CN106867273A - Modified phthalocyanine blue pigment for the coloring of PLA system and preparation method thereof - Google Patents
Modified phthalocyanine blue pigment for the coloring of PLA system and preparation method thereof Download PDFInfo
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- CN106867273A CN106867273A CN201710089537.3A CN201710089537A CN106867273A CN 106867273 A CN106867273 A CN 106867273A CN 201710089537 A CN201710089537 A CN 201710089537A CN 106867273 A CN106867273 A CN 106867273A
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- blue pigment
- phthalocyanine blue
- coloring
- modified
- lactic acid
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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
- C09B67/0032—Treatment of phthalocyanine pigments
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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
- C09B67/0008—Coated particulate pigments or dyes with organic coatings
- C09B67/0009—Coated particulate pigments or dyes with organic coatings containing organic acid derivatives
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- Chemical Kinetics & Catalysis (AREA)
- Organic Chemistry (AREA)
- Compositions Of Macromolecular Compounds (AREA)
- Biological Depolymerization Polymers (AREA)
Abstract
The invention belongs to phthalocyanine blue pigment production technical field, and in particular to a kind of modified phthalocyanine blue pigment for the coloring of PLA system and preparation method thereof；The modified phthalocyanine blue pigment, including following weight proportion raw material：Copper phthalocyanine：Lactic acid：Tetrahydrofuran：Pure water=1：0.01~0.5：0.5~10：0.5~10；The modified phthalocyanine blue pigment that the present invention is provided can be coloured to acid fiber by polylactic, and be had the following advantages that：1. phthalocyanine blue pigment carries out that surface is modified through lactic acid or its oligomer, and pigment particles are good with the compatibility of polylactic resin system, the characteristics of possessing superfine, easily disperse.2. coloring process is environment friendly and pollution-free：Pigment is water insoluble, almost can absolutely be utilized in coloring, emits no waste water, environmentally friendly.3. because pigment is dispersed in the form of particle in fiber system, so the fiber light fastness after coloring is more excellent, not fugitive color.
Description
Technical field
The invention belongs to phthalocyanine blue pigment production technical field, and in particular to a kind of for the modified of PLA system coloring
Phthalocyanine blue pigment and preparation method thereof.
Background technology
Acid fiber by polylactic is a kind of synthesis macromolecular material with the machine-shaping property such as weave cotton cloth, dye.At present, to poly-
The method that acid fiber is coloured is dyeed with dyestuff, and the problem that the method is present mainly has：First, during dye bath
Dye utilization rate it is relatively low；Second, dyeing and finishing wastewater amount is big, and environmental pollution is serious, and cost of sewage disposal is high；3rd, due to dye
The light resistance of material is poor, so coloured fiber easily fades；4th, because acid fiber by polylactic water-resistance is poor, in harsh dye
Under shelf-regulating Conditions, acid fiber by polylactic is easily degraded, mechanical strength reduction.Although also having fine to PLA using phthalocyanine blue pigment at present
Dimension is coloured, but is mismatched because phthalocyanine blue pigment and polylactic resin system have polarity, so phthalocyanine blue pigment is poly-
Poor dispersion in lactic acid resin system, its tinctorial property has to be strengthened.
The content of the invention
It is an object of the invention to provide a kind of good, environment friendly and pollution-free the changing for the coloring of PLA system of tinctorial property
Property phthalocyanine blue pigment.
To achieve the above object, the technical solution adopted by the present invention is：
It is a kind of for PLA system coloring modified phthalocyanine blue pigment, including following weight proportion raw material：Copper phthalocyanine：
Lactic acid：Tetrahydrofuran：Pure water=1：0.01~0.5：0.5~10：0.5~10.
Above-mentioned technical proposal produce beneficial effect be：
The modified phthalocyanine blue pigment that the present invention is provided can be coloured to acid fiber by polylactic, and be had the following advantages that：1. phthalein
Cyanines indigo plant pigment carries out that surface is modified through lactic acid or its oligomer, and pigment particles are good with the compatibility of polylactic resin system,
The characteristics of possessing superfine, easily disperse.2. coloring process is environment friendly and pollution-free：Pigment is water insoluble, almost can be by hundred in coloring
/ hundred utilize, and emit no waste water, environmentally friendly.3. because pigment is that fiber system is dispersed in the form of particle
In, so the fiber light fastness after coloring is more excellent, not fugitive color.
Additionally, simple, good product performance for PLA body it is another object of the present invention to provide a kind of method
It is the preparation method of the modified phthalocyanine blue pigment of coloring.
A kind of preparation method of modified phthalocyanine blue pigment for the coloring of PLA system, comprises the following steps：
(1) copper phthalocyanine is added in pure water, and carries out dispersed with stirring；
(2) to lactic acid is added in above-mentioned material, by wet lapping pump normal temperature circulation, it is ground to fineness of materials micro- less than 1
Rice；
(3) to tetrahydrofuran is added in the material of step (2), 60~65 DEG C are warming up to, are flowed back 4-6 hours；
(4) after backflow terminates, 66~70 DEG C are continuously heating to, reclaim product of distillation tetrahydrofuran；
(5) material to step (4) is vacuum dried, and 0.1% is less than to material moisture；
(6) finally material is taken out, be milled, packed, is detected.
Above-mentioned technical proposal produce beneficial effect be：
The present invention is modified by using lactic acid or its oligomer to pigment particles, can effectively improve pigment particles poly-
Dispersive property and application performance in lactic acid resin system.Specifically, it is thin to be effectively reduced pigment particles by wet lapping
Degree；Lactic acid is added in process of production, is passed to Van der Waals force absorption on pigment particles surface, and by being vacuum dried condition
Polycondensation reaction can occur between lower lactic acid molecules, form lactic acid oligomer and effectively coat pigment particles, pigment particles are in poly- breast
Application performance in acid resin system is good.Additionally, the preparation method that the present invention is provided is simple, low production cost.
Brief description of the drawings
Fig. 1 is process chart of the invention.
Specific embodiment
To further illustrate technical scheme disclosed by the invention, illustrated below by way of 7 embodiments：
Embodiment 1：A kind of preparation method of modified phthalocyanine blue pigment for the coloring of PLA system comprises the following steps：
(1) 100kg copper phthalocyanines are added in 100kg pure water, and carries out dispersed with stirring；Wherein, copper phthalocyanine purity >=
98.5%, dissociate copper content≤500ppm；During stirring, running speed is 800-2000r/min, and mixing time is that 1.5-2.5 is small
When；
(2) to the lactic acid that copper phthalocyanine weight 2kg is added in above-mentioned material, by wet lapping pump normal temperature circulation, it is ground to
Fineness of materials is less than 1 micron；
(3) to the solvents tetrahydrofurane that 300kg is added in the material of step (2), 60~65 DEG C are warming up to, 4-6 is small for backflow
When；
(4) after backflow terminates, 66~70 DEG C are continuously heating to, reclaim product of distillation tetrahydrofuran；
(5) material to step (4) is placed in vacuum drier, at 80 DEG C, vacuum is carried out under the conditions of vacuum 0.05Mpa
Dry, 0.1% is less than to material moisture；
(6) finally material is taken out, be milled, packed, is detected.
Embodiment 2-7：A kind of preparation method of modified phthalocyanine blue pigment for the coloring of PLA system, its preparation process
With embodiment 1, raw materials used formula is as shown in table 1：
Table 1：Each composition of raw materials in embodiment 2-7：
Comparative example 1：Raw material is free of lactic acid, and remaining step is with embodiment 1.
Testing result in embodiment 1-7 and comparative example 1 is contrasted, as shown in table 2：
Table 2：Testing result contrast in embodiment 1-7 and comparative example 1
As seen from Table 2, after adding lactic acid to be modified in phthalocyanine blue pigment, its pigment fineness is small, and tinctorial strength is high,
Filter value is low.
Claims (8)
1. it is a kind of for PLA system coloring modified phthalocyanine blue pigment, it is characterised in that the original including following weight proportion
Material：
Copper phthalocyanine：Lactic acid：Tetrahydrofuran：Pure water=1：0.01~0.5：0.5~10：0.5~10.
2. it is as claimed in claim 1 to be used for the modified phthalocyanine blue pigment that PLA system is coloured, it is characterised in that including as follows
The raw material of weight proportion：
Copper phthalocyanine：Lactic acid：Tetrahydrofuran：Pure water=1：0.02~0.1：1~5：1~5.
3. it is as claimed in claim 1 to be used for the modified phthalocyanine blue pigment that PLA system is coloured, it is characterised in that including as follows
The raw material of weight proportion：
Copper phthalocyanine：Lactic acid：Tetrahydrofuran：Pure water=1：0.05：3：4.
4. the modified phthalocyanine blue pigment for the coloring of PLA system as any one of claim 1-3, its feature exists
In purity >=98.5% of the copper phthalocyanine.
5. it is as claimed in claim 4 to be used for the modified phthalocyanine blue pigment that PLA system is coloured, it is characterised in that the copper phthalein
Content≤the 500ppm of free copper in cyanines.
6. the preparation of a kind of modified phthalocyanine blue pigment for the coloring of PLA system as any one of claim 1-3
Method, it is characterised in that comprise the following steps：
(1) copper phthalocyanine is added in pure water, and carries out dispersed with stirring；
(2) to lactic acid is added in above-mentioned material, by wet lapping pump normal temperature circulation, fineness of materials is ground to less than 1 micron；
(3) to tetrahydrofuran is added in the material of step (2), 60~65 DEG C are warming up to, are flowed back 4-6 hours；
(4) after backflow terminates, 66~70 DEG C are continuously heating to, reclaim product of distillation tetrahydrofuran；
(5) material to step (4) is vacuum dried, and 0.1% is less than to material moisture；
(6) finally material is taken out, be milled, packed, is detected.
7. the preparation method of the modified phthalocyanine blue pigment of PLA system coloring is used for as claimed in claim 6, and its feature exists
In in stirring, running speed is 800-2000r/min to the step (1)；Mixing time is 1.5-2.5 hours.
8. the preparation method of the modified phthalocyanine blue pigment of PLA system coloring is used for as claimed in claim 6, and its feature exists
In the drying temperature of the step (5) is 80 DEG C, and environment vacuum degree is 0.05Mpa.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710089537.3A CN106867273B (en) | 2017-02-20 | 2017-02-20 | Modification phthalocyanine blue pigment and preparation method thereof for the coloring of polylactic acid system |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710089537.3A CN106867273B (en) | 2017-02-20 | 2017-02-20 | Modification phthalocyanine blue pigment and preparation method thereof for the coloring of polylactic acid system |
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| CN106867273A true CN106867273A (en) | 2017-06-20 |
| CN106867273B CN106867273B (en) | 2019-05-03 |
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| CN201710089537.3A Active CN106867273B (en) | 2017-02-20 | 2017-02-20 | Modification phthalocyanine blue pigment and preparation method thereof for the coloring of polylactic acid system |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116023799A (en) * | 2022-12-28 | 2023-04-28 | 宇虹颜料股份有限公司 | Degradable superfine pigment preparation and preparation method thereof |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1702091A (en) * | 2005-06-22 | 2005-11-30 | 西北师范大学 | Process for preparing nontoxic poly lactic acid by direct condensation polymerization of lactic acid |
| CN101153070A (en) * | 2006-09-28 | 2008-04-02 | 东丽纤维研究所（中国）有限公司 | High melting point polylactic acid by direct condensation and polymerization of lactic acid, and method of producing the same |
| CN101679767A (en) * | 2007-07-17 | 2010-03-24 | 科莱恩金融(Bvi)有限公司 | Based on the C.I. pigment Blue 15: 6 pigment preparation |
| CN101864198A (en) * | 2010-06-11 | 2010-10-20 | 丽王化工(南通)有限公司 | Production process of novel phthalocyanine blue pigment |
| CN105803553A (en) * | 2016-03-14 | 2016-07-27 | 浙江金彩新材料有限公司 | Heat discoloration color master batches for polylactic acid fiber and preparing method thereof |
-
2017
- 2017-02-20 CN CN201710089537.3A patent/CN106867273B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1702091A (en) * | 2005-06-22 | 2005-11-30 | 西北师范大学 | Process for preparing nontoxic poly lactic acid by direct condensation polymerization of lactic acid |
| CN101153070A (en) * | 2006-09-28 | 2008-04-02 | 东丽纤维研究所（中国）有限公司 | High melting point polylactic acid by direct condensation and polymerization of lactic acid, and method of producing the same |
| CN101679767A (en) * | 2007-07-17 | 2010-03-24 | 科莱恩金融(Bvi)有限公司 | Based on the C.I. pigment Blue 15: 6 pigment preparation |
| CN101864198A (en) * | 2010-06-11 | 2010-10-20 | 丽王化工(南通)有限公司 | Production process of novel phthalocyanine blue pigment |
| CN105803553A (en) * | 2016-03-14 | 2016-07-27 | 浙江金彩新材料有限公司 | Heat discoloration color master batches for polylactic acid fiber and preparing method thereof |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116023799A (en) * | 2022-12-28 | 2023-04-28 | 宇虹颜料股份有限公司 | Degradable superfine pigment preparation and preparation method thereof |
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| CN106867273B (en) | 2019-05-03 |
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Address after: 242000 No.70, Beimen Industrial Road, Xuancheng City, Anhui Province Patentee after: Anhui shenlanhua color material Co.,Ltd. Address before: 242000 No.70, Beimen Industrial Road, Xuancheng City, Anhui Province Patentee before: XUANCHENG YABANG CHEMICAL Co.,Ltd. |
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Address after: 242000 No.70, Beimen Industrial Road, Xuancheng City, Anhui Province Patentee after: Anhui Shenlanhua Color Material Co.,Ltd. Address before: 242000 No.70, Beimen Industrial Road, Xuancheng City, Anhui Province Patentee before: Anhui shenlanhua color material Co.,Ltd. |
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| PE01 | Entry into force of the registration of the contract for pledge of patent right |
Denomination of invention: Modified phthalocyanine blue pigment for coloring polylactic acid system and its preparation method Effective date of registration: 20230811 Granted publication date: 20190503 Pledgee: Xuancheng Branch of China Construction Bank Corp. Pledgor: Anhui Shenlanhua Color Material Co.,Ltd. Registration number: Y2023980051780 |
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