CN106118140B - A kind of preparation method of high whiteness high-temperature resistant color masterbatch grade titanium dioxide - Google Patents
A kind of preparation method of high whiteness high-temperature resistant color masterbatch grade titanium dioxide Download PDFInfo
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- CN106118140B CN106118140B CN201610423711.9A CN201610423711A CN106118140B CN 106118140 B CN106118140 B CN 106118140B CN 201610423711 A CN201610423711 A CN 201610423711A CN 106118140 B CN106118140 B CN 106118140B
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Abstract
The invention discloses a kind of high whiteness, the preparation methods of high-temperature resistant color masterbatch grade titanium dioxide, the rutile-type color masterbatch special titanium pigment is based on a kind of Production By Sulfuric Acid Process technique, by fully bleach, wash and salt treatment after, it carries out calcining the rutile base-material being prepared without surface treatment, has good whiteness and particle fineness；After the abundant crushing being sanded using wet-milling, inorganic coating and expansion drying are carried out, in air-flow crushing by organic coated processing, to prepare the color masterbatch grade special titanium white of the low moisture absorption, fine grain, high whiteness, high-temperature resistant.The standby color masterbatch grade titanium dioxide of patent system of the present invention can significantly improve titanium dioxide in the heatproof situation of down-stream enterprise and the application performance of resin, it, which has, can be used for different industrial uses and can manufacture the broad mass market foreground of different colored plastic articles for use.
Description
Technical field
The invention belongs to the technologies of Titanium White Production By Sulfuric Acid Process, and in particular to carry out inorganic coating and organic to titanium dioxide
Cladding, improving product has the preparation method of color masterbatch grade titanium dioxide of better application performance in plastic masterbatch system.
Background technology
The physicochemical properties of titanium dioxide are stablized, and have best opacity, whiteness and highest brightness, are to work as
This life circle can not be substituted, most outstanding white pigment, be widely used in the industries such as coating, plastics, papermaking, ink.
The production method of titanium dioxide mainly has sulfuric acid process and chloridising.The primary raw material of wherein Titanium White Production By Sulfuric Acid Process is
Ilmenite and sulfuric acid, typical process flow include：The preparation of metatitanic acid, metatitanic acid bleaching rinsing, salt treatment, calcining smashing, after
The stages such as processing.The preparation of metatitanic acid mainly with industrial sulfuric acid decomposition through magnetic separation, drying, it is levigate after ilmenite, add water logging
Take plus iron powder reducing after titanium liquid is made, through settling, be separated by filtration the solid impurities such as ferrous sulfate, colloid, clear titanium liquid is made,
It concentrates again, hydrolyze metatitanic acid (hydrated titanium dioxide) is made.
Plastics are the second largest application fields of titanium dioxide, basic pigment of the titanium dioxide as plastic filler, except requiring
Outside the convention pigments performance such as good glossiness, covering power and reducing power, it is very good to be required in Masterbatch preparation process
Surface wettability performance, require good dispersion effect and excellent hot-working character when being mixed with the other auxiliary agents of plastics,
There is good heat resistance in plastic moulding process, there is good light resistance during solar exposure, so titanium dioxide
Properties for follow in, as temperature tolerance becomes the key technical index of plastics titanium dioxide.Obtain excellent processability
Can, other than carrying out inorganic coating processing to titanium dioxide, it is necessary to organic coated processing is carried out to it, wherein organic coated processing
Directly determine the heat resistance of titanium dioxide.
The machine coating agent of common are is broadly divided into polyalcohols, organic silicon and organic amine three categories.Sulfuric acid process is general
Titanium white and coating grade titanium white are often used polyalcohols as organic coated dose, and domestic color masterbatch grade titanium dioxide has commonly using small molecule
The problems such as machine silicon is as organic coated dose, but that there are temperature tolerances is poor, is easy xanthochromia for this type organic, poor processability.
Domestic few to the existing research and product manufacturing of color masterbatch grade titanium dioxide at present, existing producer passes through to titanium dioxide
The selection of organic agent carries out the preparation of titanium dioxide for producing color master batch, such as：CN200810045510.5 discloses proposition using a kind of
Special organosilicon material carries out organic coated processing to titanium dioxide, obtains with polymolecularity, yellowing resistance and high working property
The method of the titanium dioxide of energy.Show that Masterbatch titanium dioxide is very heavy using which kind of organic process in laboratory test by us
It wants, but the inorganic coating of titanium dioxide influences also very greatly, if the two not taken into account uniformly, in the white of plastic masterbatch system
Degree, dispersibility, covering power, processing torque cannot be guaranteed.
In addition a very crucial basic pigment performance index of titanium dioxide is whiteness, and whiteness is an optics of titanium dioxide
Property is two kinds of optical effects of bright intensity and tone that people feel white pigment, indicates to absorb between reflection natural light
Proportion, be in natural light different wave length light wave absorb and degree of reflection mark, can to it is red, orange, yellow in natural light wave,
Green, indigo, indigo plant, purple seven kinds of light waves are universal and uniformly reflect presentation white.According to Kubelka-Munk theories, the film of infinite thickness
The brightness of (opaque coating) or reflectivity R are inversely proportional to the ratio between the absorption coefficient K and scattering coefficient S of light (K/S) with pigment, i.e. K
It reduces or S increases, whiteness and brightness just increase.Therefore, in the actual production process of titanium white, it is mainly adjusted by and controls two
The grain size of titanium oxide and particle diameter distribution enhance dispersibility, and improve S；And the impurity being reduced as far as in titanium dioxide contains
Amount, and chemical purity is improved, avoid titanium dioxide from lattice defect occur, to reduce the mode of K, to obtain good whiteness.
Invention content
The technical problem to be solved by the present invention is to：In prior art basis, by adding zinc salt, sylvite, microcosmic salt salt
Treatment formulations are combined to realize effective control to rutile titanium white Powder Particle Size and size distribution by inorganic and organic coating
Mode, to obtain a kind of high whiteness high-temperature resistant color masterbatch grade titanium dioxide.
Technical scheme is as follows：
A kind of preparation method of high whiteness high-temperature resistant color masterbatch grade titanium dioxide, includes the following steps：
(1) metatitanic acid is once washed, adds the Ti of 0.8g/L3+It is bleached with sulfuric acid, then carries out secondary washing,
Fully wash off the iron ion in filter cake, after the completion of washing press filtration obtain iron content be less than 15ppm metatitanic acid filter cake；
(2) after the slurry of 200-400g/L concentration being made in the mashing dispersion of metatitanic acid filter cake, with zinc salt, sylvite and microcosmic salt into
Row combination salt treatment, then at 950-980 DEG C, calcining obtains object under the kiln that rutile conversion ratio is 94-98%；
(3) object addition water and sodium metasilicate under calcining kiln are passed through into ball after dispersant is prepared into the slurry of 300-700g/L
After well dispersed slurry being obtained after grinding machine coarse crushing and sand mill are finely divided, water use regulation concentration to 200-400g/L and pH value
To 8.0-10.0；
(4) above-mentioned slurry is subjected to inorganic coating processing with sodium metaaluminate, coating agent additive amount is with Al2O3Meter is TiO2Matter
The 1.0-2.0% of amount；
(5) slurry after coating is subjected to press filtration and desalination water washing, filter cake carries out expansion drying；
(6) material after expansion drying is carried out air-flow crushing, and organic coated dose is added in air-flow crushing, then existed
Vapour flour bag filter is collected by fully crushing and organic coated powder, obtains the titanium dioxide pigment, the product is thin
It is coated with polymeric type organic film on the surface of small titanium dioxide granule, titanium dioxide TiO in the pigment2Content range be 97~
99%, C element content range is 0.05-0.2%.
Wherein, zinc salt, sylvite and microcosmic salt are embedded under the calcining kiln described in step (2) in the crystal structure of object, at the salt
Reason realizes salt treatment using the combination of zinc sulfate, potassium carbonate and phosphoric acid；
Its addition of zinc salt is TiO in terms of ZnO mass in salt treatment described in step (2)2The 0.05-0.2% of quality；
Its addition of sylvite is with K in salt treatment described in step (2)2O mass meters are TiO2The 0.25-0.45% of quality；
Its addition of microcosmic salt is with P in salt treatment described in step (2)2O5Quality meter is TiO2The 0.2-0.4% of quality；
It is the polydimethylsiloxanes of 50-500cp that organic coated dose in step (6), which refers to the viscosity of both ends methyl blocking,
Alkane, additive amount are the 0.05%-0.2% of carbon content in titanium dioxide.
Bleaching rinsing mainly washes off Fe in step (1)2+, because as pH value increases in water-washing process, Fe2+It can oxygen
It is melted into Fe3+, ferric iron can hydrolyze in pH ＞ 2.5 and be precipitated as colloidal ferric hydroxide, be adsorbed in metatitanic acid, to influence to produce
Product whiteness needs metatitanic acid zinc powder, aluminium powder or trivalent titanium solution after washing to carry out bleaching, also by ferric iron thus
Originally it was that the ferrous sulfate of low price is washed with water, while can also remove the impurity such as the chromium adsorbed in metatitanic acid, vanadium.If using a water
Washing method removes iron, and washing for a long time is also difficult to remove impurity iron completely.Industrial common method for bleaching has zinc powder-sulfuric acid, aluminium
The bleaching of powder-sulfuric acid and titanous-sulfuric acid bleaching, wherein titanous is widely used due to not generating secondary pollution to product,
So the present invention is using titanous-sulfuric acid bleaching.
After the washed removal foreign ion of metatitanic acid that titanium hydrolysis generates, if being fed directly to turn round without salt treatment
Kiln is calcined, and titanium dioxide pigment quality requirement is much not achieved in whiteness, reducing power, oil absorption, the covering power etc. of finished product.However it is same
Metatitanic acid will produce the finished product of high pigment performance by salt treatment appropriate and calcining, greatly improve economic benefit, so
The salt treatment stage is very important in Producing Titanium Dioxide.In fact, being required for metatitanic acid quality and the different of final product quality, it is added
The type and quantity of salt treatment are different.Experiments have shown that phosphate is added in metatitanic acid before calcination, keep the iron in metatitanic acid miscellaneous
Matter aoxidizes the ferric phosphate for becoming lark in high-temperature calcination, and the brownish red that compares iron oxide wants small by one to product whiteness influence
A bit, thus can partially obscured impurity iron colour developing, the whiteness of product can be improved indirectly, sylvite can make calcined particle loose, adjust
Whole rutile crystal type, zinc salt, which can play, inhibits particle crystal form rapid conversion, is conducive to particle during transformation of crystal at a slow speed
It uniformly grows up, has the function that improve particle diameter distribution and round and smooth particle morphology.
The advantage of the invention is that by the stringent control of process conditions, salt is combined using zinc salt, sylvite and microcosmic salt
Processing, and Calcine Strength is adjusted according to the difference of salt treatment formula, to realize the simple grain size and granularity of titanium dioxide crude product
Effective control of distribution improves titanium dioxide whiteness, and by inorganic coating mode, is coated on titanium dioxide granule surface one layer thin
Thin pellumina, when making three washing after coating, slurry will not largely wear filter, while because covering amount is less, make titanium dioxide
With preferable covering, lubricity, dispersibility, then by the further organic coated processing of siloxanes, titanium dioxide is made to exist
Plastic masterbatch system has very high color inhibition shape and more high application performance.
Specific implementation mode
The present invention is described in detail below
In order to make the purpose , technical scheme and advantage of the present invention be clearer, with reference to embodiments, to the present invention
It is described in further detail.It should be appreciated that described herein, specific examples are only used to explain the present invention, does not limit
In the present invention.
Embodiment 1：
(1) metatitanic acid is added into Ti by primary washing3+It is bleached with sulfuric acid, then carries out secondary washing, washing is completed
Press filtration obtains the metatitanic acid filter cake that iron content is less than 10ppm afterwards；
(2) after the slurry of 300g/L concentration being made in the mashing dispersion of metatitanic acid filter cake, group is carried out with zinc salt, sylvite and microcosmic salt
Salt treatment is closed, the addition of zinc sulfate, potassium carbonate and phosphoric acid is respectively 0.05%, 0.35%, 0.3% (based on titanium dioxide
Mass fraction, addition is respectively with oxide ZnO, K2O, P2O5Quality meter), then at 950 DEG C calcining obtain rutile conversion
Object under the kiln that rate is 94%；
(3) object adds water and sodium metasilicate after dispersant is prepared into the slurry of 500g/L under the rutile-type kiln after calcining,
It is roughly ground into ball mill, finely divided, then water use regulation pulp density to 200g/L and pH is carried out subsequently into sand mill
It is worth to after 9.0；
(4) sodium metaaluminate inorganic coating processing is carried out, covering additive amount is with Al2O3Quality meter is TiO2Quality
1.0%；
(5) material after coating is subjected to press filtration and desalination water washing, filter cake carries out expansion drying；
(6) material after expansion drying is carried out air-flow crushing, in air-flow crushing, organosiloxane is added, then exists
Vapour flour bag filter is collected by fully crushing and organic coated powder, and the titanium dioxide pigment, carbon content TiO are obtained2
The 0.1% of quality.
Embodiment 2
(1) metatitanic acid is added into Ti by primary washing3+It is bleached with sulfuric acid, then carries out secondary washing, washing is completed
Press filtration obtains the metatitanic acid filter cake that iron content is less than 10ppm afterwards；
(2) after the slurry of 200g/L concentration being made in the mashing dispersion of metatitanic acid filter cake, group is carried out with zinc salt, sylvite and microcosmic salt
Salt treatment is closed, the addition of zinc sulfate, potassium carbonate and phosphoric acid is respectively 0.2%, 0.25%, 0.20% (based on titanium dioxide
Mass fraction, addition is respectively with oxide ZnO, K2O, P2O5Quality meter), then at 950 DEG C calcining obtain rutile conversion
Object under the kiln that rate is 96%；
(3) object adds water and sodium metasilicate after dispersant is prepared into the slurry of 300g/L under the rutile-type kiln after calcining,
It is roughly ground into ball mill, finely divided, then water use regulation pulp density to 300g/L and pH is carried out subsequently into sand mill
It is worth to after 8.0；
(4) inorganic coating processing is carried out, covering additive amount is with Al2O3Quality meter is TiO2The 1.5% of quality；
(5) material after coating is subjected to press filtration and desalination water washing, filter cake carries out expansion drying；
(6) material after expansion drying is carried out air-flow crushing, in air-flow crushing, organosiloxane is added, then exists
Vapour flour bag filter is collected by fully crushing and organic coated powder, and the titanium dioxide pigment is obtained.Carbon content is TiO2
The 0.05% of quality.
Embodiment 3
(1) metatitanic acid is added into Ti by primary washing3+It is bleached with sulfuric acid, then carries out secondary washing, washing is completed
Press filtration obtains the metatitanic acid filter cake that iron content is less than 10ppm afterwards；
(2) after the slurry of 400g/L concentration being made in the mashing dispersion of metatitanic acid filter cake, group is carried out with zinc salt, sylvite and microcosmic salt
Salt treatment is closed, the addition of zinc sulfate, potassium carbonate and phosphoric acid is respectively 0.15%, 0.45%, 0.4% (based on titanium dioxide
Mass fraction, addition is respectively with oxide ZnO, K2O, P2O5Quality meter), then at 950 DEG C calcining obtain rutile conversion
Object under the kiln that rate is 98%；
(3) object adds water and sodium metasilicate after dispersant is prepared into the slurry of 700g/L under the rutile-type kiln after calcining,
It is roughly ground into ball mill, finely divided, then water use regulation pulp density to 400g/L and pH is carried out subsequently into sand mill
It is worth to after 10.0；
(4) inorganic coating processing is carried out, covering additive amount is with Al2O3Quality meter is TiO2The 2.0% of quality；
(5) material after coating is subjected to press filtration and desalination water washing, filter cake carries out expansion drying；
Last material enters airslide disintegrating mill and crushes, and in air-flow crushing, organosiloxane, carbon content control is added
0.2%；
(6) material after expansion drying is carried out air-flow crushing, in air-flow crushing, organosiloxane is added, then exists
Vapour flour bag filter is collected by fully crushing and organic coated powder, and the titanium dioxide pigment is obtained.Carbon content is TiO2
The 0.2% of quality.
Performance detection：
1, temperature tolerance
Since titanium dioxide surface is surrounded by one layer organic coated dose, when titanium dioxide heats to a certain extent, surfactant
It can be carbonized, influence product form and aspect to which xanthochromia occur.The temperature tolerance test method is based on this principle, and titanium dioxide is put in
For a period of time, the aberration after preceding and heating is heated in then test to the baking oven of certain temperature.The specific method is as follows：By titanium white obtained
Powder is placed in Muffle furnace and heats 10 minutes, so respectively at 260,280,300,320,330,340,360,380,400,420 DEG C
Dry powder L, a, b value of titanium dioxide is tested afterwards, and is compared with the titanium dioxide before heating, and aberration △ E are calculated.
2, whiteness
Whiteness of the titanium dioxide in resin is extremely important, and this time experiment is added titanium dioxide obtained by 1.5% mass ratio
It is added in low density polyethylene (LDPE), after mixing, carries out injection molding and re-pack, then use the whiteness of color difference meter test sample plate.
Claims (3)
1. a kind of preparation method of high whiteness high-temperature resistant color masterbatch grade titanium dioxide, it is characterised in that：Include the following steps：
(1) metatitanic acid is added into Ti by primary washing3+It is bleached with sulfuric acid, then carries out secondary washing, pressed after the completion of washing
Filter obtains the metatitanic acid filter cake that iron content is less than 15ppm；
(2) after the slurry of 200-400g/L concentration being made in the mashing dispersion of metatitanic acid filter cake, group is carried out with zinc salt, sylvite and microcosmic salt
Salt treatment is closed, then calcining obtains object under the kiln that rutile conversion ratio is 94-98% at 950-980 DEG C；
(3) object addition water and sodium metasilicate under calcining kiln are passed through into ball mill after dispersant is prepared into the slurry of 300-700g/L
After obtaining well dispersed slurry after coarse crushing and sand mill are finely divided, water use regulation concentration to 200-400g/L and pH value are extremely
8.0-10.0；
(4) above-mentioned slurry is subjected to inorganic coating processing with sodium metaaluminate, coating agent additive amount is with Al2O3Meter is TiO2Quality
1.0-2.0%；
(5) slurry after coating is subjected to press filtration and desalination water washing, filter cake carries out expansion drying；
(6) material after expansion drying is carried out air-flow crushing, and organic coated dose is added in air-flow crushing, then in vapour powder
Bag hose is collected by fully crushing and organic coated powder, obtains titanium dioxide pigment, the pigment is in tiny titanium dioxide
It is coated with polymeric type organic film on the surface of titanium particle, titanium dioxide TiO in the pigment2Content range is 97~99%, C members
Cellulose content ranging from 0.05-0.3%；
Its addition of microcosmic salt is with P in salt treatment described in step (2)2O5Quality meter is TiO2The 0.4% of quality；
Its addition of zinc salt is TiO in terms of ZnO mass in salt treatment described in step (2)2The 0.05-0.2% of quality；
Its addition of sylvite is with K in salt treatment described in step (2)2O mass meters are TiO2The 0.25-0.45% of quality.
2. a kind of preparation method of high whiteness high-temperature resistant color masterbatch grade titanium dioxide according to claim 1, it is characterised in that：Step
Suddenly zinc salt, sylvite and microcosmic salt are embedded under the calcining kiln described in (2) in the crystal structure of object, the salt treatment is using zinc sulfate, carbon
Salt treatment is realized in the combination of sour potassium and phosphoric acid.
3. a kind of preparation method of high whiteness high-temperature resistant color masterbatch grade titanium dioxide according to claim 1, it is characterised in that：Step
Suddenly it is the dimethyl silicone polymer of 50-500cp that organic coated dose in (6), which refers to the viscosity of both ends methyl blocking, and additive amount is
It is calculated for 0.05%-0.2% according to carbon content in titanium dioxide is made.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610423711.9A CN106118140B (en) | 2016-06-13 | 2016-06-13 | A kind of preparation method of high whiteness high-temperature resistant color masterbatch grade titanium dioxide |
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|---|---|---|---|
| CN201610423711.9A CN106118140B (en) | 2016-06-13 | 2016-06-13 | A kind of preparation method of high whiteness high-temperature resistant color masterbatch grade titanium dioxide |
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| CN106118140A CN106118140A (en) | 2016-11-16 |
| CN106118140B true CN106118140B (en) | 2018-09-11 |
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| KR100273601B1 (en) * | 1996-03-26 | 2001-03-02 | 곤도 요시카즈 | Method of manufacturing inorganic pigment |
| CN101880479B (en) * | 2010-06-25 | 2013-04-24 | 宁波新福钛白粉有限公司 | Method for producing special rutile type titanium white powder for power coating |
| CN102936040B (en) * | 2012-11-28 | 2014-07-09 | 四川龙蟒钛业股份有限公司 | Production method of high-gloss and high-covering-capability rutile titanium dioxide |
| CN104817105B (en) * | 2015-04-21 | 2017-01-11 | 江苏镇钛化工有限公司 | Preparation method for treating titanium white by high zinc salt |
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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. |