CN101074329A - Pigment surface modification and production of dispersed pigment - Google Patents
Pigment surface modification and production of dispersed pigment Download PDFInfo
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- CN101074329A CN101074329A CN 200710042821 CN200710042821A CN101074329A CN 101074329 A CN101074329 A CN 101074329A CN 200710042821 CN200710042821 CN 200710042821 CN 200710042821 A CN200710042821 A CN 200710042821A CN 101074329 A CN101074329 A CN 101074329A
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- pigment
- surface modification
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- easily dispersible
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Abstract
Production of pigment surface modification and dispersing pigment is carried out by putting pigment dry powders into plasma vacuum chamber, supplying vacuum, inducing into air, re-supplying vacuum while inducing into air to needed reactive pressure, cryogenic plasma glow discharging or corona discharge treating, dispersing treated pigment into polar resin or solvent or adding residual ammonia or organic ammonia into pigment color paste as dispersing stabilized accessory. It has better dispersion.
Description
Technical field
The invention belongs to the pigment prepared field, particularly relate to a kind of surface modification of pigment and the preparation method of easily dispersible pigment.
Background technology
Pigment is applied in the media such as coating, Yin Mo, plastics, rubber and fiber with insoluble minuteness particle, and most of pigment to be nanometer arrive micron-sized particle, surface energy is very big, so their are difficult to be dispersed in uniformly in resin or the solvent.Introduce polar group for the surface at pigment, traditional way is with wet processing methods pigment to be carried out surface modification.But this procedure complexity can produce a certain amount of pollutent, and is bigger to the influence of environment.And Cement Composite Treated by Plasma is a dry process, and energy-saving and water-saving can not pollute environment.
The generation of plasma body has dual mode: apply significant high temperature or apply energy by accelerated electron, speeding-up ion etc. to material to material, the neutral material will be dissociated into electronics, ion and free radical.Constantly apply energy from the outside, material is dissociated into the charged ionic state of yin, yang and is called plasma body, and it is that electric charge is neutral gas.Be called high-temperature plasma by the mode that applies high temperature acquisition plasma body, modes that other forms by non high temperature obtain plasma body are called low-temperature plasma.
Comprise electronics, ion, ground state atom or molecule in the plasma body, intensify molecule or multiple particle such as atom and free radical, so it is a kind of chemically reactive special gas that has.The gas that is in plasmoid can be followed surface of pigments generation chemical reaction, introduces carboxyl, hydroxyl, carbonyl, ester group isopolarity group on the surface of pigment, thereby pigment is disperseed in resin and solvent easily.
United States Patent (USP) 4,478,643 disclose a kind of method with Low Temperature Plasma Treating pigment prepared additives of pigments, add to as additive in the pigment dispersion system that contains polar resin or solvent by the pigment with Cement Composite Treated by Plasma, can effectively improve dispersing of pigments.
T.Takada etc. [" surface modification and characterization of carbon black with oxygenplasma ", Carbon Vol.34, No.9, pp 1087-1091,1996] by the oxygen plasma treatment carbon black, carbonyl, carboxyl and ester group isopolarity group have been introduced in the XPS analysis discovery on the sooty surface.
Gao Yueying etc. [" plasma modification is to the influence of CuPc dispersion stabilization in water ", applied chemistry, 2000,17,615-619] changed the surface properties of CuPc pigment by the methyl acrylate plasma modification, increased the dispersion stabilization of CuPc in water.But methyl acrylate is to add behind plasma discharge in this article, and the CuPc pigment of article on plasma body after handling further handles employing is 2,2,2-trifluoroacetic anhydride and 2,2,2 tfifluoroethyl alcohol.
Li Yong [" research of plasma body carbon black graft polymerization ", coatings industry, 2000,6,3-5] causes vinyl monomer by the Cement Composite Treated by Plasma carbon black and carries out graft polymerization reaction, has increased the dispersion stabilization of carbon black in solvent.
But above-mentioned research and be untreated after the dispersiveness of pigment in solvent or resin study, do not mix yet and use with further raising pigment-dispersing with ammonia or organic amine.
Summary of the invention
The surface modifying method that the purpose of this invention is to provide a kind of pigment, be slightly acidic by the pigment of introducing groups such as carboxyl, carbonyl, can be dispersed in preferably in the resin or solvent of application system, mix in water with weakly alkaline amine again as this pigment, both connect with sat linkage, cause dispersing of pigments stability further to improve.
The surface modification of a kind of pigment of the present invention and the preparation method of easily dispersible pigment comprise the following steps:
(1) pigment dry powder is put into the plasma vacuum chamber, vacuumize the back and feed gas, repeat to vacuumize ventilation to required reaction pressure;
(2) pigment carries out low-temperature plasma glow discharge or Corona discharge Treatment;
(3) colo(u)rant dispersion after will handling is in polar resin or solvent;
(4) or further add little ammonia or organic amine in the dispersible pigment color paste as the stably dispersing auxiliary agent.
Described pigment is pigment dyestuff or mineral dye, mineral dye is a carbon black, pigment dyestuff is to be selected from containing metal or containing metal phthalocyanine pigment not, and azo pigment is beta naphthal class pigment, azoic coupling component AS class pigment, azo condensation pigment or benzimidazolone heterocycle azo pigment; Heterocycle and condensed ring ketone pigment are quinacridine ketone serial pigment, dioxazines pigment, 1,4-diketopyrrolo-pyrrole serial pigment; Condensed ring anthraquinone ketone pigment, perylene system or pyrene series pigments, chloro isoindolinone, isoindoline class pigment, quinophthalone class pigment or pyrazoloquinazolone class pigment;
Described gas is reactivity and/or non-reactive gas, is selected from one or more mixed gas of gases such as ammonia, carbonic acid gas, air, oxygen, hydrogen, nitrogen and argon gas;
The power supply of described generation plasma body is high frequency, microwave, interchange or direct supply;
Described plasma discharge is meant air pressure at 10～100Pa, and the power of plasma discharge is 1～1000W, 1～3600 second time of plasma discharge;
Described resin is selected from resol, aminoresin, isocyanate resin, acrylic resin, vibrin, Synolac, vinyl chloride-vinyl acetate resin, vinyl chloride-vinylidene chloride resin, Resins, epoxy, Vinylite or polyamide resin.
Described solvent is water or organic solvent, and organic solvent is to be selected from the solvent that contains hydroxyl, carboxyl, ester group, ketone group group;
Described ammonia stably dispersing auxiliary agent is ammonia (NH
3) or its aqueous solution;
Described organic amine stably dispersing auxiliary agent is meant the organic alcohol amine compound that contains at least one hydroxyl and at least one organic amine structure simultaneously, preferred alcohol amine, diethanolamine or trolamine, 2-amido-2-methyl isophthalic acid-propyl alcohol or N-Propylamino-methyl-thanomin etc.; Or polyetheramine (CH
3[OCH
2CH
2]
x-[OCH
2CH (CH
3)]
yNH
2, wherein x is 0～10000, y is 0～10000).
Beneficial effect of the present invention:
(1) pigment has good dispersiveness in polar resin or solvent after Low Temperature Plasma Treating;
(2) in this dispersing of pigments system, add little ammonia or organic amine, can further improve its dispersion stabilization in dispersion system.
Embodiment
Below in conjunction with specific embodiment, further set forth the present invention.Should be understood that these embodiment only to be used to the present invention is described and be not used in and limit the scope of the invention.Should be understood that in addition those skilled in the art can make various changes or modifications the present invention after the content of having read the present invention's instruction, these equivalent form of values fall within the application's appended claims institute restricted portion equally.
Embodiment 1
The 1g carbon black is put into vacuum chamber at culture dish middle berth open form lamellar, and vacuum chamber is airtight, is evacuated to about 10Pa, behind oxygen gas washing 2 times, is evacuated to 20Pa, and discharge is 1 minute under 30W power, takes out sample.Add distilled water 100mL in the sample, carry out following operation respectively:
(1) 30min that under the 1800r/min condition, pulls an oar, or
(2) add the 4g polyetheramine, the 30min that under the condition of 1800r/min, pulls an oar, afterwards, centrifugal 30min under the 2500r/min condition gets supernatant liquor and survey transmitance on spectrophotometer, uses following formulate dispersing of pigments:
Dispersed %=1-transmitance %
Its dispersion stabilization sees the following form 1.
Take by weighing the carbon black of 1g without Cement Composite Treated by Plasma, be the contrast experiment as stated above, its dispersion stabilization sees the following form 1.
Table 1 dispersity of carbon black
| Condition | Dispersed % |
| Carbon black without oxygen plasma treatment | 0 |
| The carbon black of oxygen plasma treatment | 75 |
| The carbon black of oxygen plasma treatment mixes with amine | 96 |
Embodiment 2
1g quinacridone PR122 puts into vacuum chamber at culture dish middle berth open form lamellar, with the vacuum chamber sealing, is evacuated to about 10Pa, behind oxygen gas washing 2 times, is evacuated to 40Pa, and discharge is 20 minutes under 100W power, takes out sample.Add distilled water 100mL in the sample, carry out following operation respectively:
(1) 30min that under the 1800r/min condition, pulls an oar, or
(2) add the 4g polyetheramine, the 30min that under the condition of 1800r/min, pulls an oar, afterwards, centrifugal 30min under the 2500r/min condition gets supernatant liquor and survey transmitance on spectrophotometer, uses following formulate dispersing of pigments:
Dispersed %=1-transmitance %
Its dispersion stabilization sees the following form 2.
Take by weighing the quinacridone PR122 of 1g without Cement Composite Treated by Plasma, be the contrast experiment as stated above, its dispersion stabilization sees the following form 2.
The dispersiveness of table 2 quinacridone PR122
| Condition | Dispersed % |
| Quinacridone PR122 without oxygen plasma treatment | 47 |
| The quinacridone PR122 of oxygen plasma treatment | 65 |
| The quinacridone PR122 of oxygen plasma treatment mixes with amine | 97 |
Embodiment 3
1g Pigment Yellow 73 PY83 puts into vacuum chamber at culture dish middle berth open form lamellar, with the vacuum chamber sealing, is evacuated to about 10Pa, behind oxygen gas washing 2 times, is evacuated to 50Pa, and discharge is 10 minutes under 150W power, takes out sample.Add distilled water 100ml in the sample, carry out following operation respectively:
(1) 30min that under the 1800r/min condition, pulls an oar, or
(2) add the 5g diethanolamine, the 30min that under the condition of 1800r/min, pulls an oar, afterwards, centrifugal 30min under the 2500r/min condition gets supernatant liquor and survey transmitance on spectrophotometer, uses following formulate dispersing of pigments:
Dispersed %=1-transmitance %
Its dispersion stabilization sees the following form 3.
Take by weighing the Pigment Yellow 73 PY83 of 1g without Cement Composite Treated by Plasma, be the contrast experiment as stated above, its dispersion stabilization sees the following form 3
The dispersiveness of table 3 Pigment Yellow 73 PY83
| Condition | Dispersed % |
| Pigment Yellow 73 PY83 without oxygen plasma treatment | 35 |
| The Pigment Yellow 73 PY83 of oxygen plasma treatment | 67 |
| The Pigment Yellow 73 PY83 of oxygen plasma treatment mixes with amine | 96 |
Embodiment 4
1g Pigment blue PB15:1 puts into vacuum chamber at culture dish middle berth open form lamellar, with the vacuum chamber sealing, is evacuated to about 10Pa, behind oxygen gas washing 2 times, is evacuated to 40Pa, and discharge is 20 minutes under 100W power, takes out sample.Add distilled water 100ml in the sample, carry out following operation respectively:
(1) 30min that under the 1800r/min condition, pulls an oar, or
(2) add the 3.8g thanomin, the 30min that under the condition of 1800r/min, pulls an oar, afterwards, centrifugal 30min under the 2500r/min condition gets supernatant liquor and survey transmitance on spectrophotometer, uses following formulate dispersing of pigments:
Dispersed %=1-transmitance %
Its dispersion stabilization sees the following form 4.
Take by weighing the Pigment blue PB15:1 of 1g without Cement Composite Treated by Plasma, be the contrast experiment as stated above, its dispersion stabilization sees the following form 4.
The dispersiveness of table 4 Pigment blue PB15:1
| Condition | Dispersed % |
| Pigment blue PB15:1 without oxygen plasma treatment | 43 |
| The Pigment blue PB15:1 of oxygen plasma treatment | 72 |
| The Pigment blue PB15:1 of oxygen plasma treatment mixes with amine | 98 |
Embodiment 5
0.1g carbon black is put into vacuum chamber at culture dish middle berth open form lamellar, with the vacuum chamber sealing, is evacuated to about 10Pa, behind oxygen gas washing 2 times, is evacuated to 40Pa, discharge is 10 minutes under 100W power, takes out sample.Add 2-Butoxyethyl acetate 40g in the sample, carry out following operation respectively:
(1) thermal agitation 5min, or
(2) add the 2g polyetheramine, vigorous stirring 1 hour afterwards, left standstill 5 hours, and 1cm gets 1ml in the place under liquid level, dilute 4 times after, on spectrophotometer, survey transmitance, use following formulate dispersing of pigments:
Dispersed %=1-transmitance %
Its dispersion stabilization sees the following form 5.
Take by weighing the carbon black of 0.1g without Cement Composite Treated by Plasma, be the contrast experiment as stated above, its dispersion stabilization sees the following form 5.
Table 5 dispersity of carbon black
| Condition | Dispersed % |
| Carbon black without oxygen plasma treatment | 32 |
| The carbon black of oxygen plasma treatment | 49 |
| The carbon black of oxygen plasma treatment mixes with amine | 91 |
Claims (11)
1. the preparation method of the surface modification of a pigment and easily dispersible pigment comprises the following steps:
(1) pigment dry powder is put into the plasma vacuum chamber, vacuumize the back and feed gas, repeat to vacuumize ventilation to required reaction pressure;
(2) pigment carries out low-temperature plasma glow discharge or Corona discharge Treatment;
(3) colo(u)rant dispersion after will handling is in polar resin or solvent;
(4) or further add little ammonia or organic amine in the dispersible pigment color paste as the stably dispersing auxiliary agent.
2. the preparation method of the surface modification of a kind of pigment according to claim 1 and easily dispersible pigment, it is characterized in that: described pigment is pigment dyestuff or mineral dye, mineral dye is a carbon black, pigment dyestuff is selected from containing metal or containing metal phthalocyanine pigment not, and azo pigment is beta naphthal class pigment, azoic coupling component AS class pigment, azo condensation pigment or benzimidazolone heterocycle azo pigment; Heterocycle and condensed ring ketone pigment are quinacridine ketone serial pigment, dioxazines pigment, 1,4-diketopyrrolo-pyrrole serial pigment; Condensed ring anthraquinone ketone pigment, perylene system or pyrene series pigments, chloro isoindolinone, isoindoline class pigment, quinophthalone class pigment or pyrazoloquinazolone class pigment.
3. the preparation method of the surface modification of a kind of pigment according to claim 1 and easily dispersible pigment, it is characterized in that: described gas is reactivity and/or non-reactive gas, is selected from one or more mixed gas of gases such as ammonia, carbonic acid gas, air, oxygen, hydrogen, nitrogen and argon gas.
4. the preparation method of the surface modification of a kind of pigment according to claim 1 and easily dispersible pigment, it is characterized in that: the power supply of described generation plasma body is high frequency, microwave, interchange or direct supply.
5. the preparation method of the surface modification of a kind of pigment according to claim 1 and easily dispersible pigment, it is characterized in that: described plasma discharge is meant that air pressure is at 10 ~ 100Pa, the power of plasma discharge is 1 ~ 1000W, 1 ~ 3600 second time of plasma discharge.
6. the preparation method of the surface modification of a kind of pigment according to claim 1 and easily dispersible pigment is characterized in that: described resin is selected from a kind of in resol, aminoresin, isocyanate resin, acrylic resin, vibrin, Synolac, vinyl chloride-vinyl acetate resin, vinyl chloride-vinylidene chloride resin, Resins, epoxy, Vinylite or the polyamide resin.
7. the preparation method of the surface modification of a kind of pigment according to claim 1 and easily dispersible pigment, it is characterized in that: described solvent is water or organic solvent, organic solvent is selected from the solvent that contains hydroxyl, carboxyl, ester group, ketone group, ether group.
8. the preparation method of the surface modification of a kind of pigment according to claim 1 and easily dispersible pigment, it is characterized in that: described ammonia stably dispersing auxiliary agent is ammonia (NH
3) or its aqueous solution.
9. the preparation method of the surface modification of a kind of pigment according to claim 1 and easily dispersible pigment, it is characterized in that: described organic amine stably dispersing auxiliary agent is organic alcohol amine compounds or polyetheramine.
10. the preparation method of the surface modification of a kind of pigment according to claim 9 and easily dispersible pigment, it is characterized in that: described organic alcohol amine compounds is meant the organic compound that contains at least one hydroxyl and at least one organic amine structure simultaneously, wherein the amido structure comprises primary amine groups, secondary amine, tertiary amine groups and quaternary amine base, typical organic alcohol amine compound such as thanomin, diethanolamine or trolamine, 2-amido-2-methyl isophthalic acid-propyl alcohol, N-Propylamino-methyl-thanomin etc.
11. the surface modification of a kind of pigment according to claim 9 and the preparation method of easily dispersible pigment is characterized in that: the general structure of described polyetheramine is CH
3[OCH
2CH
2]
x-[OCH
2CH (CH
3)]
yNH
2, wherein x is 0～10000, y is 0～10000.
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|---|---|---|---|
| CN 200710042821 CN101074329A (en) | 2007-06-27 | 2007-06-27 | Pigment surface modification and production of dispersed pigment |
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|---|---|---|---|
| CN 200710042821 CN101074329A (en) | 2007-06-27 | 2007-06-27 | Pigment surface modification and production of dispersed pigment |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102791807A (en) * | 2010-02-03 | 2012-11-21 | 埃迪亚贝拉科技有限公司 | A process for the preparation of carbon black pellets |
| CN103963382A (en) * | 2014-04-23 | 2014-08-06 | 福建省晋江市夜光达反光材料有限公司 | PET light-reflecting sequin and manufacturing method thereof |
| CN108794970A (en) * | 2018-06-11 | 2018-11-13 | 安徽四季能源科技有限公司 | A kind of preparation method for the nano metal pigment master batch that coloring effect is good |
| CN110511592A (en) * | 2019-07-19 | 2019-11-29 | 杭州红妍颜料化工有限公司 | A kind of preparation method of pigment yellow 83 |
| CN113462188A (en) * | 2021-06-16 | 2021-10-01 | 潍坊泰兴生物化工有限责任公司 | Pigment yellow 138 easily dispersible in weak solvent and preparation method thereof |
| CN114539847A (en) * | 2020-11-25 | 2022-05-27 | 阪田油墨株式会社 | Pigment dispersion composition for black matrix, resist composition for black matrix, and black matrix |
| CN114800921A (en) * | 2022-04-29 | 2022-07-29 | 青岛科技大学 | Preparation method of carbon black/natural rubber composite material |
-
2007
- 2007-06-27 CN CN 200710042821 patent/CN101074329A/en active Pending
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102791807A (en) * | 2010-02-03 | 2012-11-21 | 埃迪亚贝拉科技有限公司 | A process for the preparation of carbon black pellets |
| CN102791807B (en) * | 2010-02-03 | 2015-06-10 | 埃迪亚贝拉科技有限公司 | A process for the preparation of carbon black pellets |
| CN103963382A (en) * | 2014-04-23 | 2014-08-06 | 福建省晋江市夜光达反光材料有限公司 | PET light-reflecting sequin and manufacturing method thereof |
| CN108794970A (en) * | 2018-06-11 | 2018-11-13 | 安徽四季能源科技有限公司 | A kind of preparation method for the nano metal pigment master batch that coloring effect is good |
| CN110511592A (en) * | 2019-07-19 | 2019-11-29 | 杭州红妍颜料化工有限公司 | A kind of preparation method of pigment yellow 83 |
| CN114539847A (en) * | 2020-11-25 | 2022-05-27 | 阪田油墨株式会社 | Pigment dispersion composition for black matrix, resist composition for black matrix, and black matrix |
| CN113462188A (en) * | 2021-06-16 | 2021-10-01 | 潍坊泰兴生物化工有限责任公司 | Pigment yellow 138 easily dispersible in weak solvent and preparation method thereof |
| CN113462188B (en) * | 2021-06-16 | 2023-12-01 | 潍坊泰兴生物化工有限责任公司 | Pigment yellow 138 easy to disperse in weak solvent and preparation method thereof |
| CN114800921A (en) * | 2022-04-29 | 2022-07-29 | 青岛科技大学 | Preparation method of carbon black/natural rubber composite material |
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