Method of preparing rutile conductive titanium white powder through dry doping

Dry miserable hybrid method for preparing a conductive iron rutile white powder

TECHNICAL FIELD

[0001] The present invention belongs to the field of functional materials powdery iron, concrete and provided a dry method infiltration method for preparing hybrid conductive iron rutile white powder.

Background technique

[0002] In recent years, with the rapid development of coating technology, coating technology for people it adds infinite color space, but in some areas, after paint spraying, influenced by the environment, such as airborne particles, dust, water vapor etc., easily lead to the generation of static electricity, static electricity generated when accumulated to a certain extent it will be dangerous. For this reason the development of anti-static coating and more attention. Anti-static conductive coating must be added iron white powder, white powder and other conductive pigments with iron, easy to prepare a permanent conductive nearly white and other colors, anti-static products, has been widely used in petroleum, chemicals, building materials, electronics, electrical, communications, automotive, pharmaceuticals, paper, textiles, packaging, printing, shipbuilding, ceramics, aerospace, weapons and other industrial fields and daily life of a conductive, anti-static fields. White also has a conductive iron and non-toxic, odorless, acid, alkali, salt, organic solvent resistance, light resistance and so on, at 800 ° CW stable, non-oxidizing, non-flammable and has a flame retardant. Suitable for almost any conductive requirements, anti-static environments and events, the W and broad development prospects.

[0003] Currently, the preparation method disclosed in the patent CN1385862A- species method of preparing a light-colored conductive powder and conductive titanium oxide species patent CN102583524A- powders are prepared in the presence of particle distribution is not uniform and do not have pigment properties, particle agglomeration serious and other issues, the crystal structure is flawed, in the course of whiteness, tinting strength pigments such indicators is not ideal, affecting the use of the product and difficult to W industrial production. And preparation of patent CN102583524A- kinds conductive titanium oxide powder prepared iron salt complex and a single raw material, iron particles formed are uniform enough, and a colloidal iron salt is prepared, it is difficult to achieve subsequent filtering wash coating and cladding.

SUMMARY

[0004] for the deficiencies of the prior art, an object of the present invention is to provide a method of dry infiltration hybrid conductive iron preparation rutile white powder, low production cost and easy to implement, less iron absorption resulting conductive light white powder, granular distributed evenly and will not reunite, large scattering capacity, good gloss, whiteness, achromatic power, covering power and other optical properties.

[0005] The present invention is a dry method for producing doped rutile white powder conductive iron, tin oxide and mixed oxide and chain = added to the white powder of iron sulfate process rutile production has been added to the seed of intermediate goods partial iron oxalic acid solution to obtain a product.

Intermediate goods partial ferrite [0006] The present invention is a white powder produced iron sulphate, iron sulphate that heroin production is conventional processes in the art. Oxalic acid solution has been added rutile seed of intermediate goods partial iron acid sulphate of iron heroin production is: join rutile seed in sulfuric acid iron white powder produced intermediate goods partial iron acid, and then added together to oxalic acid solution. Wherein rutile seed and partial ferrite in Ti mass ratio of 3-5%; rutile species are known in the art products.

[0007] The present invention is a dry method for producing rutile doped conductive iron white powder, comprising the steps of W:

[000 primer (1) the production of sulfuric acid has been added powdery iron rutile seed of intermediate goods partial iron was added to the oxalic acid solution, formulated as a suspension;

[0009] (2) tin oxide and oxide and chain = shear mixing;

Mixed powder [0010] (3) the step (2) was added to the step (1) to give a suspension;

[0011] (4) The step (3) the product obtained was filtered, washed until no coating oxalate;

[0012] (5) in step (4) drying the filter cake obtained;

[0013] (6) grinding the material after drying, the material after grinding burn lose, then cooled to room temperature;

[0014] (7) to pay cooked crushed material; a conductive iron to give white powder.

[0015] wherein;

[0016] Ferrite quality bias should meet: D50 in 0.25-0.30um, the number of particles of less than 0 m is not more than 4%, the number of particles larger than 0.5um is not more than 10% of the particles into a normal distribution; laser. particle size distribution analyzer for testing;

[0017] The oxalic acid solution is an aqueous solution of oxalic acid, oxalic acid concentration of 15-30%. The percentage by mass suspension containing titanium oxide is 20-35%.

[001 tin oxide and lead oxide and chain S mass ratio of 1: 1-1: 15.

Mass [0019] Step (2) mixing the powder obtained in step (1) to give a suspension ratio of 1 to 10%, in step (1) to give a suspension of W Ti mass.

[0020] Step (4) the drying temperature of 100-150 ° C, in 8-12 hours time control.

[0021] Step (4) of the step (3) the product obtained was filtered, washed painted to no oxalate; oxalate ions using ammonia oxidation clever solution to detect the wash filtrate painted after addition of ammonia oxidation clever solution, no white precipitate formed, you can.

[0022] Step (6) was burned to lose: Temperature controlled at 0-300 ° C, the heating time of 1 hour, 300-400 ° C, the heating time of 2 hours, 400-500 ° C, the heating time is three hours, 500-600 ° C, the heating time of 2 hours, 600-700 ° C, the heating time of 2 hours, 700-800 ° C, the heating time is three hours.

[0023] Step (7) pulverized to: be crushed by rolling Luk grinding pressure, will lose burn process sintered agglomerated particles broken, the grinding pressure grinding glistening sheet material again after Raymond machine pulverized to fine reaches the 99.9% W; using 45um, 320 sieves detection purposes.

[0024] As a preferred aspect, the present invention is a dry method for producing rutile doped conductive iron white powder, comprising the steps of W:

[0025] (1) the production of sulfuric acid has been added powdery iron rutile seed of intermediate goods partial iron was added to the oxalic acid solution, mix olive rate of 3 rev / min and takes 30-60 minutes to mix, formulated as a suspension ;

[00%] (2) = the tin oxide and oxide and chain, a mass ratio of 1: 1-1: 15 was added to the powder mixing device, shear mixing, mixing and grinding 3-6 times;

[0027] (3) the step (2) was added to the mixed powder obtained in step (1) to obtain a suspension, mix embrace speed 10-30 rev / min, olive mix for 30-60 minutes;

[Cited 002 (4) of step (3) the product obtained was filtered, washed until no coating oxalate;

[0029] (5) in step (4) was not induced into the steel cake tray drying temperature of 100-150 ° C, in 8-12 hours time control;

[0030] (6) the material after drying using a coffee grinder or ball mill grinding, the material is milled into steel trays were not induced to lose firing temperature controlled at 0-300 ° C, the heating time of 1 hour, 300-400 ° C, the heating time of 2 hours, 400-500 ° C, the heating time is three hours, 500-600 ° C, the heating time of 2 hours, 600-700 ° C, the heating time of 2 hours, 700-800 ° C, It was heated 3 hours, then cooled to room temperature;

[0031] (7) to pay cooked through glistening material grinding pressure roll crushing, burning process will lose sintered agglomerated particles broken, the grinding pressure grinding glistening sheet material again after Raymond grinding machine, so fineness reach the 99.9% W; get a conductive iron white powder.

[0032] In summary, the present invention has the following advantages W:

[0033] (1) prepared by the invention of conductive iron white powder, crushed powder after detecting polishing Hunter whiteness on 92% W, achromatic force reaches the 95% W, the gloss on the L value reached 93.5 W, rutile content greater than 90% on the W, powder resistivity 20-60 Q • Hata.

[0034] (2) Since the present invention W sulfuric acid iron heroin production has joined rutile seed of intermediate goods biased ferrite-based raw materials, with the primary particles and pigment properties iron white powder pigments, conductive iron W prepared white rutile content, with excellent weather resistance, whiteness pigment properties by tin oxide and oxide and chain = dry-blended particles lose doped semiconductor burn treatment to the substrate surface to form a conductive oxide layer, thereby preparing a new class of semiconductor electronic conductive functional pigments. White light absorbing conductive iron fewer large scattering capacity, good gloss, whiteness, achromatic power, covering power and other optical properties. It can be made nearly white and other light colored permanent conductive, anti-static products. In the whiteness of higher electrical conductivity, anti-static products and environments is particularly applicable.

[0035] (3) Preparation method of the present invention provides a simple operation, excellent electrical conductivity effects, using sulfuric acid iron heroin production process intermediate products partial ferrite, prepare a conductive iron white powder, low production cost and easy to implement, since the sulfuric acid method iron White production of intermediate products is the result of partial iron acid preparation from hydrolysis, thus ensuring the original morphology of conductive powdery iron particles, the particle size distribution is uniform and excellent characteristics reunion.

detailed description

[0036] The following combination of embodiments of the present invention will be further described below.

[0037] Example 1

[0038] 1) sulfuric acid Calafate heroin production has joined rutile seed of intermediate goods partial ferrite 2000g (off Ti of the quality of 1600g) was added to oxalic acid solution containing 15% (by mass percent), and formulated to contain two iron 20% (W Ti of mass%) of the suspension, mix olive rate of 3 rev / min, embrace stirred for 30 minutes.

[0039] 2) tin oxide and S-oxide and chain 50g 50g powder in a 1: 1 ratio (mass ratio) was added to the powder mixing device, shear mixing, mixed and ground three times requested.

[0040] 3) were slowly added to the mixed powder 16g Step 1) two iron suspension of the mixed oxide powder and two mass ratio of 1%, a rate of 10 football mix rev / min, stirred for 30 minutes football .

[0041] 4) The suspension was filtered, washed until no oxalate coating can be. Oxalate ions using a solution of ammonia oxidation coincidence detection, the filtrate was washed painted after addition of ammonia oxidation clever solution, no white precipitate formed, you can.

[0042] 5) The cake was put into the wash coat does not induce steel tray, drying, temperature requirements at 100 ° C, 8 hours time-control.

[0043] 6) the material after drying using a ball mill grinding, grinding the material was put into a steel tray does not induce crystalline lose burn temperature control 0-300 ° C, the heating time of 1 hour, 300-400 ° C, the heating time of 2 hours, 400-500 ° C, the heating time is three hours, 500-600 ° C, the heating time of 2 hours, 600-700 ° C, the heating time of 2 hours, 700-800 ° C, the heating time of 3 hours , then cooled to room temperature.

[0044] 7) will pay cooked through glistening material grinding pressure roll crushing, burning process will lose sintered agglomerated particles broken, the grinding pressure grinding glistening sheet material again after Raymond grinding machine to make it fineness of the 99.9% W (using 45um, 320 sieves detection purposes), to obtain a conductive iron white powder.

[0045] Example 2

[0046] I) sulfate Calafate heroin production has joined rutile seed of intermediate goods partial ferrite 2000g (off Ti of the quality of 1600g) was added to oxalic acid solution containing 20% ​​(by mass percent), and formulated to contain two iron 25% (W Ti of mass%) of the suspension, mix olive rate of 3 rev / min, olive mix for 40 minutes.

[0047] 2) tin oxide and S-oxide and chain 50g 250g powder ratio of 1: 5 (mass ratio) was added to a coffee grinder, shear mixing, mixing requires grinding four times.

[0048] 3) The mixed powder was slowly added to a 4¾ step 1) two iron suspension of the mixed oxide powder and two mass ratio of 3% olive mix rate of 20 rev / min, 40 minutes football mix .

[0049] 4) The suspension was filtered to wash coat can no oxalate. Oxalate ions using a solution of ammonia oxidation coincidence detection, the filtrate was washed painted after addition of ammonia oxidation clever solution, no white precipitate formed, you can.

[0050] 5) The cake was put into the wash coat does not induce steel tray, drying, temperature requirements at 120 ° C, time-controlled to 9 hours.

[0051] 6) the material after drying using a ball mill grinding, grinding the material was put into a steel tray does not induce crystalline lose burn temperature control 0-300 ° C, the heating time of 1 hour, 300-400 ° C, the heating time of 2 hours, 400-500 ° C, the heating time is three hours, 500-600 ° C, the heating time of 2 hours, 600-700 ° C, the heating time of 2 hours, 700-800 ° C, the heating time of 3 hours , then cooled to room temperature.

[0052] 7) will pay cooked through glistening material grinding pressure roll crushing, burning process will lose sintered agglomerated particles broken, the grinding pressure grinding glistening sheet material again after Raymond machine and pulverized to yield conductive iron white powder.

[0 of 3] Example 3

[0054] 1) sulfuric acid Calafate heroin production has joined rutile seed of intermediate goods partial ferrite 2000g (off Ti of the quality of 1600g) was added to oxalic acid solution containing 25% (by mass percent), and formulated to contain two iron 30% (W Ti of mass%) of the suspension, mix olive rate of 3 rev / min, olive mix for 50 minutes.

[0055] 2) tin oxide and S-oxide and chain 50g 500g powder according to 1:10 (mass ratio) was added to the powder mixing device, shear mixing, mixing and grinding claim 5 times.

[0056] 3) were slowly added to the mixed powder SOg step 1) two iron suspension of the mixed oxide powder and two mass ratio of 5%, a rate of 25 football mix rev / min and takes 50 minutes mix .

[0057] 4) The suspension was filtered to wash coat can no oxalate. Oxalate ions using a solution of ammonia oxidation coincidence detection, the filtrate was washed painted after addition of ammonia oxidation clever solution, no white precipitate formed, you can.

[0058] 5) The cake was put into the wash coat does not induce steel tray, drying, temperature requirements at 130 ° C, time-controlled for 10 hours.

[0059] 6) the material after drying using the coffee grinder for grinding, milling the material was put into a steel tray does not induce crystalline lose burn temperature control 0-300 ° C, the heating time of 1 hour, 300-400 ° C, the heating time of 2 hours, 400-500 ° C, the heating time is three hours, 500-600 ° C, the heating time of 2 hours, 600-700 ° C, the heating time of 2 hours, 700-800 ° C, the heating time 3 hours, then cooled to room temperature.

[0060] 7) will pay cooked through glistening material grinding pressure roll crushing, burning process will lose sintered agglomerated particles broken, the grinding pressure grinding glistening sheet material again after Raymond machine and pulverized to yield conductive iron white powder.

[0061] Example 4

[0062] 1) sulfuric acid Calafate heroin production has joined rutile seed of intermediate goods partial ferrite 2000g (off Ti of the quality of 1600g) was added to oxalic acid solution containing 30% (by mass percent), and formulated to contain two iron 35% (W Ti of mass%) of the suspension, mix olive rate of 3 rev / min, olive mix for 60 minutes.

[0063] 2) tin oxide and S-oxide and chain 50g 750g powder according to 1:15 (mass ratio) was added to the coffee powder mill or other mixing device, shear mixing, mixing requires grinding 6 times.

[0064] 3) will 160g mixed powder was slowly added to the step 1) two iron suspension of the mixed oxide powder and two mass ratio of 10%, a rate of 30 football mix rev / min and takes 60 minutes mix .

[0065] 4) The suspension was filtered to wash coat can no oxalate. Oxalate ions using a solution of ammonia oxidation coincidence detection, the filtrate was washed painted after addition of ammonia oxidation clever solution, no white precipitate formed, you can.

[0066] 5) The cake was put into the wash coat does not induce steel tray, drying, temperature requirements at 150 ° C, time-controlled in 12 hours.

[0067] 6) the material after drying using the coffee grinder for grinding, milling the material was put into a steel tray does not induce crystalline lose burn temperature control 0-300 ° C, the heating time of 1 hour, 300-400 ° C, the heating time of 2 hours, 400-500 ° C, the heating time is three hours, 500-600 ° C, the heating time of 2 hours, 600-700 ° C, the heating time of 2 hours, 700-800 ° C, the heating time 3 hours, then cooled to room temperature.

[0068] 7) will pay cooked through glistening material grinding pressure roll crushing, burning process will lose sintered agglomerated particles broken, the grinding pressure grinding glistening sheet material again after Raymond machine and pulverized to yield conductive iron white powder.

[0069] Preparation Example 1-4 to obtain a conductive powdery iron implement performance testing, test results are shown in Table 1.

Performance Test Results [0070] Table 1 prepared in Example 1-4 to give white powder of conductive iron

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