CN116478560A - Black pearlescent pigment and preparation method thereof - Google Patents
Black pearlescent pigment and preparation method thereof Download PDFInfo
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- CN116478560A CN116478560A CN202310294156.4A CN202310294156A CN116478560A CN 116478560 A CN116478560 A CN 116478560A CN 202310294156 A CN202310294156 A CN 202310294156A CN 116478560 A CN116478560 A CN 116478560A
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- 239000000049 pigment Substances 0.000 title claims abstract description 183
- 238000002360 preparation method Methods 0.000 title abstract description 13
- 239000002243 precursor Substances 0.000 claims abstract description 93
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 75
- 239000000843 powder Substances 0.000 claims abstract description 46
- 239000004408 titanium dioxide Substances 0.000 claims abstract description 37
- 238000000034 method Methods 0.000 claims abstract description 13
- 239000007789 gas Substances 0.000 claims description 32
- 239000002245 particle Substances 0.000 claims description 20
- 238000012216 screening Methods 0.000 claims description 18
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 16
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims description 16
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 14
- 239000001257 hydrogen Substances 0.000 claims description 12
- 229910052739 hydrogen Inorganic materials 0.000 claims description 12
- 239000012495 reaction gas Substances 0.000 claims description 12
- 239000000758 substrate Substances 0.000 claims description 11
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 claims description 10
- 229910002091 carbon monoxide Inorganic materials 0.000 claims description 10
- 230000035484 reaction time Effects 0.000 claims description 10
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 8
- 229910052786 argon Inorganic materials 0.000 claims description 8
- 238000006243 chemical reaction Methods 0.000 claims description 8
- 239000010445 mica Substances 0.000 claims description 7
- 229910052618 mica group Inorganic materials 0.000 claims description 7
- 229910052757 nitrogen Inorganic materials 0.000 claims description 7
- 239000003570 air Substances 0.000 claims description 6
- 230000004048 modification Effects 0.000 claims description 6
- 238000012986 modification Methods 0.000 claims description 6
- RJDOZRNNYVAULJ-UHFFFAOYSA-L [O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[F-].[F-].[Mg++].[Mg++].[Mg++].[Al+3].[Si+4].[Si+4].[Si+4].[K+] Chemical compound [O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[F-].[F-].[Mg++].[Mg++].[Mg++].[Al+3].[Si+4].[Si+4].[Si+4].[K+] RJDOZRNNYVAULJ-UHFFFAOYSA-L 0.000 claims description 5
- 238000005507 spraying Methods 0.000 claims description 5
- 239000010985 leather Substances 0.000 claims description 4
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims description 4
- 239000003973 paint Substances 0.000 claims description 4
- 239000004033 plastic Substances 0.000 claims description 4
- 229920003023 plastic Polymers 0.000 claims description 4
- 235000012239 silicon dioxide Nutrition 0.000 claims description 4
- 239000000377 silicon dioxide Substances 0.000 claims description 4
- 241000276425 Xiphophorus maculatus Species 0.000 claims description 2
- 125000004435 hydrogen atom Chemical class [H]* 0.000 claims 2
- 230000009467 reduction Effects 0.000 abstract description 12
- 239000011248 coating agent Substances 0.000 abstract description 7
- 238000000576 coating method Methods 0.000 abstract description 7
- 239000000126 substance Substances 0.000 abstract description 5
- 238000005516 engineering process Methods 0.000 abstract description 4
- 230000008569 process Effects 0.000 abstract description 3
- 238000011946 reduction process Methods 0.000 abstract description 3
- 230000000694 effects Effects 0.000 description 7
- 150000002431 hydrogen Chemical class 0.000 description 7
- 238000012512 characterization method Methods 0.000 description 6
- 238000004458 analytical method Methods 0.000 description 5
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- 229910044991 metal oxide Inorganic materials 0.000 description 3
- 150000004706 metal oxides Chemical class 0.000 description 3
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 2
- GXDVEXJTVGRLNW-UHFFFAOYSA-N [Cr].[Cu] Chemical compound [Cr].[Cu] GXDVEXJTVGRLNW-UHFFFAOYSA-N 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 239000006229 carbon black Substances 0.000 description 2
- 238000005253 cladding Methods 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- SZVJSHCCFOBDDC-UHFFFAOYSA-N ferrosoferric oxide Chemical compound O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 description 2
- DALUDRGQOYMVLD-UHFFFAOYSA-N iron manganese Chemical compound [Mn].[Fe] DALUDRGQOYMVLD-UHFFFAOYSA-N 0.000 description 2
- 238000007639 printing Methods 0.000 description 2
- 238000005728 strengthening Methods 0.000 description 2
- 239000010936 titanium Substances 0.000 description 2
- 229910052719 titanium Inorganic materials 0.000 description 2
- QVYYOKWPCQYKEY-UHFFFAOYSA-N [Fe].[Co] Chemical compound [Fe].[Co] QVYYOKWPCQYKEY-UHFFFAOYSA-N 0.000 description 1
- BQCFCWXSRCETDO-UHFFFAOYSA-N [Fe].[Mn].[Cu] Chemical compound [Fe].[Mn].[Cu] BQCFCWXSRCETDO-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 230000003796 beauty Effects 0.000 description 1
- 239000004566 building material Substances 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 239000003086 colorant Substances 0.000 description 1
- 230000000295 complement effect Effects 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 239000002537 cosmetic Substances 0.000 description 1
- 238000005034 decoration Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 210000003298 dental enamel Anatomy 0.000 description 1
- -1 enamel Substances 0.000 description 1
- 239000000976 ink Substances 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 239000002932 luster Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 230000005012 migration Effects 0.000 description 1
- 238000013508 migration Methods 0.000 description 1
- 239000011050 natural pearl Substances 0.000 description 1
- 231100000956 nontoxicity Toxicity 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 239000012860 organic pigment Substances 0.000 description 1
- 238000004806 packaging method and process Methods 0.000 description 1
- 239000000123 paper Substances 0.000 description 1
- 239000011049 pearl Substances 0.000 description 1
- 239000005060 rubber Substances 0.000 description 1
- 239000000344 soap Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000004753 textile Substances 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
- 230000000007 visual effect Effects 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
- C09C1/0015—Pigments exhibiting interference colours, e.g. transparent platelets of appropriate thinness or flaky substrates, e.g. mica, bearing appropriate thin transparent coatings
- C09C1/0021—Pigments exhibiting interference colours, e.g. transparent platelets of appropriate thinness or flaky substrates, e.g. mica, bearing appropriate thin transparent coatings comprising a core coated with only one layer having a high or low refractive index
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
- C09C3/06—Treatment with inorganic compounds
- C09C3/063—Coating
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/60—Optical properties, e.g. expressed in CIELAB-values
Abstract
The invention discloses a black pearlescent pigment and a preparation method thereof, and belongs to the technical field of pearlescent pigments. According to the invention, titanium dioxide of the pearlescent pigment is reduced to titanium dioxide, the black pearlescent pigment is prepared by utilizing the black pigment characteristic of titanium dioxide, no coating modified substance or complex mixed oxide is additionally added, the purity of the pearlescent pigment is maximally maintained, excellent blackness and brightness are ensured to be obtained at the same time, the surface reduction treatment is carried out on the pearlescent pigment precursor by adopting a gas phase reduction technology, a flowing powder reinforced reduction process is designed, the reduction temperature is reduced, the reduction efficiency is improved, and the process is simple, the economy is good and the environment is protected.
Description
Technical Field
The invention belongs to the technical field of pearlescent pigments, and particularly relates to a black pearlescent pigment and a preparation method thereof.
Background
The pearlescent pigment is an optical effect pigment, has the glittering effect of metal pigment, can generate soft color of natural pearl, can generate multi-level reflection when being irradiated by sunlight, and has the characteristics of soft and attractive or colorful luster and color due to interaction of reflected light, strong covering power, high refractive index, excellent chemical stability, rich color, acid and alkali resistance, no toxicity and the like, and has been widely applied to various fields of paint, plastics, rubber, printing ink, paper, textiles, cosmetics, ornaments, artware, leather, enamel, ceramics, packaging articles, printing decoration, building materials and the like. These filters divide the incident light that reaches the interface between materials of different refractive indices at a suitable angle into the complementary reflected and transmitted portions (other angles of incident light can also be absorbed and reflected) as observed in our daily lives, such as soap bubbles, spilled oils, and pearl colors.
The titanium dioxide mica pearlescent pigment is the most widely studied and mature technology, and due to the different refractive indexes of titanium dioxide and mica substrates, better pearlescent effect, color effect and visual angle color flashing effect are generated through the multiple reflection and interference effects of light, and along with the development of society and economy, people have pursued higher levels of beauty and color, and the industry development of the pearlescent pigment is very rapid.
Among pigments, black pigments are pigments which are extremely widely used, mainly comprise carbon black, titanium dioxide, iron manganese black, iron oxide black, copper chromium black and the like, and compared with the black pearlescent pigments, the types and markets of the black pearlescent pigments are far fewer, and the black pearlescent pigment products on the market mainly comprise the following two types: firstly, the pearlescent pigment is dyed black by an organic pigment.
For example, patent CN106009784B reports that carbon black and pearlescent pigment form black pearlescent pigment through chemical combination or physical adsorption, but the product is easy to have quality problem and has poor thermal stability because the blackness and brightness are hard to match and color migration is easy to occur; secondly, black metal oxide "cladding" type pearlescent pigment, through cladding a layer of black composite metal oxide such as iron cobalt compound (patent CN 109054457B), ferroferric oxide, iron manganese black (patent CN114316630 a), copper chromium black, copper iron manganese black, etc. on the surface of the flaky substrate, black pearlescent is formed by the natural color of the metal oxide, and the blackness and brightness of the product are relatively poor.
Therefore, the application field of the above products is limited to a certain extent.
Disclosure of Invention
(one) solving the technical problems
In order to overcome the defects of the prior art, the invention provides the black pearlescent pigment and the preparation method thereof, which solve the problems of difficult matching of blackness and brightness and poor thermal temperature property of the existing black pearlescent pigment.
(II) technical scheme
In order to achieve the above purpose, the present invention provides the following technical solutions: a black pearlescent pigment, which is made from a pearlescent pigment precursor comprising titanium suboxide, the pearlescent pigment precursor being a titanium dioxide coated medium pearlescent pigment.
As a further aspect of the invention: the platy substrate in the pearlescent pigment precursor is one or more of natural mica, synthetic mica, silicon dioxide and aluminum oxide.
Preferably, the particle size of the pearlescent pigment precursor is 5-125 μm, more preferably, the particle size of the pearlescent pigment precursor is 10-60 μm, and preferably, the ratio of diameter to thickness of the pearlescent pigment precursor is not less than 50.
As a further aspect of the invention: the titanium dioxide in the black pearlescent pigment is reduced, in whole or in part, to titanium dioxide.
As a further aspect of the invention: the content of the titanium suboxide is 50 to 100%, preferably 80 to 90%.
A preparation method of black pearlescent pigment comprises the following steps:
s100, screening the pearlescent pigment precursor to enable the particle size of the pearlescent pigment precursor to be 10-60 mu m, wherein the diameter-thickness ratio of the pearlescent pigment precursor is more than or equal to 50.
S200, placing the pearlescent pigment precursor after screening treatment into a reactor, setting the reactor to be heated to a certain temperature, maintaining a constant temperature state, and adjusting control parameters to enable the pearlescent pigment precursor powder to be in a continuous motion state.
And S300, introducing a reducing reaction gas into the reactor, fully contacting with pearlescent pigment precursor powder, and reacting for a certain reaction time.
S400, taking out the prepared black pearlescent pigment after the temperature of the reactor is reduced.
As a further aspect of the invention: in S300, the reducing reaction gas is a mixed gas of one or more of hydrogen, carbon monoxide and methane and one or two of nitrogen and argon.
As a further aspect of the invention: the gas percentage of hydrogen, carbon monoxide, methane is not more than 10%, preferably not more than 5%.
As a further aspect of the invention: the reactor is one of a fluidized bed, a vibrating bed and a rotary furnace.
The operating gas of the reactor is one or more of nitrogen, argon and air.
The operating gas velocity of the fluidized bed is 0.05-0.5 m/s.
The vibration knocking frequency of the vibration bed is 60-300 times/min.
The rotation speed of the rotary furnace is 5-60 r/min.
As a further aspect of the invention: in S300, the chemical reaction temperature in the reactor is 400 to 700 ℃, preferably, the modification chemical reaction temperature is 500 to 600 ℃.
The modification chemical reaction duration is 30 to 120min, preferably 60 to 90min.
As a further aspect of the invention: the black pearlescent pigment is applied in electrostatic powder spraying, paint, plastics, leather or wallpaper.
(III) beneficial effects
Compared with the prior art, the invention has the beneficial effects that:
1. according to the invention, the titanium dioxide of the pearlescent pigment is reduced to titanium dioxide, and the black pearlescent pigment is prepared by utilizing the black pigment characteristic of titanium dioxide, and a coating modified substance or a complex mixed oxide is not added, so that the purity of the pearlescent pigment is maintained to the maximum extent, and excellent blackness and brightness are ensured to be obtained at the same time.
2. According to the invention, the surface reduction treatment is carried out on the pearlescent pigment precursor by adopting a gas phase reduction technology, the flowing powder strengthening reduction process is designed, the reduction temperature is reduced, the reduction efficiency is improved, the process is simple, the economy is good, the environment is protected, and meanwhile, the pearlescent pigment is applied to the electrostatic powder coating, so that the high powder coating rate and the excellent spraying effect are obtained.
Drawings
FIG. 1 is a schematic flow chart of the present invention;
FIG. 2 is a schematic illustration of pretreatment of pearlescent pigment precursors of the present invention;
FIG. 3 is a schematic block diagram of the reactor control of the present invention;
fig. 4 is a schematic diagram of step S300 of the present invention.
Detailed Description
The technical scheme of the patent is further described in detail below with reference to the specific embodiments.
As shown in fig. 1-4, the present invention provides a technical solution: a black pearlescent pigment is prepared from pearlescent pigment precursor, wherein the black pearlescent pigment contains titanium dioxide, and the pearlescent pigment precursor is titanium dioxide coated medium pearlescent pigment.
The flaky substrate in the pearlescent pigment precursor is one or more of natural mica, synthetic mica, silicon dioxide and aluminum oxide.
Preferably, the particle size of the pearlescent pigment precursor is 5-125 μm, more preferably, the particle size of the pearlescent pigment precursor is 10-60 μm, and preferably, the ratio of the diameter to the thickness of the pearlescent pigment precursor is not less than 50.
The titanium dioxide in the black pearlescent pigment is reduced, in whole or in part, to titanium dioxide.
The content of titanium oxide is 50 to 100%, preferably 80 to 90%.
A preparation method of black pearlescent pigment comprises the following steps:
s100, screening the pearlescent pigment precursor to enable the particle size of the pearlescent pigment precursor to be 10-60 mu m, wherein the diameter-thickness ratio of the pearlescent pigment precursor is more than or equal to 50.
S200, placing the pearlescent pigment precursor after screening treatment into a reactor, setting the reactor to be heated to a certain temperature, maintaining a constant temperature state, and adjusting control parameters to enable the pearlescent pigment precursor powder to be in a continuous motion state.
And S300, introducing a reducing reaction gas into the reactor, fully contacting with pearlescent pigment precursor powder, and reacting for a certain reaction time.
S400, taking out the prepared black pearlescent pigment after the temperature of the reactor is reduced.
In S300, the reducing reaction gas is a mixed gas of one or more of hydrogen, carbon monoxide and methane and one or two of nitrogen and argon.
The gas percentages of hydrogen, carbon monoxide, methane are not more than 10%, preferably not more than 5%.
The reactor is one of a fluidized bed, a vibrating bed and a rotary furnace.
The operating gas of the reactor is one or more of nitrogen, argon and air.
The operating gas velocity of the fluidized bed is 0.05-0.5 m/s.
The vibration knocking frequency of the vibration bed is 60-300 times/min.
The rotation speed of the rotary furnace is 5-60 r/min.
In S300, the chemical reaction temperature in the reactor is 400 to 700 ℃, preferably, the modification chemical reaction temperature is 500 to 600 ℃.
The modification chemical reaction duration is 30 to 120min, preferably 60 to 90min.
The black pearlescent pigment is applied in electrostatic powder spraying, paint, plastics, leather or wallpaper.
Example 1
A preparation method of black pearlescent pigment comprises the following steps:
s100, screening the pearlescent pigment precursor to enable the particle size of the pearlescent pigment precursor to be 10-60 mu m.
S200, placing the pearlescent pigment precursor after screening treatment into a reactor, setting the reactor to be heated to a certain temperature, maintaining a constant temperature state, and adjusting control parameters to enable the pearlescent pigment precursor powder to be in a continuous motion state.
And S300, introducing a reducing reaction gas into the reactor, fully contacting with pearlescent pigment precursor powder, and reacting for a certain reaction time.
S400, taking out the prepared black pearlescent pigment after the temperature of the reactor is reduced.
The method comprises the steps of selecting a natural mica substrate pearlescent pigment (the particle size is 5 mu m, the diameter-thickness ratio is more than or equal to 50) containing titanium dioxide as a precursor, setting a fluidized bed reactor, heating to 400 ℃, maintaining a constant temperature state, putting pearlescent pigment precursor powder into the reactor, taking nitrogen as operation gas of the reactor, controlling the gas speed to be 0.05m/s, and adjusting the operation parameters to enable the pearlescent pigment precursor powder to be in a continuous motion state; introducing hydrogen, wherein the gas percentage of the hydrogen is 10%, and fully contacting with pearlescent pigment precursor powder; reacting for 30min; and taking out the modified black pearlescent pigment after the temperature of the reactor is reduced.
The prepared black pearlescent pigment is found to have a titanium dioxide content of 50% by analytical characterization.
Example 2
A preparation method of black pearlescent pigment comprises the following steps:
s100, screening the pearlescent pigment precursor to enable the particle size of the pearlescent pigment precursor to be 10-60 mu m.
S200, placing the pearlescent pigment precursor after screening treatment into a reactor, setting the reactor to be heated to a certain temperature, maintaining a constant temperature state, and adjusting control parameters to enable the pearlescent pigment precursor powder to be in a continuous motion state.
And S300, introducing a reducing reaction gas into the reactor, fully contacting with pearlescent pigment precursor powder, and reacting for a certain reaction time.
S400, taking out the prepared black pearlescent pigment after the temperature of the reactor is reduced.
The method comprises the steps of selecting a synthetic mica substrate pearlescent pigment (the particle size is 125 mu m, the diameter-thickness ratio is more than or equal to 60) containing titanium dioxide as a precursor, setting a vibrating bed reactor to be heated to 700 ℃, maintaining a constant temperature state, putting pearlescent pigment precursor powder into the reactor, taking argon as operation gas of the reactor, controlling the operation gas speed to be 0.5m/s, controlling the vibrating knocking frequency of a vibrating bed to be 60 times/min, and adjusting control parameters to enable the pearlescent pigment precursor powder to be in a continuous motion state; introducing carbon monoxide, wherein the gas percentage of the carbon monoxide is 7%, and fully contacting with pearlescent pigment precursor powder; reacting for 120min; and taking out the modified black pearlescent pigment after the temperature of the reactor is reduced.
The prepared black pearlescent pigment is found by analysis and characterization to have the titanium dioxide content of 100%.
Example 3
A preparation method of black pearlescent pigment comprises the following steps:
s100, screening the pearlescent pigment precursor to enable the particle size of the pearlescent pigment precursor to be 10-60 mu m.
S200, placing the pearlescent pigment precursor after screening treatment into a reactor, setting the reactor to be heated to a certain temperature, maintaining a constant temperature state, and adjusting control parameters to enable the pearlescent pigment precursor powder to be in a continuous motion state.
And S300, introducing a reducing reaction gas into the reactor, fully contacting with pearlescent pigment precursor powder, and reacting for a certain reaction time.
S400, taking out the prepared black pearlescent pigment after the temperature of the reactor is reduced.
The method comprises the steps of selecting a natural mica substrate pearlescent pigment (the particle size is 25 mu m, the diameter-thickness ratio is more than or equal to 70) containing titanium dioxide as a precursor, setting a fluidized bed reactor, heating to 600 ℃, maintaining a constant temperature state, putting pearlescent pigment precursor powder into the reactor, taking air as operation gas of the reactor, controlling the gas speed to be 0.5m/s, and adjusting the operation parameters to enable the pearlescent pigment precursor powder to be in a continuous motion state; introducing methane, wherein the gas percentage of the methane is 5%, and fully contacting with pearlescent pigment precursor powder; reacting for 66min; and taking out the modified black pearlescent pigment after the temperature of the reactor is reduced.
The prepared black pearlescent pigment is found to have titanium dioxide content of 80% by analysis and characterization.
Example 4
A preparation method of black pearlescent pigment comprises the following steps:
s100, screening the pearlescent pigment precursor to enable the particle size of the pearlescent pigment precursor to be 10-60 mu m.
S200, placing the pearlescent pigment precursor after screening treatment into a reactor, setting the reactor to be heated to a certain temperature, maintaining a constant temperature state, and adjusting control parameters to enable the pearlescent pigment precursor powder to be in a continuous motion state.
And S300, introducing a reducing reaction gas into the reactor, fully contacting with pearlescent pigment precursor powder, and reacting for a certain reaction time.
S400, taking out the prepared black pearlescent pigment after the temperature of the reactor is reduced.
Selecting a titanium dioxide-containing silicon dioxide substrate pearlescent pigment (particle size is 60 mu m, diameter-thickness ratio is more than or equal to 100) as a precursor, setting a vibrating bed reactor, heating to 500 ℃, maintaining a constant temperature state, placing pearlescent pigment precursor powder into the reactor, taking argon as operation gas of the reactor, operating the gas speed to be 0.1m/s, vibrating the vibrating bed to beat at a frequency of 300 times/min, and adjusting control parameters to enable the pearlescent pigment precursor powder to be in a continuous motion state; introducing hydrogen, wherein the gas percentage of the hydrogen is 4%, and fully contacting with pearlescent pigment precursor powder; reacting for a certain reaction time of 100min; and taking out the modified black pearlescent pigment after the temperature of the reactor is reduced.
The prepared black pearlescent pigment is found by analysis and characterization to have the titanium dioxide content of 90%.
Example 5
A preparation method of black pearlescent pigment comprises the following steps:
s100, screening the pearlescent pigment precursor to enable the particle size of the pearlescent pigment precursor to be 10-60 mu m.
S200, placing the pearlescent pigment precursor after screening treatment into a reactor, setting the reactor to be heated to a certain temperature, maintaining a constant temperature state, and adjusting control parameters to enable the pearlescent pigment precursor powder to be in a continuous motion state.
And S300, introducing a reducing reaction gas into the reactor, fully contacting with pearlescent pigment precursor powder, and reacting for a certain reaction time.
S400, taking out the prepared black pearlescent pigment after the temperature of the reactor is reduced.
Selecting titanium dioxide-containing aluminum oxide substrate pearlescent pigment (particle size is 20 mu m, diameter-thickness ratio is more than or equal to 50) as a precursor, setting a rotary furnace reactor to be heated to 650 ℃, maintaining a constant temperature state, putting pearlescent pigment precursor powder into the reactor, taking air as operation gas of the reactor, operating the gas at the speed of 0.3m/s, rotating the rotary furnace at the speed of 5r/min, and adjusting control parameters to enable the pearlescent pigment precursor powder to be in a continuous motion state; introducing carbon monoxide, wherein the gas percentage of the carbon monoxide is 6%, and fully contacting with pearlescent pigment precursor powder; reacting for 95min; and taking out the modified black pearlescent pigment after the temperature of the reactor is reduced.
The prepared black pearlescent pigment is found to have titanium dioxide content of 78% by analysis and characterization.
Example 6
A preparation method of black pearlescent pigment comprises the following steps:
s100, screening the pearlescent pigment precursor to enable the particle size of the pearlescent pigment precursor to be 10-60 mu m.
S200, placing the pearlescent pigment precursor after screening treatment into a reactor, setting the reactor to be heated to a certain temperature, maintaining a constant temperature state, and adjusting control parameters to enable the pearlescent pigment precursor powder to be in a continuous motion state.
And S300, introducing a reducing reaction gas into the reactor, fully contacting with pearlescent pigment precursor powder, and reacting for a certain reaction time.
S400, taking out the prepared black pearlescent pigment after the temperature of the reactor is reduced.
The method comprises the steps of selecting a synthetic mica substrate pearlescent pigment (particle size is 10 mu m, diameter-thickness ratio is more than or equal to 100) containing titanium dioxide as a precursor, setting a rotary furnace reactor to be heated to 450 ℃ and then maintaining a constant temperature state, putting pearlescent pigment precursor powder into the reactor, taking air as operation gas of the reactor, controlling the operation gas speed to be 0.4m/s, controlling the rotation speed of the rotary furnace to be 60r/min, and adjusting control parameters to enable the pearlescent pigment precursor powder to be in a continuous motion state; introducing hydrogen, wherein the gas percentage of the hydrogen is 10%, and fully contacting with pearlescent pigment precursor powder; reacting for 110min; and taking out the modified black pearlescent pigment after the temperature of the reactor is reduced.
The prepared black pearlescent pigment is found by analysis and characterization to have the titanium dioxide content of 95%.
The following table is derived according to examples 1-6:
from the above table it is known that: titanium dioxide content is obtained on the basis of different reactors and conditions.
The method comprises the following steps:
the titanium dioxide of the pearlescent pigment is reduced to titanium dioxide, and the black pearlescent pigment is prepared by utilizing the black pigment characteristic of the titanium dioxide, and a coating modified substance or a complex mixed oxide is not added, so that the purity of the pearlescent pigment is maintained to the maximum extent, and excellent blackness and brightness are ensured to be obtained at the same time.
The pearlescent pigment precursor is subjected to surface reduction treatment by adopting a gas phase reduction technology, a flowing powder strengthening reduction process is designed, the reduction temperature is reduced, the reduction efficiency is improved, the process is simple, the economy is good, the environment is protected, and meanwhile, the pearlescent pigment is applied to electrostatic powder coating, so that high powder coating rate and excellent spraying effect are obtained.
The last points to be described are: while the invention has been described in detail in the foregoing general description and with reference to specific embodiments, the foregoing embodiments are merely illustrative of the technical aspects of the invention and are not limiting thereof; although the invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical scheme described in the foregoing embodiments can be modified or some or all of the technical features thereof can be replaced by equivalents; such modifications and substitutions do not depart from the spirit of the invention.
Claims (10)
1. The black pearlescent pigment is characterized in that the black pearlescent pigment is prepared from a pearlescent pigment precursor, the black pearlescent pigment contains titanium dioxide, and the pearlescent pigment precursor is a titanium dioxide coated medium pearlescent pigment.
2. A black pearlescent pigment according to claim 1 wherein: the platy substrate in the pearlescent pigment precursor is one or more of natural mica, synthetic mica, silicon dioxide and aluminum oxide;
the particle size of the pearlescent pigment precursor is 5-125 mu m, and the diameter-thickness ratio of the pearlescent pigment precursor is more than or equal to 50.
3. A black pearlescent pigment according to claim 1 wherein: the titanium dioxide in the black pearlescent pigment is reduced, in whole or in part, to titanium dioxide.
4. A black pearlescent pigment according to claim 3 wherein: the content of the titanium dioxide is 50-100%.
5. A method for preparing a black pearlescent pigment according to any one of claims 1 to 4, comprising the steps of:
s100, screening the pearlescent pigment precursor to enable the particle size of the pearlescent pigment precursor to be 10-60 mu m, wherein the diameter-thickness ratio of the pearlescent pigment precursor is more than or equal to 50;
s200, placing the pearlescent pigment precursor after screening treatment into a reactor, setting the reactor to be heated to a certain temperature, maintaining a constant temperature state, and adjusting control parameters to enable the pearlescent pigment precursor powder to be in a continuous motion state;
s300, introducing a reducing reaction gas into the reactor, fully contacting with pearlescent pigment precursor powder, and reacting for a certain reaction time;
s400, taking out the prepared black pearlescent pigment after the temperature of the reactor is reduced.
6. The method for preparing a black pearlescent pigment according to claim 5, wherein: in S300, the reducing reaction gas is a mixed gas of one or more of hydrogen, carbon monoxide and methane and one or two of nitrogen and argon.
7. The method for preparing a black pearlescent pigment according to claim 6, wherein: the gas percentages of the hydrogen, the carbon monoxide and the methane are not more than 10 percent.
8. The method for preparing a black pearlescent pigment according to claim 5, wherein: the reactor is one of a fluidized bed, a vibrating bed and a rotary furnace;
the operating gas of the reactor is one or more of nitrogen, argon and air;
the operation gas speed of the fluidized bed is 0.05-0.5 m/s;
the vibration knocking frequency of the vibration bed is 60-300 times/min;
the rotation speed of the rotary furnace is 5-60 r/min.
9. The method for preparing a black pearlescent pigment according to claim 5, wherein: in the step S300, the chemical reaction temperature in the reactor is 400-700 ℃;
the duration of the modification chemical reaction is 30-120 min.
10. A black pearlescent pigment according to any one of claims 1 to 4 wherein: the black pearlescent pigment is applied in electrostatic powder spraying, paint, plastics, leather or wallpaper.
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| CN202310294156.4A CN116478560A (en) | 2023-03-24 | 2023-03-24 | Black pearlescent pigment and preparation method thereof |
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| CN202310294156.4A CN116478560A (en) | 2023-03-24 | 2023-03-24 | Black pearlescent pigment and preparation method thereof |
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