added, titanium white first product whiteness is easy
Reduce.Crystal seed usage amount is more, although conversion rate is fast, can increase production cost, the excessively few then metatitanic acid of dosage is difficult short
Rutile-type is completely converted into time；And sylvite crosses the conversion that can at most influence crystal form.And the proportioning of the present invention, except that can have
Effect reduces calcining heat, and can cause
4th, final products of the present invention possess following superperformance：
Titanium dioxide TiO2Content range is 95~97%, and wherein rutile content is not less than 99.7%；S constituent contents
No more than 3ppm；
350~370m of specific surface area2/g；Aggregated particle size D50For 0.10~0.20 μm；Aggregated particle size D90≤0.5μm；
Fugitive constituent (105 DEG C, 2h)≤1.5%；Calcination loss (600 DEG C of calcination 1h of sample after 105 DEG C of 2h drying)≤8%；
Water slurry pH value 6.5~7.5；Water absorption (30~35) g/50g；45 μm of residue on sieve≤0.04%；Oil absorption 23
~25 (g/100g)；Fe2O3≤ 0.005%；(K2O+Na2O)≤0.008%.
Color CIE performances：
Brightness L*：98.5~98.8；Tone a*：(0.9~1.0)；Tone b*：1.4~1.5
Embodiment
The present invention will be described in detail by the specific embodiment of following exemplary, but the spirit and right of the present invention will
The protection domain of book is sought from the restriction of these specific embodiments.
Embodiment 1
7) hydrolyze
The purpose of hydrolysis is to obtain metatitanic acid, its basic process includes forming nucleus of crystal, and the growth of nucleus is with sinking
The change of the formation in shallow lake, metatitanic acid particle coacervation precipitation and solution composition.Need to add anatase titanium dioxide crystal seed in hydrolytic process.
It is as follows to hydrolyze concrete technology：
7.1) the titanium liquid prepared by technological requirement is measured and squeezes into hydrolysis foreheater and crystal seed titanium liquid bath respectively, work as liquid level
When reaching agitating paddle, that is, foreheater stirring is opened, the ammonium hydroxide for preparing concentration is measured to throw crystal seed ammonia vessel into spare；
7.2) after having broken material, crystal seed to be added is waited.Start crystal seed and make groove stirring, open ammonia vessel baiting valve ammonium hydroxide is quick
Put crystal seed into and make groove, and, used during then opening crystal seed titanium liquid bath baiting valve makes crystal seed titanium liquid and ammonium hydroxide in crystal seed making groove
The ammonium hydroxide that mass percent concentration is 20% neutralizes, and to pH value 9.5, when N-process holding 1 is small, side stirring, side neutralizes.Neutralize
After the completion of material be warming up to 90 DEG C, 1 DEG C/min of heating rate, when insulation 1 is small.75 DEG C are subsequently cooled to, quickly detects its stabilization
Property, crystal seed is quickly opened when stability is in 90ml and makes groove outlet valve, the crystal seed made quickly is put into and is preheating to 96 DEG C
Foreheater titanium liquid in；Have to allow the titanium liquid of foreheater to be warming up to 96 DEG C waits crystal seed to carry out again, crystal seed must not be allowed to make
Titanium liquid heats up, and otherwise crystal seed stability can drastically decline, and influence whole pot quality.
9) salt treatment
Salt treatment process step is specific as follows：1st step, the meta-titanium acid solution after bleaching add 4% calcining rutile
Type crystal seed；2nd step, adds ZnO, addition 0.10%, is stirred 30 minutes after addition.Add NH4H2PO4Powder 0.65%, is stirred
Mix 12 minutes, add KOH solution 1.0%, be eventually adding Al2(SO4)3Powder 0.5%, is then stirred for 150 minutes.With pump
It is sent into kiln tail storage tank.Mass ratio between rutilization nuclei and zinc salt, ammonium salt, sylvite and aluminium salt needs to meet such as ShiShimonoseki
System, wherein each salt is all with oxidation material gauge, crystal seeds of rutile：ZnO∶P2O5∶K2O∶Al2O3Mass percent should control
9: 1: 1: 1.3: 1.
Embodiment 2
7) hydrolyze
The purpose of hydrolysis is to obtain metatitanic acid, its basic process includes forming nucleus of crystal, and the growth of nucleus is with sinking
The change of the formation in shallow lake, metatitanic acid particle coacervation precipitation and solution composition.Need to add anatase titanium dioxide crystal seed in hydrolytic process.
It is as follows to hydrolyze concrete technology：
7.1) the titanium liquid prepared by technological requirement is measured and squeezes into hydrolysis foreheater and crystal seed titanium liquid bath respectively, work as liquid level
When reaching agitating paddle, that is, foreheater stirring is opened, the ammonium hydroxide for preparing concentration is measured to throw crystal seed ammonia vessel into spare；
7.2) after having broken material, crystal seed to be added is waited.Start crystal seed and make groove stirring, open ammonia vessel baiting valve ammonium hydroxide is quick
Put crystal seed into and make groove, and, used during then opening crystal seed titanium liquid bath baiting valve makes crystal seed titanium liquid and ammonium hydroxide in crystal seed making groove
The ammonium hydroxide that mass percent concentration is 18% neutralizes, and to pH value 9.8, when N-process holding 1 is small, side stirring, side neutralizes.Neutralize
After the completion of material be warming up to 90 DEG C, 1 DEG C/min of heating rate, when insulation 1 is small.75 DEG C are subsequently cooled to, quickly detects its stabilization
Property, crystal seed is quickly opened when stability is in 90ml and makes groove outlet valve, the crystal seed made quickly is put into and is preheating to 96 DEG C
Foreheater titanium liquid in；Have to allow the titanium liquid of foreheater to be warming up to 96 DEG C waits crystal seed to carry out again, crystal seed must not be allowed to make
Titanium liquid heats up, and otherwise crystal seed stability can drastically decline, and influence whole pot quality.
9) salt treatment
Salt treatment process step is specific as follows：1st step, the meta-titanium acid solution after bleaching add 5% calcining rutile
Type crystal seed；2nd step, adds ZnO, addition 0.10%, is stirred 30 minutes after addition.Add NH4H2PO4Powder 0.55%, is stirred
Mix 12 minutes, add KOH solution 0.9%, be eventually adding Al2(SO4)3Powder 0.2%, is then stirred for 150 minutes.With pump
It is sent into kiln tail storage tank.Mass ratio between rutilization nuclei and zinc salt, ammonium salt, sylvite and aluminium salt needs to meet such as ShiShimonoseki
System, wherein each salt is all with oxidation material gauge, crystal seeds of rutile：ZnO∶P2O5∶K2O∶Al2O3Mass percent should control
18: 1: 2: 2.5: 8.
Embodiment described above is only that the preferred embodiment of the present invention is described, not to the model of the present invention
Enclose and be defined, on the premise of design spirit of the present invention is not departed from, those skilled in the art make technical scheme
The various modifications gone out and improvement, should all include in the protection domain that claims of the present invention determines.
Claims (5)
1. a kind of preparation process of Masterbatch special titanium pigment, has following characteristics：1st, raw ore crushes, 2, acidolysis, 3, leaching, 4,
Reduction, 5, sedimentation, 6, the concentration of titanium liquid, 7, hydrolysis, 8, washing and bleaching, 9, salt treatment, 10, filtering, calcining, surface treatment,
11st, dry, dedusting.
2. the preparation process of Masterbatch special titanium pigment as claimed in claim 1, it is characterised in that the technique of step 7 includes：
7.1) the titanium liquid prepared by technological requirement is measured and squeezes into hydrolysis foreheater and crystal seed titanium liquid bath respectively, stirred when liquid level reaches
During paddle, that is, foreheater stirring is opened, the ammonium hydroxide for preparing concentration is measured to throw crystal seed ammonia vessel into spare；7.2) after having broken material,
Etc. crystal seed to be added.Start crystal seed and make groove stirring, open ammonia vessel baiting valve and ammonium hydroxide is quickly put into crystal seed making groove, then beat
Open crystal seed titanium liquid bath baiting valve make crystal seed titanium liquid and ammonium hydroxide in crystal seed is made in groove and, with mass percent concentration for 18~
20% ammonium hydroxide neutralizes, and to pH value 9~10, when N-process holding 1 is small, side stirring, side neutralizes.Material heats up after the completion of neutralization
To 90 DEG C, 1 DEG C/min of heating rate, when insulation 1 is small.75 DEG C are subsequently cooled to, quickly detects its stability, when stability exists
Crystal seed is quickly opened during 90ml and makes groove outlet valve, the crystal seed made quickly is put into and is preheating to 96 DEG C of foreheater titanium liquid
In；Have to allow the titanium liquid of foreheater to be warming up to 96 DEG C waits crystal seed to carry out again, and crystal seed must not be allowed to make and wait titanium liquid to heat up, otherwise
Crystal seed stability can drastically decline, and influence whole pot quality.
3. the preparation process of Masterbatch special titanium pigment as claimed in claim 1, it is characterised in that the technique of step 9 includes：
Salt treatment process step is specific as follows：1st step, the meta-titanium acid solution after bleaching add 3~6%；2nd step, adds ZnO, adds
Enter amount 0.05~0.25%, stirred 30 minutes after addition；Add NH4H2PO4Powder 0.5~0.7%, is stirred 10~15 minutes
Afterwards, KOH solution 0.85~1.1% is added, is eventually adding Al2(SO4)3Powder 0.1~0.8%, is then stirred for 100~160
Minute；With being pumped into kiln tail storage tank.
4. the preparation process of Masterbatch special titanium pigment as claimed in claim 2, it is characterised in that step 9 further includes：Golden red
Stone crystal seed: ZnO: P2O5∶K2O∶Al2O3Mass percent should control in (9~18): 1: (1~2): (1.3~2.5): (1~
8)。
5. the preparation process of Masterbatch special titanium pigment as claimed in claim 3, it is characterised in that step 9 further includes：At salt
The specific preparation method of reason rutilization nuclei is as follows：A. the preparation of positive sodium titanate：Filter press filtration washing qualification iron is washed through two
Content is less than the TiO of 50ppm2Hydrate, is divided with metatitanic acid heating measuring tank, NaOH is pumped into after alkali heating measuring tank metering
After not being heated to 60 DEG C and 90 DEG C, by TiO2It is anti-with 50%NaOH solution that hydrate NaOH and being put into alkali fusion tank carries out reaction
Should, generate positive sodium titanate.After cooling with pump squeeze into filter press by upper piece, washing, discharging, filter cake mashing, positive sodium titanate
Separated from the filtrate containing a large amount of free NaOH solution, 15%NaOH filtrates flow into ammonium hydroxide collecting tank, then outer with pumping
System is used as tail gas spray.The NaOH in positive sodium titanate filter cake is washed with filter press, when measurement filtrate NaOH content is less than
After 1500ppm, discharging enters hollander tub, is then neutralized to pH value in 3.5~4.0 scopes with 10% hydrochloric acid again, press filtration is squeezed into pump
Machine again by upper piece, washing, until when washing filtrate pH value is more than 7, discharging, filter cake mashing, are made TiO2Concentration is controlled 200
~220g/l, the positive metatitanic acid intermediate products prepared for crystal seed.B. prepared by crystal seed：The positive sodium titanate of step A and 30% salt
Acid reaction generation rutile type calcining seeds, the crystal seed made are squeezed into storage tank with pump.
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| CN108946806A (en) * | 2018-09-05 | 2018-12-07 | 襄阳龙蟒钛业有限公司 | A kind of production method of high covering power titanium dioxide |
| CN110668495A (en) * | 2019-10-31 | 2020-01-10 | 襄阳龙蟒钛业有限公司 | Method for reducing acidolysis solid-phase substance in titanium dioxide production process |
| CN111422902A (en) * | 2020-03-31 | 2020-07-17 | 广西金茂钛业有限公司 | Method for preparing high-achromatism rutile titanium dioxide |
| CN113549345A (en) * | 2021-08-26 | 2021-10-26 | 苏州市宏丰钛业有限公司 | Preparation method and system of titanium dioxide for plastics |
| CN114988465A (en) * | 2022-04-22 | 2022-09-02 | 甘肃东方钛业有限公司 | Efficient recycling method for scale in acidolysis premixing tank |
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Address after: 543399 Tengxian Chemical Industry Zone, Wuzhou City, Guangxi Zhuang Autonomous Region Patentee after: Guangxi Jinmao Titanium Industry Co.,Ltd. Address before: 543300 Teng County Industrial Zone, Wuzhou City, Guangxi Patentee before: GUANGXI JINMAO TITANIUM Co.,Ltd. |
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Denomination of invention: Preparation process of titanium dioxide powder for plastic color masterbatch Effective date of registration: 20230822 Granted publication date: 20200529 Pledgee: Tengxian Rural Credit Cooperative Association Pledgor: Guangxi Jinmao Titanium Industry Co.,Ltd. Registration number: Y2023980053145 |