CN106675094A - Preparation process of phthalocyanine blue 15:2 pigment for automotive paint - Google Patents

Preparation process of phthalocyanine blue 15:2 pigment for automotive paint Download PDF

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Publication number
CN106675094A
CN106675094A CN201611232807.3A CN201611232807A CN106675094A CN 106675094 A CN106675094 A CN 106675094A CN 201611232807 A CN201611232807 A CN 201611232807A CN 106675094 A CN106675094 A CN 106675094A
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China
Prior art keywords
pigment
blue
phthalocyanine
phthalocyanine blue
resistive connection
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CN201611232807.3A
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Chinese (zh)
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CN106675094B (en
Inventor
李庆豹
郑进峰
王西元
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MEILIDA PIGMENT INDUSTRY Co Ltd
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MEILIDA PIGMENT INDUSTRY Co Ltd
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    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09BORGANIC DYES OR CLOSELY-RELATED COMPOUNDS FOR PRODUCING DYES, e.g. PIGMENTS; MORDANTS; LAKES
    • C09B67/00Influencing 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
    • C09B67/0025Crystal modifications; Special X-ray patterns
    • C09B67/0026Crystal modifications; Special X-ray patterns of phthalocyanine pigments
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09BORGANIC DYES OR CLOSELY-RELATED COMPOUNDS FOR PRODUCING DYES, e.g. PIGMENTS; MORDANTS; LAKES
    • C09B67/00Influencing 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
    • C09B67/0001Post-treatment of organic pigments or dyes
    • C09B67/0002Grinding; Milling with solid grinding or milling assistants
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09BORGANIC DYES OR CLOSELY-RELATED COMPOUNDS FOR PRODUCING DYES, e.g. PIGMENTS; MORDANTS; LAKES
    • C09B67/00Influencing 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
    • C09B67/0032Treatment of phthalocyanine pigments
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09DCOATING 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
    • C09D7/00Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
    • C09D7/40Additives
    • C09D7/60Additives non-macromolecular
    • C09D7/63Additives 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 invention relates to a preparation process of a phthalocyanine blue 15:2 pigment for automotive paint and belongs to the technical field of preparation of automotive paint. The preparation process comprises the following steps: firstly, adding a copper phthalocyanine crude product, a copper phthalocyanine derivative and a pigment stabilizer into a grinding machine, and grinding and activating to prepare crystallization-resisting activated copper phthalocyanine; stirring the crystallization-resisting activated copper phthalocyanine, sulfuric acid and the copper phthalocyanine derivative, diluting, washing with acid, washing with water, washing with alkali and filtering and rinsing to obtain a crystallization-resisting phthalocyanine blue 15:1 pigment filter cake; finally, stirring the crystallization-resisting phthalocyanine blue 15:1 pigment filter cake and the copper phthalocyanine derivative to generate paste; pressing and filtering the paste to obtain a filter cake; finally, spraying and drying the filter cake by utilizing a spraying dryer; finally, preparing the crystallization-resisting and flocculation-resisting phthalocyanine blue 15:2 pigment. The pigment is applied to the automotive paint so that crystals formed by the paint and flocculated and agglomerated particles formed by the paint can be prevented; uniform color and luster of the automotive paint are easy to form.

Description

A kind of car paint phthalocyanine blue 15:The preparation technology of 2 pigment
Technical field
The invention belongs to phthalocyanine color production technical field, and in particular to a kind of car paint phthalocyanine blue 15:2 pigment Preparation technology.
Background technology
Phthalocyanine blue 15 in prior art:2 pigment have disadvantages that especially which is applied in car paint in the application, Easily there is flocculation and crystallization, spray lacquer painting easily general flower, more crucially weather-proof sun-proof performance not enough, easily occurs colour fading, coating The phenomenon of cracking or uneven shade, for above-mentioned phenomenon, it is weather-proof that relevant industries start research and development resistive connection crystalline substance, deflocculation, sun-proof Phthalocyanine blue 15:2 pigment, but there is no a kind of producer that more ripe and product using effect is significantly improved in prior art The problems such as method, the selection of the derivant needed for existing preparation process, addition and addition manner still do not obtain compared with Good solution.
The content of the invention
Instant invention overcomes the shortcoming that prior art is present, there is provided a kind of preparation technology of car paint phthalocyanine blue, The preparation technology is by resistive connection crystalline substance phthalocyanine blue 15:Resistive connection is brilliant, antiflocculating phthalocyanine indigo plant 15 to produce for 1 pigment:2 pigment, reduce life Dystocia degree, simplifies production technology.
The present invention concrete technical scheme be:
A kind of car paint phthalocyanine blue 15:The preparation technology of 2 pigment, key point is, described preparation technology include with Lower step:
A, prepare the brilliant activation C.I. Pigment Blue 15 of resistive connection
C.I. Pigment Blue 15 crude product, copper phthalocyanine derivative and pigment stabiliser are put in grinder jointly and is ground, pigment stabiliser For benzene class, alcohols, amine or furans, more than 98%, particle diameter is 10-200 μm to the purity of C.I. Pigment Blue 15 crude product, C.I. Pigment Blue 15 crude product Inventory be respectively C.I. Pigment Blue 15 crude product inventory for the inventory of 30-1800kg, copper phthalocyanine derivative and pigment stabiliser 1%-18% and 0.1%-2%, the milling time of grinder is 1-30h, and grinding temperature is 100-120 DEG C, polished to obtain The brilliant activation C.I. Pigment Blue 15 of resistive connection, particle diameter is 0.01-0.2 μm;
B, prepare resistive connection crystalline substance phthalocyanine blue 15:1 pigment
C.I. Pigment Blue 15,98% sulphuric acid and copper phthalocyanine derivative are activated according to 1 by resistive connection brilliant:3-8:The quality of 0.03-0.15 It is stirred in ratio input chuck glassed steel reaction vessels, mixing time 2-6h, temperature are maintained at 20-45 DEG C, subsequently carry out dilute Release, 4-8h is boiled in acid, dilution water used is 40 with the weight ratio of activation C.I. Pigment Blue 15:1, it is 6-7 then to filter, be washed to ph values, Then soda boiling 5-8h again, it is 8 then to squeeze into chamber filter press and rinse to ph values, and resistive connection crystalline substance phthalocyanine blue is obtained after pressure filter discharging 15:1 pigment filter cake;
C, prepare that resistive connection is brilliant, antiflocculating phthalocyanine indigo plant 15:2 pigment
By resistive connection crystalline substance phthalocyanine blue 15:High-speed stirred beating is carried out in 1 pigment filter cake input beating tank, mixing speed is 3000-6000r/min, is beaten to uniform, is subsequently adding copper phthalocyanine derivative and is stirred, and input amount is resistive connection crystalline substance phthalocyanine blue 15:The 3%-15% of 1 pigment filter cake input amount, mixing time 0.5-2h obtain phthalocyanine blue 15:2 pigment slurries, slurry send into pressure Filter makes phthalocyanine blue 15:2 pigment filter cakes, with spray dryer to phthalocyanine blue 15:2 pigment filter cakes are spray-dried, work Temperature is 150-180 DEG C, and drying finally obtains resistive connection crystalline substance, antiflocculating phthalocyanine indigo plant 15 after terminating:2 pigment finished products.
In described step A, the inventory of C.I. Pigment Blue 15 crude product is the throwing of 1000kg, copper phthalocyanine derivative and pigment stabiliser Doses is respectively the 10% and 1% of C.I. Pigment Blue 15 crude product inventory, and the milling time of grinder is 15h.
In described step A, grinder is ball mill, and cooling water jecket is provided with ball mill, and ball mill is 300- The vertical lapping machine of 500L, 10m3-15m3Horizontal mill or 200L-700L vibromill, mill ball is added in ball mill Amount be 120kg-12000kg, a diameter of 2mm-250mm of mill ball, weight 20g-2000g, the material of mill ball are cast steel, oxygen Change aluminum or zirconium oxide.
In described step A, described grinder is passed through noble gases in process of lapping.
In described step B, the mass ratio of the brilliant activation C.I. Pigment Blue 15 of resistive connection, 98% sulphuric acid and copper phthalocyanine derivative is 1: 5:0.1.
In described step C, the input amount of described copper phthalocyanine derivative is resistive connection crystalline substance phthalocyanine blue 15:1 pigment filter cake is thrown Enter the 8% of amount.
The invention has the beneficial effects as follows:Phthalocyanine blue 15:1 pigment only possesses preferable anti-crystallization energy, and flocculation resistance energy It is poor, other phthalocyanine blue pigments, such as phthalocyanine blue 15:Although 1 pigment possess that resistive connection is brilliant and flocculation resistance energy, but sun-proof and weather-proof Poor performance, does not reach the non-fading functional requirements of Automobile paint 8-10, and the present invention is by resistive connection crystalline substance phthalocyanine blue 15:1 pigment comes Production resistive connection is brilliant, antiflocculating phthalocyanine indigo plant 15:2 pigment, resistive connection crystalline substance phthalocyanine blue 15:The production of 1 pigment can be activated by resistive connection is brilliant Then which mixed with sulphuric acid and copper phthalocyanine derivative and improve phthalocyanine blue 15 after pickling and alkali cleaning obtaining by C.I. Pigment Blue 15:1 The flocculation resistance energy of pigment, finally by copper phthalocyanine derivative by phthalocyanine blue 15:1 pigment is converted to phthalocyanine blue 15:2 pigment, phthalein Cyanines indigo plant 15:2 pigment finished products possess preferable resistive connection crystalline substance, deflocculation characteristic, and the difficulty of whole preparation technology is substantially reduced, technique step Suddenly it is simplified, the input of equipment, manpower and time is all significantly reduced, 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 phthalocyanine blue 15:The preparation technology of 2 pigment, the technique is by phthalocyanine blue 15:1 Resistive connection is brilliant, antiflocculating phthalocyanine indigo plant 15 to produce for pigment:2 pigment, apply in the middle of car paint, first with C.I. Pigment Blue 15 crude product system The brilliant activation C.I. Pigment Blue 15 of resistive connection is taken, resistive connection crystalline substance phthalocyanine blue 15 is subsequently produced:1 pigment, finally obtains resistive connection crystalline substance, antiflocculating phthalocyanine blue 15:2 pigment.
Specific embodiment, raw materials for production include C.I. Pigment Blue 15 crude product, copper phthalocyanine derivative and pigment stabiliser, and C.I. Pigment Blue 15 is thick The purity of product is more than 98%, and particle diameter is 10-200 μm, and selection Solsperse is serial for copper phthalocyanine derivative, and pigment stabiliser is benzene Class, alcohols, amine or furans, preparation technology are comprised the following steps:
A, prepare the brilliant activation C.I. Pigment Blue 15 of resistive connection
C.I. Pigment Blue 15 crude product, copper phthalocyanine derivative and pigment stabiliser are put in grinder jointly and is ground, copper phthalocyanine derivative Thing selects Solsperse5000, and pigment stabiliser is alcohols, such as Polyethylene Glycol, isopropanol etc., and the purity of C.I. Pigment Blue 15 crude product is more than 98%, particle diameter is 100 μm, and the inventory of C.I. Pigment Blue 15 crude product is the inventory of 1000kg, copper phthalocyanine derivative and pigment stabiliser Respectively the 10% and 1% of C.I. Pigment Blue 15 crude product inventory, grinder is ball mill, and cooling water jecket is provided with ball mill, Formula of having a rest produce when from 300-500L vertical lapping machine, 10m3-15m3Horizontal mill, continuous schedule produce when select 200L- The vibromill of 700L, additionally, mill ball 120kg-12000kg, a diameter of 2mm-250mm of mill ball, weight are added in ball mill 20g-2000g, the material selection cast steel of mill ball are passed through noble gases in process of lapping, the milling time of grinder is 15h, Grinding temperature is 110 DEG C, polished to obtain the brilliant activation C.I. Pigment Blue 15 of resistive connection, and particle diameter is qualified at 0.01-0.2 μm;
Anti- brilliant phthalocyanine blue 15 is tied in B, preparation:1 pigment
C.I. Pigment Blue 15,98% sulphuric acid and copper phthalocyanine derivative are activated according to 1 by resistive connection brilliant:5:0.1 mass ratio input It is stirred in chuck glassed steel reaction vessels, mixing time 4h, temperature is maintained at 30 DEG C, is subsequently diluted, 6h is boiled in acid, dilution Water used is 40 with the weight ratio of activation C.I. Pigment Blue 15:1, it is 6-7 then to filter and be washed to ph values, then soda boiling 6h again, then It is 8 to squeeze into chamber filter press and rinse to ph values, and resistive connection crystalline substance phthalocyanine blue 15 is obtained after pressure filter discharging:1 pigment filter cake;
C, prepare that resistive connection is brilliant, antiflocculating phthalocyanine indigo plant 15:2 pigment
By resistive connection crystalline substance phthalocyanine blue 15:High-speed stirred beating is carried out in 1 pigment filter cake input beating tank, mixing speed is 5000r/min, is beaten to uniform, is subsequently adding copper phthalocyanine derivative and is stirred, and input amount is resistive connection crystalline substance phthalocyanine blue 15:1 face The 8% of material filter cake input amount, mixing time 1.2h obtains phthalocyanine blue 15:2 pigment slurries, slurry are sent into pressure filter and make phthalocyanine Blue 15:2 pigment filter cakes, with spray dryer to phthalocyanine blue 15:2 pigment filter cakes are spray-dried, and operating temperature is 160-180 DEG C, drying obtains resistive connection crystalline substance, antiflocculating phthalocyanine indigo plant 15 after terminating:2 pigment finished products.
Phthalocyanine blue 15 is chosen in the present invention:Resistive connection is brilliant, antiflocculating phthalocyanine indigo plant 15 to carry out for 1 pigment:The preparation of 2 pigment, leads to Cross the brilliant activation C.I. Pigment Blue 15 of resistive connection to prepare phthalocyanine blue 15:1 pigment, is improved on the basis of its anti-crystallization energy, and is strengthened Its flocculation resistance energy, then by copper phthalocyanine derivative by phthalocyanine blue 15:1 pigment is converted into phthalocyanine blue 15:2 pigment, C.I. Pigment Blue 15 Derivant can select existing C.I. Pigment Blue 15 sulfamide derivative, phthalocyanine blue 15:It is brilliant, anti-that 2 pigment finished products possess preferable resistive connection Flocculating property, such preparation method is compared to directly improving phthalocyanine blue 15:The resistive connection crystalline substance of 2 pigment and flocculation resistance energy, not only Difficulty is low, low cost, and preparation process is simple, and without the need for environment under high pressure, safe preparation process, efficiently is that resistive connection is brilliant, deflocculation The weather-proof phthalocyanine blue of sun-proof 15:2 pigment provide stable, the efficient and preferable preparation technology of finished product using effect, are applied to automobile In coating, it is not susceptible to flocculate and crystallizes, the phenomenon for spraying the general flower of lacquer painting is substantially reduced, while weather-proof sun-proof performance is significantly carried Height, is not susceptible to the phenomenon of colour fading, coating cracking or uneven shade.

Claims (6)

1. a kind of car paint phthalocyanine blue 15:The preparation technology of 2 pigment, it is characterised in that described preparation technology include with Lower step:
A, prepare the brilliant activation C.I. Pigment Blue 15 of resistive connection
C.I. Pigment Blue 15 crude product, copper phthalocyanine derivative and pigment stabiliser are put in grinder jointly and is ground, pigment stabiliser is benzene Class, alcohols, amine or furans, the purity of C.I. Pigment Blue 15 crude product are more than 98%, and particle diameter is 10-200 μm, the throwing of C.I. Pigment Blue 15 crude product Doses is the 1%- that the inventory of 30-1800kg, copper phthalocyanine derivative and pigment stabiliser is respectively C.I. Pigment Blue 15 crude product inventory 18% and 0.1%-2%, the milling time of grinder is 1-30h, and grinding temperature is 100-120 DEG C, polished to obtain resistive connection Brilliant activation C.I. Pigment Blue 15, particle diameter is 0.01-0.2 μm;
B, prepare resistive connection crystalline substance phthalocyanine blue 15:1 pigment
C.I. Pigment Blue 15,98% sulphuric acid and copper phthalocyanine derivative are activated according to 1 by resistive connection brilliant:3-8:The mass ratio of 0.03-0.15 Input chuck glassed steel reaction vessels in be stirred, mixing time 2-6h, temperature are maintained at 20-45 DEG C, be subsequently diluted, acid 4-8h is boiled, dilution water used is 40 with the weight ratio of activation C.I. Pigment Blue 15:1, then filter, ph values are washed to for 6-7, Ran Houzai Soda boiling 5-8h, it is 8 then to squeeze into chamber filter press and rinse to ph values, and resistive connection crystalline substance phthalocyanine blue 15 is obtained after pressure filter discharging:1 face Material filter cake;
C, prepare that resistive connection is brilliant, antiflocculating phthalocyanine indigo plant 15:2 pigment
By resistive connection crystalline substance phthalocyanine blue 15:High-speed stirred beating is carried out in 1 pigment filter cake input beating tank, mixing speed is 3000- 6000r/min, is beaten to uniform, is subsequently adding copper phthalocyanine derivative and is stirred, and input amount is resistive connection crystalline substance phthalocyanine blue 15:1 face The 3%-15% of material filter cake input amount, mixing time 0.5-2h obtain phthalocyanine blue 15:2 pigment slurries, slurry send into filter pressing mechanism Into phthalocyanine blue 15:2 pigment filter cakes, with spray dryer to phthalocyanine blue 15:2 pigment filter cakes are spray-dried, and operating temperature is 150-180 DEG C, drying finally obtains resistive connection crystalline substance, antiflocculating phthalocyanine indigo plant 15 after terminating:2 pigment finished products.
2. the preparation technology of a kind of car paint phthalocyanine blue according to claim 1, it is characterised in that:Described step In A, the inventory of C.I. Pigment Blue 15 crude product is thick for the inventory respectively C.I. Pigment Blue 15 of 1000kg, copper phthalocyanine derivative and pigment stabiliser The 10% of product inventory and 1%, the milling time of grinder is 15h.
3. the preparation technology of a kind of car paint phthalocyanine blue according to claim 1, it is characterised in that:Described step In A, grinder is ball mill, is provided with cooling water jecket in ball mill, ball mill for 300-500L vertical lapping machine, 10m3-15m3Horizontal mill or 200L-700L vibromill, in ball mill add mill ball amount be 120kg- 12000kg, a diameter of 2mm-250mm of mill ball, weight 20g-2000g, the material of mill ball is cast steel, aluminium oxide or oxidation Zirconium.
4. the preparation technology of a kind of car paint phthalocyanine blue according to claim 1, it is characterised in that:Described step In A, described grinder is passed through noble gases in process of lapping.
5. the preparation technology of a kind of car paint phthalocyanine blue according to claim 1, it is characterised in that:Described step In B, the mass ratio of the brilliant activation C.I. Pigment Blue 15 of resistive connection, 98% sulphuric acid and copper phthalocyanine derivative is 1:5:0.1.
6. the preparation technology of a kind of car paint phthalocyanine blue according to claim 1, it is characterised in that:Described step In C, the input amount of described copper phthalocyanine derivative is resistive connection crystalline substance phthalocyanine blue 15:The 8% of 1 pigment filter cake input amount.
CN201611232807.3A 2016-12-28 2016-12-28 A kind of preparation process of car paint phthalocyanine blue 15:2 pigment Active CN106675094B (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108192385A (en) * 2018-02-14 2018-06-22 滨海康益医药化工有限公司 One kind contains phthalocyanine blue 15:2 color compositions and preparation method thereof

Citations (4)

* Cited by examiner, † Cited by third party
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

Patent Citations (4)

* Cited by examiner, † Cited by third party
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

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108192385A (en) * 2018-02-14 2018-06-22 滨海康益医药化工有限公司 One kind contains phthalocyanine blue 15:2 color compositions and preparation method thereof
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

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