CN104229873A - Preparation method of grey blue paint suitable for ink-jet printing ceramic ink - Google Patents
Preparation method of grey blue paint suitable for ink-jet printing ceramic ink Download PDFInfo
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Abstract
The invention discloses a preparation method of a grey blue paint suitable for ink-jet printing ceramic ink. The method comprises the following steps: A heating tin metal and antimony metal into a molten state, carrying out ultrasonic atomization on melt to obtain alloy fine powder; B adding the alloy fine powder and polypropylene glycol to a closed reaction kettle with a stirrer, introducing compressed air into the closed reaction kettle, and reacting to obtain a stable alloy liquid; and C spraying the stable alloy solution to the top in a fluidized bed reactor in an ultrasonic spraying manner, and simultaneously introducing oxygen at 200-450 DEG C from the bottom of the fluidized bed reactor, so as to obtain the gray blue paint doped with a little of stibium to a stannic oxide lattice suitable for ink-jet printing ceramic ink at the bottom of the fluidized bed reactor. According to the method disclosed by the invention, the grey blue paint doped with stibium in the stannic oxide lattice can be prepared. The preparation method of the high-grade ceramic paint is high in efficiency and low in cost; and the paint is high in color development efficiency, small in particle size, and suitable for ink-jet printing ceramic ink.
Description
Technical field
The present invention relates to a kind of preparation method being applicable to the dusty blue pigment of spray ink Printing ceramic ink.
Background technology
Pigment can be divided into pigment dyestuff and mineral dye, and the price of pigment dyestuff is relatively low, and the density of pigment is lower, and obtain stable ink application than being easier to by dispersing technology, but its weathering resistance is relatively poor, the temperature that can bear is usually less than 100 DEG C.Mineral dye has good weathering resistance, and some kinds can resistance to about 1300 DEG C temperature, can be applied to the industries such as pyroceramic, enamel, glass lacquer.But the price of mineral dye is relatively high, and the density of pigment is comparatively large, and granularity is comparatively thick, is difficult to obtain stable paint ink by conventional disperse technique.Reduce the use cost of mineral dye, good way is exactly improve the service efficiency of mineral dye, reduces the usage quantity that unit applies area paint.Although carry out by the mineral dye that wet ball grinding technique is relatively large to particle the granularity that ball milling significantly can reduce pigment, but the efficiency of this ball milling is lower, cost is higher, as passed through high efficiency dispersing apparatus, use small-particle, highdensity grinding medium, then the use cost of equipment is higher.So will reduce the overall use cost of mineral dye, fundamental way is exactly reduce the granularity of pigment, particularly for the InkJet printing processes representing pigment usage trend, its ink pigments used it has been generally acknowledged that granularity is less than 1 micron.
Tindioxide has the characteristics such as acidproof, alkaline-resisting, high temperature resistant, mechanical resistant impact as inorganic oxide material, when after a small amount of+5 valence state antimony ions that adulterate in its lattice, tin dioxide powder presents dusty blue and is used as dusty blue beramic color, because it maintains tindioxide crystalline phase, so the characteristic such as intrinsic acidproof, alkaline-resisting, high temperature resistant, mechanical resistant impact of tindioxide still keeps.This inorganic ceramic pigment can the high temperature of resistance to 1300 DEG C, so be widely used in high-grade ceramic colorant, enamel colorant, glass pigment.
The conventional production process of the dusty blue pigment of tindioxide antimony dopant be also existing unique industrial process for tin dioxide powder and antimonous oxide powder for raw material (Yang Youming etc.,
jiangsu pottery, 2005,
38(2): 30-31) (Li Chunwen etc.,
pottery, 2003, (4): 27-28,32), first adopt wet ball grinding to carry out mixing and powder granularity is reduced to improve reactive behavior, then drying, pulverizing, sieve, high-temperature calcination solid state reaction, pulverizes, washes away unreacted antimonous oxide with hydrochloric acid etc., carry out alkali neutralization, washing, oven dry again, pulverize and namely obtain targeted pigment.The powder pigment granularity D that this technique obtains
50substantially, more than 6 microns, then production efficiency is extremely low to prepare ink-jet printing ink with this powder pigment, and cause the production cost of ink high, market value is high, is difficult to promote in a wider context.Except the excessive ink production cost caused of powder pigment granularity caused due to the conventional production process of tindioxide antimony dopant dusty blue pigment is too high, the higher market value of overall ink that also causes of the production cost of this powder pigment itself is higher.The raw material tin dioxide powder of pigment and the production of antimonous oxide powder experienced by the step such as acid-base neutralisation, oven dry, high-temperature calcination, pulverizing required for above-mentioned pigment substantially.Production process as pigment tin dioxide powder is, metal tin slab is adopted melt water quenching Cheng Xihua, dissolves tin flower with concentrated nitric acid, obtains metastannic acid precipitation, again with the neutralization of the alkali such as sodium hydroxide, sodium carbonate, with water washing precipitation, filter, dry, high-temperature calcination, pulverize and namely obtain tin dioxide powder.Antimonous oxide powder is that to adopt take antimony as the high-temperature oxidation of raw material substantially, although the production efficiency of this technique is higher, cost is lower, but high temperature causes the reactive behavior of antimonous oxide powder lower, this is very unfavorable for the high temperature solid state reaction carried out with tin dioxide powder, increase temperature of reaction on the one hand, add production cost, also make the granularity of powder pigment too grow up on the other hand.So from starting raw material metallic tin and metallic antimony, the dusty blue pigment of tindioxide antimony dopant be obtained, also first must obtain tin dioxide powder and antimonous oxide powder.Make overall manufacturing process loaded down with trivial details, efficiency is low, and cost is high.
For reducing the granularity of tindioxide antimony dopant dusty blue powder pigment, and improving preparation efficiency, reducing preparation temperature.Bernardi etc. (
j. Euro. Ceram. Soc., 2002,
22: 2911-2919) propose employing with tindichloride, antimonous oxide is main raw material, add nitric acid and promote the dissolving of antimonous oxide, then add citric acid and ethylene glycol to promote the formation of collosol and gel, then carry out the pigment that pyrolytic decomposition obtains tindioxide antimony dopant.This method compares the high-temperature solid phase reaction method that tradition take oxide compound as raw material, greatly reduces temperature of reaction, and facilitate tin, antimony ion in the mixing of molecular level level, the granularity of pigment also significantly reduces simultaneously.But be that its price of raw material of tin will be much higher than metallic tin with tindichloride, be even the price of tin raw material higher than tin dioxide powder, a large amount of use citric acid and ethylene glycol, also greatly increase raw materials cost, make the pigment production cost finally obtained be much higher than conventional solid-state method technique simultaneously.
Have similar tindioxide adulterate a small amount of antimony the nano-powder for preparing of the relative low temperature of chemical composition be also referred to as antimony doped stannic oxide nano powder, this powder has light-coloured transparent conductive characteristic, absorb infrared rays characteristic, be widely used in the industry such as transparent antistatic light-colored, transparent heat-insulated, laser marking, laser welding, coating heating, drying.
Chinese patent CN102285683A proposes and adopts metallic tin, antimony is raw material, and adopt nitric acid dissolve to be precipitated, then carry out washing, drying, 600 DEG C of thermal treatments obtain corresponding stibium doping stannic oxide conductive powder.This technique is that nitric acid dissolve tin obtains metastannic acid precipitation in essence, and dissolve antimony and obtain weisspiessglanz or metaantimmonic acid precipitation, the precipitated solid particle of rear tin, antimony etc. obtains target product by 600 DEG C of high temperature solid state reactions.Tin in such product, antimony atoms homogeneity are still lower, and have part metals when acid dissolve tin, antimony metal can not dissolve completely, its residual quality that greatly can reduce final tindioxide antimony dopant in the product, this technique is inadvisable in actual industrial production.Chinese patent CN103533819A proposes with antimony raw materials such as the tin raw material such as tin chloride, tin sulphate and nitric acid antimony, antimony chlorides, part, dispersion agent is added again after dissolving, add precipitation agent again and be precipitated thing, carry out again washing, dry, calcine, obtain target product antimony doped stannic oxide nano powder, this method improves the monodispersity of nano-powder.But comparatively speaking, add the use cost of part, dispersion agent.The compound of tin and the compound cost of antimony also higher.The overall cost of this technique is higher than the high-temperature solid phase reaction method that traditional tindioxide is raw material.Chinese patent CN103041896A to propose with tindioxide and antimonous oxide powder as raw material, adopts lower than-180 DEG C of low temperature ball millings, then in 50-200 DEG C of denitrogenation, obtains target antimony doped stannic oxide nano powder.Although this technique process is simple, great amount of cost consumption is on low temperature liquid nitrogen, and production efficiency is extremely low simultaneously.Overall cost is high.Chinese patent CN102976396A proposes with stannic chloride pentahydrate and butter of antimony as main raw material, add dispersion agent, under reactor rotating condition, add ammonia be precipitated, then carry out washing, dry, calcine and obtain target tindioxide antimony dopant nano-powder.This process increases ammonia precipitation agent and add fashionable homogeneity.But additional rotating machinery adds production cost, the use cost of tin, antimony chemical is higher simultaneously, makes overall cost higher than high temperature solid state reaction technique.Similar Chinese 103553120A proposes with stannic chloride pentahydrate and butter of antimony as main raw material, add part, ethanol, water solvent obtain mixing solutions, add ammonia precipitation process agent again, reach precipitation, carry out again washing, component distillation, drying, calcining, obtain antimony doped stannic oxide nano powder.Chinese patent CN10327948A proposes with stannic chloride pentahydrate and butter of antimony as main raw material, be dissolved in ethanol and obtain solution, add ammonia precipitation process agent to be again precipitated, in autoclave, high-temperature water thermal response is precipitated again, product washing, oven dry, calcining, obtain target antimony doped stannic oxide nano powder.The high-temperature water thermal process increased improves the thermostability of particle, improves the agglomeration of particle, but considerably increases production cost, cannot participate in market competition.
In sum, in tindioxide lattice, the dusty blue pigment of antimony dopant cannot adapt to the industry development trend of high-level efficiency, small size, low cost as its existing production technique of high-grade ceramic pigment, is particularly applicable to the pigment market vacancy especially of spray ink Printing ceramic ink.
Summary of the invention
In order to overcome the above-mentioned deficiency of the preparation technology of the dusty blue pigment of tindioxide antimony dopant in prior art, the invention provides that a kind of production efficiency is high, cost is low, colorant color development efficiency is high, colorant particle diameter is little, can be applicable to the preparation method being applicable to the dusty blue pigment of spray ink Printing ceramic ink of InkJet printing processes.
The technical scheme that the present invention solves its technical problem is: a kind of preparation method being applicable to the dusty blue pigment of spray ink Printing ceramic ink, comprises the following steps:
A. tin metal, antimony metal are heated to 850 ~ 1100 DEG C of meltings, wherein the mass ratio of tin and antimony is 10 ~ 99:1, the melt that after tin, antimony melting, stirring forms tin, antimony is evenly distributed, carries out ultrasonic atomization by this melt, obtains granularity 1000 order ~ 1500 object alloy fine powder;
B. alloy fine powder steps A obtained and polypropylene glycol are added to in the closed reactor stirred, the quality of polypropylene glycol and the mass ratio of alloy fine powder are 1 ~ 3.5:1, pressurized air is passed in closed reactor, the mass ratio of compressed-air actuated quality and alloy fine powder is 2 ~ 6:1, compressed-air actuated pressure is 0.2 ~ 0.9MPa, mixing speed is 150 ~ 400 revs/min, and closed reactor temperature is 90 ~ 130 DEG C, reacts and obtains alloy stabilizing solution in 3 ~ 12 hours;
C. adopting ullrasonic spraying mode alloy stabilizing solution to be sprayed into temperature is top in 500 ~ 900 DEG C of fluidized-bed reactors, pass into from the bottom of fluidized-bed reactor the oxygen that temperature is 200 ~ 450 DEG C simultaneously, the pressure of oxygen is 0.1 ~ 0.3 MPa, and the mass ratio of the polypropylene glycol in the quality of oxygen and step B is 3 ~ 8:1; Namely the dusty blue pigment of a small amount of antimony that adulterates is obtained in the tindioxide lattice being applicable to spray ink Printing ceramic ink in the bottom of fluidized-bed reactor.
Beneficial effect of the present invention is: method of the present invention can prepare the dusty blue pigment of antimony dopant in tindioxide lattice, preparation method's efficiency of this high-grade ceramic pigment is high, cost is low, colorant color development efficiency is high, colorant particle diameter is little, is specially adapted to spray ink Printing ceramic ink.
Embodiment
Below in conjunction with embodiment, the present invention is described in further detail.
Embodiment one
Be applicable to a preparation method for the dusty blue pigment of spray ink Printing ceramic ink, comprise the following steps:
A. tin metal, antimony metal are heated to 900 DEG C of meltings, wherein the mass ratio of tin and antimony is 50:1, and the melt that after tin, antimony melting, stirring forms tin, antimony is evenly distributed, carries out ultrasonic atomization by this melt, obtain granularity 1000 object alloy fine powder;
B. alloy fine powder steps A obtained and polypropylene glycol are added to in the closed reactor stirred, the quality of polypropylene glycol and the mass ratio of alloy fine powder are 2.5:1, pressurized air is passed in closed reactor, the mass ratio of compressed-air actuated quality and alloy fine powder is 4:1, compressed-air actuated pressure is 0.5MPa, mixing speed is 300 revs/min, and closed reactor temperature is 120 DEG C, reacts and obtains alloy stabilizing solution in 7 hours;
C. adopting ullrasonic spraying mode alloy stabilizing solution to be sprayed into temperature is top in 700 DEG C of fluidized-bed reactors, pass into from the bottom of fluidized-bed reactor the oxygen that temperature is 300 DEG C simultaneously, the pressure of oxygen is 0.2MPa, and the mass ratio of the polypropylene glycol in the quality of oxygen and step B is 5:1; Namely obtain in the bottom of fluidized-bed reactor that X-ray diffraction test result is shown as tindioxide crystalline phase, granularity be 0.3 micron be applicable to adulterate in the tindioxide lattice of spray ink Printing ceramic ink the dusty blue pigment of a small amount of antimony.
Embodiment two
Be applicable to a preparation method for the dusty blue pigment of spray ink Printing ceramic ink, comprise the following steps:
A. tin metal, antimony metal are heated to 850 DEG C of meltings, wherein the mass ratio of tin and antimony is 40:1, and the melt that after tin, antimony melting, stirring forms tin, antimony is evenly distributed, carries out ultrasonic atomization by this melt, obtain granularity 1500 object alloy fine powder;
B. alloy fine powder steps A obtained and polypropylene glycol are added to in the closed reactor stirred, the quality of polypropylene glycol and the mass ratio of alloy fine powder are 2:1, pressurized air is passed in closed reactor, the mass ratio of compressed-air actuated quality and alloy fine powder is 4.2:1, compressed-air actuated pressure is 0.3MPa, mixing speed is 160 revs/min, and closed reactor temperature is 100 DEG C, reacts and obtains alloy stabilizing solution in 3 hours;
C. adopting ullrasonic spraying mode alloy stabilizing solution to be sprayed into temperature is top in 900 DEG C of fluidized-bed reactors, pass into from the bottom of fluidized-bed reactor the oxygen that temperature is 320 DEG C simultaneously, the pressure of oxygen is 0.15MPa, and the mass ratio of the polypropylene glycol in the quality of oxygen and step B is 7:1; Namely obtain in the bottom of fluidized-bed reactor that X-ray diffraction test result is shown as tindioxide crystalline phase, granularity be 0.5 micron be applicable to adulterate in the tindioxide lattice of spray ink Printing ceramic ink the dusty blue pigment of a small amount of antimony.
Embodiment three
Be applicable to a preparation method for the dusty blue pigment of spray ink Printing ceramic ink, comprise the following steps:
A. tin metal, antimony metal are heated to 1000 DEG C of meltings, wherein the mass ratio of tin and antimony is 10:1, and the melt that after tin, antimony melting, stirring forms tin, antimony is evenly distributed, carries out ultrasonic atomization by this melt, obtain granularity 1100 object alloy fine powder;
B. alloy fine powder steps A obtained and polypropylene glycol are added to in the closed reactor stirred, the quality of polypropylene glycol and the mass ratio of alloy fine powder are 3.5:1, pressurized air is passed in closed reactor, the mass ratio of compressed-air actuated quality and alloy fine powder is 2.5:1, compressed-air actuated pressure is 0.7MPa, mixing speed is 200 revs/min, and closed reactor temperature is 90 DEG C, reacts and obtains alloy stabilizing solution in 10 hours;
C. adopting ullrasonic spraying mode alloy stabilizing solution to be sprayed into temperature is top in 550 DEG C of fluidized-bed reactors, pass into from the bottom of fluidized-bed reactor the oxygen that temperature is 200 DEG C simultaneously, the pressure of oxygen is 0.18MPa, and the mass ratio of the polypropylene glycol in the quality of oxygen and step B is 3:1; Namely obtain in the bottom of fluidized-bed reactor that X-ray diffraction test result is shown as tindioxide crystalline phase, granularity be 0.4 micron be applicable to adulterate in the tindioxide lattice of spray ink Printing ceramic ink the dusty blue pigment of a small amount of antimony.
Embodiment four
Be applicable to a preparation method for the dusty blue pigment of spray ink Printing ceramic ink, comprise the following steps:
A. tin metal, antimony metal are heated to 860 DEG C of meltings, wherein the mass ratio of tin and antimony is 20:1, and the melt that after tin, antimony melting, stirring forms tin, antimony is evenly distributed, carries out ultrasonic atomization by this melt, obtain granularity 1300 object alloy fine powder;
B. alloy fine powder steps A obtained and polypropylene glycol are added to in the closed reactor stirred, the quality of polypropylene glycol and the mass ratio of alloy fine powder are 3.2:1, pressurized air is passed in closed reactor, the mass ratio of compressed-air actuated quality and alloy fine powder is 5.5:1, compressed-air actuated pressure is 0.2MPa, mixing speed is 320 revs/min, and closed reactor temperature is 92 DEG C, reacts and obtains alloy stabilizing solution in 4 hours;
C. adopting ullrasonic spraying mode alloy stabilizing solution to be sprayed into temperature is top in 500 DEG C of fluidized-bed reactors, pass into from the bottom of fluidized-bed reactor the oxygen that temperature is 400 DEG C simultaneously, the pressure of oxygen is 0.25MPa, and the mass ratio of the polypropylene glycol in the quality of oxygen and step B is 8:1; Namely obtain in the bottom of fluidized-bed reactor that X-ray diffraction test result is shown as tindioxide crystalline phase, granularity be 0.45 micron be applicable to adulterate in the tindioxide lattice of spray ink Printing ceramic ink the dusty blue pigment of a small amount of antimony.
Embodiment five
Be applicable to a preparation method for the dusty blue pigment of spray ink Printing ceramic ink, comprise the following steps:
A. tin metal, antimony metal are heated to 1100 DEG C of meltings, wherein the mass ratio of tin and antimony is 90:1, and the melt that after tin, antimony melting, stirring forms tin, antimony is evenly distributed, carries out ultrasonic atomization by this melt, obtain granularity 1400 object alloy fine powder;
B. alloy fine powder steps A obtained and polypropylene glycol are added to in the closed reactor stirred, the quality of polypropylene glycol and the mass ratio of alloy fine powder are 1:1, pressurized air is passed in closed reactor, the mass ratio of compressed-air actuated quality and alloy fine powder is 2:1, compressed-air actuated pressure is 0.9MPa, mixing speed is 230 revs/min, and closed reactor temperature is 91 DEG C, reacts and obtains alloy stabilizing solution in 11 hours;
C. adopting ullrasonic spraying mode alloy stabilizing solution to be sprayed into temperature is top in 850 DEG C of fluidized-bed reactors, pass into from the bottom of fluidized-bed reactor the oxygen that temperature is 450 DEG C simultaneously, the pressure of oxygen is 0.1MPa, and the mass ratio of the polypropylene glycol in the quality of oxygen and step B is 6.5:1; Namely obtain in the bottom of fluidized-bed reactor that X-ray diffraction test result is shown as tindioxide crystalline phase, granularity be 0.85 micron be applicable to adulterate in the tindioxide lattice of spray ink Printing ceramic ink the dusty blue pigment of a small amount of antimony.
Embodiment six
Be applicable to a preparation method for the dusty blue pigment of spray ink Printing ceramic ink, comprise the following steps:
A. tin metal, antimony metal are heated to 950 DEG C of meltings, wherein the mass ratio of tin and antimony is 80:1, and the melt that after tin, antimony melting, stirring forms tin, antimony is evenly distributed, carries out ultrasonic atomization by this melt, obtain granularity 1200 object alloy fine powder;
B. alloy fine powder steps A obtained and polypropylene glycol are added to in the closed reactor stirred, the quality of polypropylene glycol and the mass ratio of alloy fine powder are 3.4:1, pressurized air is passed in closed reactor, the mass ratio of compressed-air actuated quality and alloy fine powder is 6:1, compressed-air actuated pressure is 0.4MPa, mixing speed is 150 revs/min, and closed reactor temperature is 95 DEG C, reacts and obtains alloy stabilizing solution in 5 hours;
C. adopting ullrasonic spraying mode alloy stabilizing solution to be sprayed into temperature is top in 600 DEG C of fluidized-bed reactors, pass into from the bottom of fluidized-bed reactor the oxygen that temperature is 370 DEG C simultaneously, the pressure of oxygen is 0.13MPa, and the mass ratio of the polypropylene glycol in the quality of oxygen and step B is 5.5:1; Namely obtain in the bottom of fluidized-bed reactor that X-ray diffraction test result is shown as tindioxide crystalline phase, granularity be 0.7 micron be applicable to adulterate in the tindioxide lattice of spray ink Printing ceramic ink the dusty blue pigment of a small amount of antimony.
Embodiment seven
Be applicable to a preparation method for the dusty blue pigment of spray ink Printing ceramic ink, comprise the following steps:
A. tin metal, antimony metal are heated to 980 DEG C of meltings, wherein the mass ratio of tin and antimony is 99:1, and the melt that after tin, antimony melting, stirring forms tin, antimony is evenly distributed, carries out ultrasonic atomization by this melt, obtain granularity 1200 object alloy fine powder;
B. alloy fine powder steps A obtained and polypropylene glycol are added to in the closed reactor stirred, the quality of polypropylene glycol and the mass ratio of alloy fine powder are 3.3:1, pressurized air is passed in closed reactor, the mass ratio of compressed-air actuated quality and alloy fine powder is 4.5:1, compressed-air actuated pressure is 0.6MPa, mixing speed is 250 revs/min, and closed reactor temperature is 93 DEG C, reacts and obtains alloy stabilizing solution in 12 hours;
C. adopting ullrasonic spraying mode alloy stabilizing solution to be sprayed into temperature is top in 650 DEG C of fluidized-bed reactors, pass into from the bottom of fluidized-bed reactor the oxygen that temperature is 260 DEG C simultaneously, the pressure of oxygen is 0.27MPa, and the mass ratio of the polypropylene glycol in the quality of oxygen and step B is 6:1; Namely obtain in the bottom of fluidized-bed reactor that X-ray diffraction test result is shown as tindioxide crystalline phase, granularity be 0.8 micron be applicable to adulterate in the tindioxide lattice of spray ink Printing ceramic ink the dusty blue pigment of a small amount of antimony.
Embodiment eight
Be applicable to a preparation method for the dusty blue pigment of spray ink Printing ceramic ink, comprise the following steps:
A. tin metal, antimony metal are heated to 910 DEG C of meltings, wherein the mass ratio of tin and antimony is 60:1, and the melt that after tin, antimony melting, stirring forms tin, antimony is evenly distributed, carries out ultrasonic atomization by this melt, obtain granularity 1100 object alloy fine powder;
B. alloy fine powder steps A obtained and polypropylene glycol are added to in the closed reactor stirred, the quality of polypropylene glycol and the mass ratio of alloy fine powder are 1.5:1, pressurized air is passed in closed reactor, the mass ratio of compressed-air actuated quality and alloy fine powder is 5:1, compressed-air actuated pressure is 0.45MPa, mixing speed is 380 revs/min, and closed reactor temperature is 110 DEG C, reacts and obtains alloy stabilizing solution in 6 hours;
C. adopting ullrasonic spraying mode alloy stabilizing solution to be sprayed into temperature is top in 620 DEG C of fluidized-bed reactors, pass into from the bottom of fluidized-bed reactor the oxygen that temperature is 210 DEG C simultaneously, the pressure of oxygen is 0.26MPa, and the mass ratio of the polypropylene glycol in the quality of oxygen and step B is 4:1; Namely obtain in the bottom of fluidized-bed reactor that X-ray diffraction test result is shown as tindioxide crystalline phase, granularity be 0.6 micron be applicable to adulterate in the tindioxide lattice of spray ink Printing ceramic ink the dusty blue pigment of a small amount of antimony.
Embodiment nine
Be applicable to a preparation method for the dusty blue pigment of spray ink Printing ceramic ink, comprise the following steps:
A. tin metal, antimony metal are heated to 930 DEG C of meltings, wherein the mass ratio of tin and antimony is 30:1, and the melt that after tin, antimony melting, stirring forms tin, antimony is evenly distributed, carries out ultrasonic atomization by this melt, obtain granularity 1000 object alloy fine powder;
B. alloy fine powder steps A obtained and polypropylene glycol are added to in the closed reactor stirred, the quality of polypropylene glycol and the mass ratio of alloy fine powder are 3.1:1, pressurized air is passed in closed reactor, the mass ratio of compressed-air actuated quality and alloy fine powder is 3.5:1, compressed-air actuated pressure is 0.55MPa, mixing speed is 400 revs/min, and closed reactor temperature is 125 DEG C, reacts and obtains alloy stabilizing solution in 8 hours;
C. adopting ullrasonic spraying mode alloy stabilizing solution to be sprayed into temperature is top in 800 DEG C of fluidized-bed reactors, pass into from the bottom of fluidized-bed reactor the oxygen that temperature is 440 DEG C simultaneously, the pressure of oxygen is 0.3MPa, and the mass ratio of the polypropylene glycol in the quality of oxygen and step B is 3.5:1; Namely obtain in the bottom of fluidized-bed reactor that X-ray diffraction test result is shown as tindioxide crystalline phase, granularity be 0.45 micron be applicable to adulterate in the tindioxide lattice of spray ink Printing ceramic ink the dusty blue pigment of a small amount of antimony.
Embodiment ten
Be applicable to a preparation method for the dusty blue pigment of spray ink Printing ceramic ink, comprise the following steps:
A. tin metal, antimony metal are heated to 960 DEG C of meltings, wherein the mass ratio of tin and antimony is 70:1, and the melt that after tin, antimony melting, stirring forms tin, antimony is evenly distributed, carries out ultrasonic atomization by this melt, obtain granularity 1100 object alloy fine powder;
B. alloy fine powder steps A obtained and polypropylene glycol are added to in the closed reactor stirred, the quality of polypropylene glycol and the mass ratio of alloy fine powder are 3:1, pressurized air is passed in closed reactor, the mass ratio of compressed-air actuated quality and alloy fine powder is 3:1, compressed-air actuated pressure is 0.8MPa, mixing speed is 280 revs/min, and closed reactor temperature is 130 DEG C, reacts and obtains alloy stabilizing solution in 9 hours;
C. adopting ullrasonic spraying mode alloy stabilizing solution to be sprayed into temperature is top in 750 DEG C of fluidized-bed reactors, pass into from the bottom of fluidized-bed reactor the oxygen that temperature is 410 DEG C simultaneously, the pressure of oxygen is 0.22MPa, and the mass ratio of the polypropylene glycol in the quality of oxygen and step B is 4.5:1; Namely obtain in the bottom of fluidized-bed reactor that X-ray diffraction test result is shown as tindioxide crystalline phase, granularity be 0.35 micron be applicable to adulterate in the tindioxide lattice of spray ink Printing ceramic ink the dusty blue pigment of a small amount of antimony.
Claims (1)
1. be applicable to a preparation method for the dusty blue pigment of spray ink Printing ceramic ink, it is characterized in that comprising the following steps:
A. tin metal, antimony metal are heated to 850 ~ 1100 DEG C of meltings, wherein the mass ratio of tin and antimony is 10 ~ 99:1, the melt that after tin, antimony melting, stirring forms tin, antimony is evenly distributed, carries out ultrasonic atomization by this melt, obtains granularity 1000 order ~ 1500 object alloy fine powder;
B. alloy fine powder steps A obtained and polypropylene glycol are added to in the closed reactor stirred, the quality of polypropylene glycol and the mass ratio of alloy fine powder are 1 ~ 3.5:1, pressurized air is passed in closed reactor, the mass ratio of compressed-air actuated quality and alloy fine powder is 2 ~ 6:1, compressed-air actuated pressure is 0.2 ~ 0.9MPa, mixing speed is 150 ~ 400 revs/min, and closed reactor temperature is 90 ~ 130 DEG C, reacts and obtains alloy stabilizing solution in 3 ~ 12 hours;
C. adopting ullrasonic spraying mode alloy stabilizing solution to be sprayed into temperature is top in 500 ~ 900 DEG C of fluidized-bed reactors, pass into from the bottom of fluidized-bed reactor the oxygen that temperature is 200 ~ 450 DEG C simultaneously, the pressure of oxygen is 0.1 ~ 0.3 MPa, and the mass ratio of the polypropylene glycol in the quality of oxygen and step B is 3 ~ 8:1; Namely the dusty blue pigment of a small amount of antimony that adulterates is obtained in the tindioxide lattice being applicable to spray ink Printing ceramic ink in the bottom of fluidized-bed reactor.
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| CN111621169A (en) * | 2020-06-05 | 2020-09-04 | 江苏拜富科技股份有限公司 | Method for blending high-stability pigment for heat-resistant porcelain pot |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111621169A (en) * | 2020-06-05 | 2020-09-04 | 江苏拜富科技股份有限公司 | Method for blending high-stability pigment for heat-resistant porcelain pot |
| CN111621169B (en) * | 2020-06-05 | 2021-06-08 | 江苏拜富科技股份有限公司 | Method for blending high-stability pigment for heat-resistant porcelain pot |
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