CN104098932B - A kind of preparation method of white mineral-titanium dioxide composite powder pigment - Google Patents
A kind of preparation method of white mineral-titanium dioxide composite powder pigment Download PDFInfo
- Publication number
- CN104098932B CN104098932B CN201310128329.1A CN201310128329A CN104098932B CN 104098932 B CN104098932 B CN 104098932B CN 201310128329 A CN201310128329 A CN 201310128329A CN 104098932 B CN104098932 B CN 104098932B
- Authority
- CN
- China
- Prior art keywords
- titanium dioxide
- water
- powder
- slurry
- white mineral
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Fee Related
Links
Landscapes
- Inorganic Compounds Of Heavy Metals (AREA)
- Pigments, Carbon Blacks, Or Wood Stains (AREA)
- Cosmetics (AREA)
Abstract
The invention discloses a kind of preparation method of white mineral-titanium dioxide composite powder pigment. This composite granule pigment first by white mineral powder, pigmentary titanium dioxide respectively with water slurrying after, adopt organic modifiers to carry out surface modification, regulation and control pH value, then the slurry of preparation is all mixed, strong stirring, press filtration and dry, prepare white mineral-titanium dioxide composite powder pigment of the present invention. The present invention has the following advantages: 1) in preparation process, energy consumption is lower; 2) the composite particles surface of preparing has hydrophobicity, good with organic matrix compatibility; 3) preparation technology is simple, and particularly Separation of Solid and Liquid is easy, is easy to realize large-scale production; 4) production process is clean, without " three wastes " discharge, non-environmental-pollution.
Description
Technical field
The present invention relates to the technical field that a kind of powder body material is produced, concretely, relate to a kind of whiteThe preparation method of mineral-titanium dioxide composite powder pigment.
Background technology
Pigmentary titanium dioxide related to the present invention, titanium dioxide is the crystalline phase two by granularity 0.2-0.3 μ mTitanium oxide composition. Be born so far over more than 100 year from 20 beginnings of the century, pigmentary titanium dioxide coating, plastics,Numerous industrial circles such as papermaking and ink are widely applied, and have become performance the best, range of application is the widestThe Chinese white having comparative advantage with consumption. The pigmentary titanium dioxide annual production of 2009 in the whole world reaches5500000 tons, China has become the first in the world production and consumption big country at present, and the annual production of 2011 reaches 181.19Ten thousand tons. The share of TiO 2 pigment has accounted for the more than 90% of Chinese white at present, becomes national economy numerousOne of the important fine chemical material in field.
But, TiO 2 pigment produce and use procedure in the natural resources and energy resources consumption that exists large, environment is dirtyThe problems such as serious and cost price height of dying are also more and more outstanding. Along with day by day in short supply, the dilution of global titanium resourceWith the severe attack of the public to titanium dioxide production process problem of environmental pollution, pigmentary titanium dioxide is rawProduce enterprise and be faced with unprecedented challenge and test, have to strengthen cost and drop into coping resources and environmentProblem, and these measures become the main cause of continuous promotion product cost and rise in price. Pigment-level titanium dioxideTitanium rise in price causes again product cost increase, the business burden of its application to increase the weight of, and industry development is subject toGreatly restriction. In all solutions for the problems referred to above, multiple with mineral inorganic particle and titanium dioxideChinese white prepared by the approach of closing is similar to pigmentary titanium dioxide performance, and with low cost, and by actualApplication reduces amount of titanium and is considered at present one of the most effective approach. Wherein, with mineral grain tableFace cladding titanium dioxide be the composite particles of feature because replacement of titanium dioxide ratio is large, pigment performance and titanium dioxideTitanium pigment quite becomes the method for tool prospect, and related work becomes study hotspot for many years always.
At present, there is the compound of white pigment property with mineral inorganic particle and the preparation of titanium dioxide composite pathwayThe method of powder mainly contains two: chemical precipitation is coated and the coated complex method of mechanical force and chemical grain-grain, its designTarget all, taking inorganic powder particle as bag core, titanium dioxide are as coating forms composite particles, is utilized titanium dioxideMake composite particles and composite granule in the optical characteristics on composite particles surface and the cooperative effect of inorganic powder materialForm the performance of similar pigmentary titanium dioxide.
The coated composite square ratio juris of chemical precipitation is: at the titanium salt that has mineral inorganic particle, as TiOSO4、TiCl4Hydrolyzation system in, cause titanium salt hydrolysis, generate hydrated titanium dioxide and cover inorganic powder particle tableFace, then make the hydrated titanium dioxide of composite surface generate crystal type titanium dioxide coating through salt processing and roastingThing, thus make the composite particles powder taking the coated crystal type titanium dioxide in inorganic powder particle surface as feature.The advantage of the method is to form finer and close coated by titanium dioxide layer, dioxy on inorganic powder particle surfaceChange titanium firm at inorganic powder particle surface conjunction. But also there is some shortcomings and restriction problem: 1) bag core thingThe hydrated titanium dioxide on top layer is difficult to be transformed into pure rutile crystalline phase; 2) titanium salt is hydrolyzed to acid system, alkalescenceNonmetallic mineral can not be served as bag core thing and be used; 3) preparation process produces a large amount of acid waste waters etc. environment is formedPollute.
The coated composite square ratio juris of mechanical force and chemical grain-grain is: by solid matter in mechanical lapping refinementThe Mechanochemical Effect producing, causes the thin particulate matter as coating thing, i.e. titanium dioxide, with conductInterfacial reaction between the coarse particulate matter of bag core thing, forms titanium dioxide thus at the lip-deep bag of coarse granuleCover, specifically comprise dry laminating and wet method combination process. Wherein, dry process is simple, but reunites between particlePhenomenon is serious, bad dispersibility, and coated by titanium dioxide is at random, unordered, inhomogeneous, between particle, a little less than reaction, wrapsCover imperfectly, the pigment performance of the composite powder material of being prepared by composite particles is poor and unstable; Wet processingActive force between coated core particle and titanium dioxide granule is strong, so composite granule pigment performance is stable, approachesIn the pigment performance of titanium white, and production process non-environmental-pollution. But, wet method mechanical force and chemical grain-grain is coatedComplex method is at also Shortcomings and restriction problem of preparation technology, properties of product design aspect: 1) preparation processConsume energy larger. Its reason has two: the powerful grinding of mineral enforcement reaches miniature scale needs energy more; For makingParticle overcomes the effect of repelling each other in aqueous medium system, is able to occur chemically combined distance, needsApply compared with macro-energy. 2) mineral and titanium dioxide granule form to each other chemically combined distribution of particles inequality,Identity is poor cause chemical bond power a little less than, pigment performance is poor and unstable; 3) mineral-titanium dioxide of preparingComposite powder material is hydrophily, dehydrates difficulty, and during for organic matrix, compatibility is poor.
Chinese patent 200510080497.3 with white breeze as calcium carbonate, kaolin, calcined kaolin and heavySpar etc. are bag core matrix, and crystal titanium dioxide is coating thing, by the coated approach system of mechanical force and chemical grain-grainFor the composite white pigment taking mineral surfaces cladding titanium dioxide composite particles as composition. Prepared at productCheng Zhong, for ensure mineral grain surface be activated and mineral-titanium dioxide recombination process in outside energy defeatedEnter, all adopted wet ultra-fine grinding work in the preparation of mineral bag core matrix and mineral-titanium dioxide recombination processOrder, power consumption is very large. Chinese patent 200910000614.9 is with titanium dioxide and white breeze or compound white ore depositPowder is raw material, by titanium dioxide and white breeze mixture slurry are added to dispersant and pH adjusting agent adjustment, wetMethod stirs mill or sand mill segmentation is ground and dry, depolymerization processing, makes inorganic composite white pigment. This is specialIn profit method, not only white mineral-titanium dioxide recombination process adopts the energy input of segmentation wet ultra-fine grindingMode, and for ensureing that titanium dioxide is depolymerizated and disperses before compound, also adopt wet type extra-fine grinding to carry outDisperse. This causes the increase of power consumption equally. In addition, the product that prepared by above-mentioned two patent supplying methods isSurface hydrophilicity powder, poor with organic system compatibility.
Summary of the invention
The object of this invention is to provide a kind of preparation method of white mineral-titanium dioxide composite powder pigment, separateIn the existing preparation method that determines, consume energy high, the problem that the composite granule of preparation and organic matrix compatibility are poor.
The preparation method who realizes a kind of white mineral-titanium dioxide composite powder pigment of the present invention is:
One, raw-material selecting:
Using calcite, barite, wollastonite, kaolinite or calcined kaolin powder as white mineral powder,Its granularity is less than 2 μ m, content 85～90%, meso-position radius d50Be less than 1.1 μ m; With rutile type titanium white orDetitanium-ore-type titanium dioxide is pigmentary titanium dioxide; With stearate, oleic acid, oleate, containing C atom 8～16Organic ammonium salt or titante coupling agent be organic modifiers; And for regulate and control pH value dilute sulfuric acid orDilute solution of sodium hydroxide.
Two, raw material proportioning and step of preparation process:
(1) by the requirement of solid content 40～70% in white mineral powder and water formation suspended substance, measure mineral powderBody and water, mixed merga pass mixer stirs 45～90min, then will by heating tube in mixer or chuckSlurry is heated to 50～80 DEG C, keeps stable;
(2) in the white mineral powder of 50～80 DEG C and water suspension, add concentration to be to temperature after heatingThe solution of 3～8% organic modifiers, organic modifiers consumption is to account for 0.5～2.0% of white mineral powder amount,Stir 20～60min, make modified product activation index reach 90～100%, with 90～120 ° of water-wet contact angles;
(3) by the requirement of solid content 30～60% in pigmentary titanium dioxide and water formation suspended substance, measure pigmentGrade titanium dioxide and water, mixed merga pass mixer stirs, and breaks up 45～90min, then by mixerSlurry is heated to 50～80 DEG C by heating tube or chuck, keeps stable;
(4) in the pigmentary titanium dioxide of 50～80 DEG C and water suspension, add concentration to be to temperature after heatingThe solution of 3～8% organic modifiers, organic modifiers consumption is to account for pigmentary titanium dioxide amount0.5～2.0%, stir 20～60min, make modified product activation index reach 85～100%, contact with water-wet80～120 °, angle;
(5) the white mineral powder-aqueous suspension slurry after modification and pigmentary titanium dioxide-aqueous suspension slurry are pressedIts dry powder weight ratio white mineral powder: pigmentary titanium dioxide=40～70%: 30～60% ratio is mixed,Add again dilute sulfuric acid or dilute solution of sodium hydroxide to make pH value be controlled at certain value in 3～8 scopes according to mineral species,Then uniform stirring 30～60min completes compound;
(6) mixture slurry after compound is filtered into filter cake with centrifugal or vacuum filter, water content is less than35％；
(7) it is dry that filter cake step (6) being obtained is put into flash dryer, and desciccate is and will makesStandby white mineral-titanium dioxide composite powder pigment.
Composition and the weight ratio of the final white mineral-titanium dioxide composite powder pigment forming of the present invention are: whiteLook mineral powder 39.5～69.5%, pigmentary titanium dioxide 29.5～59.5%, modifier 0.5%～1.5%.
As follows to principles illustrated of the present invention:
In water slurry body, white mineral and pigmentary titanium dioxide are carried out respectively to surface organic modification, make twoThe outward extending organic carbochain of person's particle surface absorption, and form thus Induced drainage. This makes white ore depositBetween the particle of the same race of thing and titanium dioxide granule and between xenogenesis particle, in aqueous medium, be close to microcosmicWhen operating distance scope 5～6nm, can form strong Hydrophobic aggregation sucking action; The regulation and control of pH value can changeThe surface potential of white mineral and titanium dioxide granule, and then, their particles of the same race increased in long distance on the one handFrom between electronic double layer repulsion effect, make on the other hand their xenogenesis particles present sucking action between remote,Or repulsive interaction is reduced.
With this understanding, then through suitable strong stirring effect, between white mineral and titanium dioxide granule because ofAttract each other, or only there is weak repulsive interaction, and be close to short range from, be less than 5～6nm, reachBetween particle, produce the scope of Hydrophobic aggregation sucking action, so white mineral and titanium dioxide granule are by strongHydrophobic aggregation sucking action forms coated compound. And between white mineral and titanium dioxide granule particle of the same race because ofRepulsive interaction is strong, thus can not be close to the scope that Hydrophobic aggregation effect produces, therefore between particle of the same raceBe difficult in conjunction with and exist with dispersing morphology, it is intergranular compound that this is conducive to above-mentioned xenogenesis.
The present invention regulates and controls the hydrophobization degree on white mineral and titanium dioxide granule surface with regulation and control by modificationThe Hydrophobic aggregation sucking action of intergranular, by regulating and controlling particle surface current potential to regulate and control intergranular Effect of Electric Double LayerBehavior and degree, be finally formed in long-range distance range 5～50nm white mineral and titanium dioxide granuleBetween particle of the same race, have between strong repulsive interaction, xenogenesis particle and mainly have sucking action, next hasBe weaker than the result of the repulsive interaction between particle of the same race. Like this, under suitable strong stirring effect, whiteMineral and titanium dioxide granule be close to each other short range from, be less than 5～6nm, reach between particle and produceThe scope of Hydrophobic aggregation sucking action, so white mineral and titanium dioxide granule are inhaled by strong Hydrophobic aggregationThe effect of drawing forms coated compound. And between white mineral and titanium dioxide granule particle of the same race because repulsive interaction is strongStrong, so can not be close to the scope that Hydrophobic aggregation effect produces, be conducive to xenogenesis particle therefore keep disperseingBetween coated compound.
The present invention has the following advantages: 1) in preparation process, energy consumption is lower; 2) the composite particles surface of preparingThere is hydrophobicity, good with organic matrix compatibility; 3) preparation technology is simple, and particularly Separation of Solid and Liquid is easy,Be easy to realize large-scale production; 4) production process is clean, without " three wastes " discharge, non-environmental-pollution.
Detailed description of the invention
Embodiment 1:
One, raw-material selecting:
Taking calcite as white mineral powder, its granularity is less than 2 μ m, content 85%, meso-position radius d50Be 1.0 μ m;Taking Detitanium-ore-type titanium dioxide as pigmentary titanium dioxide; Taking odium stearate as organic modifiers.
Two, raw material proportioning and step of preparation process:
(1) according to mass ratio, measure calcite powder 40%, water 60% is placed in the mixer that can heat,Mix and stir 60min, then slurry being heated to 60 DEG C, keeping stable;
(2) be 6% sodium stearate solution to adding concentration in the calcite powder after heating and water suspension,Wherein the odium stearate amount in solution is 1% of calcite in powder weight, stirs 40min, modified product activationIndex reaches 99%, with 112 ° of water-wet contact angles;
(3), according to mass ratio, measure Detitanium-ore-type titanium dioxide 40%, water 60% is placed in the mixer that can heatIn, mix and stir 60min, then slurry is heated to 60 DEG C, keep stable;
(4) be that 6% odium stearate is molten to adding concentration in the Detitanium-ore-type titanium dioxide after heating and water suspensionLiquid, wherein the odium stearate amount in solution is 1% of Detitanium-ore-type titanium dioxide quality, stirs 40min, modificationProduct activation index reaches 95%, with 105 ° of water-wet contact angles;
(5) by the slurry of the calcite powder after modification and Detitanium-ore-type titanium dioxide slurry mixed in equal amounts by weightAnd stir, then to add dilute sulfuric acid to make pH value be 7.5, uniform stirring 50min completes compound;
(6) mixture slurry after compound is filtered into filter cake with vacuum filter;
(7) it is dry that filter cake step (6) being obtained is put into flash dryer, and desciccate is and will makesStandby white mineral-titanium dioxide composite powder pigment.
Embodiment 2:
One, raw-material selecting:
Taking calcite as white mineral powder, its granularity is less than 2 μ m, content 85%, meso-position radius d50Be 1.0 μ m;Taking rutile type titanium white as pigmentary titanium dioxide; Taking odium stearate as organic modifiers.
Two, raw material proportioning and step of preparation process:
(1) according to mass ratio, measure calcite powder 40%, water 60% is placed in the mixer that can heat,Mix and stir 60min, then slurry being heated to 60 DEG C, keeping stable;
(2) be 7% sodium stearate solution to adding concentration in the calcite powder after heating and water suspension,Wherein the odium stearate amount in solution is 1% of calcite in powder weight, stirs 40min, modified product activationIndex reaches 99%, with 112 ° of water-wet contact angles;
(3), according to mass ratio, measure rutile type titanium white 40%, water 60% is placed in the mixer that can heatIn, mix and stir 60min, then slurry is heated to 60 DEG C, keep stable;
(4) be that 7% odium stearate is molten to adding concentration in the rutile type titanium white after heating and water suspensionLiquid, wherein the odium stearate amount in solution is 1% of rutile type titanium white quality, stirs 40min, modificationProduct activation index reaches 95%, with 100 ° of water-wet contact angles;
(5) by the slurry of the calcite powder after modification and rutile type titanium white slurry mixed in equal amounts by weightAnd stir, then to add dilute sulfuric acid to make pH value be 7.5, uniform stirring 50min completes compound;
(6) mixture slurry after compound is filtered into filter cake with centrifugal filter;
(7) it is dry that filter cake step (6) being obtained is put into flash dryer, and desciccate is and will makesStandby white mineral-titanium dioxide composite powder pigment.
Embodiment 3:
One, raw-material selecting:
Taking barite as white mineral powder, its granularity is less than 2 μ m, content 88%, meso-position radius d50Be 1.0 μ m;Taking Detitanium-ore-type titanium dioxide as pigmentary titanium dioxide; Taking enuatrol as organic modifiers.
Two, raw material proportioning and step of preparation process:
(1) according to mass ratio, measure barite powder 40%, water 60% is placed in the mixer that can heat,Mix and stir 60min, then slurry being heated to 60 DEG C, keeping stable;
(2) be 7% sodium oleate solution to adding concentration in the barite powder after heating and water suspension, itsEnuatrol amount in middle solution is 1% of barite powder quality, stirs 40min, modified product activation indexReach 95%, with 108 ° of water-wet contact angles;
(3) according to mass ratio, measure Detitanium-ore-type titanium dioxide 40%, water 60%, be placed in the stirring that can heatIn machine, mix and stir 60min, then slurry being heated to 60 DEG C, keeping stable;
(4) be that 7% enuatrol is molten to adding concentration in the Detitanium-ore-type titanium dioxide after heating and water suspensionLiquid, wherein the enuatrol amount in solution is 1% of Detitanium-ore-type titanium dioxide quality, stirs 40min, modification is producedThing activation index reaches 95%, with 105 ° of water-wet contact angles;
(5) by the slurry of the barite powder after modification and Detitanium-ore-type titanium dioxide slurry mixed in equal amounts by weightAnd stir, then to add dilute sulfuric acid adjust pH be 7, uniform stirring 50min completes compound;
(6) mixture slurry after compound is filtered into filter cake with vacuum filter;
(7) it is dry that filter cake step (6) being obtained is put into flash dryer, and desciccate is and will makesStandby white mineral-titanium dioxide composite powder pigment.
Three kinds of white mineral-titanium dioxide making respectively by embodiment 1, embodiment 2 and embodiment 3 are compoundThe main performance of powder pigment is listed in table 1.
The performance of the prepared white mineral-titanium dioxide composite powder of table 1 pigment
Claims (4)
1. a preparation method for white mineral-titanium dioxide composite powder pigment, is characterized in that:
One, raw-material selecting:
Using calcite, barite, wollastonite, kaolinite or calcined kaolin powder as white mineral powder,Its granularity is less than 2 μ m, content 85～90%, meso-position radius d50Be less than 1.1 μ m; With rutile type titanium white orDetitanium-ore-type titanium dioxide is pigmentary titanium dioxide; With stearate, oleic acid, oleate, containing C atom 8～16Organic ammonium salt or titante coupling agent be organic modifiers; And for regulating and controlling dilute sulfuric acid or the hydrogen of pH valueSodium oxide molybdena weak solution;
Two, raw material proportioning and step of preparation process:
(1) by the requirement of solid content 40～70% in white mineral powder and water formation suspended substance, measure mineral powderBody and water, mixed merga pass mixer stirs 45～90min, then will by heating tube in mixer or chuckSlurry is heated to 50～80 DEG C, keeps stable;
(2) in the white mineral powder of 50～80 DEG C and water suspension, add concentration to be to temperature after heatingThe solution of 3～8% organic modifiers, organic modifiers consumption is to account for 0.5～2.0% of white mineral powder amount,Stir 20～60min, make modified product activation index reach 90～100%, with 90～120 ° of water-wet contact angles;
(3) by the requirement of solid content 30～60% in pigmentary titanium dioxide and water formation suspended substance, measure pigmentGrade titanium dioxide and water, mixed merga pass mixer stirs, and breaks up 45～90min, then by mixerSlurry is heated to 50～80 DEG C by heating tube or chuck, keeps stable;
(4) in the pigmentary titanium dioxide of 50～80 DEG C and water suspension, add concentration to be to temperature after heatingThe solution of 3～8% organic modifiers, organic modifiers consumption is to account for 0.5～2.0% of pigmentary titanium dioxide amount,Stir 20～60min, make modified product activation index reach 85～100%, with 80～120 ° of water-wet contact angles;
(5) the white mineral powder-aqueous suspension slurry after modification and pigmentary titanium dioxide-aqueous suspension slurry are pressedIts dry powder weight ratio white mineral powder: pigmentary titanium dioxide=40～70%: 30～60% ratio is mixed,Add again dilute sulfuric acid or dilute solution of sodium hydroxide to make pH value be controlled at certain value in 3～8 scopes according to mineral species,Then uniform stirring 30～60min completes compound;
(6) mixture slurry after compound is filtered into filter cake with centrifugal or vacuum filter, water content is less than35％；
(7) it is dry that filter cake step (6) being obtained is put into flash dryer, and desciccate is and will makesStandby white mineral-titanium dioxide composite powder pigment.
2. the preparation method of a kind of white mineral-titanium dioxide composite powder pigment according to claim 1,It is characterized in that:
One, raw-material selecting:
Taking calcite as white mineral powder, its granularity is less than 2 μ m, content 85%, meso-position radius d50Be 1.0 μ m;Taking Detitanium-ore-type titanium dioxide as pigmentary titanium dioxide; Taking odium stearate as organic modifiers;
Two, raw material proportioning and step of preparation process:
(1) according to mass ratio, measure calcite powder 40%, water 60% is placed in the mixer that can heat,Mix and stir 60min, then slurry being heated to 60 DEG C, keeping stable;
(2) be 6% sodium stearate solution to adding concentration in the calcite powder after heating and water suspension,Wherein the odium stearate amount in solution is 1% of calcite in powder weight, stirs 40min, modified product activationIndex reaches 99%, with 112 ° of water-wet contact angles;
(3), according to mass ratio, measure Detitanium-ore-type titanium dioxide 40%, water 60% is placed in the mixer that can heatIn, mix and stir 60min, then slurry is heated to 60 DEG C, keep stable;
(4) be that 6% odium stearate is molten to adding concentration in the Detitanium-ore-type titanium dioxide after heating and water suspensionLiquid, wherein the odium stearate amount in solution is 1% of Detitanium-ore-type titanium dioxide quality, stirs 40min, modificationProduct activation index reaches 95%, with 105 ° of water-wet contact angles;
(5) by the slurry of the calcite powder after modification and Detitanium-ore-type titanium dioxide slurry mixed in equal amounts by weightAnd stir, then to add dilute sulfuric acid to make pH value be 7.5, uniform stirring 50min completes compound;
(6) mixture slurry after compound is filtered into filter cake with vacuum filter;
(7) it is dry that filter cake step (6) being obtained is put into flash dryer, and desciccate is and will makesStandby white mineral-titanium dioxide composite powder pigment.
3. the preparation method of a kind of white mineral-titanium dioxide composite powder pigment according to claim 1,It is characterized in that:
One, raw-material selecting:
Taking calcite as white mineral powder, its granularity is less than 2 μ m, content 85%, meso-position radius d50Be 1.0 μ m;Taking rutile type titanium white as pigmentary titanium dioxide; Taking odium stearate as organic modifiers;
Two, raw material proportioning and step of preparation process:
(1) according to mass ratio, measure calcite powder 40%, water 60% is placed in the mixer that can heat,Mix and stir 60min, then slurry being heated to 60 DEG C, keeping stable;
(2) be 7% sodium stearate solution to adding concentration in the calcite powder after heating and water suspension,Wherein the odium stearate amount in solution is 1% of calcite in powder weight, stirs 40min, modified product activationIndex reaches 99%, with 112 ° of water-wet contact angles;
(3), according to mass ratio, measure rutile type titanium white 40%, water 60% is placed in the mixer that can heatIn, mix and stir 60min, then slurry is heated to 60 DEG C, keep stable;
(4) be that 7% odium stearate is molten to adding concentration in the rutile type titanium white after heating and water suspensionLiquid, wherein the odium stearate amount in solution is 1% of rutile type titanium white quality, stirs 40min, modificationProduct activation index reaches 95%, with 100 ° of water-wet contact angles;
(5) by the slurry of the calcite powder after modification and rutile type titanium white slurry mixed in equal amounts by weightAnd stir, then to add dilute sulfuric acid to make pH value be 7.5, uniform stirring 50min completes compound;
(6) mixture slurry after compound is filtered into filter cake with centrifugal filter;
(7) it is dry that filter cake step (6) being obtained is put into flash dryer, and desciccate is and will makesStandby white mineral-titanium dioxide composite powder pigment.
4. the preparation method of a kind of white mineral-titanium dioxide composite powder pigment according to claim 1,It is characterized in that:
One, raw-material selecting:
Taking barite as white mineral powder, its granularity is less than 2 μ m, content 88%, meso-position radius d50Be 1.0 μ m;Taking Detitanium-ore-type titanium dioxide as pigmentary titanium dioxide; Taking enuatrol as organic modifiers;
Two, raw material proportioning and step of preparation process:
(1) according to mass ratio, measure barite powder 40%, water 60% is placed in the mixer that can heat,Mix and stir 60min, then slurry being heated to 60 DEG C, keeping stable;
(2) be 7% sodium oleate solution to adding concentration in the barite powder after heating and water suspension, itsEnuatrol amount in middle solution is 1% of barite powder quality, stirs 40min, modified product activation indexReach 95%, with 108 ° of water-wet contact angles;
(3) according to mass ratio, measure Detitanium-ore-type titanium dioxide 40%, water 60%, be placed in the stirring that can heatIn machine, mix and stir 60min, then slurry being heated to 60 DEG C, keeping stable;
(4) be that 7% enuatrol is molten to adding concentration in the Detitanium-ore-type titanium dioxide after heating and water suspensionLiquid, wherein the enuatrol amount in solution is 1% of Detitanium-ore-type titanium dioxide quality, stirs 40min, modification is producedThing activation index reaches 95%, with 105 ° of water-wet contact angles;
(5) by the slurry of the barite powder after modification and Detitanium-ore-type titanium dioxide slurry mixed in equal amounts by weightAnd stir, then to add dilute sulfuric acid adjust pH be 7, uniform stirring 50min completes compound;
(6) mixture slurry after compound is filtered into filter cake with vacuum filter;
(7) it is dry that filter cake step (6) being obtained is put into flash dryer, and desciccate is and will makesStandby white mineral-titanium dioxide composite powder pigment.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310128329.1A CN104098932B (en) | 2013-04-15 | 2013-04-15 | A kind of preparation method of white mineral-titanium dioxide composite powder pigment |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310128329.1A CN104098932B (en) | 2013-04-15 | 2013-04-15 | A kind of preparation method of white mineral-titanium dioxide composite powder pigment |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN104098932A CN104098932A (en) | 2014-10-15 |
| CN104098932B true CN104098932B (en) | 2016-05-25 |
Family
ID=51667496
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201310128329.1A Expired - Fee Related CN104098932B (en) | 2013-04-15 | 2013-04-15 | A kind of preparation method of white mineral-titanium dioxide composite powder pigment |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN104098932B (en) |
Families Citing this family (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104893364A (en) * | 2015-06-03 | 2015-09-09 | 安徽省铜陵县牛山矿业有限责任公司 | Production technique and production line of mineral/TiO2 composite granular material |
| CN105440739A (en) * | 2015-12-15 | 2016-03-30 | 常熟市环虹化工颜料厂 | Preparation method of nanometer filling material-doped compound titanium dioxide pigment |
| CN105542517B (en) * | 2016-01-14 | 2018-07-06 | 广西七色珠光材料股份有限公司 | White and interference colours dumb light sheet coated pigment and preparation method |
| CN106479247B (en) * | 2016-08-18 | 2018-09-14 | 西藏亚吐克工贸有限公司 | The application of barium sulfate and titanium white compound powder on coating |
| CN106479246B (en) * | 2016-08-18 | 2018-09-14 | 西藏亚吐克工贸有限公司 | The application of calcium activated and titanium white compound powder on coating |
| CN106243500B (en) * | 2016-08-22 | 2019-06-18 | 江西广源化工有限责任公司 | A kind of preparation method and its product of polypropylene modification composite material |
| CN108070280B (en) * | 2016-11-11 | 2020-06-09 | 中国地质大学（北京） | Preparation method of silicon dioxide microsphere-titanium dioxide composite powder pigment |
| CN106590062A (en) * | 2016-12-06 | 2017-04-26 | 大连环球矿产股份有限公司 | Preparation method of composite titanium dioxide pigment with wollastonite coated with titanium dioxide |
| CN107254195A (en) * | 2017-06-20 | 2017-10-17 | 江苏特丰新材料科技有限公司 | Composite titanium dioxide and preparation method thereof |
| CN109183497B (en) * | 2018-09-18 | 2021-07-13 | 吉林大学 | Nano TiO for papermaking2Preparation method of/wollastonite compound |
| CN111748223A (en) * | 2020-05-07 | 2020-10-09 | 阳泉灿坤工贸有限公司 | Coated titanium dioxide and preparation method thereof |
| CN114716846A (en) * | 2021-01-04 | 2022-07-08 | 北京橡胶工业研究设计院有限公司 | Method for preparing composite titanium dioxide by using titanium dioxide coated calcium carbonate |
| CN113416434B (en) * | 2021-06-07 | 2022-05-17 | 淮阴工学院 | Preparation method and application of vegetable oil modified titanium dioxide/Maya blue-like composite pigment |
| KR20230104300A (en) * | 2021-12-30 | 2023-07-10 | 주식회사 코스메카코리아 | manufacturing method of titanium dioxide composite pigment and titanium dioxide composite pigment manufactured through the same |
Citations (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH10204316A (en) * | 1997-01-24 | 1998-08-04 | Kanebo Ltd | Composite powder and cosmetic |
| CN1724595A (en) * | 2005-07-07 | 2006-01-25 | 北京天之岩健康科技有限公司 | White minera powder TiO2 composite white pigment and its preparation method |
| JP2006152466A (en) * | 2004-11-26 | 2006-06-15 | Nippon Paper Industries Co Ltd | Method for milling calcium carbonate |
| CN1970486A (en) * | 2006-10-16 | 2007-05-30 | 大连理工大学 | Method for removing brucite powder chromophore impurity |
| CN101041748A (en) * | 2007-04-23 | 2007-09-26 | 恩施州瀑源化工有限责任公司 | TiO2 complex ore powder and preparation method thereof |
| JP2007332223A (en) * | 2006-06-13 | 2007-12-27 | Toda Kogyo Corp | Heat-shielding composite particle powder and heat-shielding coating composition using it |
| CN101210117A (en) * | 2006-12-25 | 2008-07-02 | 中国地质大学（北京） | Sericite/TiO2 composite material with white pigment property |
| CN101245198A (en) * | 2008-03-13 | 2008-08-20 | 常州市美伦钛业有限公司 | Coated titanium dioxide and manufacture method thereof |
| CN101418139A (en) * | 2007-10-25 | 2009-04-29 | 中国地质大学（北京） | Magnesium hydroxide/TiO2 composite material with flame resistance property and pigment |
| CN101775239A (en) * | 2009-01-09 | 2010-07-14 | 中国矿业大学(北京) | Preparation method of inorganic composite white pigment with high covering power |
| JP2010280763A (en) * | 2009-06-02 | 2010-12-16 | Okutama Kogyo Co Ltd | Pigment composition for coating |
| CN102260422A (en) * | 2010-05-25 | 2011-11-30 | 中国地质大学（北京） | Method for preparing TiO2/powdered quartz composite powder material |
-
2013
- 2013-04-15 CN CN201310128329.1A patent/CN104098932B/en not_active Expired - Fee Related
Patent Citations (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH10204316A (en) * | 1997-01-24 | 1998-08-04 | Kanebo Ltd | Composite powder and cosmetic |
| JP2006152466A (en) * | 2004-11-26 | 2006-06-15 | Nippon Paper Industries Co Ltd | Method for milling calcium carbonate |
| CN1724595A (en) * | 2005-07-07 | 2006-01-25 | 北京天之岩健康科技有限公司 | White minera powder TiO2 composite white pigment and its preparation method |
| JP2007332223A (en) * | 2006-06-13 | 2007-12-27 | Toda Kogyo Corp | Heat-shielding composite particle powder and heat-shielding coating composition using it |
| CN1970486A (en) * | 2006-10-16 | 2007-05-30 | 大连理工大学 | Method for removing brucite powder chromophore impurity |
| CN101210117A (en) * | 2006-12-25 | 2008-07-02 | 中国地质大学（北京） | Sericite/TiO2 composite material with white pigment property |
| CN101041748A (en) * | 2007-04-23 | 2007-09-26 | 恩施州瀑源化工有限责任公司 | TiO2 complex ore powder and preparation method thereof |
| CN101418139A (en) * | 2007-10-25 | 2009-04-29 | 中国地质大学（北京） | Magnesium hydroxide/TiO2 composite material with flame resistance property and pigment |
| CN101245198A (en) * | 2008-03-13 | 2008-08-20 | 常州市美伦钛业有限公司 | Coated titanium dioxide and manufacture method thereof |
| CN101775239A (en) * | 2009-01-09 | 2010-07-14 | 中国矿业大学(北京) | Preparation method of inorganic composite white pigment with high covering power |
| JP2010280763A (en) * | 2009-06-02 | 2010-12-16 | Okutama Kogyo Co Ltd | Pigment composition for coating |
| CN102260422A (en) * | 2010-05-25 | 2011-11-30 | 中国地质大学（北京） | Method for preparing TiO2/powdered quartz composite powder material |
Non-Patent Citations (1)
| Title |
|---|
| 机械力活化制备碳酸钙/TiO2复合颗粒材料及表征;檀倩等;《中国非金属矿工业导刊》;20110825(第4期);28-32 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN104098932A (en) | 2014-10-15 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN104098932B (en) | A kind of preparation method of white mineral-titanium dioxide composite powder pigment | |
| CN104119701B (en) | A kind of preparation method of inorganic composite white pigment of replacement of titanium dioxide at high proportion | |
| CN108083331B (en) | A kind of preparation method of rutile titanium dioxide superfine powder | |
| CN101418140B (en) | Preparation method of surface modified barium sulfate base ultrafine function powder material | |
| CN103194098B (en) | Preparation method of composite titanium dioxide | |
| CN101585539B (en) | Prepartion method of highly anti-yellow resistance white carbon black for silastic | |
| CN102924979B (en) | Method for preparing inorganic and organic coating titanium dioxide | |
| CN101429348B (en) | Process for producing nano-titanium dioxide-zinc oxide composite powder | |
| CN102993785B (en) | Preparation method for TiO2/opal composite powder material | |
| CN102924980B (en) | Surface modified titanium dioxide particles and preparation method thereof | |
| CN103740139B (en) | Composite titanium dioxide and preparation method thereof | |
| CN105271363B (en) | A kind of preparation method of super fine zinc oxide powder | |
| WO2013020430A1 (en) | Method for preparing high dispersion rutile product | |
| CN101318684A (en) | Method for preparing ultra-fine active nano-calcium carbonate with low-ore grade limestone wet-process activation | |
| CN103756367A (en) | Preparation method of novel coated anatase titanium dioxide | |
| CN103980739A (en) | Multiple modified ultrafine non-metal powder partially replacing titanium dioxide powder, and preparation method thereof | |
| CN101775239A (en) | Preparation method of inorganic composite white pigment with high covering power | |
| WO2010078821A1 (en) | Method for preparing subsphaeroidal barium sulfate by sulfuric acid process and its use in copper foil substrate | |
| CN104495900A (en) | Method for preparing nanometer calcium carbonate powder by mechanochemical method of shells | |
| CN103450712B (en) | Illite-based composite titanium dioxide and preparation method thereof | |
| CN1887973A (en) | Assembling modification and integration process for preparing functional white dye | |
| CN105271344A (en) | Preparation method of pine-cone-shaped calcite type micron-size calcium carbonate particles | |
| CN102616791A (en) | Method for preparing white carbon black from diatomite in situ | |
| CN106543795B (en) | A kind of preparation method for the nano zinc oxide slurry that suspended dispersed is stable | |
| CN101805017B (en) | Preparation method of rutile type titanium dioxide nano particle |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20160525 Termination date: 20170415 |
|
| CF01 | Termination of patent right due to non-payment of annual fee |