CN106675094B - A kind of preparation process of car paint phthalocyanine blue 15:2 pigment - Google Patents
A kind of preparation process of car paint phthalocyanine blue 15:2 pigment Download PDFInfo
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- CN106675094B CN106675094B CN201611232807.3A CN201611232807A CN106675094B CN 106675094 B CN106675094 B CN 106675094B CN 201611232807 A CN201611232807 A CN 201611232807A CN 106675094 B CN106675094 B CN 106675094B
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- pigment
- copper phthalocyanine
- phthalocyanine
- crystalline substance
- resistive connection
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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
- 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
- C09B67/0025—Crystal modifications; Special X-ray patterns
- C09B67/0026—Crystal modifications; Special X-ray patterns 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
- C09B67/0001—Post-treatment of organic pigments or dyes
- C09B67/0002—Grinding; Milling with solid grinding or milling assistants
-
- 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
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/60—Additives non-macromolecular
- C09D7/63—Additives non-macromolecular organic
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Wood Science & Technology (AREA)
- Paints Or Removers (AREA)
Abstract
The present invention relates to a kind of car paint preparation processes of phthalocyanine blue 15:2 pigment, belong to car paint preparation technical field, in the preparation process, first, by copper phthalocyanine crude product, grinding activation is carried out in copper phthalocyanine derivative and pigment stabiliser investment grinder, resistive connection crystalline substance is made and activates copper phthalocyanine, then resistive connection crystalline substance is activated into copper phthalocyanine again, sulfuric acid and copper phthalocyanine derivative are stirred, dilution, pickling, washing, resistive connection crystalline substance phthalocyanine blue 15:1 pigment filter cake is obtained after alkali cleaning and filtering rinsing, resistive connection crystalline substance phthalocyanine blue 15:1 pigment filter cake and copper phthalocyanine derivative are then stirred generation slurry, filter cake is made after filters pressing, finally filter cake is spray-dried with spray dryer, it is brilliant that resistive connection is finally made, antiflocculating phthalocyanine indigo plant 15:2 pigment, the pigment is applied in car paint, it can prevent coating from generating Crystallization forms flocculation agglomerated particle, is conducive to the uniform color of car paint.
Description
Technical field
The invention belongs to phthalocyanine color production technical fields, and in particular to a kind of car paint phthalocyanine blue 15:2 pigment
Preparation process.
Background technique
Phthalocyanine blue 15:2 pigment has disadvantages that especially it is applied in car paint in the application in the prior art,
Easily generation flocculation and crystallization, spray the easily general flower of lacquer painting, and more crucially weather-proof sun-proof performance is inadequate, and colour fading, coating easily occurs
Cracking or the phenomenon that uneven shade, for above-mentioned phenomenon, relevant industries start to research and develop resistive connection crystalline substance, deflocculation, sun-proof weather-proof
Phthalocyanine blue 15:2 pigment, but the producer being significantly improved in the prior art without the more mature and product using effect of one kind
The problems such as method, the selection of derivative needed for existing preparation process, additive amount and addition manner do not obtain still compared with
Good solution.
Summary of the invention
The present invention overcomes disadvantages of the existing technology, provide a kind of preparation process of car paint phthalocyanine blue,
The preparation process produces resistive connection crystalline substance, antiflocculating phthalocyanine indigo plant 15:2 pigment by resistive connection crystalline substance phthalocyanine blue 15:1 pigment, reduces life
Difficulty is produced, production technology is simplified.
The specific technical solution of the present invention is:
A kind of preparation process of car paint phthalocyanine blue 15:2 pigment, key point be, the preparation process include with
Lower step:
A, resistive connection crystalline substance activation copper phthalocyanine is prepared
Copper phthalocyanine crude product, copper phthalocyanine derivative and pigment stabiliser are put into grinder jointly and ground, pigment stabiliser
For benzene class, alcohols, amine or furans, the purity of copper phthalocyanine crude product is greater than 98%, and partial size is 10-200 μm, copper phthalocyanine crude product
Inventory be 30-1800kg, the inventory of copper phthalocyanine derivative and pigment stabiliser is respectively copper phthalocyanine crude product inventory
1%-18% and 0.1%-2%, the milling time of grinder are 1-30h, and grinding temperature is 100-120 DEG C, polished to obtain
Resistive connection crystalline substance activates copper phthalocyanine, and partial size is 0.01-0.2 μm；
B, resistive connection crystalline substance phthalocyanine blue 15:1 pigment is prepared
Resistive connection crystalline substance is activated into copper phthalocyanine, 98% sulfuric acid and copper phthalocyanine derivative according to the quality of 1:3-8:0.03-0.15
It is stirred in ratio investment collet glassed steel reaction vessels, mixing time 2-6h, temperature is maintained at 20-45 DEG C, then carries out dilute
Release, acid boils 4-8h, the weight ratio for diluting used water and activation copper phthalocyanine is 40:1, and then filtering, being washed to ph value is 6-7,
Then soda boiling 5-8h again, then squeezing into chamber filter press and rinsing to ph value is 8, and resistive connection crystalline substance phthalocyanine blue is obtained after filter press discharging
15:1 pigment filter cake；
C, resistive connection crystalline substance, antiflocculating phthalocyanine indigo plant 15:2 pigment are prepared
Resistive connection crystalline substance phthalocyanine blue 15:1 pigment filter cake is put into mashing tank and carries out high-speed stirred mashing, mixing speed is
Then 3000-6000r/min, mashing are added copper phthalocyanine derivative and are stirred, input amount is resistive connection crystalline substance phthalocyanine blue to uniform
The 3%-15% of 15:1 pigment filter cake input amount, mixing time 0.5-2h, obtain phthalocyanine blue 15:2 pigment slurry, and slurry is sent into pressure
Phthalocyanine blue 15:2 pigment filter cake is made in filter, is spray-dried with spray dryer to phthalocyanine blue 15:2 pigment filter cake, work
Temperature is 150-180 DEG C, finally obtains resistive connection crystalline substance, antiflocculating phthalocyanine indigo plant 15:2 pigment finished product after drying.
In the step A, the inventory of copper phthalocyanine crude product is 1000kg, the throwing of copper phthalocyanine derivative and pigment stabiliser
Doses is respectively the 10% and 1% of copper phthalocyanine crude product inventory, and the milling time of grinder is 15h.
In the step A, grinder is ball mill, and cooling water jecket, ball mill 300- are provided in ball mill
Vertical lapping machine, the 10m of 500L3-15m3Horizontal mill or 200L-700L vibromill, mill ball is added in ball mill
Amount be 120kg-12000kg, the diameter of mill ball is 2mm-250mm, and weight 20g-2000g, the material of mill ball is cast steel, oxygen
Change aluminium or zirconium oxide.
In the step A, the grinder is passed through inert gas during the grinding process.
In the step B, the mass ratio that resistive connection crystalline substance activates copper phthalocyanine, 98% sulfuric acid and copper phthalocyanine derivative is 1:
5:0.1.
In the step C, the input amount of the copper phthalocyanine derivative is the throwing of resistive connection crystalline substance phthalocyanine blue 15:1 pigment filter cake
Enter the 8% of amount.
The beneficial effects of the present invention are: phthalocyanine blue 15:1 pigment only has a preferable anti-crystallization energy, and flocculation resistance energy
Poor, although other phthalocyanine blue pigments, such as phthalocyanine blue 15:1 pigment have resistive connection crystalline substance and flocculation resistance energy, but sun-proof and weather-proof
Performance is poor, and the non-fading functional requirement of Automobile paint 8-10 is not achieved, and the present invention comes by resistive connection crystalline substance phthalocyanine blue 15:1 pigment
Resistive connection crystalline substance, antiflocculating phthalocyanine indigo plant 15:2 pigment are produced, the production of resistive connection crystalline substance phthalocyanine blue 15:1 pigment can be activated by resistive connection crystalline substance
Copper phthalocyanine obtains, and then mixes it with sulfuric acid and copper phthalocyanine derivative and improves phthalocyanine blue 15:1 after overpickling and alkali cleaning
Phthalocyanine blue 15:1 pigment is converted to phthalocyanine blue 15:2 pigment, phthalein finally by copper phthalocyanine derivative by the flocculation resistance energy of pigment
Cyanines indigo plant 15:2 pigment finished product has preferable resistive connection crystalline substance, deflocculation characteristic, and the difficulty of entire preparation process substantially reduces, technique step
Suddenly it is simplified, equipment, manpower and the investment of time are all significantly reduced, and resistive connection is brilliant, antiflocculating phthalocyanine indigo plant 15:2 pigment
Preparation efficiency is substantially improved.
Specific embodiment
The present invention relates to a kind of car paint preparation processes of phthalocyanine blue 15:2 pigment, and the technique is by phthalocyanine blue 15:1
Resistive connection is brilliant, antiflocculating phthalocyanine indigo plant 15:2 pigment producing for pigment, applies in car paint, first with copper phthalocyanine crude product system
It takes resistive connection crystalline substance to activate copper phthalocyanine, then produces resistive connection crystalline substance phthalocyanine blue 15:1 pigment, it is blue to finally obtain resistive connection crystalline substance, antiflocculating phthalocyanine
15:2 pigment.
Specific embodiment, raw materials for production include copper phthalocyanine crude product, copper phthalocyanine derivative and pigment stabiliser, and copper phthalocyanine is thick
The purity of product is greater than 98%, and partial size is 10-200 μm, and copper phthalocyanine derivative chooses Solsperse series, and pigment stabiliser is benzene
Class, alcohols, amine or furans, preparation process the following steps are included:
A, resistive connection crystalline substance activation copper phthalocyanine is prepared
Copper phthalocyanine crude product, copper phthalocyanine derivative and pigment stabiliser are put into grinder jointly and ground, copper phthalocyanine derivative
Object selects Solsperse5000, and pigment stabiliser is alcohols, such as polyethylene glycol, isopropanol, and the purity of copper phthalocyanine crude product is greater than
98%, partial size is 100 μm, and the inventory of copper phthalocyanine crude product is 1000kg, the inventory of copper phthalocyanine derivative and pigment stabiliser
Respectively the 10% and 1% of copper phthalocyanine crude product inventory, grinder are ball mill, are provided with cooling water jecket in ball mill,
Vertical lapping machine, the 10m of 300-500L are selected when formula of having a rest produces3-15m3Horizontal mill, continuous schedule produce when select 200L-
The vibromill of 700L, in addition, mill ball 120kg-12000kg is added in ball mill, the diameter of mill ball is 2mm-250mm, weight
20g-2000g, the material selection cast steel of mill ball are passed through inert gas in process of lapping, and the milling time of grinder is 15h,
Grinding temperature is 110 DEG C, polished to obtain resistive connection crystalline substance activation copper phthalocyanine, and partial size is qualification at 0.01-0.2 μm；
B, the anti-brilliant phthalocyanine blue 15:1 pigment of preparation knot
Resistive connection crystalline substance is activated copper phthalocyanine, 98% sulfuric acid and copper phthalocyanine derivative to put into according to the mass ratio of 1:5:0.1
It is stirred in collet glassed steel reaction vessels, mixing time 4h, temperature is maintained at 30 DEG C, is then diluted, acid boils 6h, dilution
The weight ratio of water used and activation copper phthalocyanine is 40:1, and it is 6-7 that then filtering, which is washed to ph value, then soda boiling 6h again, then
Squeezing into chamber filter press and rinsing to ph value is 8, and resistive connection crystalline substance phthalocyanine blue 15:1 pigment filter cake is obtained after filter press discharging；
C, resistive connection crystalline substance, antiflocculating phthalocyanine indigo plant 15:2 pigment are prepared
Resistive connection crystalline substance phthalocyanine blue 15:1 pigment filter cake is put into mashing tank and carries out high-speed stirred mashing, mixing speed is
Then 5000r/min, mashing are added copper phthalocyanine derivative and are stirred, input amount is resistive connection crystalline substance phthalocyanine blue 15:1 face to uniform
8%, the mixing time 1.2h for expecting filter cake input amount, obtain phthalocyanine blue 15:2 pigment slurry, and slurry is sent into filter press and phthalocyanine is made
Blue 15:2 pigment filter cake is spray-dried phthalocyanine blue 15:2 pigment filter cake with spray dryer, operating temperature 160-180
DEG C, resistive connection crystalline substance, antiflocculating phthalocyanine indigo plant 15:2 pigment finished product are obtained after drying.
Phthalocyanine blue 15:1 pigment is chosen in the present invention to carry out the preparation of resistive connection crystalline substance, antiflocculating phthalocyanine indigo plant 15:2 pigment, is led to
Resistive connection crystalline substance activation copper phthalocyanine is crossed to prepare phthalocyanine blue 15:1 pigment, is improved on the basis of its anti-crystallization energy, and enhance
Then its flocculation resistance energy converts phthalocyanine blue 15:2 pigment, copper phthalocyanine for phthalocyanine blue 15:1 pigment by copper phthalocyanine derivative
Derivative can choose existing copper phthalocyanine sulfamide derivative, and it is brilliant, anti-that phthalocyanine blue 15:2 pigment finished product has preferable resistive connection
Flocculating property, such preparation method is compared to the resistive connection crystalline substance and flocculation resistance energy for directly improving phthalocyanine blue 15:2 pigment, not only
Difficulty is low, at low cost, and preparation process is simple, is not necessarily to hyperbaric environment, safe preparation process, efficiently, is that resistive connection is brilliant, deflocculation
Sun-proof weather-proof phthalocyanine blue 15:2 pigment provides stable, the efficient and preferable preparation process of finished product using effect, is applied to automobile
It in coating, is not susceptible to flocculate and crystallize, the phenomenon of the spraying general flower of lacquer painting substantially reduces, while weather-proof sun-proof performance significantly mentions
Height is not susceptible to fade, coating cracking or the phenomenon that uneven shade.
Claims (6)
1. a kind of car paint preparation process of phthalocyanine blue 15:2 pigment, which is characterized in that the preparation process include with
Lower step:
A, resistive connection crystalline substance activation copper phthalocyanine is prepared
Copper phthalocyanine crude product, copper phthalocyanine derivative and pigment stabiliser are put into grinder jointly and ground, pigment stabiliser is benzene
Class, alcohols, amine or furans, the purity of copper phthalocyanine crude product are greater than 98%, and partial size is 10-200 μm, the throwing of copper phthalocyanine crude product
Doses is 30-1800kg, and the inventory of copper phthalocyanine derivative and pigment stabiliser is respectively the 1%- of copper phthalocyanine crude product inventory
18% and 0.1%-2%, the milling time of grinder are 1-30h, and grinding temperature is 100-120 DEG C, polished to obtain resistive connection
Crystalline substance activation copper phthalocyanine, partial size are 0.01-0.2 μm；
B, resistive connection crystalline substance phthalocyanine blue 15:1 pigment is prepared
Resistive connection crystalline substance is activated into copper phthalocyanine, 98% sulfuric acid and copper phthalocyanine derivative according to the mass ratio of 1:3-8:0.03-0.15
It is stirred in investment collet glassed steel reaction vessels, mixing time 2-6h, temperature is maintained at 20-45 DEG C, is then diluted, acid
4-8h is boiled, the weight ratio for diluting water and activation copper phthalocyanine used is 40:1, and then filtering, being washed to ph value is 6-7, then again
Soda boiling 5-8h, then squeezing into chamber filter press and rinsing to ph value is 8, and resistive connection crystalline substance phthalocyanine blue 15:1 face is obtained after filter press discharging
Expect filter cake；
C, resistive connection crystalline substance, antiflocculating phthalocyanine indigo plant 15:2 pigment are prepared
Resistive connection crystalline substance phthalocyanine blue 15:1 pigment filter cake is put into mashing tank and carries out high-speed stirred mashing, mixing speed 3000-
Then 6000r/min, mashing are added copper phthalocyanine derivative and are stirred, input amount is resistive connection crystalline substance phthalocyanine blue 15:1 face to uniform
3%-15%, the mixing time 0.5-2h for expecting filter cake input amount, obtain phthalocyanine blue 15:2 pigment slurry, and slurry is sent into filters pressing mechanism
At phthalocyanine blue 15:2 pigment filter cake, phthalocyanine blue 15:2 pigment filter cake is spray-dried with spray dryer, operating temperature is
150-180 DEG C, resistive connection crystalline substance, antiflocculating phthalocyanine indigo plant 15:2 pigment finished product are finally obtained after drying.
2. a kind of preparation process of car paint phthalocyanine blue 15:2 pigment according to claim 1, it is characterised in that: institute
In the step A stated, the inventory of copper phthalocyanine crude product is 1000kg, and the inventory of copper phthalocyanine derivative and pigment stabiliser is respectively
The 10% and 1% of copper phthalocyanine crude product inventory, the milling time of grinder are 15h.
3. a kind of preparation process of car paint phthalocyanine blue 15:2 pigment according to claim 1, it is characterised in that: institute
In the step A stated, grinder is ball mill, and cooling water jecket is provided in ball mill, and ball mill is that the vertical of 300-500L is ground
Grinding machine, 10m3-15m3Horizontal mill or 200L-700L vibromill, the amount that mill ball is added in ball mill is 120kg-
12000kg, the diameter of mill ball are 2mm-250mm, and weight 20g-2000g, the material of mill ball is cast steel, aluminium oxide or oxidation
Zirconium.
4. a kind of preparation process of car paint phthalocyanine blue 15:2 pigment according to claim 1, it is characterised in that: institute
In the step A stated, the grinder is passed through inert gas during the grinding process.
5. a kind of preparation process of car paint phthalocyanine blue 15:2 pigment according to claim 1, it is characterised in that: institute
In the step B stated, the mass ratio that resistive connection crystalline substance activates copper phthalocyanine, 98% sulfuric acid and copper phthalocyanine derivative is 1:5:0.1.
6. a kind of preparation process of car paint phthalocyanine blue 15:2 pigment according to claim 1, it is characterised in that: institute
In the step C stated, the input amount of the copper phthalocyanine derivative is the 8% of resistive connection crystalline substance phthalocyanine blue 15:1 pigment filter cake input amount.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611232807.3A CN106675094B (en) | 2016-12-28 | 2016-12-28 | A kind of preparation process of car paint phthalocyanine blue 15:2 pigment |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611232807.3A CN106675094B (en) | 2016-12-28 | 2016-12-28 | A kind of preparation process of car paint phthalocyanine blue 15:2 pigment |
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| CN106675094A CN106675094A (en) | 2017-05-17 |
| CN106675094B true CN106675094B (en) | 2019-03-08 |
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| CN108192385B (en) * | 2018-02-14 | 2019-06-07 | 滨海康益医药化工有限公司 | A kind of color compositions and preparation method thereof containing phthalocyanine blue 15:2 |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5393339A (en) * | 1994-05-11 | 1995-02-28 | Miles Inc. | Preparation of phthalocyanine pigments |
| 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 |
| CN102964868A (en) * | 2012-11-28 | 2013-03-13 | 江苏双乐化工颜料有限公司 | Preparation method for easily-dispersed phthalocyanine blue 15: 4 |
| CN103146253A (en) * | 2013-03-19 | 2013-06-12 | 江苏双乐化工颜料有限公司 | Preparation method of special phthalocyamine blue 15:4 pigment for methylbenzene ink |
-
2016
- 2016-12-28 CN CN201611232807.3A patent/CN106675094B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5393339A (en) * | 1994-05-11 | 1995-02-28 | Miles Inc. | Preparation of phthalocyanine pigments |
| 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 |
| CN102964868A (en) * | 2012-11-28 | 2013-03-13 | 江苏双乐化工颜料有限公司 | Preparation method for easily-dispersed phthalocyanine blue 15: 4 |
| CN103146253A (en) * | 2013-03-19 | 2013-06-12 | 江苏双乐化工颜料有限公司 | Preparation method of special phthalocyamine blue 15:4 pigment for methylbenzene ink |
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