CN103642278B - There is titanium system environmental-friendly pigment and the preparation method of composite mineralizer - Google Patents
There is titanium system environmental-friendly pigment and the preparation method of composite mineralizer Download PDFInfo
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- CN103642278B CN103642278B CN201310631786.2A CN201310631786A CN103642278B CN 103642278 B CN103642278 B CN 103642278B CN 201310631786 A CN201310631786 A CN 201310631786A CN 103642278 B CN103642278 B CN 103642278B
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Abstract
There is the titanium system environmental-friendly pigment of composite mineralizer, comprise titanium dioxide 60-80 part, nitrate 15-40 part, composite mineralizer 3-20 part, also comprise antimonous oxide 10-15 part.Preparation method: titanium dioxide or titanium dioxide and antimonous oxide are joined and is dissolved with in the aqueous solution of tensio-active agent, add water-fast mineralizer and nitrate after being uniformly dispersed; Slow dropping alkali lye clear liquor, the nucleation and growth speed of control dropwise reaction speed, nano material and pH value, then ageing, the Nanometer hydroxide pattern making it to be formed on titanium dioxide surface is subsphaeroidal, and particle diameter is at about 25-40nm; Rinsing, makes foreign matter content lower than 20ppm, during solution pH value weakly acidic pH; The mineralizer being dissolved in water is joined the good slurry of rinsing again and carry out spraying dry, then calcined in retort furnace by dried powder, namely obtain bright after insulation, size distribution interval is narrow, the powder pigment of strong coloring force.
Description
Technical field
The present invention relates to field of powder metallurgy preparation, especially relate to the application of composite mineralizer in environmental protection titanium pigment.
Background technology
Energy-saving and emission-reduction problem is more and more subject to the extensive concern of international community, promotes low-carbon environment-friendly product, and strengthening energy-saving and emission-reduction is the important means tackling environment and the shortage of resources gone from bad to worse.At present, product many employings solid-phase process preparation comparatively ripe on market, solid phase method technique is that required starting material are carried out high speed ball milling, then is dried by the powder after ball milling, the techniques such as calcining.This preparation method is low for equipment requirements, and technique is simple and easy to control, and product cost is lower, is therefore adopted by a lot of producer.But, solid phase method technology does not reach the contact of molecular level due to starting material in mechanical milling process, dispersion can be caused uneven, and in the process of calcining, form substitutional solid solution between powder abundant not, on the other hand, part starting material just defined stable crystalline structure before ball milling, in the process of calcining, need higher temperature and soaking time that coloring ion can be made to enter in titanium dioxide lattice, power consumption is serious.Liquid phase method is raw material is at other batch mixing of molecular level, and can reach the dispersed of height, just, strong coloring force, can reduce Calcine Strength to the product look of preparation to a certain extent, but can bring more serious agglomeration traits equally.
Summary of the invention
The object of the invention is to the titanium pigment quality defect existed for prior art, there is provided a kind of product quality excellent, and cost is significantly lower than market-ripe product, what be easy to suitability for industrialized production has the titanium system environmental-friendly pigment of composite mineralizer and the preparation method of this pigment.
The present invention provide firstly a kind of titanium system environmental-friendly pigment with composite mineralizer, comprises the raw material of following weight parts:
Titanium dioxide 60-80 part, nitrate 15-40 part, composite mineralizer 3-20 part.
The titanium system environmental-friendly pigment that the present invention has composite mineralizer also can comprise antimonous oxide 10-15 part further.
Above-mentioned have in the titanium system environmental-friendly pigment of composite mineralizer, described composite mineralizer comprises water-fast mineralizer and water-soluble mineralizer, any one or more than one the combination in zinc oxide or magnesium oxide or cerium oxide or stannic oxide selected by described water-fast mineralizer, and it accounts for the 0.2%-5% of titanium dioxide weight; Described water-soluble mineralizer comprises: account for any one or more than one the combination in the borax of described titanium dioxide weight 0.1%-10% or boric acid or potassiumphosphate, account for the sodium chlorate of titanium dioxide weight 0.1%-0.5%, and account for the sucrose of described titanium dioxide weight 0.4%-5%.
Above-mentioned have in the titanium system environmental-friendly pigment of composite mineralizer, and described nitrate is any one or more than one the combination in nickelous nitrate, chromium nitrate, Jing Ti/Bao Pian COBALT NITRATE CRYSTALS/FLAKES or zinc nitrate.
The titanium system environmental-friendly pigment with composite mineralizer provided by the invention, by adding a certain amount of composite mineralizer in the pigment being major ingredient with titanium dioxide raw material, the dispersion of raw material effectively can be ensured in preparation process, significantly reduce calcining temperature and soaking time to a certain extent, reach effects of energy saving and emission reduction, and can ensure in calcination process, coloring ion can fully enter in titanium dioxide lattice, promote that crystal formation fully transforms, improve the painted quality of product.
The titanium system environmental-friendly pigment preparation technology with composite mineralizer provided by the invention comprises the steps:
(1) take a certain amount of titanium dioxide or titanium dioxide and antimonous oxide by weight, join and be dissolved with in the aqueous solution of tensio-active agent, be uniformly dispersed, then add water-fast mineralizer;
(3) take a certain amount of nitrate by weight, after being added to the water dissolving, pouring in step (1), stir;
(3) by concentration be 0.5-2mol the alkali lye clear liquor of L be slowly added drop-wise in step (2), by controlling dropwise reaction speed, controlling the nucleation and growth speed of nano material, controlling pH value simultaneously, during titration end point to be achieved, stop instillation alkali lye;
(4) after Keep agitation 10-30min, close to stir and carry out ageing to system, the Nanometer hydroxide pattern making it to be formed on titanium dioxide surface is subsphaeroidal, and size is at about 25-40nm;
(5) carry out rinsing to system, remove unnecessary foreign ion, in the process of rinsing, constantly detect the content of foreign ion and the pH value of system in solution, treat that foreign matter content is lower than 20ppm, during solution pH value weakly acidic pH, rinsing is complete;
(6) after the mineralizer being dissolved in water being prepared solution, join the good slurry of rinsing and carry out spraying dry, control spray drying parameters, then dried powder is calcined in retort furnace, after insulation, namely obtain required powder pigment.
In above-mentioned steps:
Described tensio-active agent is Sodium hexametaphosphate 99, accounts for the 0.2-0.5% of titanium dioxide weight.
The technique adding mineralizer in described step (1) is: add water-fast mineralizer zinc oxide or/and magnesium oxide by proportioning, carry out supersound process before interpolation.
In described step (3), the speed of response that alkali lye clear liquor drips controls in 10-15ml/min, and control pH value is 8-11.
In described step (4), digestion time is 24 hours.
The drying parameter of described step (6) is: charging total amount 10-12kg h, in tower, negative pressure is 400-600Kpa, inlet temperature 150-165 DEG C, temperature of outgoing air 60-65 DEG C; Calcining temperature controls at about 900-1200 DEG C, and soaking time is 1-2h.
Compared to solid phase method technique, in preparation technology of the present invention, add different mineralizers, and adopt segmentation add pattern is set, the powder bright obtained, size distribution interval is narrow, strong coloring force; Meanwhile, calcining temperature comparatively solid phase method reduces 100-200 DEG C, reduces cost significantly.Compared to liquid phase method technique, preparation technology of the present invention is easy, reduces workman's cost.
Embodiment
In order to make object of the present invention, technical scheme and advantage clearly understand, below in conjunction with embodiment, the present invention is further elaborated.Should be appreciated that specific embodiment described herein only in order to explain the present invention, be not intended to limit the present invention.
The present invention provide firstly a kind of titanium system environmental-friendly pigment with composite mineralizer, comprises the raw material of following weight parts:
Titanium dioxide 60-80 part, nitrate 15-40 part, composite mineralizer 3-20 part.
In above-mentioned pigment component, by adding a certain amount of mineralizer in the pigment being major ingredient with titanium dioxide raw material, significantly calcining temperature and soaking time can be reduced to a certain extent in preparation process, reach effects of energy saving and emission reduction, and can ensure in calcination process, promote that crystal formation fully transforms, to improve the quality of product.Literature search result shows, does not still have relevant report both at home and abroad at present for the application of composite mineralizer in titanium pigment.
As the more excellent combination of pigment of the present invention, in said components, antimonous oxide 10-15 part also can be added.Add antimonous oxide in temperature raises in follow-up pigment preparation process, antimony peroxide to be changed under the atmosphere that antimonous oxide exists at oxygen, provide electric charge supplementary, avoid occurring lattice imperfection.
Particularly, described composite mineralizer comprises water-fast mineralizer and water-soluble mineralizer, any one or more than one the combination in zinc oxide or magnesium oxide or cerium oxide or stannic oxide selected by wherein said water-fast mineralizer, and it accounts for the 0.2%-5% of titanium dioxide weight; Described water-soluble mineralizer comprises: account for any one or more than one the combination in the borax of titanium dioxide weight 0.1%-10% or boric acid or potassiumphosphate, account for the sodium chlorate of titanium dioxide weight 0.1%-0.5% and account for the sucrose of titanium dioxide weight 0.4%-5%.
Wherein, zinc oxide, magnesium oxide, cerium oxide, stannic oxide or its combination can add when powder pigment synthesis in early stage, can promote that coloring ion enters in the octahedra lattice of titanium dioxide.Adding of borax can promote that lattice transforms, and reduces calcining temperature 100 DEG C-200 DEG C in preparation process; Sodium chlorate can make in calcination process, releasing oxygen, makes calcining be in oxygen enrichment atmosphere, avoids producing lattice imperfection; Sucrose can select organic sucrose; powder is when carrying out spraying dry; sucrose pyrolytic decomposition; the protective membrane of one deck densification can be formed at nano powder surface; hinder growing up further of nanoparticle self, meanwhile, the existence of nano-carbon film; significantly can reduce the reunion of powder, improve the dispersiveness of powder.
Particularly, described nitrate is one or more in nickelous nitrate, chromium nitrate, Jing Ti/Bao Pian COBALT NITRATE CRYSTALS/FLAKES or zinc nitrate, and above-mentioned nitrate has coloring ion R
+(Ni
2+, Cr
3+, Co
2+, Zn
2+).Select nitrate to be to be formed with alkali lye when precipitating, it is little and precipitate uniformly that monovalent salt more easily forms particle diameter.
Present invention also offers a kind of titanium system environmental-friendly pigment preparation method with composite mineralizer, specifically comprise the steps:
(1) take a certain amount of titanium dioxide or titanium dioxide and antimonous oxide by above-mentioned weight part, join and be dissolved with in the aqueous solution of tensio-active agent, be uniformly dispersed, then add the water-fast mineralizer of part.Wherein said tensio-active agent is Sodium hexametaphosphate 99, it is the 0.2-0.5% of titanium dioxide quality, can be used as dispersion agent, and the surface tension of titanium dioxide raw material is reduced, titanium dioxide and not water-fast mineralizer can be made to disperse in the solution uniformly, and make the state that the particulate after dispersion keeps stable.The concrete technology adding mineralizer can be: add water-fast mineralizer zinc oxide or/and magnesium oxide by proportioning, carry out supersound process before interpolation.
(2) take a certain amount of nitrate by proportioning, after being added to the water dissolving, pouring in step (1), stir;
(3) by concentration be 0.5-2mol the alkali lye clear liquor (sodium hydroxide or other oxyhydroxide) of L be slowly added drop-wise in step (2), by controlling dropwise reaction speed in 10-15ml/min, to control the nucleation and growth speed of nano material, when controlling pH value 8-12 titration end point to be achieved, stop instillation alkali lye simultaneously.
The dropping of alkali lye has activated the surface tissue of titanium dioxide on the one hand, changes the acid-basicity of system, makes its surface form great amount of hydroxy group chemical bond, as the coloring ion R of its instillation nitrate
+(Ni
2+, Cr
3+, Co
2+, Zn
2+) time, coloring ion R
+can be uniform at titanium dioxide surface deposition, form fine and close coating film, form Ti-O-R
+chemical bond, when later stage high-temperature calcination, coloring ion can enter in titanium dioxide lattice uniformly, forms substitutional solid solution, reduces calcining temperature, save energy; And when titanium dioxide surface processes, the surface of the titanium dioxide after process can be made to form the more weak sodium titanate of alkalescence, be conducive to reducing speed of response, control nano material fineness.
(4) after Keep agitation 10-30min, close and stir, solution is placed ageing in 24 hours in air, the nano-sized nickel hydroxide pattern making it to be formed on titanium dioxide surface is subsphaeroidal, and size is at about 25-40nm;
(5) carry out rinsing to solution, go out except undesired impurities ion, in the process of rinsing, constantly detect the content of foreign ion and the pH value of system in solution, treat that foreign matter content is lower than 20ppm, during solution pH value weakly acidic pH, rinsing is complete;
(6) after the mineralizer being dissolved in water being prepared solution, join the good slurry of rinsing and carry out drying process with atomizing, control spray drying parameters: charging total amount 10-12kg h, in tower, negative pressure is 400-600Kpa, inlet temperature 150-165 DEG C, temperature of outgoing air 60-65 DEG C.Then calcined in retort furnace by dried powder, calcining temperature controls at about 900-1200 DEG C, obtains required powder after insulation 1-2h.
In above-mentioned preparation method, what mineralizer adopted segmentation to add arranges pattern, first water-fast mineralizer is added when powder synthesizes in earlier stage, by controlling reaction conditions, the existence of mineralizer adjustable reaction system on the one hand can be made like this, promote the carrying out of reaction, on the other hand, mineralizer itself reaches the object of uniform dispersion; Secondly, in the process of drying, because nano-powder there will be agglomeration traits, water-soluble mineralizer was added before the drying of powder later stage, fine and close carbon coating film can be formed in xeraphium surface, inhibit the reunion of nano material, finally obtain particle diameter little, the powder of good dispersity; 3rd. adding of the zwitterion mineralizer of small radii, when powder high-temperature calcination, the conversion of rutile-type can be promoted, be conducive to forming substitutional solid solution, significantly reduce calcining temperature; 4th, have adding of the mineralizer of oxidisability, when high-temperature calcination, meeting release portion oxygen, makes calcining system be in the atmosphere of oxygen enrichment, crystal formation is fully transformed, reduce calcining temperature, reduce calcination time.
Below in conjunction with specific embodiment, the present invention is further described.
Embodiment 1:
1) join in 750ml water by 65g titanium dioxide and 10g antimonous oxide respectively, 30g nickelous nitrate joins in 300ml water, for subsequent use after nickel nitrate solution clarification;
2) join after taking the sodium hexametaphosphate solution of titanium dioxide weight 0.2% in the mixed solution of titanium dioxide, dispersion 0.5h is carried out to it.
3) in step 2) in add magnesium oxide 0.3g, zinc oxide 0.3g, cerium oxide 0.4, stannic oxide 0.3, be uniformly dispersed before magnesium oxide, zinc oxide, cerium oxide, stannic oxide in ultrasonic;
4) in step 2) in add the nickel nitrate solution dissolved, stir 10-30min;
5) by the concentration prepared be 0.5-2mol the sodium hydroxide clear liquor of L be added drop-wise in step 4) nickel nitrate solution slowly, control rate of addition is 15ml/min, treat that nickelous nitrate precipitation terminates, stop sodium hydroxide clear liquor to drip, regulate reacting system PH value about 8;
6) after Keep agitation 10min, ageing 24h, the nano-sized nickel hydroxide pattern that titanium dioxide surface is formed is subsphaeroidal, even particle size distribution, and size is at about 20nm;
7) solution repetitive scrubbing step 6) prepared three times, detects solution pH value to neutral, foreign ion NO
3when-content is lower than 20ppm, rinsing terminates;
8) water-soluble mineralizer is weighed, wherein sodium chlorate 0.3g, borax 3g, sucrose 3.0g, join in the good solution of rinsing;
9) solution of step 8) gained is carried out spray drying treatment, control drying parameter: charging total amount 10kg h, in drying tower, negative pressure is 500Kpa, inlet temperature 165 DEG C, temperature of outgoing air 65 DEG C;
10) dried powder is put into retort furnace to calcine, heat-up rate be 5 DEG C min, be warming up to 900 DEG C, insulation 1h, namely obtain required powder pigment.
Embodiment 2:
1) join in 850ml water by 75g titanium dioxide and 10g antimonous oxide respectively, 20g nickelous nitrate joins in 200ml water, for subsequent use after nickel nitrate solution clarification;
2) join after taking the sodium hexametaphosphate solution of titanium dioxide weight 0.3% in the mixed solution of titanium dioxide, dispersion 0.5h is carried out to it.
3) in step 2) in add magnesium oxide 0.25g, zinc oxide 0.25g, cerium oxide 0.4, be uniformly dispersed in ultrasonic before magnesium oxide and zinc oxide, cerium oxide;
4) in step 2) in add the nickel nitrate solution dissolved, stir 10-30min;
5) by the concentration prepared be 0.5-2mol the sodium hydroxide clear liquor of L be added drop-wise in step 4) nickel nitrate solution slowly, control rate of addition is 15ml/min, treat that nickelous nitrate precipitation terminates, stop sodium hydroxide clear liquor to drip, regulate reacting system PH value about 9;
6) after Keep agitation 15min, ageing 24h, the nano-sized nickel hydroxide pattern that titanium dioxide surface is formed is subsphaeroidal, even particle size distribution, and size is at about 35nm;
7) solution repetitive scrubbing step 6) prepared three times, detects solution pH value to neutral, foreign ion NO
3when-content is lower than 20ppm, rinsing terminates;
8) water-soluble mineralizer is weighed, wherein sodium chlorate 0.25g, borax 0.75g, boric acid 1g, sucrose 3g, join in the good solution of rinsing;
9) solution of step 8) gained is carried out spray drying treatment, control drying parameter: charging total amount 12kg h, in drying tower, negative pressure is 500Kpa, inlet temperature 165 DEG C, temperature of outgoing air 65 DEG C;
10) dried powder is put into retort furnace to calcine, heat-up rate be 5 DEG C min, be warming up to 1000 DEG C, insulation 1.5h, namely obtain required powder pigment.
Embodiment 3:
1) join in 950ml water by 80g titanium dioxide and 15g antimonous oxide, 15g chromium nitrate joins in 150ml water, for subsequent use after chromium nitrate solution clarification;
2) join after taking the sodium hexametaphosphate solution of titanium dioxide weight 0.4% in the mixed solution of titanium dioxide, dispersion 0.5h is carried out to it;
3) in step 2) in add magnesium oxide 1.0g, zinc oxide 1.0g.Be uniformly dispersed in ultrasonic before magnesium oxide, zinc oxide;
4) in step 2) in add the chromium nitrate solution dissolved, stir 10-30min;
5) by the concentration prepared be 0.5-2mol the potassium hydroxide clear liquor of L be added drop-wise in step 4) chromium nitrate solution slowly, control rate of addition is 10ml/min, treat that chromium nitrate precipitation terminates, stop potassium hydroxide clear liquor to drip, regulate reacting system PH value about 10;
6) after Keep agitation 20min, ageing 24h, the nanometer chromium hydroxide pattern that titanium dioxide surface is formed is subsphaeroidal, even particle size distribution, and size is at about 40nm;
7) solution repetitive scrubbing step 6) prepared three times, detects solution pH value to neutral, foreign ion NO
3-content is lower than 20ppm, and rinsing terminates;
8) water-soluble mineralizer is weighed, wherein sodium chlorate 0.4g, borax 1.5g, potassiumphosphate 1.5g, sucrose 4g, join in the good solution of rinsing;
9) slurry in step 8) is carried out spray drying treatment, control drying parameter: charging total amount 11kg h, in drying tower, negative pressure is 600Kpa, inlet temperature 155 DEG C, temperature of outgoing air 60 DEG C;
10) dried powder is put into retort furnace to calcine, heat-up rate be 5 DEG C min, be warming up to 1100 DEG C, insulation 2h, namely obtain required powder pigment.
Embodiment 4:
1) join in 700ml water by 70g titanium dioxide respectively, 10g nickelous nitrate, 15g Jing Ti/Bao Pian COBALT NITRATE CRYSTALS/FLAKES, 10g zinc nitrate joins in 350ml water, nickelous nitrate, Jing Ti/Bao Pian COBALT NITRATE CRYSTALS/FLAKES, for subsequent use after zinc nitrate solution clarification;
2) join after taking the sodium hexametaphosphate solution of titanium dioxide weight 0.5% in the mixed solution of titanium dioxide, dispersion 0.5h is carried out to it;
3) in step 2) in add titanium dioxide content magnesium oxide 1.5g, zinc oxide 1.5g.Magnesium oxide, is uniformly dispersed before zinc oxide in ultrasonic;
4) in step 2) in add the nickelous nitrate dissolved, Jing Ti/Bao Pian COBALT NITRATE CRYSTALS/FLAKES and zinc nitrate solution, stir 10-30min;
5) by the concentration prepared be 0.5-2mol the sodium hydroxide clear liquor of L be added drop-wise to step 4) nickelous nitrate slowly, in Jing Ti/Bao Pian COBALT NITRATE CRYSTALS/FLAKES and zinc nitrate solution, control rate of addition is 10ml/min, treat that nickelous nitrate, Jing Ti/Bao Pian COBALT NITRATE CRYSTALS/FLAKES and zinc nitrate precipitation terminates, stop sodium hydroxide clear liquor to drip, regulate reacting system PH value about 10;
6) after Keep agitation 30min, ageing 24h, the nano-sized nickel hydroxide that titanium dioxide surface is formed, cobaltous hydroxide, zinc hydroxide pattern are subsphaeroidal, even particle size distribution, and size is at about 30nm; 7) solution step 6) prepared, by slurry repetitive scrubbing three times, detects solution pH value to neutral, foreign ion NO
3-content is lower than 20ppm, and rinsing terminates;
8) water-soluble mineralizer is weighed, wherein sodium chlorate 0.35g, borax 0.5g, boric acid 0.5g, potassiumphosphate 0.5g, sucrose 3.5g, join in the good solution of rinsing;
9) slurry in step 8) is carried out spray drying treatment, control drying parameter: charging total amount 12kg h, in drying tower, negative pressure is 400Kpa, inlet temperature 160 DEG C, temperature of outgoing air 65 DEG C.
10) dried powder is put into retort furnace to calcine, heat-up rate be 5 DEG C min, be warming up to 1200 DEG C, insulation 2h, namely obtain required powder pigment.
The foregoing is only preferred embodiment of the present invention, not in order to limit the present invention, all any amendments done within the spirit and principles in the present invention, equivalent replacement and improvement etc., all should be included within protection scope of the present invention.
Claims (9)
1. there is a titanium system environmental-friendly pigment for composite mineralizer, it is characterized in that, comprise the raw material of following weight parts:
Titanium dioxide 60-80 part, nitrate 15-40 part, composite mineralizer 3-20 part;
Described composite mineralizer comprises water-fast mineralizer and water-soluble mineralizer, any one or more than one the combination in zinc oxide or magnesium oxide or cerium oxide or stannic oxide selected by described water-fast mineralizer, and it accounts for the 0.2%-5% of titanium dioxide weight; Described water-soluble mineralizer comprises: account for the borax of titanium dioxide weight 0.1%-10% or any one or more than one the combination of boric acid or potassiumphosphate, account for the sodium chlorate of titanium dioxide weight 0.1%-0.5%, and account for the sucrose of titanium dioxide weight 0.4%-5%.
2. the titanium system environmental-friendly pigment with composite mineralizer according to claim 1, is characterized in that, also comprise antimonous oxide 10-15 part.
3. the titanium system environmental-friendly pigment with composite mineralizer according to claim 1 and 2, is characterized in that, described nitrate is any one or more than one the combination in nickelous nitrate, chromium nitrate, Jing Ti/Bao Pian COBALT NITRATE CRYSTALS/FLAKES or zinc nitrate.
4. the titanium system environmental-friendly pigment preparation method with composite mineralizer as described in any one of claim 1-3, is characterized in that, comprise the steps:
(1) take a certain amount of titanium dioxide or titanium dioxide and antimonous oxide by weight, join and be dissolved with in the aqueous solution of tensio-active agent, be uniformly dispersed, then add water-fast mineralizer;
(2) take a certain amount of nitrate by weight, after being added to the water dissolving, pouring in step (1), stir;
(3) be that the alkali lye clear liquor of 0.5-2mol/L is slowly added drop-wise in step (2) by concentration, by controlling dropwise reaction speed, control the nucleation and growth speed of nano material, simultaneously control ph, during titration end point to be achieved, stop instillation alkali lye;
(4) after Keep agitation 10-30min, close to stir and carry out ageing to system, the Nanometer hydroxide pattern making it to be formed on titanium dioxide surface is subsphaeroidal, and size is at 25-40nm;
(5) carry out rinsing to system, remove unnecessary foreign ion, in the process of rinsing, constantly detect the content of foreign ion and the pH value of system in solution, treat that foreign matter content is lower than 20ppm, solution ph is to time neutral, and rinsing is complete;
(6) after the mineralizer being dissolved in water being prepared solution, join the good slurry of rinsing and carry out spraying dry, control spray drying parameters, then dried powder is calcined in retort furnace, after insulation, namely obtain required powder pigment.
5. the titanium system environmental-friendly pigment preparation method with composite mineralizer according to claim 4, it is characterized in that, described tensio-active agent is Sodium hexametaphosphate 99, accounts for the 0.2-0.5% of titanium dioxide weight.
6. there is the titanium system environmental-friendly pigment preparation method of composite mineralizer as claimed in claim 4, it is characterized in that, the technique adding mineralizer in described step (1) is: add water-fast mineralizer zinc oxide or/and magnesium oxide by proportioning, carry out supersound process before interpolation.
7. have the titanium system environmental-friendly pigment preparation method of composite mineralizer as claimed in claim 4, it is characterized in that: in described step (3), the speed of response that alkali lye clear liquor drips controls in 10-15mL/min, and control ph is 8-11.
8. there is the titanium system environmental-friendly pigment preparation method of composite mineralizer as claimed in claim 4, it is characterized in that, in described step (4), digestion time is 24 hours.
9. there is the titanium system environmental-friendly pigment preparation method of composite mineralizer as claimed in claim 4, it is characterized in that: described step (6) drying parameter: charging total amount 10-12kg/h, in tower, negative pressure is 400-600KPa, inlet temperature 150-165 DEG C, temperature of outgoing air 60-65 DEG C; Calcining temperature controls at 900-1200 DEG C, and soaking time is 1-2h.
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| GB534538A (en) * | 1938-09-08 | 1941-03-10 | Du Pont | Improvements in and relating to the production of titanium pigments |
| CN1044668A (en) * | 1989-09-02 | 1990-08-15 | 孙秀玲 | The manufacture method of blue inorganic pigment |
| CN1234057A (en) * | 1996-10-04 | 1999-11-03 | 千年无机化学品股份有限公司 | Method for preparing coloured pigments with titanium dioxide base |
| CN101029187A (en) * | 2006-03-03 | 2007-09-05 | 攀钢集团攀枝花钢铁研究院 | High-dispersed titanium pigment and its production |
| CN101429348A (en) * | 2008-12-12 | 2009-05-13 | 江苏河海纳米科技股份有限公司 | Process for producing nano-titanium dioxide-zinc oxide composite powder |
| CN102500375A (en) * | 2011-09-28 | 2012-06-20 | 江苏科技大学 | Method for preparing titanium dioxide codoped with boron and metal element |
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