CN105907130A - High-purity interference green effect pearlescent pigment and preparation method thereof - Google Patents

High-purity interference green effect pearlescent pigment and preparation method thereof Download PDF

Info

Publication number
CN105907130A
CN105907130A CN201610314477.6A CN201610314477A CN105907130A CN 105907130 A CN105907130 A CN 105907130A CN 201610314477 A CN201610314477 A CN 201610314477A CN 105907130 A CN105907130 A CN 105907130A
Authority
CN
China
Prior art keywords
minutes
purity
pearlescent pigment
aqueous solution
refractive index
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN201610314477.6A
Other languages
Chinese (zh)
Inventor
余青
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
JIANGSU BEILIDE NEW MATERIALS CO Ltd
Original Assignee
JIANGSU BEILIDE NEW MATERIALS CO Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by JIANGSU BEILIDE NEW MATERIALS CO Ltd filed Critical JIANGSU BEILIDE NEW MATERIALS CO Ltd
Priority to CN201610314477.6A priority Critical patent/CN105907130A/en
Publication of CN105907130A publication Critical patent/CN105907130A/en
Pending legal-status Critical Current

Links

Classifications

    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09CTREATMENT 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
    • C09C1/00Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
    • C09C1/0015Pigments exhibiting interference colours, e.g. transparent platelets of appropriate thinness or flaky substrates, e.g. mica, bearing appropriate thin transparent coatings
    • C09C1/0024Pigments exhibiting interference colours, e.g. transparent platelets of appropriate thinness or flaky substrates, e.g. mica, bearing appropriate thin transparent coatings comprising a stack of coating layers with alternating high and low refractive indices, wherein the first coating layer on the core surface has the high refractive index
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09CTREATMENT 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
    • C09C3/00Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
    • C09C3/06Treatment with inorganic compounds
    • C09C3/063Coating

Landscapes

  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Cosmetics (AREA)
  • Pigments, Carbon Blacks, Or Wood Stains (AREA)

Abstract

The invention provides high-purity interference green effect pearlescent pigment. Multiple oxide layers are sequentially covered on a natural mica base sheet; high-purity interference green effect margaritaceous pigment is generated by using different refraction indexes of different oxides; in addition, the invention also provides a production method of the pearlescent pigment. The natural mica is used as base materials; a liquid phase deposition method is used; under the conditions of the proper temperature and PH value, oxide layers with different refractive indexes are covered; finally, drying and roasting are performed to form high-purity interference green effect pearlescent pigment. The method has the advantages that the production process is simple; the operability is high; the scale production is stable; the cost is low; the pigment is suitable for industrial production.

Description

A kind of high-purity interferes green effect pearlescent pigment and preparation method thereof
Technical field
The invention belongs to pigment art, particularly relate to a kind of high-purity and interfere green effect pearlescent pigment and preparation method thereof.
Background technology
Green, belongs to environmental protection, the youth, vibrant, is the color enjoying people to like.Usually said viridine green has following several realization means: [1] chrome green pigment, chrome green is to have lead chromate yellow and titanium cyanines indigo plant, barba hispanica to be blended by certain component, the appearance luster bright-coloured title guignet's green of this pigment or art green, but because its group contains chrome yellow, when application, its leaded toxicity should be noted that, containing barba hispanica in chrome green, and containing oxidant plumbous chromate, so having the possibility of spontaneous combustion when dust meets Mars, it is both needed to warn very much careful when being dried with pulverizing, chrome green after burning completely loses the characteristic of pigment, is changed into dark-brown material;[2] on mica substrate surface, it is coated with layer of metal oxide or coloring phthalocyanine green pigment with the method for chemical deposition or physical absorption, and obtains pearly-lustre viridine green;As reached to interfere green pearl effect at mica surface cladding certain thickness titanium dioxide;The latter is liquid phase deposition coloring phthalocyanine green pigment, although two kinds of methods all can obtain green effect pearlescent pigments, but its color saturation, brightness, covering power are the most relatively poor, and produced green effect still has bigger difference compared with natural plants green;Making film and launch the most white keynote of color, lack nature youth active green phase, what these defects were serious limits the application of green pearlescent pigment.
As previously mentioned, conventional viridine green is in many defects of application aspect, surface of pigments optical phenomena is the surface metal by cladding mica substrate or nonmetal oxide multilayer coating structure layer, incident light is carried out multipath reflection, transmission and refraction, and the interference effect of light occurs;According to the principle of interference of light, there is metal and the nonmetal oxide layer of high and low refractive index in mica substrate surface multi-layer alternately cladding, by controlling the thickness of each clad, it is possible to prepare above-mentioned high-purity and interfere green effect pearlescent pigment;The green pearlescent pigment of plain interference, lot of domestic and international supplier can produce, but does not finds the pearlescent pigment with natural plants green effect.Though there are similar products in Merck KGaA company, but its complex manufacturing, process are difficult to control to, production cost high.Accordingly, it would be desirable to a kind of production technology is simple, workable, large-scale production is stable, the pearlescent pigment production technology of the natural plants of the low cost green phase high-purity green effect of interference.
Summary of the invention
For above-mentioned reason, the method that the present invention proposes to use multilayer coating structure, there is in mica substrate surface alternately cladding metal and the nonmetal oxide layer of high and low refractive index, prepare and above-mentioned inorganic viridine green, high-purity that plain interference is green, colour green pearlescent pigment has clear improvement, high glaze, the interference green effect pearlescent pigment of high covering power.
For reaching above-mentioned purpose, present invention employs following technical proposals:
A kind of high-purity interferes green effect pearlescent pigment, including natural mica substrate, mica substrate surface is coated with the first high refractive index oxide layer, the second high refractive index oxide layer, the first low-refraction oxide skin(coating), the 3rd high refractive index oxide layer and the second low-refraction oxide skin(coating) successively.
Described first high refractive index oxide layer is tin oxide.
Second, third high refractive index oxide layer described is titanium oxide
First low, the second low-refraction oxide skin(coating) described in 4 be silica, aluminum oxide one or both.
Described substrate thickness is 50 ~ 300 nanometers, first high refractive index oxide layer thickness is 1 ~ 4 nanometer, second high refractive index oxide layer thickness is 400 ~ 600 nanometers, and first, second low-refraction oxide layer thicknesses is 0.6 ~ 2.5 nanometer, the 3rd high refractive index oxide layer thickness 200 ~ 400 nanometer.
Described first, second, third high refractive index oxide refractive index is more than 2.6.
A kind of high-purity interferes the preparation method of green effect pearlescent pigment, comprises the following steps:
[1] in glass beaker, add water, throw 10 ~ 60 microns of mica substrates, open stirring 200 ~ 300 revs/min, heat up 70 ~ 75 DEG C, add hydrochloric acid or aqueous solution of nitric acid adjusts pH1.1 ~ 1.3, adjust and finish, stir 10 ~ 30 minutes;
[2] under constant temperature, stirring, butter of tin or the stannous chloride aqueous solution are dripped, and drip hydro-oxidation sodium water solution, maintain PH constant, charging is finished, and stirs 10 ~ 20 minutes;
[3] improving rotating speed 280 ~ 360 revs/min, intensification is 75 ~ 80 DEG C, promotes PH1.8 ~ 2.0 with sodium hydrate aqueous solution, and drip adds titanium tetrachloride, sodium hydrate aqueous solution, maintaining pH value constant, speed of agitator rises with liquid level and promotes rotating speed accordingly, charging is finished, and stirs 10 ~ 20 minutes;
[4] raising rotating speed is to 360 ~ 400 revs/min, and intensification is 82 ~ 85 DEG C, and single current adds sodium hydrate aqueous solution, promotes pH value 9.3 ~ 9.5, finishes, stirs 5 ~ 20 minutes;
[5] constant temperature stirring, and drip adds sodium silicate aqueous solution, with constant PH9.3 ~ 9.5 of nitric acid or aqueous hydrochloric acid solution, charging is finished, is stirred 5 ~ 20 minutes;
[6] reducing reaction temperature is 75 ~ 80 DEG C, and adjustment of rotational speed is 280 ~ 360 revs/min, adds with nitric acid or aqueous hydrochloric acid solution single current, adjusts pH1.8 ~ 2.0, finishes, stir 5 ~ 20 minutes;
[7] constant temperature stirring, and drip adds titanium tetrachloride, sodium hydrate aqueous solution, maintains temperature, pH value constant, speed of agitator rises with liquid level and promotes rotating speed accordingly, and charging is finished, and stirs 5 ~ 20 minutes;
[8] constant temperature stirring, single current dropping sodium silicate aqueous solution, charging is finished, is stirred 5 ~ 20 minutes;
[9] after reaction terminates, by material vacuum filtration in beaker, adding deionized water washing is neutrality to washings pH value;
[10] by 105 ~ 120 DEG C of forced air dryings of material 1 ~ 3 hour, calcine 10 ~ 25 minutes for 700 ~ 720 DEG C, obtain high-purity and interfere green effect pearlescent pigment.
Beneficial effects of the present invention: the product of the present invention passes through multilayer coating structure silica, different material interface is increased, light is easily linearly propagated in same medium, when running into the interface of different material when, then can be refracted away by a part of light, another part is reflected, it is possible to promote the fineness of each refracting layer, increase the effect of mirror-reflection, improve pigment purity;The inventive method production technology is simple, workable, large-scale production is stable, with low cost, be suitable for industrialized production.
Detailed description of the invention
Embodiment 1
[1] in glass beaker, add water 500 milliliters, throw 10 ~ 60 microns of mica substrates 30 grams, open stirring 200 revs/min, constant temperature 70 DEG C, add 2% hydrochloric acid and adjust pH1.1, adjust and finish, stir 10 minutes;
[2] under constant temperature, stirring, drip 10% butter of tin aqueous solution 20ml, and drip adds 20% sodium hydrate aqueous solution, maintain pH constant, control to finish for 30 minutes, continue stirring 10 minutes;
[3] rotating speed is improved to 280 revs/min, it is warming up to 75 DEG C, promote pH1.8 with 20% sodium hydrate aqueous solution, be slowly added dropwise 2M titanium tetrachloride, control time for adding 8 ~ 11 hours, and drip adds 20% sodium hydrate aqueous solution and maintains pH value constant, when dropping to water sample in interference green, stopping charging, during dropping, speed of agitator rises with liquid level and promotes rotating speed accordingly, charging is finished, and continues stirring 10 minutes;
[4] raising rotating speed is to 360 revs/min, is warming up to 82 DEG C, and single current adds 20% sodium hydrate aqueous solution, adjusts pH 9.3, finishes, and continues stirring 5 minutes;
[5] constant temperature stirring, and drip adds 20% sodium silicate aqueous solution 20 milliliters, by 8% aqueous hydrochloric acid solution constant pH 9.3, adds in controlling 40 minutes, continues stirring 5 minutes;
[6] reducing reaction temperature is 75 DEG C, and adjustment of rotational speed is 280 revs/min, adds with 8% aqueous hydrochloric acid solution single current, adjusts pH1.8, finishes, and continues stirring 5 minutes;
[7] constant temperature stirring, it is slowly added dropwise 2M titanium tetrachloride control time for adding about 6 hours and drip adds 20% sodium hydrate aqueous solution and maintains pH value constant, drop to water sample be second take turns interference green time, stop charging, during dropping, speed of agitator rises with liquid level and promotes rotating speed accordingly, charging is finished, and continues stirring 10 minutes;
[8] constant temperature stirring, single current drips 20% sodium silicate aqueous solution 10 milliliters, controls to add for 10 minutes, stirs 5 minutes;
[9] after reaction terminates, by material vacuum filtration in beaker, adding deionized water washing is neutrality to washings pH value;
[10] by 105 DEG C of forced air dryings of material 3 hours, calcine 25 minutes for 700 DEG C, obtain high-purity and interfere green effect pearlescent pigment.
Embodiment 2
[1] in glass beaker, add water 500 milliliters, throw 10 ~ 60 microns of mica substrates, open stirring 300 revs/min, constant temperature 75 DEG C, add 5% nitric acid and adjust pH1.3, adjust and finish, stir 30 minutes;
[2] under constant temperature, stirring, it is slowly added dropwise the dropping 5% stannous chloride aqueous solution 30 milliliters, and drip adds 20% sodium hydrate aqueous solution, maintain pH constant, control to finish for 50 minutes, continue stirring 20 minutes;
[3] rotating speed is improved to 360 revs/min, intensification is 80 DEG C, pH2.0 is promoted with 20% sodium hydrate aqueous solution, it is slowly added dropwise 2M titanium tetrachloride control time for adding 8 ~ 11 hours and drip adds 20% sodium hydrate aqueous solution and maintains pH value constant, when dropping to water sample in interference green, stopping charging, during dropping, speed of agitator rises with liquid level and promotes rotating speed accordingly, charging is finished, and continues stirring 20 minutes;
[4] raising rotating speed is to 400 revs/min, and intensification is 85 DEG C, and single current adds 20% sodium hydrate aqueous solution, promotes pH9.5, finishes, stirs 20 minutes;
[5] constant temperature stirring, and drip adds 20% sodium silicate aqueous solution 20 milliliters, by 8% aqueous hydrochloric acid solution constant pH 9.5, adds in controlling 40 minutes, continues stirring 20 minutes;
[6] reducing reaction temperature is 80 DEG C, and adjustment of rotational speed is 360 revs/min, adds with 8% aqueous solution of nitric acid single current, adjusts 2.0, finishes, stirs 20 minutes;
[7] constant temperature stirring, it is slowly added dropwise 2M titanium tetrachloride control time for adding 6 ~ 8 hours and drip adds 20% sodium hydrate aqueous solution and maintains pH value constant, drop to water sample be second take turns interference green time, stop charging, during dropping, speed of agitator rises with liquid level and promotes rotating speed accordingly, charging is finished, and continues stirring 10 ~ 20 minutes;
[8] constant temperature stirring, single current drips the 10% alchlor aqueous solution 5 milliliters, controls to add for 10 minutes, stirs 20 minutes;
[9] after reaction terminates, by material vacuum filtration in beaker, adding deionized water washing is neutrality to washings pH value;
[10] by 120 DEG C of forced air dryings of material 2 hours, calcine 10 minutes for 720 DEG C, obtain high-purity and interfere green effect pearlescent pigment.
Embodiment 3
[1] in glass beaker, add water 500 milliliters, throw 10 ~ 60 microns of mica substrates, open stirring 230 revs/min, heat up 72 DEG C, add 5% nitric acid and adjust pH1.2, adjust and finish, stir 20 minutes;
[2] under constant temperature, stirring, it is slowly added dropwise the dropping 10% butter of tin aqueous solution 20 milliliters, and drip adds 20% sodium hydrate aqueous solution, maintain pH constant, control to finish for 50 minutes, continue stirring 15 minutes;
[3] rotating speed 300 revs/min is improved, intensification is 77 DEG C, pH1.9 is promoted with 20% sodium hydrate aqueous solution, it is slowly added dropwise 2M titanium tetrachloride control time for adding 8 ~ 11 hours and drip adds 20% sodium hydrate aqueous solution and maintains pH value constant, when dropping to water sample in interference green, stopping charging, during dropping, speed of agitator rises with liquid level and promotes rotating speed accordingly, charging is finished, and continues stirring 15 minutes;
[4] raising rotating speed is to 380 revs/min, and intensification is 83 DEG C, and single current adds 20% sodium hydrate aqueous solution, adjusts pH value 9.4, finishes, stirs 10 minutes;
[5] constant temperature stirring, and drip adds the 10% alchlor aqueous solution 30 milliliters, by 8% aqueous hydrochloric acid solution constant pH 9.4, adds in controlling 40 minutes, continues stirring 10 minutes;
[6] reducing reaction temperature is 77 DEG C, and adjustment of rotational speed is 300 revs/min, adds with 8% aqueous solution of nitric acid single current, adjusts pH1.9, finishes, stirs 10 minutes;
[7] constant temperature stirring, it is slowly added dropwise 2M titanium tetrachloride control time for adding 6 ~ 8 hours and drip adds 20% sodium hydrate aqueous solution and maintains pH value constant, drop to water sample be second take turns interference green time, stop charging, during dropping, speed of agitator rises with liquid level and promotes rotating speed accordingly, charging is finished, and continues stirring 20 minutes;
[8] constant temperature stirring, single current drips the 10% alchlor aqueous solution 5 milliliters, controls to add for 10 minutes, stirs 15 minutes;
[9] after reaction terminates, by material vacuum filtration in beaker, adding deionized water washing is neutrality to washings pH value;
[10] by 110 DEG C of forced air drying 2h of material, calcine 15 minutes for 710 DEG C, obtain high-purity and interfere green effect pearlescent pigment.
Embodiment 4
[1] in glass beaker, add water 500 milliliters, throw 10 ~ 60 microns of mica substrates, open stirring 230 revs/min, heat up 72 DEG C, add 2% hydrochloric acid and adjust pH1.2, adjust and finish, stir 20 minutes;
[2] under constant temperature, stirring, it is slowly added dropwise the dropping 10% butter of tin aqueous solution 20 milliliters, and drip adds 20% sodium hydrate aqueous solution, maintain pH constant, control to finish for 50 minutes, continue stirring 15 minutes;
[3] rotating speed 300 revs/min is improved, intensification is 77 DEG C, pH1.9 is promoted with 20% sodium hydrate aqueous solution, it is slowly added dropwise 2M titanium tetrachloride control time for adding 8 ~ 11 hours and drip adds 20% sodium hydrate aqueous solution and maintains pH value constant, when dropping to water sample in interference green, stopping charging, during dropping, speed of agitator rises with liquid level and promotes rotating speed accordingly, charging is finished, and continues stirring 15 minutes;
[4] raising rotating speed is to 380 revs/min, and intensification is 83 DEG C, and single current adds 20% sodium hydrate aqueous solution, adjusts pH value 9.4, finishes, stirs 10 minutes;
[5] constant temperature stirring, and drip adds 20% sodium silicate aqueous solution 20 milliliters, by 8% aqueous hydrochloric acid solution constant pH 9.3, adds in controlling 40 minutes, continues stirring 15 minutes;
[6] reducing reaction temperature is 77 DEG C, and adjustment of rotational speed is 300 revs/min, adds with 8% aqueous solution of nitric acid single current, adjusts pH1.9, finishes, stirs 10 minutes;
[7] constant temperature stirring, it is slowly added dropwise 2M titanium tetrachloride control time for adding 6 ~ 8 hours and drip adds 20% sodium hydrate aqueous solution and maintains pH value constant, drop to water sample be second take turns interference green time, stop charging, during dropping, speed of agitator rises with liquid level and promotes rotating speed accordingly, charging is finished, and continues stirring 10 minutes;
[8] constant temperature stirring, single current drips the 10% alchlor aqueous solution 5 milliliters, controls to add for 10 minutes, stirs 15 minutes;
[9] after reaction terminates, by material vacuum filtration in beaker, adding deionized water washing is neutrality to washings pH value;
[10] 115 DEG C of air blast of material are dried 2 hours, calcine 20 minutes for 705 DEG C, obtain high-purity and interfere green effect pearlescent pigment.
The product that embodiment 1 ~ 4 prepares is filmed detection with Merck iriodin235, under the conditions of 45° angle, white background by color difference meter and spectrophotometer testing result is:
L lightness a b C saturation degree H look angle
iriodin235 87.1 7.0 1.0 29.31 155.47
Embodiment 1 92.3 6.3 1.1 49.32 173.62
Embodiment 2 91.7 6.2 1.1 38.61 169.53
Embodiment 3 92.1 6.2 1.0 45.83 167.45
Embodiment 4 91.6 6.3 1.2 46.49 166.76
Being proved by data above, in the case of a/b value is close, the titanium dioxide-coated mica utilizing the method for the present invention to work it out will be better than conventional products in lightness, saturation degree, is felt to be exactly that purity has obvious superiority the most intuitively by naked eyes;And the transparency of the base material of individual layer cladding itself is good, the reflecting layer at internal overall reflective interface is less, and the mirror-reflection probability of light is few, and anaclasis is poor with reflection uniformity, causes the pearlescent pigment purity difference being commonly coated with;The present invention increases low-refraction oxide skin(coating) between high refractor oxide skin(coating), promote the fineness of each refracting layer, increase the effect of mirror-reflection, by multilayer coating structure silica or aluminum oxide, different material interface is increased, and light is easily linearly propagated in same medium, when running into the interface of different material when, then can be refracted away by a part of light, another part is reflected;The present invention, according to this principle cladding two-layer silica or aluminum oxide, strengthens the reflectivity of light;The surface smoothness made by interpolation silica or aluminum oxide is increased, and the mirror-reflection probability of light increases, and promotes pigment colour purity.
Specific embodiments described herein, is only to present invention spirit explanation for example.

Claims (7)

1. a high-purity interferes green effect pearlescent pigment, it is characterized in that: described pearlescent pigment includes natural mica substrate, mica substrate surface is coated with the first high refractive index oxide layer, the second high refractive index oxide layer, the first low-refraction oxide skin(coating), the 3rd high refractive index oxide layer and the second low-refraction oxide skin(coating) successively.
A kind of high-purity the most according to claim 1 interferes green effect pearlescent pigment, it is characterised in that: described first high refractive index oxide layer is tin oxide.
A kind of high-purity the most according to claim 1 interferes green effect pearlescent pigment, it is characterised in that: second, third high refractive index oxide layer described is titanium oxide.
A kind of high-purity the most according to claim 1 interferes green effect pearlescent pigment, it is characterised in that: described first low, the second low-refraction oxide skin(coating) be silica, aluminum oxide one or both.
A kind of high-purity the most according to claim 1 interferes green effect pearlescent pigment, it is characterized in that: described substrate thickness is 50 ~ 300 nanometers, first high refractive index oxide layer thickness is 1 ~ 4 nanometer, second high refractive index oxide layer thickness is 400 ~ 600 nanometers, first, second low-refraction oxide layer thicknesses is 0.6 ~ 2.5 nanometer, the 3rd high refractive index oxide layer thickness 200 ~ 400 nanometer.
A kind of high-purity the most according to claim 1 interferes green effect pearlescent pigment, it is characterised in that: described first, second, third high refractive index oxide refractive index is more than 2.6.
A kind of high-purity the most according to claim 1 interferes green effect pearlescent pigment, it is characterised in that: the preparation method of described pearlescent pigment, comprise the following steps:
[1] in glass beaker, add water, throw 10 ~ 60 microns of mica substrates, open stirring 200 ~ 300 revs/min, heat up 70 ~ 75 DEG C, add hydrochloric acid or aqueous solution of nitric acid adjusts pH1.1 ~ 1.3, adjust and finish, stir 10 ~ 30 minutes;
[2] under constant temperature, stirring, butter of tin or the stannous chloride aqueous solution are dripped, and drip hydro-oxidation sodium water solution, maintain pH constant, charging is finished, and stirs 10 ~ 20 minutes;
[3] improving rotating speed 280 ~ 360 revs/min, intensification is 75 ~ 80 DEG C, promotes pH1.8 ~ 2.0 with sodium hydrate aqueous solution, and drip adds titanium tetrachloride, sodium hydrate aqueous solution, maintaining pH value constant, speed of agitator rises with liquid level and promotes rotating speed accordingly, charging is finished, and stirs 10 ~ 20 minutes;
[4] raising rotating speed is to 360 ~ 400 revs/min, and intensification is 82 ~ 85 DEG C, and single current adds sodium hydrate aqueous solution, promotes pH value 9.3 ~ 9.5, finishes, stirs 5 ~ 20 minutes;
[5] constant temperature stirring, and drip adds sodium silicate aqueous solution, by nitric acid or aqueous hydrochloric acid solution constant pH 9.3 ~ 9.5, charging is finished, is stirred 5 ~ 20 minutes;
[6] reducing reaction temperature is 75 ~ 80 DEG C, and adjustment of rotational speed is 280 ~ 360 revs/min, adds with nitric acid or aqueous hydrochloric acid solution single current, adjusts pH1.8 ~ 2.0, finishes, stir 5 ~ 20 minutes;
[7] constant temperature stirring, and drip adds titanium tetrachloride, sodium hydrate aqueous solution, maintains temperature, pH value constant, speed of agitator rises with liquid level and promotes rotating speed accordingly, and charging is finished, and stirs 5 ~ 20 minutes;
[8] constant temperature stirring, single current dropping sodium silicate aqueous solution, charging is finished, is stirred 5 ~ 20 minutes;
[9] after reaction terminates, by material vacuum filtration in beaker, adding deionized water washing is neutrality to washings pH value;
[10] by 105 ~ 120 DEG C of forced air dryings of material 1 ~ 3 hour, calcine 10 ~ 25 minutes for 700 ~ 720 DEG C, obtain high-purity and interfere green effect pearlescent pigment.
CN201610314477.6A 2016-05-13 2016-05-13 High-purity interference green effect pearlescent pigment and preparation method thereof Pending CN105907130A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201610314477.6A CN105907130A (en) 2016-05-13 2016-05-13 High-purity interference green effect pearlescent pigment and preparation method thereof

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201610314477.6A CN105907130A (en) 2016-05-13 2016-05-13 High-purity interference green effect pearlescent pigment and preparation method thereof

Publications (1)

Publication Number Publication Date
CN105907130A true CN105907130A (en) 2016-08-31

Family

ID=56748844

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201610314477.6A Pending CN105907130A (en) 2016-05-13 2016-05-13 High-purity interference green effect pearlescent pigment and preparation method thereof

Country Status (1)

Country Link
CN (1) CN105907130A (en)

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108997792A (en) * 2018-07-18 2018-12-14 黄山幻彩颜料科技有限公司 A kind of preparation method of artificial synthesized bloom iris pearlescent pigment
CN112226100A (en) * 2020-11-12 2021-01-15 江苏贝丽得新材料有限公司 Method for enhancing whiteness of white pearlescent pigment

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1270615A (en) * 1997-10-17 2000-10-18 默克专利股份有限公司 Interference pigments
CN101235227A (en) * 2008-03-13 2008-08-06 北京首创纳米科技有限公司 Method for preparing mica titanium nacreous material
CN101343424A (en) * 2008-08-26 2009-01-14 攀钢集团研究院有限公司 Pearlescent pigment and preparation thereof
CN103788719A (en) * 2014-01-18 2014-05-14 南京理工大学 Preparation method of single-coating cobalt chromite green coating mica pearlescent compound pigment
CN103834196A (en) * 2014-03-31 2014-06-04 福建师范大学 Method for preparing mica titanium pearlescent pigment with carbonate as neutralizing solution

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1270615A (en) * 1997-10-17 2000-10-18 默克专利股份有限公司 Interference pigments
CN101235227A (en) * 2008-03-13 2008-08-06 北京首创纳米科技有限公司 Method for preparing mica titanium nacreous material
CN101343424A (en) * 2008-08-26 2009-01-14 攀钢集团研究院有限公司 Pearlescent pigment and preparation thereof
CN103788719A (en) * 2014-01-18 2014-05-14 南京理工大学 Preparation method of single-coating cobalt chromite green coating mica pearlescent compound pigment
CN103834196A (en) * 2014-03-31 2014-06-04 福建师范大学 Method for preparing mica titanium pearlescent pigment with carbonate as neutralizing solution

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108997792A (en) * 2018-07-18 2018-12-14 黄山幻彩颜料科技有限公司 A kind of preparation method of artificial synthesized bloom iris pearlescent pigment
CN112226100A (en) * 2020-11-12 2021-01-15 江苏贝丽得新材料有限公司 Method for enhancing whiteness of white pearlescent pigment

Similar Documents

Publication Publication Date Title
CN101870842B (en) Aqueous cold pigment double-coat multifunctional thermal-insulation external wall paint and preparation method thereof
US3978272A (en) Coated article for solar control and process for its production
CN101891395B (en) Method for preparing thermal-insulation, self-cleaning and film-coated toughened glass
US6936348B1 (en) Method for deposition of rutile-type titanium dioxide, and substrate and glass flakes having the oxide attached thereto
US20090090275A1 (en) Pigment having angle dependence of the interference colors and the production processes thereof
CN103539365B (en) A kind of reflective solar controls low radiation coated glass and preparation method thereof
CN107325589A (en) A kind of glittering Gold production effect pearlescent pigment of high-purity titanium ferroalloy and preparation method thereof
CN101434759B (en) Preparation of high glaze glass-based pearlescent pigment
CN102951849B (en) A kind of colorful glass microbead and preparation method thereof of interfering
CN102260421A (en) Magic-color nacreous aluminum powder pigment and preparation method thereof
CN102765231A (en) Thermochromic substrate and pair-glass with thermochromic thin film
CN105859153A (en) Antifogging antireflection visible-light double-function coated glass and preparation method thereof
CN111171602B (en) Preparation method of pearlescent pigment
CN102127321A (en) Method for preparing gold pearlescent pigment with high hue and high brightness
Pi et al. Superhydrophobic and thermochromic VO2-Based composite coatings for energy-saving smart windows
Kursawe et al. Nano-particles by wet chemical processing in commercial applications
CN105907130A (en) High-purity interference green effect pearlescent pigment and preparation method thereof
US3440075A (en) Golden flake pigments coated with silver and hydrous oxides
CN205787185U (en) A kind of LCDs two-in-one plated film of anti-dazzle antireflective
CN104071988A (en) Preparation method of wear-resistant long-acting self-cleaning anti-reflecting coating, and wear-resistant long-acting self-cleaning anti-reflecting coating
CN110408239B (en) High rutile type titanium dioxide hollow glass bead, preparation method thereof and heat insulation filler
CN108084743A (en) Rutile-type high color saturation interference colours pearlescent pigment and preparation method thereof
CN111995884A (en) Production process of color-changing pearlescent pigment
CN2712932Y (en) Strongly flaring coloring materials
TWI784312B (en) Broadband splitter with photocatalytic coating and fabrication method thereof

Legal Events

Date Code Title Description
C06 Publication
PB01 Publication
C10 Entry into substantive examination
SE01 Entry into force of request for substantive examination
WD01 Invention patent application deemed withdrawn after publication
WD01 Invention patent application deemed withdrawn after publication

Application publication date: 20160831