CN101469140B - Preparation of active titanium dioxide - Google Patents
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- CN101469140B CN101469140B CN2007103078629A CN200710307862A CN101469140B CN 101469140 B CN101469140 B CN 101469140B CN 2007103078629 A CN2007103078629 A CN 2007103078629A CN 200710307862 A CN200710307862 A CN 200710307862A CN 101469140 B CN101469140 B CN 101469140B
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Abstract
The invention provides a method for preparing activated titanium pigment. The method comprises the contact between titanium pigment and a plating solution in a form of impact flow; the plating solution contains optical titanium, a solvent, a stabilizing agent and dimethyl silicon oil; the weight ratio of the optical titanium to the solvent to the stabilizing agent to the dimethyl silicon oil is (1.3-30):(10-50):(8-27):100. The activity index of the activated titanium pigment prepared through the embodiment of the method is between 70 and 99 percent and is obviously higher than the activity of commercially-purchased unactivated titanium pigment of between 15 and 19 percent.
Description
Technical field
The invention relates to a kind of preparation method of active titanium dioxide.
Background technology
Generally titanium oxide is called white titanium pigment in the industry; White titanium pigment adularescent pigment king's title; Have characteristics such as nontoxic, high whiteness, high refractive index, physicochemical property are stable; And the superfine titanium white body has characteristics such as the UVA function is strong, visible light permeability good, chemically reactive height can be used for preparing UV light absorber, photocatalyst, makeup, high-grade paint etc.But the white titanium pigment seed activity that is purchased is lower, and its sterilization, deodorizing, effect such as anticorrosion are relatively poor, therefore have and must carry out surface-treated to it, it is become have surface-active filler.But at present, the preparation method of " active titanium dioxide " does not also appear in the newspapers.
Summary of the invention
The objective of the invention is provides the preparation method of the higher active titanium dioxide of a kind of activity in order to overcome the present lower defective of white titanium pigment activity.
The invention provides a kind of preparation method of active titanium dioxide; Wherein, This method comprises makes white titanium pigment contact with the form of plating bath with percussion flow; Said plating bath contains light titanium, solvent, stablizer, dimethyl silicone oil, and the weight ratio of light titanium, solvent, stablizer and membrane-forming agent is (1.3-30): (10-50): (8-27): 100.
The present invention contacts with plating bath through making white titanium pigment, makes that the white titanium pigment after the contact has activity, becomes active titanium dioxide.According to preferred implementation of the present invention,, can obviously improve the activity of gained active titanium dioxide through reducing the particle dia of white titanium pigment.Through reducing the content of the metallic impurity such as iron in the white titanium pigment, can further make active titanium dioxide be applied to makeup, high-grade paint etc., thereby widen the range of application of white titanium pigment.
Can know that from the activity index test result activity index of the active titanium dioxide of embodiment of the invention 1-9 preparation is 70-99%, apparently higher than the activity of the 15-19% of the non-activated white titanium pigment that is purchased.
Embodiment
The invention provides a kind of preparation method of active titanium dioxide; Wherein, This method comprises makes white titanium pigment contact with the form of plating bath with percussion flow; Said plating bath contains light titanium, solvent, stablizer, dimethyl silicone oil, and the weight ratio of light titanium, solvent, stablizer and membrane-forming agent is (1.3-30): (10-50): (8-27): 100.
The weight ratio of said white titanium pigment and plating bath can be 100: 2-10.
Wherein, Said smooth titanium has been conventionally known to one of skill in the art; Being a kind ofly can the Conversion of energy of the light photocatalyst for preparation hydroxyl free radical and negative oxygen ion institute energy requirement mainly be contained nano titanium oxide, is benchmark with the total amount of light titanium; The content of said titanium oxide is 40-80 weight %, and this smooth titanium can be commercially available.For example, can protect Science and Technology Ltd. available from Guangzhou light titanium subring.Said solvent can be absolute ethyl alcohol, and said stablizer can be sodium hypophosphite, and said membrane-forming agent can be dimethyl silicone oil.
The condition of said contact comprises that the contact temperature is 55-100 ℃, and the time is 2-10 minute, and the speed of percussion flow is the 2-3.8 Mach number, is preferably the 2.2-3.0 Mach number; Said Mach number is meant the fluid velocity of percussion flow and the ratio of local velocity of sound.
The present invention contacts with the form of plating bath with percussion flow through making white titanium pigment under these conditions, makes plating bath fully to contact with white titanium pigment, gives the white titanium pigment activity.
Said white titanium pigment and plating bath can contact in any instrument that can form percussion flow, and preferred said contact is carried out in fluidized bed jet mill, and said fluidized bed jet mill can be commercially available.
When in fluidized bed jet mill, carrying out, control following parameter and can realize the object of the invention, input speed is that 60-250 rev/min, stream pressure are that 0.5-1.2 MPa, air flow rate are the 5-12 cubic meters per minute; The contact temperature is 55-100 ℃; Said air-flow is a dry air stream, in general, and when under identical condition, preparing active titanium dioxide; The water cut of airflow is low more; Then the activity of the active titanium dioxide of preparation is high more, and the water cut of said dry air stream generally can be 0.01-0.2 weight %, and preferred water content is 0.01-0.15 weight %.This dry air stream obtains after for example can having heat regeneration compressed air drier with the air heating drying with the QZ-12/12A type.When the active titanium dioxide of said preparation is used for makeup, preferably air is being carried out oil removing, removal of impurities with before the dry air.Concrete oil removing, impurity-removing method have been conventionally known to one of skill in the art, repeat no more at this.
Said white titanium pigment can be the anatase thpe white powder of coating not and/or the Rutile type Titanium Dioxide of coating not, and in general, anatase thpe white powder is softer, and Rutile type Titanium Dioxide is harder, therefore, as makeup the time, preferably uses anatase thpe white powder; As purposes such as UV light absorber, photocatalyst, high-grade paint the time, can use anatase thpe white powder and/or Rutile type Titanium Dioxide.
The anatase thpe white powder of said not coating can be commercially available or make through following method; Preferably make the not anatase thpe white powder of coating through following method; The preparation method of said anatase thpe white powder comprises the mixture calcining back grinding that contains metatitanic acid, salt of wormwood, Sodium hexametaphosphate 99 and phosphoric acid; Said calcining comprises earlier calcined 2-3 hour down at 150-580 ℃; Calcined 2.5-3 hour down at 590-790 ℃, the weight ratio of metatitanic acid, salt of wormwood, Sodium hexametaphosphate 99 and phosphoric acid is 100 in the said mixture: (0.2-1.6): (0.3-1.8): (0.1-0.8) again.Product after the calcining can confirm to contain in the product anatase thpe white powder through the XRD spectrum map analysis.
Above-mentioned metatitanic acid is the intermediate product of method for producing gtitanium dioxide with sulphuric acid, is available commercially.
Compare with the white titanium pigment that is purchased, use the white titanium pigment of metatitanic acid preparation more to be prone to realize less particle dia and dispersed preferably.
According to the present invention, as long as according to method provided by the invention, white titanium pigment is contacted with the form of plating bath with percussion flow, can realize the active purpose of raising white titanium pigment of the present invention; But; Activity for the active titanium dioxide that improves preparation; The average particle diameter of the anatase thpe white powder of coating and Rutile type Titanium Dioxide is not preferably 50-400 nanometer (the white titanium pigment median size of the not coating that is purchased in general, is the 500-700 nanometer) separately; But, when the makeup, the more preferably average particle diameter of the anatase thpe white powder of coating and the Rutile type Titanium Dioxide 150-250 nanometer of respectively doing for oneself not, and the median size of the active anatase thpe white powder of preferred preparation is the 200-300 nanometer.
The white titanium pigment of the anatase thpe white powder of the not coating of above-mentioned granularity and/or white titanium pigment that Rutile type Titanium Dioxide of coating can be through the not coating that will be purchased or the not coating that makes through above-mentioned use metatitanic acid grinds in the presence of grinding aid and solvent and obtains; Said abrasive method can be for well known to a person skilled in the art any method, if the anatase thpe white powder of said not coating and/or not the Rutile type Titanium Dioxide of coating reach above-mentioned particle diameter.
During grinding, the weight ratio of said white titanium pigment, grinding aid and solvent can be (57-77): (0.2-0.6): 100, and said grinding aid can be Sodium hexametaphosphate 99, said solvent is a water, is preferably deionized water.
The present invention does not have special qualification for the purity of anatase thpe white powder and/or Rutile type Titanium Dioxide; But, as makeup the time, higher to the purity requirement of white titanium pigment; The content of iron is no more than 30ppm in the active titanium dioxide after the preferred activation, and does not contain harmful material.The present invention to the anatase thpe white powder of coating not and/or not the water cut of the Rutile type Titanium Dioxide of coating certain restriction is arranged, the content of preferably water is 0.01-1.5 weight %, more preferably 0.01-1 weight %.
In general; The anatase thpe white powder of the not coating that is purchased and not the major impurity in the Rutile type Titanium Dioxide of coating be red oxide of iron, manganese, Vanadium Pentoxide in FLAKES, sulfate ion etc.; Wherein, The content of ferric ion is greater than 30ppm to 150ppm, therefore, is no more than 30ppm as long as the content of ferric ion dropped to.Partial impurities in the anatase thpe white powder of the not coating that can will be purchased through following method and the anatase thpe white powder that do not obtain after Rutile type Titanium Dioxide and the metatitanic acid calcining that is purchased of coating is removed, and reaches above-mentioned purity requirement.
Above-mentioned purity not coating anatase thpe white powder and/or not the preparation method of the Rutile type Titanium Dioxide of coating comprise white titanium pigment bleached the removal of impurities after drying.The method of said bleaching removal of impurities comprises white titanium pigment is contacted in water with SYNTHETIC OPTICAL WHITNER; Washing, filtration and drying obtain solid product, preferably white titanium pigment are contacted in deionized water with SYNTHETIC OPTICAL WHITNER, and the temperature of said contact is 50-90 ℃; Be 0.5-0.8 hour duration of contact; The pH of the mixed solution of white titanium pigment, SYNTHETIC OPTICAL WHITNER and water is 1-6, and preferred pH is 3-5, and the weight ratio of said white titanium pigment, SYNTHETIC OPTICAL WHITNER and water is 100: (0.2-1.6): (66-200).Can fully contact and wash the back with SYNTHETIC OPTICAL WHITNER at white titanium pigment and regulate mixture according to the difference of the purposes of the active titanium dioxide after the activation, be the pH of the active titanium dioxide of preparation to required pH, for example can be with the pH regulator of this mixture to 6-9.Said drying can be for well known to a person skilled in the art the whole bag of tricks, and preferred drying means comprises the white titanium pigment after the bleaching removal of impurities with the pressure filter after drying that dewaters.
The whiteness of above-mentioned bleaching removal of impurities and dried anatase thpe white powder is greater than 96% to 98%, can reach that whiteness is the requirement more than 96% in the makeup.Whiteness can record with blancometer.
Said exsiccant method can be for well known to a person skilled in the art the whole bag of tricks, and preferred drying means comprises the white titanium pigment after the bleaching removal of impurities with the pressure filter after drying that dewaters.
Said SYNTHETIC OPTICAL WHITNER can be tin protochloride, is preferably the technical grade tin protochloride.
In general; Lump easily through dried white titanium pigment, therefore, contact more fully with plating bath in order to make white titanium pigment; Preferably before plated film coats, dried white titanium pigment is hit carefully below 120 orders, under 80-150 ℃ of condition, hit carefully with hammer slice type loose powder machine in the embodiment of the invention.
Activity described in the present invention is to measure according to the activity index testing method among the embodiment, and as conventionally known to one of skill in the art, activity index is high more, and then white titanium pigment and organic consistency are good more, dispersiveness is good more, flowability is good more and wetting ability is poor more.The active titanium dioxide of the present invention's preparation can be used for every field, for example, can be used to prepare UV light absorber, photocatalyst, makeup, high-grade paint, particular adhesive, seabed water-proof cable coating etc.
To do further description to the present invention through embodiment below.
Embodiment 1
Present embodiment is used to explain the preparation method of active titanium dioxide provided by the invention.
With 3000 gram average particle diameters is that the average particle diameter that use is ground to white titanium pigment in pump delivery to the JWS-30 sand Mill was 400 nanometers after the deionized water of Rutile type Titanium Dioxide (productions of Shandong Dong Jia company), 10.4 gram Sodium hexametaphosphate 99s, 5200 grams of the not coating of 700 nanometers mixed.And then the white titanium pigment after levigate is used pressure filter dehydration after drying to water cut is 1 weight %.
Deliver to after the above-mentioned levigate and dried Rutile type Titanium Dioxide of 2500 grams, 0.6 gram light titanium (Guangzhou light titanium subring protect Science and Technology Ltd. produce), 4.4 gram absolute ethyl alcohols, 3.6 gram sodium hypophosphites and 40 gram dimethyl silicone oils (Chinese magnificent source chemical company produce) are mixed during FJM-400 type fluidized bed gas grinds; Spiral quantitative charging and airshed are carried out synchronously; Control spiral quantitative input speed is 60 rev/mins; The water cut of dry air stream is 0.15 weight %, and stream pressure is 0.5 MPa, air flow rate 5 cubic meters per minute; The contact temperature is 55 ℃; Time is 2 minutes, and the speed of the percussion flow of white titanium pigment and plating bath is 2.2 Mach numbers, and zirconium sheet grading wheel rotating speed is 5500 rev/mins.At last the white titanium pigment after the activation is discharged to deliver in the pulse receipts powder jar from the airduct of fluidized-bed and receive powder, promptly obtaining particle dia of the present invention is the active titanium dioxide A1 below 430 nanometers.
Embodiment 2
Present embodiment is used to explain the preparation method of active titanium dioxide provided by the invention.
With 3000 gram average particle diameters is that using the average particle diameter that is ground to white titanium pigment in pump delivery to the JWS-30 sand Mill was 80 nanometers after the deionized water of anatase thpe white powder (Jiangxi add light company produce), 23.4 gram Sodium hexametaphosphate 99s, 3900 grams of the not coating of 500 nanometers mixed.And then the white titanium pigment after levigate is used pressure filter dehydration after drying to water cut is 0.01 weight %, it is hit carefully to 120 orders with hammer slice type loose powder machine down at 120 ℃ then.
Deliver to after the above-mentioned levigate and dried anatase thpe white powder of 2500 grams, 34.8 gram light titaniums (Guangzhou light titanium subring is protected Science and Technology Ltd. and produced), 58.8 gram absolute ethyl alcohols, 31.2 gram sodium hypophosphites and 120 gram dimethyl silicone oils (Chinese magnificent source chemical company produce) are mixed during FJM-400 type fluidized bed gas grinds; Spiral quantitative charging and airshed are carried out synchronously; Control spiral quantitative input speed is 150 rev/mins; The water cut of dry air stream is 0.01 weight %, and stream pressure is 0.8 MPa, and air flow rate is 9 cubic meters per minute; The contact temperature is 80 ℃; Time is 6 minutes, and the speed of the percussion flow of white titanium pigment and plating bath is 3.0 Mach numbers, and zirconium sheet grading wheel rotating speed is 15000 rev/mins.At last the white titanium pigment after the activation is discharged to deliver in the pulse receipts powder jar from the airduct of fluidized-bed and receive powder, promptly obtaining particle dia of the present invention is the active titanium dioxide A2 below 100 nanometers.
Embodiment 3
Present embodiment is used to explain the preparation method of active titanium dioxide provided by the invention.
With 3000 gram average particle diameters is that the metatitanic acid (Yunnan rich people's titanium powder plant) of 600 nanometers, the mixture that 6 gram salt of wormwood, 9 restrain Sodium hexametaphosphate 99s and 3 gram phosphoric acid are warmed up to 650 ℃ in calcining under 300 ℃ after 2.5 hours again, calcines 2.5 hours down at 650 ℃.Product after the calcining is measured with X-ray diffractometer, obtained XRD spectrum figure, analyze this collection of illustrative plates, can confirm to contain in the product anatase thpe white powder.
After the deionized water of the product that contains anatase thpe white powder of the above-mentioned preparation of 3000 grams, 18.4 gram Sodium hexametaphosphate 99s, 4600 grams mixed, using the average particle diameter that is ground to white titanium pigment in pump delivery to the JWS-30 sand Mill was 250 nanometers.And then the white titanium pigment after levigate is used pressure filter dehydration after drying to water cut is 0.5 weight %, it is hit carefully to 120 orders with hammer slice type loose powder machine down at 120 ℃ then.
Above-mentioned the hitting of 2500 grams after mixing, product after thin, 15 gram light titaniums (Guangzhou light titanium subring protect Science and Technology Ltd. produce), 25 gram absolute ethyl alcohols, 18 gram sodium hypophosphites and 100 gram dimethyl silicone oils (Chinese magnificent source chemical company produce) delivered to during FJM-400 type fluidized bed gas grinds; Spiral quantitative charging and airshed are carried out synchronously; Control spiral quantitative input speed is 250 rev/mins; The water cut of dry air stream is 0.08 weight %, and stream pressure is 1.2 MPas, and air flow rate is 12 cubic meters per minute; The contact temperature is 100 ℃; Time is 10 minutes, and the speed of the percussion flow of white titanium pigment and plating bath is 2.6 Mach numbers, and zirconium sheet grading wheel rotating speed is 6800 rev/mins.At last the white titanium pigment after the activation is discharged to deliver in the pulse receipts powder jar from the airduct of fluidized-bed and receive powder, promptly obtaining particle dia of the present invention is the active titanium dioxide A3 below 300 nanometers.
Embodiment 4
Present embodiment is used to explain the preparation method of active titanium dioxide provided by the invention.
With 3000 gram average particle diameters is that the metatitanic acid (Baise of Guangxi titanium powder plant) of 600 nanometers, the mixture that 48 gram salt of wormwood, 54 restrain Sodium hexametaphosphate 99s and 24 gram phosphoric acid are warmed up to 600 ℃ in calcining under 180 ℃ after 3 hours again, calcines 3 hours down at 600 ℃.Product after the calcining is measured with X-ray diffractometer, obtained XRD spectrum figure, analyze this collection of illustrative plates, can confirm to contain in the product anatase thpe white powder.
The product that contains anatase thpe white powder according to preparing with embodiment 3 identical methods is levigate, dry and hit thin back and in fluidized bed jet mill, contact with plating bath, making particle dia of the present invention is the following active titanium dioxide A4 of 300 nanometers.
Embodiment 5
Present embodiment is used to explain the preparation method of active titanium dioxide provided by the invention.
With 3000 gram average particle diameters is that the metatitanic acid (Teng County, Guangxi titanium powder plant) of 600 nanometers, the mixture that 24 gram salt of wormwood, 30 restrain Sodium hexametaphosphate 99s and 12 gram phosphoric acid are warmed up to 790 ℃ in calcining under 580 ℃ after 2 hours again, calcines 2.5 hours down at 650 ℃.Product after the calcining is measured with X-ray diffractometer, obtained XRD spectrum figure, analyze this collection of illustrative plates, can confirm to contain in the product anatase thpe white powder.
The product that contains anatase thpe white powder according to preparing with embodiment 3 identical methods is levigate, dry and hit thin back and in fluidized bed jet mill, contact with plating bath, making particle dia of the present invention is the following active titanium dioxide A5 of 300 nanometers.
Embodiment 6
Present embodiment is used to explain the preparation method of active titanium dioxide provided by the invention.
According to preparing active titanium dioxide with embodiment 2 identical methods, different is, that anatase thpe white powder is not levigate.
Promptly; Be that the water cut of 500 nanometers is to deliver to after anatase thpe white powder (productions of Shandong Dong Jia company), 34.8 gram light titaniums (Guangzhou light titanium subring is protected Science and Technology Ltd. and produced), 58.8 gram absolute ethyl alcohols, 31.2 gram sodium hypophosphites and 120 gram dimethyl silicone oils (the Chinese magnificent source chemical company produce) mixing of 2.5 weight % during FJM-400 type fluidized bed gas grinds directly with 2500 gram average particle diameters; Spiral quantitative charging and air flow rate carry out synchronously, and control spiral quantitative input speed is 150 rev/mins, and the water cut of dry air stream is 0.01 weight %; Stream pressure is 0.8 MPa; Air flow rate is 9 cubic meters per minute, and the contact temperature is 80 ℃, and the time is 6 minutes; The speed of the percussion flow of white titanium pigment and plating bath is 3.0 Mach numbers, and zirconium sheet grading wheel rotating speed is 4800 rev/mins.At last the white titanium pigment after the activation is discharged to deliver in the pulse receipts powder jar from the airduct of fluidized-bed and receive powder, promptly obtaining particle dia of the present invention is the active titanium dioxide A6 below 550 nanometers.
Embodiment 7
Present embodiment is used to explain the preparation method of active titanium dioxide provided by the invention.
According to preparing active titanium dioxide with embodiment 2 identical methods, different is before activation treatment after the levigate drying with anatase thpe white powder, white titanium pigment to be bleached removal of impurities handle, promptly
Anatase thpe white powder, the 6 gram tin protochlorides and 1980 of 3000 grams after levigate are restrained deionized waters and mix; And the pH that uses hydrochloric acid to regulate mixture is 3; React after 0.5 hour, with deionized water wash mixture after-filtration, then; White titanium pigment after using pressure filter to filter dewater to water cut be 0.01 weight %, it is hit carefully to 120 orders with hammer slice type loose powder machine at 120 ℃ times then.The content that is recorded the iron in the white titanium pigment by ICP is 25ppm, and the whiteness of using blancometer to record this white titanium pigment is 97%.Make active titanium dioxide A7 provided by the invention.
Embodiment 8
Present embodiment is used to explain the preparation method of active titanium dioxide provided by the invention.
According to preparing active titanium dioxide with embodiment 2 identical methods, different is before activation treatment after the levigate drying with anatase thpe white powder, white titanium pigment to be bleached removal of impurities handle, promptly
Anatase thpe white powder, the 48 gram tin protochlorides and 6000 of 3000 grams after levigate are restrained deionized waters and mix; And the pH that uses hydrochloric acid to regulate mixture is 5; React after 0.8 hour, with deionized water wash mixture after-filtration, then; White titanium pigment after using pressure filter to filter dewater to water cut be 0.01 weight %, it is hit carefully to 120 orders with hammer slice type loose powder machine at 120 ℃ times then.The content that is recorded the iron in the white titanium pigment by ICP is 20ppm, and the whiteness of using blancometer to record this white titanium pigment is 98%.Make active titanium dioxide A8 provided by the invention.
Embodiment 9
Present embodiment is used to explain the preparation method of active titanium dioxide provided by the invention.
According to preparing active titanium dioxide with embodiment 2 identical methods, different is before activation treatment after the levigate drying with anatase thpe white powder, white titanium pigment to be bleached removal of impurities handle, promptly
Anatase thpe white powder, the 30 gram tin protochlorides and 3000 of 3000 grams after levigate are restrained deionized waters and mix; And the pH that uses hydrochloric acid to regulate mixture is 4; React after 0.6 hour, with deionized water wash mixture after-filtration, then; White titanium pigment after using pressure filter to filter dewater to water cut be 0.01 weight %, it is hit carefully to 120 orders with hammer slice type loose powder machine at 120 ℃ times then.The content that is recorded the iron in the white titanium pigment by ICP is 20ppm, and the whiteness of using blancometer to record this white titanium pigment is 97%.Make active titanium dioxide A9 provided by the invention.
Embodiment 10-18
Present embodiment is used to explain the activity of the active titanium dioxide of embodiment of the invention preparation.
The activity of active titanium dioxide is weighed with activation index, and activation index is high more, and then the activity of active titanium dioxide is strong more.
The testing method of activation index is: respectively the active titanium dioxide of 100 gram embodiment 1-9 preparations is put into deionized water; Blasting under the conditions of air; Stir after 10 minutes, left standstill 24 hours, measure the quality of buoyant active titanium dioxide on the water surface; And calculating its activation index respectively according to following formula, the result is as shown in table 1 below.
Comparative Examples 1-2
This Comparative Examples is used to explain the activity of existing white titanium pigment.
Measure the activity index of Rutile type Titanium Dioxide AC1 (production of Shandong Dong Jia company) and anatase thpe white powder AC2 (Jiangxi is added light company and produced) respectively according to the method identical with embodiment 10-18.The result is as shown in table 1 below.
Table 1
| Embodiment 10 | Embodiment 11 | Embodiment 12 | Embodiment 13 | Embodiment 14 | Embodiment 15 | Embodiment 16 | Embodiment 17 | Embodiment 18 | Comparative Examples 1 | Comparative Examples 2 | |
| Active titanium dioxide or white titanium pigment | A1 | A2 | A3 | A4 | A5 | A6 | A7 | A8 | A9 | AC1 | AC2 |
| Activity index (%) | 70 | 98 | 83 | 85 | 85 | 80 | 98 | 98 | 99 | 15 | 19 |
Can find out that from the data of table 1 activity index of the active titanium dioxide of embodiment of the invention 1-9 preparation is 70-99%, apparently higher than the activity of the 15-19% of the non-activated white titanium pigment that is purchased.
Claims (11)
1. the preparation method of an active titanium dioxide; It is characterized in that; This method comprises makes white titanium pigment contact with the form of plating bath with percussion flow; Said plating bath contains light titanium, solvent 1, stablizer, dimethyl silicone oil, and the weight ratio of light titanium, solvent 1, stablizer and dimethyl silicone oil is (1.3-30): (10-50): (8-27): 100; Said solvent 1 is an absolute ethyl alcohol; Said stablizer is a sodium hypophosphite.
2. method according to claim 1, wherein, the weight ratio of said white titanium pigment and plating bath is 100: 2-10.
3. method according to claim 1, wherein, the condition of said contact comprises that temperature is 55-100 ℃, and the time is 2-10 minute, and the speed of percussion flow is the 2-3.8 Mach number.
4. method according to claim 3, wherein, said contact is carried out in fluidized bed jet mill, and input speed is that 60-250 rev/min, stream pressure are that 0.5-1.2 MPa, air flow rate are the 5-12 cubic meters per minute, and the contact temperature is 55-100 ℃; Said air-flow is a dry air stream, and the water cut of said dry air stream is 0.01-0.2 weight %.
5. method according to claim 1; Wherein, said white titanium pigment is the anatase thpe white powder of not coating and/or the Rutile type Titanium Dioxide of coating not, and is benchmark with the gross weight of white titanium pigment; The content of iron is no more than 30ppm, and the content of water is 0.01-1.5 weight %.
6. method according to claim 5, wherein, the anatase thpe white powder of said not coating and the average particle diameter of the Rutile type Titanium Dioxide of the coating 50-400 nanometer of respectively doing for oneself not.
7. method according to claim 6, wherein, the anatase thpe white powder of said not coating and the average particle diameter of the Rutile type Titanium Dioxide of the coating 150-250 nanometer of respectively doing for oneself not.
8. according to claim 6 or 7 described methods; Wherein, The anatase thpe white powder of said not coating and/or not the preparation method of the Rutile type Titanium Dioxide of coating comprise with average particle diameter being that the white titanium pigment of 500-700 nanometer grinds in the presence of grinding aid and solvent 2; Dry then, said average particle diameter is that the weight ratio of white titanium pigment, grinding aid and the solvent 2 of 500-700 nanometer is (57-77): (0.2-0.6):
100, said grinding aid is a Sodium hexametaphosphate 99, and said solvent 2 is a water.
9. method according to claim 5; Wherein, The anatase thpe white powder of said not coating and/or not the preparation method of the Rutile type Titanium Dioxide of coating comprise that white titanium pigment contacts in water with SYNTHETIC OPTICAL WHITNER, washing, filter and drying obtains solid product, the temperature of said contact is 50-90 ℃; Be 0.5-0.8 hour duration of contact; The pH of the mixed solution of white titanium pigment, SYNTHETIC OPTICAL WHITNER and water is 1-6, and the content of iron is greater than 30ppm to 150ppm in the white titanium pigment, and the weight ratio of white titanium pigment, SYNTHETIC OPTICAL WHITNER and water is 100: (0.2-1.6): (66-200).
10. method according to claim 9, wherein, said SYNTHETIC OPTICAL WHITNER is a tin protochloride.
11. according to any described method among the claim 5-7; Wherein, The preparation method of the anatase thpe white powder of said not coating comprises the mixture calcining back grinding that contains metatitanic acid, salt of wormwood, Sodium hexametaphosphate 99 and phosphoric acid; Said calcining comprises earlier calcined 2-3 hour down at 150-580 ℃, calcined 2.5-3 hour down at 590-790 ℃ again, and said grinding comprises grinds calcining back products therefrom in the presence of grinding aid and solvent 2; The weight ratio of metatitanic acid, salt of wormwood, Sodium hexametaphosphate 99 and phosphoric acid is 100 in the said mixture: (0.2-1.6): (0.3-1.8): (0.1-0.8); The weight ratio of said calcining back products therefrom, grinding aid and solvent 2 is (57-77): (0.2-0.6): 100, and said grinding aid is a Sodium hexametaphosphate 99, said solvent 2 is a water.
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| CN114806225B (en) * | 2022-03-28 | 2023-08-29 | 浙江恒逸石化研究院有限公司 | Preparation method of liquid titanium dioxide |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3847640A (en) * | 1973-03-26 | 1974-11-12 | A L Ind Inc | Titanium pigment slurries for preparation of latex-base coating compositions |
| CN1778685A (en) * | 2005-10-14 | 2006-05-31 | 浙江大学 | Production of titanium dioxide optical catalyst sol |
| CN1982349A (en) * | 2005-12-16 | 2007-06-20 | 中国科学院福建物质结构研究所 | Nano-titanium dioxide surface treatment |
-
2007
- 2007-12-29 CN CN2007103078629A patent/CN101469140B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3847640A (en) * | 1973-03-26 | 1974-11-12 | A L Ind Inc | Titanium pigment slurries for preparation of latex-base coating compositions |
| CN1778685A (en) * | 2005-10-14 | 2006-05-31 | 浙江大学 | Production of titanium dioxide optical catalyst sol |
| CN1982349A (en) * | 2005-12-16 | 2007-06-20 | 中国科学院福建物质结构研究所 | Nano-titanium dioxide surface treatment |
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| CN101469140A (en) | 2009-07-01 |
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