CN101864198A - Production process of novel phthalocyanine blue pigment - Google Patents
Production process of novel phthalocyanine blue pigment Download PDFInfo
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- CN101864198A CN101864198A CN201010197528A CN201010197528A CN101864198A CN 101864198 A CN101864198 A CN 101864198A CN 201010197528 A CN201010197528 A CN 201010197528A CN 201010197528 A CN201010197528 A CN 201010197528A CN 101864198 A CN101864198 A CN 101864198A
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- phthalocyanine blue
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- blue pigment
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Abstract
The invention discloses a production process of novel phthalocyanine blue pigment, which combines the methods of two kinds of pigmentation: combining an acid treatment method and a grinding method by different modes to prepare the phthalocyanine blue pigment. Duding the process of acid treatment of phthalocyanine blue, crystals are transformed into needed crystal forms such as an alpha form which is partial red through controlling proper conditions such as through adjusting the concentration of the acid, the temperature of the acid treatment, the temperature of precipitation, and the like; and the acid treatment can be carried out before the grinding or during the grinding. The novel phthalocyanine blue organic pigment component provided by the invention has bigger red light, excellent heat resistance and weather resistance fastness, and can be used in printing ink, painting and plastic coloring.
Description
Technical field
The present invention relates to a kind of production technique of blue pigment dyestuff, be specifically related to a kind of production technique of novel phthalocyanine blue pigment.
Background technology
The crude product phthalocyanine blue can be made into pigment with appropriate means, and the pigment call number is C.I.P.B.15, because its superior thermotolerance and fastness to weathering are applied in printing ink, coating and plastic cement.
Phthalocyanine blue has multiple crystal formation, is respectively α, β, γ etc., relative coloured light, wherein α and the inclined to one side ruddiness of γ type, the inclined to one side green glow of β type.β is for to stablize crystal formation, and other are metastable-state crystal.Be α and β type as what pigment used.
The general synthetic phthalocyanine blue that obtains is α, β type, needs to carry out pigmenting through a series of suitable methods.The method of general pigmenting has acidic treatment, polishing, solvent treatment method etc.The purpose of pigmenting, the one, change crystal formation to stable α type, also have in order to obtain the product of bigger ruddiness.The 2nd, the control particle is to active in solvent and particle shape.The 3rd, carry out surface treatment, improve the dispersiveness in the application-specific medium, and suitability.By above adjustment, obtain the high products of fastness ability such as coloured light is bright-coloured, tinting strength is high, good dispersity, and is weather-proof, heat-resisting.
Acid pasting is to utilize phthalocyanine blue can be dissolved in the character of the vitriol oil, with its dissolving, and then separates out crystallization, obtains the evenly pigment of tiny particle of α type.In order to control the reunion of particle, can carry out surface treatment, for example add rosined soap, tensio-active agent, pigment derivative processing etc.
Polishing can use ball mill, kneader etc., with the particle of strong shearing force and impact force agglomerated separately, no longer reunites in order to control particle simultaneously, and obtains the crystal formation that needs, needs to add auxiliary agents such as organic solvent, tensio-active agent.
Solvent treatment method mainly is to utilize pigment that this character of certain dissolving is arranged in solvent, and pigment dissolved is separated out again, makes fine crystallization that growing up to a certain degree be taken place, thereby has reduced reunion, and crystal formation changes simultaneously sometimes.
Summary of the invention
Goal of the invention: the production technique that the object of the present invention is to provide a kind of novel phthalocyanine blue pigment.
Another object of the present invention is to provide a kind of novel phthalocyanine blue pigment dyestuff constituent that makes by the production technique of novel phthalocyanine blue pigment and the coating that comprises described phthalocyanine blue pigment constituent.
The technical solution used in the present invention: a kind of production technique of novel phthalocyanine blue pigment: phthalocyanine blue is carried out acid treatment and milled processed, described acid treatment can be carried out before grinding, also can carry out in grinding, acid-treated temperature is 10-80 ℃, and the time is 2-30 hour; After the acid treatment, the sour molten mixture that obtains added in the entry stir, water temperature is 0-90 ℃, the quality of water be sour quality 3-20 doubly; By adjusting concentration, the acid-treated temperature of acid, the temperature of separating out etc., making crystalline transition is the crystal formation that the phthalocyanine blue pigment that needs uses.
As preferably, the acid that described acid treatment is used is sulfuric acid, phosphoric acid or chlorsulfonic acid, and acid-treated temperature is 40-60 ℃.
As preferably, the acid that described acid treatment is used is sulfuric acid, and concentration is 60-100%, 75-98% preferably, consumption be described phthalocyanine blue weight 2-10 doubly, be preferably 3.5-8 doubly.
As preferably, after the acid treatment the above-mentioned sour molten mixture that obtains is joined in the salt solution, can reduce temperature.
The general look power of the pigment that acid treatment obtains is lower, and color is gloomy, can not satisfy the requirement of use, need carry out aftertreatment, for example grinds.Milled processed can be carried out in ball mill, also can finish in kneader.Acid treatment can be carried out before grinding, also can carry out in grinding.Can add the inorganic salt grinding aid during grinding, for example sodium-chlor, sodium sulfate, sodium-acetate etc.The fineness of inorganic salt is preferably less than 325 orders.Can add the material that prevents particle aggregation during grinding, for example organic aliphatic acid etc.Grinding back pigment will purify, and removes impurity, washes.In order to improve dispersiveness, can carry out surface treatment, for example add rosined soap, tensio-active agent, organic solvent etc., preferably add the derivative of phthalocyanine blue, for example pass through methyne, on molecule, connect the phthalimide derivative, perhaps connect aminocompound, perhaps diamine compounds, on the nitrogen-atoms of described aminocompound or diamine compounds, alkyl substituent can be arranged, and perhaps hydroxyl substituting group is as the polymkeric substance of polyoxyethylene, polyoxypropylene etc.
Beneficial effect: the present invention adopts new complex method, and phthalocyanine blue is carried out pigmenting, and the pigment color that obtains is bright-coloured, Se Ligao, scattered.Product is applicable to high-grade paint and coloring plastic.Because its excellent thermotolerance, described pigment is specially adapted to plastics, for example polystyrene and mixed polymer thereof, polyolefine, especially polyethylene and polypropylene and corresponding mixed polymer, polyvinyl chloride and polyester, especially polyethylene terephthalate and polybutylene terephthalate and based on the corresponding mixing condensation product of polyester, and composition thereof with the mass pigmentation of multipolymer, can be used in the plastics, fiber dope dyeing of high-grade automobile finish and high temperature process.
Embodiment
The invention will be further described below in conjunction with embodiment:
Embodiment 1
A. ground pigmentization:
In a 500L ball mill, add 1 part of CuPc, 0.3 part in calcium chloride, 0.05 part of dimethylbenzene ground 3 hours at 100-110 ℃.The mixture that grinds, put in 2000 parts of water then, be warmed up to 80 ℃, stir and make the calcium chloride dissolving fully, vacuum filtration is washed calcium chloride and is removed fully.Oven dry is pulverized and is obtained blue powder 1.
B. acid treatment:
In the beaker of a 100ml, 15 parts in the sulfuric acid of adding 68%, temperature is at 30 degree.Drop into 3 parts of blue powders 1 that ground pigmentization obtains in the stirring, temperature keeps 50 to 55 ℃, stirred 4 hours, and then in part of 0 ℃ water of blowing to 30, stirring half an hour.Neutrality is washed in vacuum filtration then.In 90 degree oven dry, pulverizing obtains blue powder 2 and is described novel phthalocyanine blue pigment.
Embodiment 2
Carry out ground pigmentization according to routine 1a., obtain blue powder 1.
Acid treatment: in the beaker of a 100ml, 11 parts in the sulfuric acid of adding 68%, temperature is at 30 degree.Drop into 3 parts of blue powders 1 that ground pigmentization obtains in the stirring, temperature keeps 40 to 45 ℃, stirs 4 hours, in blowing to the 50 part normal-temperature water, stirs half an hour then.Neutrality is washed in vacuum filtration then.In 90 degree oven dry, pulverizing obtains blue powder 2 and is described novel phthalocyanine blue pigment.
Embodiment 3
Carry out ground pigmentization according to routine 1a., obtain blue powder 1.
Acid treatment: in the beaker of a 100ml, 24 parts in the sulfuric acid of adding 68%, temperature is at 30 degree.Drop into 3 parts of blue powders 1 that ground pigmentization obtains in the stirring, temperature keeps 55 to 60 ℃, stirred 4 hours, and then in parts of 90 ℃ water of blowing to 200, stirring half an hour.Neutrality is washed in vacuum filtration then.In 90 degree oven dry, pulverizing obtains blue powder 2 and is described novel phthalocyanine blue pigment.
Claims (10)
1. the production technique of a novel phthalocyanine blue pigment, it is characterized in that: phthalocyanine blue is carried out acid treatment and milled processed, and described acid treatment is carried out before grinding, perhaps carries out in grinding, and acid-treated temperature is 10-80 ℃, and the time is 2-30 hour; After the acid treatment, the sour molten mixture that obtains added in the entry stir, water temperature is 0-90 ℃, the quality of water be sour quality 3-20 doubly; By adjusting concentration, the acid-treated temperature of acid, the temperature of separating out, making crystalline transition is the crystal formation that phthalocyanine blue pigment needs.
2. the production technique of a kind of novel phthalocyanine blue pigment according to claim 1, it is characterized in that: the acid that described acid treatment is used is sulfuric acid, phosphoric acid or chlorsulfonic acid, acid-treated temperature is 40-60 ℃.
3. the production technique of a kind of novel phthalocyanine blue pigment according to claim 2, it is characterized in that: the acid that described acid treatment is used is sulfuric acid, concentration is 60-100%, consumption be described phthalocyanine blue weight 2-10 doubly.
4. the production technique of a kind of novel phthalocyanine blue pigment according to claim 3, it is characterized in that: described vitriolic concentration is 75-98%, consumption be phthalocyanine blue weight 3.5-8 doubly.
5. the production technique of a kind of novel phthalocyanine blue pigment according to claim 1 is characterized in that: after the acid treatment the above-mentioned sour molten mixture that obtains is joined in the salt solution.
6. the production technique of a kind of novel phthalocyanine blue pigment according to claim 1 is characterized in that: add organic aliphatic acid in above-mentioned milled processed.
7. the production technique of a kind of novel phthalocyanine blue pigment according to claim 1 is characterized in that: add rosined soap, tensio-active agent or organic solvent and carry out surface treatment in above-mentioned milled processed.
8. the production technique of a kind of novel phthalocyanine blue pigment according to claim 7, it is characterized in that: the derivative that in described surface treatment, adds phthalocyanine blue, the derivative of described phthalocyanine blue passes through methyne, on molecule, connect phthalimide derivative, aminocompound, or diamine compounds; On the nitrogen-atoms of described aminocompound or diamine compounds alkyl substituent is arranged, or hydroxyl substituting group.
9. the production technique of a kind of novel phthalocyanine blue pigment according to claim 1 is characterized in that: add the inorganic salt grinding aid in above-mentioned milled processed, the fineness of described inorganic salt grinding aid is less than 325 orders.
10. the novel phthalocyanine blue pigment dyestuff constituent that makes of the production technique of a novel phthalocyanine blue pigment as claimed in claim 1 and the coating that comprises described phthalocyanine blue pigment constituent.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201010197528A CN101864198A (en) | 2010-06-11 | 2010-06-11 | Production process of novel phthalocyanine blue pigment |
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| CN201010197528A CN101864198A (en) | 2010-06-11 | 2010-06-11 | Production process of novel phthalocyanine blue pigment |
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| CN101864198A true CN101864198A (en) | 2010-10-20 |
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| CN201010197528A Pending CN101864198A (en) | 2010-06-11 | 2010-06-11 | Production process of novel phthalocyanine blue pigment |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102766351A (en) * | 2011-05-04 | 2012-11-07 | 丽王化工(南通)有限公司 | Preparation method of novel phthalocyanine blue organic pigment |
| CN106675094A (en) * | 2016-12-28 | 2017-05-17 | 美利达颜料工业有限公司 | Preparation process of phthalocyanine blue 15:2 pigment for automotive paint |
| CN106867273A (en) * | 2017-02-20 | 2017-06-20 | 宣城亚邦化工有限公司 | Modified phthalocyanine blue pigment for the coloring of PLA system and preparation method thereof |
| CN113150577A (en) * | 2021-01-02 | 2021-07-23 | 宣城亚邦化工有限公司 | Preparation method and application of small-particle-size phthalocyanine blue pigment |
| CN113288820A (en) * | 2021-05-25 | 2021-08-24 | 台州学院 | Organically modified attapulgite-dye hybrid pigment and preparation method and application thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1161993A (en) * | 1996-04-06 | 1997-10-15 | 龙口太行颜料有限公司 | Phthalocyanine blue and production technology thereof |
| CN101457029A (en) * | 2007-12-14 | 2009-06-17 | 上海捷虹颜料化工集团股份有限公司 | Phthalocyanine blue pigment for LCD and preparation method thereof |
-
2010
- 2010-06-11 CN CN201010197528A patent/CN101864198A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1161993A (en) * | 1996-04-06 | 1997-10-15 | 龙口太行颜料有限公司 | Phthalocyanine blue and production technology thereof |
| CN101457029A (en) * | 2007-12-14 | 2009-06-17 | 上海捷虹颜料化工集团股份有限公司 | Phthalocyanine blue pigment for LCD and preparation method thereof |
Non-Patent Citations (2)
| Title |
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| 《染料与染色》 19811231 北青 酞菁蓝的制备-酸处理制备alpha酞菁蓝 第10-14页 6 , 第2期 * |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102766351A (en) * | 2011-05-04 | 2012-11-07 | 丽王化工(南通)有限公司 | Preparation method of novel phthalocyanine blue organic pigment |
| CN106675094A (en) * | 2016-12-28 | 2017-05-17 | 美利达颜料工业有限公司 | Preparation process of phthalocyanine blue 15:2 pigment for automotive paint |
| CN106675094B (en) * | 2016-12-28 | 2019-03-08 | 美利达颜料工业有限公司 | A kind of preparation process of car paint phthalocyanine blue 15:2 pigment |
| CN106867273A (en) * | 2017-02-20 | 2017-06-20 | 宣城亚邦化工有限公司 | Modified phthalocyanine blue pigment for the coloring of PLA system and preparation method thereof |
| CN113150577A (en) * | 2021-01-02 | 2021-07-23 | 宣城亚邦化工有限公司 | Preparation method and application of small-particle-size phthalocyanine blue pigment |
| CN113150577B (en) * | 2021-01-02 | 2024-02-02 | 安徽申兰华色材股份有限公司 | Preparation method and application of small-granularity phthalocyanine blue pigment |
| CN113288820A (en) * | 2021-05-25 | 2021-08-24 | 台州学院 | Organically modified attapulgite-dye hybrid pigment and preparation method and application thereof |
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Application publication date: 20101020 |