CN106398307A - Preparation process of phthalocyanine blue for PU inkjet printing - Google Patents
Preparation process of phthalocyanine blue for PU inkjet printing Download PDFInfo
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- CN106398307A CN106398307A CN201610796211.XA CN201610796211A CN106398307A CN 106398307 A CN106398307 A CN 106398307A CN 201610796211 A CN201610796211 A CN 201610796211A CN 106398307 A CN106398307 A CN 106398307A
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- Prior art keywords
- phthalocyanine blue
- blue
- water
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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
- C09B67/0033—Blends of pigments; Mixtured crystals; Solid solutions
- C09B67/0034—Mixtures of two or more pigments or dyes of the same type
- C09B67/0035—Mixtures of phthalocyanines
Abstract
The invention discloses a preparation process of phthalocyanine blue for PU inkjet printing. The preparation process comprises the following steps: taking 1 part by drying weight of coarse phthalocyanine blue, and adding 0.05 to 0.15 part by drying weight of phthalocyanine derivative; then adding 8 to 12 parts of water, stirring, and raising the temperature to be 60 to 70 DEG C; adding 0.02 to 0.06 part of hyperdispersant, stirring, filtering, washing and drying, thus finally obtaining a finished product. According to the preparation process disclosed by the invention, the phthalocyanine derivative is added into the coarse phthalocyanine blue by adopting the proportion, so that prepared phthalocyanine blue for the PU inkjet printing has remarkable improvement effects on glossiness, transparency and tinting strength. Besides, by correct selection and use of the hyperdispersant, the compatibility between a pigment product and a resin system can be improved, the pigment product and the resin system are combined more firmly, and the printing glossiness is good.
Description
Technical field
The present invention relates to pigment manufacture field, it is specifically related to a kind of preparation technology of PU ink phthalocyanine blue.
Background technology
Existing Phthalocyanine Blue BGS is (also known as pigment blue 15:3) can be widely applied to the systems such as offset printing ink, ink, but its
Itself does not possess deflocculation performance, if therefore Phthalocyanine Blue BGS is used for solvent type ink, it can shape in the resin system of ink
Become g., jelly-like, lose flowability, therefore cannot use.
Show through research, add some phthalocyanine derivates in Phthalocyanine Blue BGS that such as sulfonated copper phthalocyanine so can improve
The deflocculation performance of phthalocyanine blue product, the phthalocyanine blue being obtained using this method is referred to as pigment blue 15 in the market:4, but existing
Or some sulfonated copper phthalocyanines pollute environment in process of production, yield is low, or sulfonation degree is difficult to control to, thus leading to product
Quality stability poor.In addition, different solvent type inks is also different to the performance requirement of pigment.Therefore, for different molten
Based ink prepares corresponding pigment, and this is significant to the serviceability improving ink.
Content of the invention
It is an object of the invention to provide a kind of using effect is good, have deflocculation PU ink phthalocyanine blue preparation
Technique.
For achieving the above object, the technical solution used in the present invention is：A kind of preparation technology of PU ink phthalocyanine blue, its
Step is as follows：
Take the thick phthalocyanine blue of 1 part of weight of giving money as a gift, add the peacock blue derivative of 0.05～0.15 part of weight of giving money as a gift, then plus 8
～12 parts of water stirrings, are warming up to 60～70 DEG C, add 0.02～0.06 part of hyper-dispersant stirring, filter, washing, be dried, obtain final product.
Using having the beneficial effects that technique scheme produces：The present invention adopts above ratio will to add in thick phthalocyanine blue
Peacock blue derivative, the phthalocyanine blue being so obtained has significantly for PU ink in terms of glossiness, transparency and tinting strength, tinting power
Lifting effect.Specifically, described hyper-dispersant is poly- ten dihydroxystearic acids, and poly- ten dihydroxystearic acids are the ice using 10 times
Add after acetate dissolution.By correct selection and the use of hyper-dispersant, so can improve pigment product and resin system it
Between the compatibility, make both combinations more firm, the glossiness of printing is good, and color and luster is good.
Specific scheme is that the preparation process of described thick phthalocyanine blue is as follows：
According to 1～10:5～15 weight puts into anhydrous sodium sulfate and C.I. Pigment Blue 15 than in ball mill, at 50～95 DEG C
Grind 5～35h, making beating, acid is boiled except ferrum, afterwards with tetrahydrofuran solvent backflow 2～3h, distillation removes solvent, filter pressing, washes with water
Wash to electrical conductivity ＜ 300 μ s/cm, the filter cake unloading is thick phthalocyanine blue.
The preparation process of described peacock blue derivative is as follows：
Under agitation, put into the concentrated sulphuric acid that 480～680 weight portion concentration are 101%～105% in reactor,
At 30～40 DEG C, slow input 60～80 weight portion C.I. Pigment Blue 15s, are warming up to 70～95 DEG C with the speed of 3～5 DEG C/min, insulation
1.5～2.5h, sequentially add 500～1000 weight portion water, 20～30 weight portion C8～C14 alkyl trimethyl ammonium chloride, 55～
65 weight portion C16～C20 Dialkyl dimethyl ammonium chloride, are warming up to 45～55 DEG C, insulation, when mensuration absorbance is 0.3～0.5
Reach sulfonation terminal, open recirculated cooling water and be less than 80 DEG C with controlling reaction temperature, be then slowly added into 8～10 times of water dilute
Release, terminate after 30～40min, filter pressing, water washing is peacock blue derivative to electrical conductivity≤500 μ s/cm, the filter cake unloading.Phthalein
The difficult point of cyanines derivant synthesis is the control of sulfonation degree, too low, does not reach optimal modified effect, too high and can make product water
Dissolubility increases it is difficult to be used for commercial production, and in addition ammonium salt intensification, insulating process, timing sampling carries out absorbance to the present invention
Detection, thus judging sulfonating reaction degree, so guarantee prepare phthalocyanine derivates using effect.
Wherein, described C8～C14 alkyl trimethyl ammonium chloride molecular formula is N (CH3)3(CmHn), m=8～14, n=2m
+1；The molecular formula of C16～C20 Dialkyl dimethyl ammonium chloride is N (CH3)2(CmHn)2, m=16～20, n=2m+1.
Preferably, in the preparation process of thick phthalocyanine blue the weight of anhydrous sodium sulfate and C.I. Pigment Blue 15 than for 5～8:10～12, no
Aqueous sodium persulfate and C.I. Pigment Blue 15 are grinding 20～25h at 70～75 DEG C；The each raw material putting in the preparation process of peacock blue derivative
Weight fraction be：Concentrated sulphuric acid 500～520, C.I. Pigment Blue 15 65～75, put into added between C8～C14 alkyl trimethyl ammonium chloride
Water 700～750, C8～C14 alkyl trimethyl ammonium chloride 20～25, C16～C20 Dialkyl dimethyl ammonium chloride 55～65.
The C.I. Pigment Blue 15 that reality is prepared used by thick phthalocyanine blue and phthalocyanine derivates can be by existing conventional technique preparation
Processed using solvent method afterwards and obtain.
Pigment blue 15 on the phthalocyanine blue being prepared using technique disclosed by the invention and market:3 production cost is big
Body phase is same, but its price can be with common pigment blue 15 on market:4 is low more than 10,000 yuan/ton, in addition domestic for pigment blue 15:
The annual requirement of 4 such products is 10000 tons about, therefore replaces the phthalocyanine blue that method disclosed by the invention prepares existing
Some pigment blue 15s:4 will have the huge market space.
Specific embodiment
1～3 technical scheme disclosed by the invention is further described by the following examples：
Embodiment 1：The preparation of phthalocyanine blue
1) put into anhydrous sodium sulfate 600kg, C.I. Pigment Blue 15 900kg into the horizontal ball mill of 15000L, grind at 75 DEG C
20 hours, making beating, acid were boiled except ferrum, were flowed back 3h with tetrahydrofuran solvent afterwards, and distillation removes solvent, filter pressing, is washed with water to electricity
Conductance ＜ 300 μ s/cm, the filter cake unloading is thick phthalocyanine blue；
2) under agitation, put into the concentrated sulphuric acid that 6000kg concentration is 101% in reactor, slowly throw at 40 DEG C
Enter 700kg C.I. Pigment Blue 15, be warming up to 70 DEG C with the speed of 3～5 DEG C/min, be incubated 2h, sequentially add the C14 alkyl of 8t water, 260kg
Trimethyl ammonium chloride, the C18 Dialkyl dimethyl ammonium chloride of 60kg, are warming up to 50 DEG C, insulation, and mensuration absorbance is to arrive when 0.5
Reach sulfonation terminal, open recirculated cooling water and be less than 80 DEG C with controlling reaction temperature, be then slowly added into 10 times of water dilutions,
Terminate after 30min, filter pressing, water washing is peacock blue derivative to electrical conductivity≤500 μ s/cm, the filter cake unloading, specifically, inhale
The detection method of luminosity is：Take 9g reactant liquor, plus 250 grams of water, 5g concentration is 5% NaOH solution, and adjusting PH is 10～11, rises
Temperature, to 70 DEG C, stirs 10min, detection absorbance (similarly hereinafter) on 721 type spectrophotometers, at wavelength 480～680nm；
3) by step 1) the thick phthalocyanine blue filter cake prepared takes 100 parts in terms of giving money as a gift, procedure of processing 2) phthalein prepared is blue or green derivative
Thing filter cake takes 10 parts in terms of giving money as a gift, and both and 1000 parts of water mix and blends in the lump is warming up to 65 DEG C, adds 4 parts of poly- ten dihydroxies
Base stearic acid (poly- ten dihydroxystearic acids are to add using after 10 times of glacial acetic acid dissolving) stirring, filters, washing, is dried, that is,
?.
Embodiment 2：The preparation of phthalocyanine blue
1) put into anhydrous sodium sulfate 600kg, C.I. Pigment Blue 15 1800kg into the horizontal ball mill of 15000L, grind at 60 DEG C
8 hours, making beating, acid were boiled except ferrum, were flowed back 2.5h with tetrahydrofuran solvent afterwards, and distillation removes solvent, filter pressing, is washed with water to electricity
Conductance ＜ 300 μ s/cm, the filter cake unloading is thick phthalocyanine blue；
2) under agitation, put into the concentrated sulphuric acid that 6000kg concentration is 102% in reactor, slowly throw at 35 DEG C
Enter 800kg C.I. Pigment Blue 15, be warming up to 80 DEG C with the speed of 3～5 DEG C/min, be incubated 2.5h, sequentially add the C14 alkane of 6t water, 230kg
Base trimethyl ammonium chloride, the C20 Dialkyl dimethyl ammonium chloride of 65kg, are warming up to 55 DEG C, insulation, when mensuration absorbance is 0.5
Reach sulfonation terminal, open recirculated cooling water and be less than 80 DEG C with controlling reaction temperature, be then slowly added into 8 times of water dilutions,
Terminate after 35min, filter pressing, water washing is peacock blue derivative to electrical conductivity≤500 μ s/cm, the filter cake unloading；
3) by step 1) the thick phthalocyanine blue filter cake prepared takes 100 parts in terms of giving money as a gift, procedure of processing 2) phthalein prepared is blue or green derivative
Thing filter cake takes 15 parts in terms of giving money as a gift, and both and 1000 parts of water mix and blends in the lump is warming up to 70 DEG C, adds 6 parts of poly- ten dihydroxies
Base stearic acid (poly- ten dihydroxystearic acids are to add using after 10 times of glacial acetic acid dissolving) stirring, filters, washing, is dried, that is,
?.
Embodiment 3：The preparation of phthalocyanine blue
1) put into anhydrous sodium sulfate 600kg, C.I. Pigment Blue 15 1500kg into the horizontal ball mill of 15000L, grind at 80 DEG C
30 hours, making beating, acid were boiled except ferrum, were flowed back 2h with tetrahydrofuran solvent afterwards, and distillation removes solvent, filter pressing, is washed with water to electricity
Conductance ＜ 300 μ s/cm, the filter cake unloading is thick phthalocyanine blue；
2) under agitation, put into the concentrated sulphuric acid that 6000kg concentration is 105% in reactor, slowly throw at 30 DEG C
Enter 500kg C.I. Pigment Blue 15, be warming up to 70 DEG C with the speed of 3～5 DEG C/min, be incubated 2h, sequentially add the C14 alkyl of 5t water, 290kg
Trimethyl ammonium chloride, the C18 Dialkyl dimethyl ammonium chloride of 55kg, are warming up to 50 DEG C, insulation, and mensuration absorbance is to arrive when 0.5
Reach sulfonation terminal, open recirculated cooling water and be less than 80 DEG C with controlling reaction temperature, be then slowly added into 10 times of water dilutions,
Terminate after 40min, filter pressing, water washing is peacock blue derivative to electrical conductivity≤500 μ s/cm, the filter cake unloading；
3) by step 1) the thick phthalocyanine blue filter cake prepared takes 100 parts in terms of giving money as a gift, procedure of processing 2) phthalein prepared is blue or green derivative
Thing filter cake takes 5 parts in terms of giving money as a gift, and both and 1000 parts of water mix and blends in the lump is warming up to 65 DEG C, adds 2 parts of poly- ten dihydroxy
Stearic acid (poly- ten dihydroxystearic acids are to add using after 10 times of glacial acetic acid dissolving) stirring, filters, washing, is dried, obtains final product.
The product that embodiment 1-3 is prepared grinds respectively makes PU ink, and the PU ink then being provided with client is used
The PU ink standard specimen that phthalocyanine blue is made is detected in the lump, specifically, weighs the bead of 125 grams of diameter 2mm, 90 grams of PU ink
Resin system, 10 grams of phthalocyanine blue powders, it is placed in 200mL vial, Red Devil shaker vibrates 2 hours, makes ink,
Colour atla is made on OPP film, tests glossiness, transparency, tinctorial strength, in addition, testing initial viscosity and 1 with rotating cylinder viscometer
Stability viscosity after week, result shows, grinds the viscous of the composite ink obtaining using the product of embodiments of the invention 1-3 preparation
Degree, glossiness, transparency and tinctorial strength are all more or less the same with the performance of client's standard specimen, shown in table 1 specific as follows.
The performance detection of the PU ink that the different phthalocyanine blue grinding of table 1 is made
Claims (6)
1. a kind of preparation technology of PU ink phthalocyanine blue, its step is as follows：
Take the thick phthalocyanine blue of 1 part of weight of giving money as a gift, add the peacock blue derivative of 0.05～0.15 part of weight of giving money as a gift, then plus 8～12
Part water stirring, is warming up to 60～70 DEG C, adds 0.02～0.06 part of hyper-dispersant stirring, filters, wash, be dried, obtain final product.
2. PU ink phthalocyanine blue according to claim 1 preparation technology it is characterised in that：Described hyper-dispersant is poly-
Ten dihydroxystearic acids, poly- ten dihydroxystearic acids are to add using after 10 times of glacial acetic acid dissolving.
3. PU ink phthalocyanine blue according to claim 2 preparation technology it is characterised in that：The system of described thick phthalocyanine blue
Standby step is as follows：
According to 1～10:5～15 weight puts into anhydrous sodium sulfate and C.I. Pigment Blue 15 than in ball mill, grinds 5 at 50～95 DEG C
～35h, making beating, acid is boiled except ferrum, and afterwards with tetrahydrofuran solvent backflow 2～3h, distillation removes solvent, filter pressing, is washed with water to
Electrical conductivity ＜ 300 μ s/cm, the filter cake unloading is thick phthalocyanine blue.
4. PU ink phthalocyanine blue according to claim 3 preparation technology it is characterised in that：Described peacock blue derivative
Preparation process is as follows：
Under agitation, put into the concentrated sulphuric acid that 480～680 weight portion concentration are 101%～105% in reactor, 30
Slow at～40 DEG C put into 60～80 weight portion C.I. Pigment Blue 15s, be warming up to 70～95 DEG C with the speed of 3～5 DEG C/min, insulation 1.5～
2.5h, sequentially adds 500～1000 weight portion water, 20～30 weight portion C8～C14 alkyl trimethyl ammonium chloride, 55～65 weight
Part C16～C20 Dialkyl dimethyl ammonium chloride, is warming up to 45～55 DEG C, insulation, and mensuration absorbance is to reach sulphur when 0.3～0.5
Change terminal, open recirculated cooling water and be less than 80 DEG C with controlling reaction temperature, be then slowly added into 8～10 times of water and dilute, 30～
Terminate after 40min, filter pressing, water washing is peacock blue derivative to electrical conductivity≤500 μ s/cm, the filter cake unloading.
5. the PU ink phthalocyanine blue according to claim 3 or 4 preparation technology it is characterised in that：The system of thick phthalocyanine blue
During standby, the weight of anhydrous sodium sulfate and C.I. Pigment Blue 15 ratio is for 5～8:10～12, anhydrous sodium sulfate and C.I. Pigment Blue 15 are 70～75
20～25h is ground at DEG C.
6. PU ink phthalocyanine blue according to claim 5 preparation technology it is characterised in that：The preparation of peacock blue derivative
During the weight fraction of each raw material that puts into be：
Concentrated sulphuric acid 500～520, C.I. Pigment Blue 15 65～75, put between C8～C14 alkyl trimethyl ammonium chloride added water 700～
750, C8～C14 alkyl trimethyl ammonium chloride 20～25, C16～C20 Dialkyl dimethyl ammonium chloride 55～65.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201610796211.XA CN106398307A (en) | 2016-08-31 | 2016-08-31 | Preparation process of phthalocyanine blue for PU inkjet printing |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201610796211.XA CN106398307A (en) | 2016-08-31 | 2016-08-31 | Preparation process of phthalocyanine blue for PU inkjet printing |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108864746A (en) * | 2018-06-04 | 2018-11-23 | 宣城亚邦化工有限公司 | A kind of phthalocyanine blue pigment lotion of good dispersion and preparation method thereof |
| CN115785697A (en) * | 2022-10-04 | 2023-03-14 | 青岛大学 | Method for improving low-temperature resistance stability of phthalocyanine blue pigment dispersion liquid |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1182103A (en) * | 1996-10-31 | 1998-05-20 | 巴斯福股份公司 | Preparation of sulfo-containing copper phthalcyanine |
| CN102702782A (en) * | 2012-05-25 | 2012-10-03 | 宣城亚邦化工有限公司 | Synthesis method of pigment blue |
| CN105001706A (en) * | 2015-07-03 | 2015-10-28 | 宣城亚邦化工有限公司 | Special phthalocyanine blue pigment for UV printing ink and manufacturing method of special phthalocyanine blue pigment |
-
2016
- 2016-08-31 CN CN201610796211.XA patent/CN106398307A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1182103A (en) * | 1996-10-31 | 1998-05-20 | 巴斯福股份公司 | Preparation of sulfo-containing copper phthalcyanine |
| CN102702782A (en) * | 2012-05-25 | 2012-10-03 | 宣城亚邦化工有限公司 | Synthesis method of pigment blue |
| CN105001706A (en) * | 2015-07-03 | 2015-10-28 | 宣城亚邦化工有限公司 | Special phthalocyanine blue pigment for UV printing ink and manufacturing method of special phthalocyanine blue pigment |
Non-Patent Citations (1)
| Title |
|---|
| 郑少琴: "有机颜料酞菁蓝的合成与颜料化", 《染料与染色》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108864746A (en) * | 2018-06-04 | 2018-11-23 | 宣城亚邦化工有限公司 | A kind of phthalocyanine blue pigment lotion of good dispersion and preparation method thereof |
| CN115785697A (en) * | 2022-10-04 | 2023-03-14 | 青岛大学 | Method for improving low-temperature resistance stability of phthalocyanine blue pigment dispersion liquid |
| CN115785697B (en) * | 2022-10-04 | 2023-10-17 | 青岛大学 | Method for improving low temperature resistance stability of phthalocyanine blue pigment dispersion liquid |
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Application publication date: 20170215 |
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