CN108084729A - A kind of preparation method of high energy-saving environment protection type phthalocyanine green pigment - Google Patents
A kind of preparation method of high energy-saving environment protection type phthalocyanine green pigment Download PDFInfo
- Publication number
- CN108084729A CN108084729A CN201711423082.0A CN201711423082A CN108084729A CN 108084729 A CN108084729 A CN 108084729A CN 201711423082 A CN201711423082 A CN 201711423082A CN 108084729 A CN108084729 A CN 108084729A
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- phthalocyanine green
- preparation
- high energy
- environment protection
- protection type
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Classifications
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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
- C09B47/00—Porphines; Azaporphines
- C09B47/04—Phthalocyanines abbreviation: Pc
- C09B47/08—Preparation from other phthalocyanine compounds, e.g. cobaltphthalocyanineamine complex
- C09B47/10—Obtaining compounds having halogen atoms directly bound to the phthalocyanine skeleton
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D487/00—Heterocyclic compounds containing nitrogen atoms as the only ring hetero atoms in the condensed system, not provided for by groups C07D451/00 - C07D477/00
- C07D487/22—Heterocyclic compounds containing nitrogen atoms as the only ring hetero atoms in the condensed system, not provided for by groups C07D451/00 - C07D477/00 in which the condensed system contains four or more hetero rings
-
- 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
-
- 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
- C09B67/006—Preparation of organic pigments
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Compositions Of Macromolecular Compounds (AREA)
- Inks, Pencil-Leads, Or Crayons (AREA)
Abstract
The invention discloses a kind of preparation methods of high energy-saving environment protection type phthalocyanine green pigment of organic pigment preparing technical field, it is characterised in that：This method is as follows：S1：After the blue or green dissolving in advance of copper phthalein, the catalyst of 6~8g is added in, 100~120 DEG C is warming up to and carries out logical chlorine reaction；S2：Phthalocyanine green crude product is obtained after filtering；S3：The surfactant for then adding in 5~7g is sufficiently stirred, and removes organic media with steam distillation, and phthalocyanine green fine work is obtained after filtration drying；S4：Phthalocyanine green fine work is mixed into 400~600ml water-base resins, phthalocyanine green pigment finished product is made after stirring and evenly mixing, the present invention is by increasing atmospheric pressure, reaction temperature is reduced, reduces required power consumption when promoting temperature, while the present invention can reduce system viscosity, so that the abundant color development of pigment, improve color, and in preparation process no acidic sewage discharge, the problem of environmental pollution will not be caused.
Description
Technical field
The invention discloses a kind of preparation methods of high energy-saving environment protection type phthalocyanine green pigment, are specially that organic pigment prepares skill
Art field.
Background technology
Phthalocyanine pigment is widely used in ink, coating and plastic cement since its advantageous heat resistance and weatherability are secured
Field, the method for general pigmentation have acidic treatment, polishing and solvent treatment method.Acidic treatment is can be molten using crude product
It in the property of the concentrated sulfuric acid, is dissolved, crystallization is then precipitated again, obtain the pigment of smaller particless；Polishing be using ball mill,
Kneader etc., the particle that with Strong shear power and impact force when reunites separate, while in order to which particle is controlled no longer to reunite and obtain
The crystal form needed is, it is necessary to add in the auxiliary agents such as organic solvent and surfactant；Solvent treatment method is then to utilize pigment in a solvent
There are certain dissolution properties, pigment dissolved is made to be precipitated again, make subtle crystalline growth, reunite so as to reduce.It is but above-mentioned
Method there is：Acidic treatment can generate substantial amounts of sour water because using substantial amounts of sulfuric acid, so as to cause dirt to environment
Dye；Polishing need to make grinding aid using inorganic salts, while the electric energy needed is higher, belongs to the Product Process of highly energy-consuming；At solvent
Logos is not only dangerous big because using alcohols, benzene class equal solvent in process of production, but also needs to recycle, while its residual part
Can also environment be caused a degree of pollution by dividing.For this purpose, we have proposed a kind of systems of high energy-saving environment protection type phthalocyanine green pigment
Preparation Method comes into operation, to solve the above problems.
The content of the invention
It is an object of the invention to provide a kind of preparation method of high energy-saving environment protection type phthalocyanine green pigment, to solve the above-mentioned back of the body
The problem of being proposed in scape technology.
To achieve the above object, the present invention provides following technical solution：A kind of system of high energy-saving environment protection type phthalocyanine green pigment
Preparation Method, this method are as follows：
S1：After the blue or green dissolving in advance of copper phthalein, the catalyst of 6~8g is added in, 100~120 DEG C is warming up to and carries out logical chlorine reaction；
S2：Reactant is diluted with the deionized water of 200~300ml, and phthalocyanine green crude product is obtained after filtering；
S3：Phthalocyanine green crude product is put into organic media, 1~3h is stirred at a certain temperature, is allowed in organic media
In it is fully dispersed, then add in 5~7g surfactant be sufficiently stirred, and with steam distillation remove organic media, cross be filtered dry
Phthalocyanine green fine work is obtained after dry；
S4：Phthalocyanine green fine work is mixed into 400~600ml water-base resins, adds 20~30ml of thickener, wetting successively
Phthalocyanine green pigment finished product is made in 5~10ml of 10~20ml of agent and dispersant after stirring and evenly mixing.
Preferably, in the step S1, logical chlorine reaction carries out under the pressure of 0.3~0.5MPa, the reaction time for 1~
3h。
Preferably, in the step S1, catalyst is one kind in sulphur, ferric trichloride, antimony trichloride and potassium iodide.
Preferably, in the step S3, organic media is n-octyl alcohol, and whipping temp is 60~80 DEG C, and surfactant is
Sodium n-alkylbenzenesulfonate, sodium sulfate of polyethenoxy ether of fatty alcohol, fatty alcohol polyoxyethylene ether ammonium sulfate, sldium lauryl sulfate and
One kind in lauroyl glutamate.
Preferably, in the step S4, water-base resin is polyester resin, phenolic resin, acrylic resin, organic siliconresin
And one kind in polyurethane resin.
Preferably, in the step S4, thickener is non-ionic modified hydroxyethylcellulosadsorbing and environment-protecting polyurethane
Mixture.
Preferably, in the step S4, dispersant is modified polycarboxylic acid ammonium salt, modified polyacrylate and phosphate ester salt
The mixture of one or both of class.
Preferably, in the step S4, wetting agent is fatty acid ester sulfate, alkylphenol polyoxyethylene ether, polyoxyethylene
One or more mixtures in modifying agent.
Compared with prior art, the beneficial effects of the invention are as follows：The present invention reduces reaction temperature by increasing atmospheric pressure
Degree reduces required power consumption when promoting temperature, while the present invention can reduce system viscosity so that the abundant color development of pigment,
Improve color, and in preparation process no acidic sewage discharge, the problem of environmental pollution will not be caused.
Description of the drawings
Fig. 1 is preparation method flow chart of the present invention.
Specific embodiment
Below in conjunction with the attached drawing in the embodiment of the present invention, the technical solution in the embodiment of the present invention is carried out clear, complete
Site preparation describes, it is clear that described embodiment is only part of the embodiment of the present invention, instead of all the embodiments.It is based on
Embodiment in the present invention, those of ordinary skill in the art are obtained every other without making creative work
Embodiment belongs to the scope of protection of the invention.
Embodiment one
A kind of preparation method of high energy-saving environment protection type phthalocyanine green pigment, this method are as follows：
S1：After the blue or green dissolving in advance of copper phthalein, the ferric trichloride of 6g is added in, 100 DEG C is warming up to and carries out logical chlorine reaction, it is anti-to lead to chlorine
It should be carried out under the pressure of 0.3MPa, reaction time 1h；
S2：Reactant is diluted with the deionized water of 200ml, and phthalocyanine green crude product is obtained after filtering；
S3：Phthalocyanine green crude product is put into n-octyl alcohol, stirs 1h at a certain temperature, whipping temp is 60 DEG C, is allowed to
Fully dispersed in n-octyl alcohol, the sodium n-alkylbenzenesulfonate for then adding in 5g is sufficiently stirred, and just pungent with steam distillation removing
Alcohol obtains phthalocyanine green fine work after filtration drying；
S4：Phthalocyanine green fine work is mixed into 400ml polyester resin, adds thickener 20ml, fatty acid ester sulfuric acid successively
Phthalocyanine green pigment finished product is made in salt 10ml and modified polycarboxylic acid ammonium salt 5ml after stirring and evenly mixing.
Embodiment two
A kind of preparation method of high energy-saving environment protection type phthalocyanine green pigment, this method are as follows：
S1：After the blue or green dissolving in advance of copper phthalein, the antimony trichloride of 8g is added in, 120 DEG C is warming up to and carries out logical chlorine reaction, it is anti-to lead to chlorine
It should be carried out under the pressure of 0.5MPa, reaction time 3h；
S2：Reactant is diluted with the deionized water of 300ml, and phthalocyanine green crude product is obtained after filtering；
S3：Phthalocyanine green crude product is put into n-octyl alcohol, stirs 3h at a certain temperature, whipping temp is 80 DEG C, is allowed to
Fully dispersed in n-octyl alcohol, the sodium sulfate of polyethenoxy ether of fatty alcohol for then adding in 7g is sufficiently stirred, and is removed with steam distillation
N-octyl alcohol is removed, phthalocyanine green fine work is obtained after filtration drying；
S4：Phthalocyanine green fine work is mixed into 600ml phenolic resin, adds thickener 30ml, alkyl phenol polyoxy second successively
Phthalocyanine green pigment finished product is made in alkene ether 20ml and modified polyacrylate 10ml after stirring and evenly mixing.
Embodiment three
A kind of preparation method of high energy-saving environment protection type phthalocyanine green pigment, this method are as follows：
S1：After the blue or green dissolving in advance of copper phthalein, the sulphur of 7g is added in, 110 DEG C is warming up to and carries out logical chlorine reaction, lead to chlorine reaction and exist
It is carried out under the pressure of 0.4MPa, reaction time 2h；
S2：Reactant is diluted with the deionized water of 280ml, and phthalocyanine green crude product is obtained after filtering；
S3：Phthalocyanine green crude product is put into n-octyl alcohol, stirs 2h at a certain temperature, whipping temp is 70 DEG C, is allowed to
Fully dispersed in n-octyl alcohol, the sldium lauryl sulfate for then adding in 6g is sufficiently stirred, and removes n-octyl alcohol, mistake with steam distillation
Be filtered dry it is dry after obtain phthalocyanine green fine work；
S4：Phthalocyanine green fine work is mixed into 500ml organic siliconresins, adds thickener 25ml successively, polyoxyethylene changes
Property agent 15ml and modified polycarboxylic acid ammonium salt 6ml, phthalocyanine green pigment finished product is made after stirring and evenly mixing.
In summary described in embodiment, highly preferred embodiment of the present invention is embodiment three, and the present invention is by increasing atmospheric pressure
Power reduces reaction temperature, reduces required power consumption when promoting temperature, while the present invention can reduce system viscosity so that
The abundant color development of pigment, improve color, and in preparation process no acidic sewage discharge, asking for environmental pollution will not be caused
Topic.
It although an embodiment of the present invention has been shown and described, for the ordinary skill in the art, can be with
Understanding without departing from the principles and spirit of the present invention can carry out these embodiments a variety of variations, modification, replace
And modification, the scope of the present invention is defined by the appended.
Claims (8)
1. a kind of preparation method of high energy-saving environment protection type phthalocyanine green pigment, it is characterised in that：This method is as follows：
S1：After the blue or green dissolving in advance of copper phthalein, the catalyst of 6~8g is added in, 100~120 DEG C is warming up to and carries out logical chlorine reaction；
S2：Reactant is diluted with the deionized water of 200~300ml, and phthalocyanine green crude product is obtained after filtering；
S3：Phthalocyanine green crude product is put into organic media, 1~3h is stirred at a certain temperature, is allowed to fill in organic media
Point scattered, the surfactant for then adding in 5~7g is sufficiently stirred, and removes organic media with steam distillation, after filtration drying
Obtain phthalocyanine green fine work；
S4：Phthalocyanine green fine work is mixed into 400~600ml water-base resins, adds 20~30ml of thickener, wetting agent 10 successively
Phthalocyanine green pigment finished product is made in 5~10ml of~20ml and dispersant after stirring and evenly mixing.
2. a kind of preparation method of high energy-saving environment protection type phthalocyanine green pigment according to claim 1, it is characterised in that：It is described
In step S1, logical chlorine reaction carries out under the pressure of 0.3~0.5MPa, and the reaction time is 1~3h.
3. a kind of preparation method of high energy-saving environment protection type phthalocyanine green pigment according to claim 1, it is characterised in that：It is described
In step S1, catalyst is one kind in sulphur, ferric trichloride, antimony trichloride and potassium iodide.
4. a kind of preparation method of high energy-saving environment protection type phthalocyanine green pigment according to claim 1, it is characterised in that：It is described
In step S3, organic media is n-octyl alcohol, and whipping temp is 60~80 DEG C, and surfactant is sodium n-alkylbenzenesulfonate, fat
In fat alcohol polyethenoxy ether sodium sulfate, fatty alcohol polyoxyethylene ether ammonium sulfate, sldium lauryl sulfate and lauroyl glutamate
It is a kind of.
5. a kind of preparation method of high energy-saving environment protection type phthalocyanine green pigment according to claim 1, it is characterised in that：It is described
In step S4, water-base resin is in polyester resin, phenolic resin, acrylic resin, organic siliconresin and polyurethane resin
It is a kind of.
6. a kind of preparation method of high energy-saving environment protection type phthalocyanine green pigment according to claim 1, it is characterised in that：It is described
In step S4, thickener is non-ionic modified hydroxyethylcellulosadsorbing and the mixture of environment-protecting polyurethane.
7. a kind of preparation method of high energy-saving environment protection type phthalocyanine green pigment according to claim 1, it is characterised in that：It is described
In step S4, dispersant is one or both of modified polycarboxylic acid ammonium salt, modified polyacrylate and phosphates
Mixture.
8. a kind of preparation method of high energy-saving environment protection type phthalocyanine green pigment according to claim 1, it is characterised in that：It is described
In step S4, wetting agent is fatty acid ester sulfate, the one or more in alkylphenol polyoxyethylene ether, polyoxyethylene modifier
Mixture.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711423082.0A CN108084729A (en) | 2017-12-25 | 2017-12-25 | A kind of preparation method of high energy-saving environment protection type phthalocyanine green pigment |
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| CN201711423082.0A CN108084729A (en) | 2017-12-25 | 2017-12-25 | A kind of preparation method of high energy-saving environment protection type phthalocyanine green pigment |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109181359A (en) * | 2018-08-29 | 2019-01-11 | 津正颜科技（天津）有限公司 | A kind of particle environmental-friendly pigment and its preparation process |
| CN110219033A (en) * | 2019-07-02 | 2019-09-10 | 东莞金稞电子科技有限公司 | A kind of aluminum alloy anode plane pattern colouring method |
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| CN1091444A (en) * | 1993-02-27 | 1994-08-31 | 张合义 | Phthalocyanine green and preparation method thereof |
| CN1680380A (en) * | 2004-03-15 | 2005-10-12 | 日本触媒股份有限公司 | Method for production of halogen-containing phthalocyanine compound |
| CN101538415A (en) * | 2008-03-21 | 2009-09-23 | 亚邦化工集团有限公司 | Method for preparing crude product of yellowish phthalocyanine green |
| CN101880471A (en) * | 2010-06-11 | 2010-11-10 | 丽王化工(南通)有限公司 | Process for producing high-grade phthalocyanine green pigment |
| CN102786814A (en) * | 2011-05-16 | 2012-11-21 | 南通乐彩颜料化工有限公司 | Preparation method for high energy saving environmental protection type phthalocyanine green pigment |
| CN104804465A (en) * | 2015-04-24 | 2015-07-29 | 江苏双乐化工颜料有限公司 | Fine clean production process of phthalocyanine green pigment |
| CN105647225A (en) * | 2014-12-08 | 2016-06-08 | 池州泰阳颜料有限公司 | Preparation method of phthalocyanine green G |
-
2017
- 2017-12-25 CN CN201711423082.0A patent/CN108084729A/en active Pending
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1091444A (en) * | 1993-02-27 | 1994-08-31 | 张合义 | Phthalocyanine green and preparation method thereof |
| CN1680380A (en) * | 2004-03-15 | 2005-10-12 | 日本触媒股份有限公司 | Method for production of halogen-containing phthalocyanine compound |
| CN101538415A (en) * | 2008-03-21 | 2009-09-23 | 亚邦化工集团有限公司 | Method for preparing crude product of yellowish phthalocyanine green |
| CN101880471A (en) * | 2010-06-11 | 2010-11-10 | 丽王化工(南通)有限公司 | Process for producing high-grade phthalocyanine green pigment |
| CN102786814A (en) * | 2011-05-16 | 2012-11-21 | 南通乐彩颜料化工有限公司 | Preparation method for high energy saving environmental protection type phthalocyanine green pigment |
| CN105647225A (en) * | 2014-12-08 | 2016-06-08 | 池州泰阳颜料有限公司 | Preparation method of phthalocyanine green G |
| CN104804465A (en) * | 2015-04-24 | 2015-07-29 | 江苏双乐化工颜料有限公司 | Fine clean production process of phthalocyanine green pigment |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109181359A (en) * | 2018-08-29 | 2019-01-11 | 津正颜科技（天津）有限公司 | A kind of particle environmental-friendly pigment and its preparation process |
| CN110219033A (en) * | 2019-07-02 | 2019-09-10 | 东莞金稞电子科技有限公司 | A kind of aluminum alloy anode plane pattern colouring method |
| CN110219033B (en) * | 2019-07-02 | 2021-04-30 | 东莞金稞电子科技有限公司 | Aluminum alloy anode plane pattern dyeing method |
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Application publication date: 20180529 |