CN106082319A - A kind of preparation method of sulfuric acid method titanium pigment production mixed crystal type double-effect seed crystal - Google Patents
A kind of preparation method of sulfuric acid method titanium pigment production mixed crystal type double-effect seed crystal Download PDFInfo
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- CN106082319A CN106082319A CN201610425082.3A CN201610425082A CN106082319A CN 106082319 A CN106082319 A CN 106082319A CN 201610425082 A CN201610425082 A CN 201610425082A CN 106082319 A CN106082319 A CN 106082319A
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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
- C01G23/0532—Producing by wet processes, e.g. hydrolysing titanium salts by hydrolysing sulfate-containing salts
- C01G23/0534—Producing by wet processes, e.g. hydrolysing titanium salts by hydrolysing sulfate-containing salts in the presence of seeds
Abstract
The present invention relates to the preparation method of a kind of sulfuric acid method titanium pigment production mixed crystal type double-effect seed crystal, the method comprises the following steps: alkali is molten, washing, the steps such as acid is molten, cooling.The molten reaction of alkali is that to carry out alkali with the alkali-titanium ratio of 3:1～5:1 molten；The molten reaction of acid is the hydrochloric acid of addition 0.5～1.0 times, 10～60min are dissolved at 85～95 DEG C, pole is cooled to less than 50 DEG C, obtains the double-effect seed crystal of nanoscale, mixed crystal type, and crystal seed prepared by the present invention only need to add when hydrolysis, calcining is without adding calcining seeds, save the preparation section of calcining seeds, it is achieved hydrolysis calcining seeds preparation once completes, it is to avoid the loaded down with trivial details technique that hydrolysis crystal seed and calcining seeds are prepared respectively, and cost-effective, improve product quality.
Description
Technical field
The present invention relates to a kind of sulfuric acid method titanium pigment production mixed crystal type double-effect seed crystal preparation method, particularly relate to one and receive
Meter level mixed crystal type double-effect seed crystal preparation method.
Background technology
In sulfuric acid method titanium pigment production process, relating to two class crystal seeds, hydrolysis crystal seed and calcining seeds, because of its nature and characteristic
Difference play different effect, thus its preparation technology also differs a lot of.
General hydrolysis crystal seed Main Function is the nucleus being hydrolyzed to metatitanic acid as sulphuric acid (oxygen) titanium, promotes fast hydrolyzing,
Improving hydrolysis productivity, and improve pigment performance, therefore seed particles is little, degree of crystallization is low.Its shape document is introduced and has two kinds, one
Planting is needle-like, and a length of 10～20nm, width is 5～10nm, and one is spherical, and mean diameter is 2～8nm；Calcining seeds master
Effect is to lure that metatitanic acid is converted into rutile into, reduces calcining heat, improves pigment performance, and its particle diameter is big, and degree of crystallization is high, its shape
Shape is Folium Salicis Babylonicae shape, and mean diameter is 40～100nm.
Additional hydrolyzing seed crystal technique has two classes: a class uses wide, directly utilizes titanium white production intermediate product dense
Titanium liquid or clear titanium liquid (or claiming titanyl sulfate) are prepared in alkali and crystal seed (or ammonia neutralization), such as patent CN1834019A,
CN85103475A, this kind of crystal seed is anatase titanium dioxide, and crystal outward appearance is transparent absinthe-green nanometer colloid, does not have calcining activity, forges
Burning need to additionally add calcining seeds.The another kind of crystal seed that titanium tetrachloride is raw material being to use outsourcing, is also in the world at present
New plus seed technique, this kind of crystal seed can be prepared as rutile-type and mixed crystal type nanometer two kinds, such as patent
CN101698505A announce for rutile-type hydrolysis crystal seed, GB2291052 announce for mixed crystal type nanometer hydrolysis crystal seed, two classes
Crystal seed has high hydrolysing activity, it may have necessarily calcine activity, but existing is harmful influence, transport, store, use in danger
Greatly, and need outsourcing, expensive, and it is easily subject to the influence of fluctuations of the market supply and demand, limit it and the most extensively apply.
Calcining seeds technique is essentially identical, and the intermediate metatitanic acid using titanium white production is raw material, carries out that alkali is molten, washes
Wash, (neutralize, wash), the acid key step such as molten, cooling, obtain is the 98% rutile-type crystal of 80～100nm, this kind of crystalline substance
Plant and cannot be used for hydrolysis.
Double-effect seed crystal technique has document to report, domestic patent CN102390865A uses the inclined titanium of intermediate of titanium white production
Acid is raw material, and by sulfuric acid solution, sodium carbonate precipitates, twice washing, and acid is molten, cooling, and the economic benefits and social benefits obtaining nanoscale colloidal sol shape are brilliant
Kind, 2% crystal seed is added in hydrolysis, and calcining is no longer added calcining seeds, obtained the rutile titanium white lead of good quality, this technique crystal seed
Mass activity is high, but exists and consume 4～5 times of sulphuric acid and a large amount of sodium carbonate, it is impossible to reclaiming, high expensive, crystal seed preparation flow is inclined
Problem long, that quality is unstable, and there is no industrialization promotion.
Also domestic patent CN1415548A is had to describe a kind of SnO2+TiO2Double-effect seed crystal, containing SnO in crystal seed2, because becoming
Basis and technical problem, it is impossible to put into reality application.Patent CN101565201A was reported, used the gold that calcining seeds technique obtains
Red stone content is 90～98% suspension crystal seed, referred to as double-effect seed crystal, but the most concrete hydrolysis and calcining activity experiment number
It is said that bright, only give the rutile content analysis result of this crystal seed, if for real double-effect seed crystal, need to be investigated.
Summary of the invention
It is an object of the invention to overcome defect present in prior art, it is provided that a kind of sulfuric acid method titanium pigment produces with mixed
The preparation method of crystal formation double-effect seed crystal.
For achieving the above object, the technical scheme is that
A kind of preparation method of sulfuric acid method titanium pigment production mixed crystal type double-effect seed crystal, including following step:
A, alkali are molten: will through bleaching pretreatment metatitanic acid making beating, add solid base, be warming up to boiling, protect boiling 2.5～
3h, cools down ＜ 50 DEG C；
B, washing: the molten slip of alkali that will be cooled to less than 50 DEG C filters, in room temperature desalted water washing to filtrate wash water
Alkali content≤2g/L；
C, acid are molten: by qualified for washing alkali molten cake making beating, and it is molten to add hydrochloric acid acid, and controlling hydrochloric acid addition is metatitanic acid quality
0.5～1.0 times, acid solubility temperature 85～～95 DEG C, the time 10～60min, obtain crystal seed；
D, cooling: rapidly join isopyknic cold water in the crystal seed after acid cementing bundle, be chilled to less than 50 DEG C.
In described step A, metatitanic acid beating consistency controls more than 10%, and solid base with the mass ratio of metatitanic acid is: 3:1
～5:1.Described solid base is selected from any one in sodium hydroxide, potassium hydroxide, sodium carbonate, potassium carbonate.
The concentration of alkali and metatitanic acid and mass ratio, determine alkali molten time boiling temperature, also determine metatitanic acid depolymerization effect,
Determine the quality of crystal seed the most at last.Because alkali is on the low side with metatitanic acid concentration and mass ratio, when alkali is molten, boiling point is low, and metatitanic acid depolymerization is not
Thoroughly, alkali is higher with metatitanic acid concentration and mass ratio, causes aqueous slkali viscosity big, and poor fluidity is heated uneven, also will impact
The molten effect of alkali.In general calcining seeds technique, alkali-titanium ratio is between 1.2～2.5, and alkali is the liquid base of more than 40%, alkali and inclined titanium
After acid preheats, metatitanic acid is added directly in the alkali of heat, needs steam that metatitanic acid and alkali liquor are preheated, alkali molten boiling temperature
Below 110 DEG C, there are two kinds of reactions, obtain two kinds of titanates, TiO in degree2+ 2NaOH=Na2TiO3+H2O and TiO2+ 4NaOH=
Na4TiO4+2H2O, obtain is meta-titanium perborate and positive sodium titanate, hydrolysis exist two kinds of acid, metatitanic acid and positive metatitanic acid, molten with acid after
System is that suspension matches.The present invention uses the alkali of 3～5 times to react with metatitanic acid, TiO2+ 4NaOH=Na4TiO4+2H2O,
The molten boiling temperature of alkali more than 120 DEG C, it is ensured that all positive sodium titanates of titanate obtained, all positive metatitanic acids after hydrolysis.
Washing described in step B, when the molten suspension of alkali carries out filtration washing, leading portion filtrate is recyclable, for the molten inclined titanium of alkali
Acid making beating, reduces the consumption of alkali, uses room temperature desalted water to wash to alkali content≤2g/L in filtrate, mainly control filter during washing
Alkali content in cake, reduce sour molten time consume hydrochloric acid, use room temperature desalted water washing, change conventional calcination crystal seed process heat washing
Washing, one is steam saving heat, and two is that to prevent titanate pyrohydrolysis be metatitanic acid, affects crystal seed quality.
In described step C, acid is molten: the molten cake of described alkali is pulled an oar 50～200g/L, and hydrochloric acid dosage is metatitanic acid quality
0.5～1.0 times, temperature controls at 85～95 DEG C, the time 10～60min.
In described step D, add cold water after acid is molten and be chilled to 50 DEG C, change temperature and the acidity of crystal seed, prevent crystal seed from continuing
Ripening is grown up.
Advantages of the present invention and having the beneficial effects that:
1. the present invention change traditional crystal seed individually separate preparation section, save preparation technology, once complete hydrolysis
Preparation with calcining seeds, it is to avoid the trouble of outsourcing seed production raw material, reduce production to city's field dependence, Bu Shou city
Field influence of fluctuations；
2. the present invention is by reasonably controlling the condition in technique, and the crystal seed of preparation is nanoscale double-effect seed crystal, no matter water
Solve or calcining all has the highest activity, crystal seed dosage less than 2%, instead of former alkali neutralizing hydrolysis crystal seed and 4～5% forge
Burning crystal seed, percent hydrolysis is up to more than 96%, and calcining heat is low, less than in alkali and automatic growing crystal species calcining heat more than 30 DEG C, obtains
Whiteness, the more preferable product of brightness, show clear superiority；
3. the production technology of the present invention is improved on existing calcining seeds preparation technology basis, uses calcining seeds and prepares
Equipment, newly added equipment small investment, steam saving and natural gas, save production cost.
Detailed description of the invention
Below in conjunction with embodiment, the detailed description of the invention of the present invention is further described.Following example are only used for more
Add and clearly demonstrate technical scheme, and can not limit the scope of the invention with this.
Embodiment 1
By metatitanic acid bleaching to Fe≤50ppm, making beating, beating consistency is 10%, joins four-hole boiling flask, according to 5:1's
Mass ratio adds the sodium hydroxide of purity more than 94%, is warming up to boiling, protects boiling 3h, is cooled to less than 50 DEG C, filters, use room temperature
Desalted water washs to alkali content≤2g/L in filtrate；Filter cake making beating at 50g/L for concentration, adds 0.5 times of HCl, is warmed up to 85 DEG C,
Insulation 60min, adds same volume room temperature desalted water and is quickly cooled to less than 50 DEG C, i.e. obtain nanosize seeds.
Embodiment 2
By metatitanic acid bleaching to Fe≤50ppm, making beating, beating consistency is 12%, joins four-hole boiling flask, according to 4:1's
Mass ratio adds the potassium hydroxide of purity more than 94%, is warming up to boiling, protects boiling 3h, is cooled to less than 50 DEG C, filters, use room temperature
Desalted water washs to alkali content≤2g/L in filtrate；Filter cake making beating at 100g/L for concentration, adds 0.8 times of HCl, is warmed up to 90
DEG C, it is incubated 30min, adds same volume room temperature desalted water and be quickly cooled to less than 50 DEG C, i.e. obtain nanosize seeds.
Embodiment 3
By metatitanic acid bleaching to Fe≤50ppm, making beating, beating consistency is 23%, joins four-hole boiling flask, according to 3:1's
Mass ratio adds the sodium carbonate of purity more than 94%, is warming up to boiling, protects boiling 3h, is cooled to less than 50 DEG C, filter, takes off by room temperature
Saline washs to alkali content≤2g/L in filtrate；Filter cake making beating at 200g/L for concentration, adds 1.0 times of HCl, is warmed up to 95 DEG C,
Insulation 10min, adds same volume room temperature desalted water and is quickly cooled to less than 50 DEG C, i.e. obtain nanosize seeds.
| Numbering | Crystal seed forms | Crystal seed BET analyzes, m<sup>2</sup>/g |
| Example 1 | A54:R46 | 175 |
| Example 2 | A52:R48 | 183 |
| Example 3 | A53:R47 | 202 |
From the analysis result of upper table, the crystal seed obtained is the nanocrystal of mixed crystal type, and specific surface area is at 175m2/ g with
On, particle diameter is at below 5nm.
Comparative example
Use in alkali and the method for titanium liquid prepares crystal seed, obtain nanoscale light green colloidal sol shape crystal seed.
Activity of crystal seed evaluation test:
Embodiment double-effect seed crystal uses the dense titanium liquid of 200g/L, is preheating to 96 DEG C, adds aforementioned according to the amount of mass ratio 2%
Crystal seed prepared by method, hydrolyzes 3h, obtains metatitanic acid, carries out bleaching, salt treatment, and calcining, under kiln, thing pigment performance is analyzed.
Comparative example plus seed hydrolysising experiment, hydrolysis crystal seed dosage 2%, (prepared by conventional method for calcining seeds dosage 5%
, 98% rutile-type, particle diameter 80～100nm), after bleaching, using the salt treatment formula identical with embodiment, calcining, under kiln
Thing pigment performance is analyzed.Concrete activity of crystal seed evaluation result see table:
| Percent hydrolysis | Calcining heat | Brightness | Whiteness | |
| Example 1 | 96.52% | 950℃ | 94.8 | 98.2 |
| Example 2 | 96.33% | 960℃ | 94.5 | 98.1 |
| Example 3 | 96.67% | 960℃ | 94.7 | 98.2 |
| Comparative example | 96.10% | 995℃ | 94.2 | 97.7 |
Note: after crystal seed composition is by neutralization precipitation crystal seed, wash Cl-After, 100 DEG C of drying, XRD analysis.
Claims (4)
1. a sulfuric acid method titanium pigment produces by the preparation method of mixed crystal type double-effect seed crystal, it is characterised in that: include following
Step:
A, alkali are molten: by the metatitanic acid making beating through bleaching pretreatment, add solid base, are warming up to boiling, protect boiling 2.5～3h, cold
But ＜ 50 DEG C；
B, washing: the molten slip of alkali that will be cooled to less than 50 DEG C filters, the washing of room temperature desalted water contains to alkali in filtrate wash water
Amount≤2g/L；
C, acid are molten: by qualified for washing alkali molten cake making beating, and it is molten to add hydrochloric acid acid, and controlling hydrochloric acid addition is metatitanic acid quality
0.5～1.0 times, acid solubility temperature 85～～95 DEG C, the time 10～60min, obtain crystal seed；
D, cooling: rapidly join isopyknic cold water in the crystal seed after acid cementing bundle, be chilled to less than 50 DEG C.
The preparation method of a kind of sulfuric acid method titanium pigment production mixed crystal type double-effect seed crystal the most according to claim 1, it is special
Levying and be: in step A, metatitanic acid beating consistency controls more than 10%, solid base with the mass ratio of metatitanic acid is: 3:1～5:1.
The preparation method of a kind of sulfuric acid method titanium pigment production mixed crystal type double-effect seed crystal the most according to claim 1, it is special
Levy and be: the solid base described in step A is selected from any one in sodium hydroxide, potassium hydroxide, sodium carbonate, potassium carbonate.
The preparation method of a kind of sulfuric acid method titanium pigment production mixed crystal type double-effect seed crystal the most according to claim 1, it is special
Levy and be: the molten cake of alkali described in step C is pulled an oar 50～200g/L.
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106966428A (en) * | 2017-03-30 | 2017-07-21 | 四川龙蟒钛业股份有限公司 | The method that calcining seeds are prepared using alkali soluble filtrate |
| CN107010659A (en) * | 2017-04-24 | 2017-08-04 | 四川龙蟒钛业股份有限公司 | The preparation method of high activity calcining seeds |
| CN107311228A (en) * | 2017-09-06 | 2017-11-03 | 四川龙蟒钛业股份有限公司 | A kind of method for improving calcining seeds activity |
| CN107686126A (en) * | 2017-09-06 | 2018-02-13 | 四川龙蟒钛业股份有限公司 | A kind of method for reducing metatitanic acid alkali soluble phosphoric acid |
| CN109336172A (en) * | 2018-10-30 | 2019-02-15 | 攀枝花学院 | The method for preparing photocatalysis nano-titanium dioxide as raw material using metatitanic acid |
| CN111333109A (en) * | 2020-04-22 | 2020-06-26 | 龙佰四川钛业有限公司 | Method for preparing calcined crystal seeds by hydrolyzing scale |
| CN112499677A (en) * | 2020-12-17 | 2021-03-16 | 襄阳龙蟒钛业有限公司 | Method for improving activity of calcined seed crystal |
| CN113213529A (en) * | 2021-05-26 | 2021-08-06 | 攀钢集团攀枝花钢铁研究院有限公司 | Method for producing titanium dioxide by sulfuric acid process and recycling metatitanic acid in titanium dioxide waste acid |
| CN114380330A (en) * | 2021-12-28 | 2022-04-22 | 龙佰襄阳钛业有限公司 | Preparation method of high-activity calcined seed crystal |
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| CN101565201A (en) * | 2009-05-05 | 2009-10-28 | 江西添光化工有限责任公司 | Preparation of white titanium pigment double action crystal seed from metatitanic acid |
| CN102153136A (en) * | 2011-02-25 | 2011-08-17 | 四川安宁铁钛股份有限公司 | Preparation method of hydrated titanium dioxide double-effect seed crystal |
| CN102390865A (en) * | 2011-08-11 | 2012-03-28 | 四川龙蟒钛业股份有限公司 | Method for preparing high-activity double-effect seed crystals from metatitanic acid |
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2016
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| CN101565201A (en) * | 2009-05-05 | 2009-10-28 | 江西添光化工有限责任公司 | Preparation of white titanium pigment double action crystal seed from metatitanic acid |
| CN102153136A (en) * | 2011-02-25 | 2011-08-17 | 四川安宁铁钛股份有限公司 | Preparation method of hydrated titanium dioxide double-effect seed crystal |
| CN102390865A (en) * | 2011-08-11 | 2012-03-28 | 四川龙蟒钛业股份有限公司 | Method for preparing high-activity double-effect seed crystals from metatitanic acid |
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106966428A (en) * | 2017-03-30 | 2017-07-21 | 四川龙蟒钛业股份有限公司 | The method that calcining seeds are prepared using alkali soluble filtrate |
| CN107010659A (en) * | 2017-04-24 | 2017-08-04 | 四川龙蟒钛业股份有限公司 | The preparation method of high activity calcining seeds |
| CN107010659B (en) * | 2017-04-24 | 2019-03-01 | 四川龙蟒钛业股份有限公司 | The preparation method of high activity calcining seeds |
| CN107311228A (en) * | 2017-09-06 | 2017-11-03 | 四川龙蟒钛业股份有限公司 | A kind of method for improving calcining seeds activity |
| CN107686126A (en) * | 2017-09-06 | 2018-02-13 | 四川龙蟒钛业股份有限公司 | A kind of method for reducing metatitanic acid alkali soluble phosphoric acid |
| CN109336172A (en) * | 2018-10-30 | 2019-02-15 | 攀枝花学院 | The method for preparing photocatalysis nano-titanium dioxide as raw material using metatitanic acid |
| CN111333109A (en) * | 2020-04-22 | 2020-06-26 | 龙佰四川钛业有限公司 | Method for preparing calcined crystal seeds by hydrolyzing scale |
| CN112499677A (en) * | 2020-12-17 | 2021-03-16 | 襄阳龙蟒钛业有限公司 | Method for improving activity of calcined seed crystal |
| CN113213529A (en) * | 2021-05-26 | 2021-08-06 | 攀钢集团攀枝花钢铁研究院有限公司 | Method for producing titanium dioxide by sulfuric acid process and recycling metatitanic acid in titanium dioxide waste acid |
| CN114380330A (en) * | 2021-12-28 | 2022-04-22 | 龙佰襄阳钛业有限公司 | Preparation method of high-activity calcined seed crystal |
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Address after: 618200 Deyang city of Sichuan province Mianzhu new industrial zone longmang Chemical Industrial Zone Patentee after: Longbai Sichuan Titanium Co., Ltd Address before: 618200 Deyang city of Sichuan province Mianzhu new industrial zone longmang Chemical Industrial Zone Patentee before: SICHUAN LOMON TITANIUM Co.,Ltd. |