CN107858014A - A kind of organic middle yellow preparation method with core shell structure - Google Patents
A kind of organic middle yellow preparation method with core shell structure Download PDFInfo
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- CN107858014A CN107858014A CN201710930228.4A CN201710930228A CN107858014A CN 107858014 A CN107858014 A CN 107858014A CN 201710930228 A CN201710930228 A CN 201710930228A CN 107858014 A CN107858014 A CN 107858014A
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- water
- huang
- pah
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09B—ORGANIC DYES OR CLOSELY-RELATED COMPOUNDS FOR PRODUCING DYES, e.g. PIGMENTS; MORDANTS; LAKES
- C09B67/00—Influencing the physical, e.g. the dyeing or printing properties of dyestuffs without chemical reactions, e.g. by treating with solvents grinding or grinding assistants, coating of pigments or dyes; Process features in the making of dyestuff preparations; Dyestuff preparations of a special physical nature, e.g. tablets, films
- C09B67/0001—Post-treatment of organic pigments or dyes
- C09B67/0004—Coated particulate pigments or dyes
- C09B67/0007—Coated particulate pigments or dyes with inorganic coatings
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09B—ORGANIC DYES OR CLOSELY-RELATED COMPOUNDS FOR PRODUCING DYES, e.g. PIGMENTS; MORDANTS; LAKES
- C09B67/00—Influencing the physical, e.g. the dyeing or printing properties of dyestuffs without chemical reactions, e.g. by treating with solvents grinding or grinding assistants, coating of pigments or dyes; Process features in the making of dyestuff preparations; Dyestuff preparations of a special physical nature, e.g. tablets, films
- C09B67/0001—Post-treatment of organic pigments or dyes
- C09B67/0002—Grinding; Milling with solid grinding or milling assistants
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- Chemical Kinetics & Catalysis (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Pigments, Carbon Blacks, Or Wood Stains (AREA)
Abstract
The present invention provides a kind of organic middle yellow preparation method with core shell structure, first in organic middle yellow adsorption multi-layer polyelectrolyte, then uses sol-gal process in organic middle yellow one layer of SiO of Surface coating2；On this basis, one layer of 5 ~ 20nm SiO is adsorbed again2Nano-particle, it is prepared with two layers of SiO2Cladding has machine yellow pigment particle.The present invention is using the method coated twice, the SiO of preparation2Shell layer surface is coarse so that product is greatly improved to the wetability of water, so as to improve organic middle yellow dispersibility in water.
Description
Technical field
The present invention relates to a kind of organic middle yellow preparation method with core shell structure, belong to organic pigment field.
Background technology
Organic middle Huang is a kind of excellent environment-friendly type organic pigment.Its color is close to medium chrome yellow, strong coloring force, alkali resistance
Well, it is not leaded, it is nontoxic, it is widely used in coating, ink and school supply and stationery.But its solvent resistant and heat resistance are poor.With
Enhancing of the people to environmental consciousness, it is solvent instead of organic matter, it is scattered a series of water-based inks, water paint etc. occur using water
The novel product of phase.Organic middle Huang poor dispersion in aqueous phase, easily reunites, therefore people have been look for various methods to change
It is apt to its dispersibility in water, wherein surface modification treatment is a kind of important means.
The composite of core shell structure, it can be asked and be designed according to our needs according to the heterogeneity of core, shell, closely
Have become study hotspot over year.Using the general principle of nucleocapsid structure, cladding processing is carried out to organic middle Huang, can be improved
Organic middle yellow solvent resistant, heat resistance, it can also select to have the shell material of hydrophilicity to improve organic middle yellow pigment pair
The wettability of water, so as to improve dispersibility of the pigment in aqueous phase.
The content of the invention
Present invention offer is a kind of to have machine Huang preparation method with core shell structure, with organic middle Huang for core, passes through silicic acid
Tetra-ethyl ester（TEOS）Hydrolysis, SiO2Cladding is handled twice for nano-particle absorption, and it is coarse to prepare layer of surface on pigment particles surface
SiO2Shell, to improve organic middle yellow dispersive property in water.
To reach above technique effect, the present invention includes following technical step：
Step 1：The preparation of dispersible pigment color paste, weigh a certain amount of kayexalate powder（PSS）It is added in deionized water
Make its dissolving, then add organic middle bloom end, stirring powder fully soaks, is put into zirconium oxide steel ball, ground in grinder
Finely dispersed organic middle yellow pigment particle mill base is prepared；
Step 2：Pigment particles are surface-treated, and above-mentioned dispersible pigment color paste is centrifuged, and deionized water is washed three times, then redisperse
Into deionized water, now pigment particles surface is negatively charged.By PAH（PAH）Solution adds pigment particles
In dispersion liquid, ultrasonic disperse 30min, centrifuge, deionized water is washed three times, and now pigment particles surface is positively charged；Weight
Multiple above-mentioned steps, are prepared surface alternating sorbent multilayer PSS-PAH polyelectrolyte, and the pigment particles of surface positively charged；
Step 3：Pigment particles are once coated, and the granules of pigments of surface positively charged is distributed in ethanol solution, are added appropriate
Water, ammoniacal liquor regulation solution pH value 9 ~ 10 is gradually added under stirring condition, was then added dropwise to tetraethyl orthosilicate in 1 hour（TEOS）
With the mixed solution of ethanol；Then, continue at room temperature stirring 24 hours, be washed with water centrifugation three times, obtain once coat it is organic
Pigment particles；
Step 4：The secondary cladding of pigment particles, an above-mentioned coated pigment particle is dispersed in water, adds polyallyl ammonium salt
Hydrochlorate（PAH）, ultrasonic disperse 30min, subsequent water washing centrifuges 3 times；The pigment particles after centrifuging will be washed, are dispersed in water,
Particle diameter 5 ~ 20nm nano silicon dioxide sols are then added, stirring and adsorbing 60min, centrifugation is washed with water three times, obtains secondary bag
The pigment particles covered, be after drying product there is core shell structure have machine yellow.
Further, in the step 1, organic middle Huang, PAH, the rate of charge of water are mOrganic middle Huang：mPSS：mWater =0.5~1:0.5
~1:100。
Further, in the step 2, organic middle Huang, PAH, PSS, the rate of charge of water are mOrganic middle Huang：mPAH：mPSS：mWater=
0.5~1:0.5~1: 0.5~1:100, the absorption number of plies of surface treatment PSS-PAH polyelectrolyte is 3 ~ 6 layers.Because granules of pigments
Surface is typically inert, obtains that adsorption capacity is weaker to polyelectrolyte, and the adsorbance of individual layer is few, is unfavorable at follow-up cladding
Reason.
Further, in the step 3, organic middle Huang, absolute ethyl alcohol, the rate of charge of water are mOrganic middle Huang：mAbsolute ethyl alcohol：mWater：
mTEOS ethanol solutions=0.5:200:20~30:40, TOSE ethanol solution mass concentration is 2% ~ 5%., can be with preparation process
By changing the quality control TEOS hydrolysis rates of system reclaimed water, change TEOS solution concentrations regulation SiO2The thickness of cladding.
Further, in the step 4, organic middle Huang, water, PAH, the rate of charge of nano silicon dioxide sol are mOrganic middle Huang：
mWater：mPAH：mSiO2=1:100:1:1~2。
Further, the second layer cladding described in step 4, on the one hand can increase and be coated on organic middle yellow pigment particle
Surface SiO2Thickness, so as to increase the stability of shell；Another aspect 20nm SiO2Particle absorption time water when first coats
Solve the SiO prepared2Film surface, surface SiO can be improved2Roughness, further improve the organic middle yellow water profit of core shell structure
Wet performance.
Based on described above, the present invention provide it is a kind of have machine Huang preparation method with core shell structure, first organic
Middle yellow adsorption multi-layer polyelectrolyte, then using sol-gel process in organic middle yellow one layer of SiO of Surface coating2；In this base
On plinth, one layer of 5 ~ 20nm SiO is adsorbed again2Nano-particle, it is prepared with two layers of SiO2Cladding has machine yellow pigment grain
Son.Due to using the SiO for coating preparation twice2Shell layer surface is coarse so that and product is greatly improved to the wetability of water, from
And improve organic middle yellow dispersibility in water.
Embodiment
The present invention is described in detail with reference to embodiment.
Embodiment 1
It is a kind of to there is machine Huang preparation method to comprise the following steps with core shell structure：
Step 1：The preparation of dispersible pigment color paste, weigh 0.5g kayexalate powder（PSS）It is added in 100g ionized waters
Make its dissolving, then add the organic middle bloom ends of 0.5g, stirring powder fully soaks, and zirconium oxide steel ball is put into, in grinder
Finely dispersed organic middle yellow uitramarine mill base is prepared in grinding；
Step 2：Pigment particles are surface-treated, and above-mentioned dispersible pigment color paste is centrifuged, and deionized water is washed three times, then redisperse
To going in 100g ionized waters, now pigment particles surface is negatively charged.By 0.5g PAHs（PAH）Solution adds
In pigment particle dispersion, ultrasonic disperse 30min, centrifuge, deionized water is washed three times, and now pigment particles surface band is being just
Electric charge.Repeat the above steps, 3 layers of PSS-PAH polyelectrolyte of surface alternating sorbent, and the pigment grain of surface positively charged is prepared
Son；
Step 3：Pigment particles are once coated, and pigment yellow particle is distributed in 100g ethanol solutions in step 2, are added appropriate
10g water, ammoniacal liquor regulation solution pH value 9 ~ 10 is gradually added under stirring condition, 20g mass fractions were then added dropwise in 1 hour
2.5% tetraethyl orthosilicate（TEOS）Ethanol solution；Then, continue stirring 24 hours at room temperature, centrifugation be washed with water three times,
Obtain a clad organic pigment particle；
Step 4：The secondary cladding of pigment particles, an above-mentioned coated pigment particle is dispersed in water, adds 0.5g polyallyls
Ammonium salt hydrochlorate（PAH）Solution, ultrasonic disperse 30min, centrifugation is then washed with water three times；By the pigment particles after centrifuge washing, divide
It is scattered in 50g water, then adds mass fraction 20%, particle diameter 20nm silicon dioxide gel 2.5g, magnetic agitation adsorbs 60min,
Centrifugation is washed with water three times, obtains the pigment particles of secondary cladding, be after drying product there is core shell structure have machine yellow.
Embodiment 2
It is a kind of to there is machine Huang preparation method to comprise the following steps with core shell structure：
Step 1：The preparation of dispersible pigment color paste, weigh 0.5g kayexalate powder（PSS）It is added in 100g ionized waters
Make its dissolving, then add the organic middle bloom ends of 0.5g, stirring powder fully soaks, and zirconium oxide steel ball is put into, in grinder
Finely dispersed organic middle yellow pigment mill base is prepared in grinding；
Step 2：Pigment particles are surface-treated, and above-mentioned dispersible pigment color paste is centrifuged, and deionized water is washed three times, then redisperse
To going in 100g ionized waters, now pigment particles surface is negatively charged；By 0.5g PAHs（PAH）Solution adds
In pigment particle dispersion, ultrasonic disperse 30min, centrifuge, deionized water is washed three times, and now pigment particles surface band is being just
Electric charge；Repeat the above steps, 3 layers of PSS-PAH polyelectrolyte of surface alternating sorbent, and the pigment grain of surface positively charged is prepared
Son；
Step 3：Pigment particles are once coated, and pigment yellow particle is distributed in 100g ethanol solutions in step 2, are added appropriate
10g water, ammoniacal liquor regulation solution pH value 9 ~ 10 is gradually added under stirring condition, 20g mass fractions were then added dropwise in 1 hour
2.5% tetraethyl orthosilicate（TEOS）Ethanol solution；Then, continue stirring 24 hours at room temperature, centrifugation be washed with water three times,
Obtain a clad organic pigment particle；
Step 4：The secondary cladding of pigment particles, an above-mentioned coated pigment particle is dispersed in water, adds 0.5g polyallyls
Ammonium salt hydrochlorate（PAH）Solution, ultrasonic disperse 30min, centrifugation 3 times is then washed with water；By the pigment particles after centrifuge washing, disperse
Into 50g water, mass fraction 20%, 5 ~ 7nm of particle diameter silicon dioxide gel 2.5g are then added, magnetic agitation adsorbs 60min,
Centrifugation is washed with water three times, obtains the pigment particles of secondary cladding, be after drying product there is core shell structure have machine yellow.
There is machine yellow with after the sample prepared in embodiment drying by what is do not processed, be pressed into disk with tablet press machine and then survey
Amount enters the contact angle test of water-filling respectively, as a result as shown in the table：
| Sample | Untreated organic middle Huang | Embodiment 1 | Embodiment 2 |
| Contact angle | 108.9° | 13.2° | 5.1° |
As shown by data in table, the sample prepared in embodiment decline to a great extent to the contact angle of water, illustrate organic middle Huang by titanium dioxide
Silicon well get up by cladding so that organic middle yellow wettability can improve.Wherein, the contact angle of the sample of embodiment 2 is less than real
Example 1 is applied, colloidal sol SiO when being because of the secondary cladding used in embodiment 22Particle diameter it is smaller, the sample shell of preparation is more coarse,
So more preferable to the wettability of water.Therefore, organic middle Huang with core shell structure that prepared by embodiment can preferably disperse
In water.
In above-described embodiment, the present invention is described in detail, but the invention is not restricted to the content in embodiment.It is right
In industry personnel, in the case of the basic thought of the present invention is not departed from, any change done to technical solution of the present invention is all
In claims of the present invention limited range.
Claims (5)
1. a kind of have machine Huang preparation method with core shell structure, it is characterised in that the preparation method comprises the following steps：
Step 1：The preparation of dispersible pigment color paste, weigh a certain amount of kayexalate powder (PSS) and be added in deionized water
Make its dissolving, then add organic middle bloom end, stirring powder fully soaks, is put into zirconium oxide steel ball, ground in grinder
Finely dispersed organic middle yellow pulp is prepared；
Step 2：Pigment particles are surface-treated, and above-mentioned dispersible pigment color paste is centrifuged, and deionized water is washed three times, Ran Houzai
It is distributed in deionized water, PAH (PAH) solution is added in organic pigment dispersion liquid, ultrasonic disperse
30min, centrifuge, deionized water is washed three times；Repeat the above steps, surface alternating sorbent multilayer PSS-PAH is prepared
Polyelectrolyte, and the pigment particles of surface positively charged；
Step 3：Pigment particles are once coated, and the granules of pigments of surface positively charged is distributed in ethanol solution, are added appropriate
Water, ammoniacal liquor regulation solution pH value 9~10 is gradually added under stirring condition, was then added dropwise to tetraethyl orthosilicate in 1 hour
(TEOS) and ethanol mixed solution.Then, continue stirring 24 hours at room temperature, centrifugation is washed with water three times, obtains and once wraps
Cover organic pigment particles；
Step 4：The secondary cladding of pigment particles, an above-mentioned coated pigment particle is dispersed in water, adds polyallyl ammonium salt
Hydrochlorate (PAH), ultrasonic disperse 30min, subsequent water washing centrifugation is three times；The pigment particles after centrifuging will be washed, are dispersed in water,
Particle diameter 5~20nm nano silicon dioxide sols are then added, stirring and adsorbing 60min, centrifugation is washed with water three times, obtains secondary bag
The pigment particles covered, be after drying product there is core shell structure have machine yellow.
A kind of there is a machine Huang preparation method with core shell structure 2. according to claim 1, it is characterised in that：The step
Organic middle Huang, PAH, the rate of charge of water are m in rapid 1Organic middle Huang：mPSS：mWater=0.5~1:0.5~1:100.
A kind of there is a machine Huang preparation method with core shell structure 3. according to claim 1, it is characterised in that：The step
In rapid 2, organic middle Huang, PAH, PSS, the rate of charge of water are mOrganic middle Huang：mPAH：mPSS：mWater=0.5~1:0.5~1:0.5~1:
100, the absorption number of plies of surface treatment PSS-PAH polyelectrolyte is 3~6 layers.
A kind of there is a machine Huang preparation method with core shell structure 4. according to claim 1, it is characterised in that：The step
Organic middle Huang, absolute ethyl alcohol, the rate of charge of water are m in rapid 3Organic middle Huang：mAbsolute ethyl alcohol：mWater：mTEOS ethanol solutions=0.5:200:20~30:
40, TOSE ethanol solution mass concentration is 2%~5%.
A kind of there is a machine Huang preparation method with core shell structure 5. according to claim 1, it is characterised in that：The step
Organic middle Huang, water, PAH, the rate of charge of nano silicon dioxide sol are m in rapid 4Organic middle Huang：mWater：mPAH：mSiO2=1:100:1:1
~2.
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| CN201710930228.4A CN107858014B (en) | 2017-10-09 | 2017-10-09 | Preparation method of organic mesochrome with core-shell structure |
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| CN201710930228.4A CN107858014B (en) | 2017-10-09 | 2017-10-09 | Preparation method of organic mesochrome with core-shell structure |
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| CN107858014A true CN107858014A (en) | 2018-03-30 |
| CN107858014B CN107858014B (en) | 2020-02-07 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108727869A (en) * | 2018-07-04 | 2018-11-02 | 南京林业大学 | Aqueous easy dispersion monoazo nanometer organic pigment of one kind and preparation method thereof |
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| US20150265508A1 (en) * | 2012-10-15 | 2015-09-24 | Ultra Ink, Llc | Removable Tattoo Ink and the Use Thereof |
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| US20090263660A1 (en) * | 2005-07-13 | 2009-10-22 | Miyoshi Kasei, Inc. | Surface-treated powder and cosmetics containing same |
| CN102015925A (en) * | 2008-03-07 | 2011-04-13 | 施乐公司 | Encapsulated nanoscale particles of organic pigments |
| US20150265508A1 (en) * | 2012-10-15 | 2015-09-24 | Ultra Ink, Llc | Removable Tattoo Ink and the Use Thereof |
| CN106349750A (en) * | 2016-08-24 | 2017-01-25 | 浙江理工大学 | Reaction type organic pigment compound particles for blue-ray curing digital printing and preparation method thereof |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108727869A (en) * | 2018-07-04 | 2018-11-02 | 南京林业大学 | Aqueous easy dispersion monoazo nanometer organic pigment of one kind and preparation method thereof |
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