CN1283727C - Organic dye/silicon carrier compound pigment and preparing method thereof - Google Patents
Organic dye/silicon carrier compound pigment and preparing method thereof Download PDFInfo
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- CN1283727C CN1283727C CN 200310107589 CN200310107589A CN1283727C CN 1283727 C CN1283727 C CN 1283727C CN 200310107589 CN200310107589 CN 200310107589 CN 200310107589 A CN200310107589 A CN 200310107589A CN 1283727 C CN1283727 C CN 1283727C
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- organic dye
- dyestuff
- silicon carrier
- basic
- pigment
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Abstract
The present invention relates to an organic dye/silicon carrier compound pigment and a preparing method thereof. The organic dye/silicon carrier compound pigment of the present invention is composed of a silicon carrier and an organic dye colorant as an object, wherein the silicon carrier is amorphous silica or amorphous aluminosilicate, and the organic dye is a basic dye or a cationic dye, and the weight percentage content of the organic dye is from 5% to 10%. The compound pigment has the advantages of bright color and homogeneous granularity, and the organic dye in the compound pigment has the advantages of high adhesion, difficult color deterioration and high water resistance. The organic dye/silicon carrier compound pigment of the present invention has the advantages of simple used devices, sufficient synthesis conditions, easy raw material obtainment and low cost, and the organic dye/silicon carrier compound pigment can widely used for various plastics, elastomers, coatings and related fields as a dye pigment.
Description
Technical field
The present invention relates to the preparation of pigment, particularly a kind of organic dye/silicon carrier composite pigment and preparation method thereof.
Background technology
Pigment at present commonly used is that to adopt organic dye and macromolecule resin be the carrier synthetic a bit, needs to use a large amount of virose solvents in the production process, pollutes greatlyyer, and the manufacturing processed time consumption and energy consumption is big.Contain heavy metal element in some pigment in addition, as cobalt, chromium etc., to the existence of HUMAN HEALTH and environment harm, the product of produced in conventional processes is the mixing of carrier and pigment simultaneously, has shortcomings such as fast light, heat-resisting, poor water resistance, has influenced result of use.Chinese patent CN1328094A discloses a kind of nm-class composite mesoporous organic/Si-base fluorescent pigment and preparation method thereof, this method is improved aspect a lot, but still have following some shortcomings: used silicon source is a tetraethoxy in the preparation process, simultaneously must use tensio-active agent to prepare MCM-41 mesoporous silicon oxide inorganic carrier, cost of material is somewhat expensive, and preparation condition is comparatively harsh, complicated.
Summary of the invention
The purpose of this invention is to provide a kind of organic dye/silicon carrier composite pigment and preparation method thereof, can overcome the shortcoming of prior art, synthesis device of the present invention is simple, and is easy to operate, and condition is loose, the energy is saved in less contamination, and raw material is simple and easy to, and is with low cost.And because organic dye is embedded in the hole of inorganic carrier in the pigment for preparing, so product color is even, machinery and thermostability height, water-tolerant.
Pigment of the present invention is to be inorganic carrier (silicon carrier) with soft silica or amorphous aluminosilicate, the composite pigment that organic dye is composited for the organic colorant object, wherein the organic dye weight percentage is 5-10%, the inorganic carrier weight percentage is 90-95%, and described organic dye is basic dyestuff or cationic dyestuff.Described amorphous aluminosilicate is a sodium silicoaluminate, wherein, and SiO
2: Al
2O
3=5～20: 0～1.
Described basic dyestuff is alkaline bright yellow O (C
17H
22N
3Cl), 2 basic orange 2 (C
12H
13N
4Cl), Basic Violet 5BN (C
25H
30N
3Cl), basic rhodamine (C
23H
31N
2O
3Cl), magenta (C
20H
10N
3Cl.4H
2Or alkali green (C O),
23H
25N
2Cl).Described cationic dyestuff is cationic red GTL (C
20H
28N
5O
6Cl), the emerald green blue X-GB (C of positively charged ion
20H
26N
3OCl
3).
The preparation method of organic dye of the present invention/silicon carrier composite pigment comprises the steps:
With water glass is the silicon source, and Tai-Ace S 150 is the aluminium source, and organic dye cationic dyestuff or basic dyestuff are tinting material.Reactant is according to mole proportioning Na
2O: SiO
2: Al
2O
3: organic dye: H
2O=3: 5～20: 0～1: 0.2～1.5: 1100 mix.Stirred 15-60 minute under the room temperature, the stainless steel still of packing into sealing, 80～120 degrees centigrade were heated 2～4 days.Take out product, use ethanol, the distilled water repetitive scrubbing is with the dyestuff of removal surface attachment, suction filtration, and target compound is finally made in 80～100 ℃ of oven dry.
Composite pigment of the present invention is bright and lustrous, epigranular, and organic dye adhesive ability wherein is strong, and is difficult for fading water-tolerant.Synthesis device of the present invention is simple, and is easy to operate, and condition is loose, the energy is saved in less contamination, and raw material is simple and easy to, and is with low cost.And because organic dye is embedded in the hole of inorganic carrier in the pigment for preparing, so product color is even, machinery and thermostability height can be used as dyeing pigment and are widely used in all types of plastic, elastomerics, coating and association area after grinding.
Embodiment
Embodiment 1:
Take by weighing 0.6g cationic red GTL (0.0024mol) and be dissolved in 8ml H
2O adds 0.2N alum liquor 10ml, water glass (SiO successively
2: 2.8836N, Na
2O:0.8587N) after 7ml, mixture evenly stir 30 minutes, the stainless steel still of packing into sealing, 100 ℃ were heated four days.Take out, suction filtration, the dyestuff of removing surface adhesion with ethanol, distilled water repetitive scrubbing is colourless to washings, 100 ℃ of oven dry.The gained composite pigment is a garnet.
Embodiment 2:
Take by weighing the bright blue X-GB of 1.5g positively charged ion (0.003mol) and be dissolved in 8ml H
2O adds 0.2N alum liquor 10ml, water glass (SiO successively
2: 2.8836N, Na
2O:0.8587N) after 7ml, mixture evenly stir 30 minutes, the stainless steel still of packing into sealing, 80 ℃ were heated four days.Take out, suction filtration, the dyestuff of removing surface adhesion with ethanol, distilled water repetitive scrubbing is colourless to washings, 80 ℃ of oven dry.The gained composite pigment is sky blue.
Embodiment 3:
Take by weighing 0.1g 2 basic orange 2 (0.0004mol) and be dissolved in 8ml H
2O adds 0.2N alum liquor 10ml, water glass (SiO successively
2: 2.8836N, Na
2O:0.8587N) after 7ml, mixture evenly stir 30 minutes, the stainless steel still of packing into sealing, 95 ℃ were heated three days.Take out, suction filtration, the dyestuff of removing surface adhesion with ethanol, distilled water repetitive scrubbing is colourless to washings, 90 ℃ of oven dry.The gained composite pigment is a light orange.
Embodiment 4:
Take by weighing 0.1g 2 basic orange 2 (0.0004mol) and be dissolved in 8ml H
2O, water glass (SiO
2: 2.8836N, Na
2O:0.8587N) after 7ml, mixture evenly stir 30 minutes, the stainless steel still of packing into sealing, 100 ℃ were heated four days.Take out, suction filtration, the dyestuff of removing surface adhesion with ethanol, distilled water repetitive scrubbing is colourless to washings, 90 ℃ of oven dry.The gained composite pigment is a bright orange.
Embodiment 5:
Take by weighing 0.1g Basic Violet 5BN (0.00025mol) and be dissolved in 8ml H
2O adds water glass (SiO successively
2: 2.8836N, Na
2O:0.8587N) after 7ml, mixture evenly stir 30 minutes, the stainless steel still of packing into sealing, 100 ℃ were heated three days.Take out, suction filtration, the dyestuff of removing surface adhesion with ethanol, distilled water repetitive scrubbing is colourless to washings, 100 ℃ of oven dry.The gained composite pigment is the brilliant violet look.
Embodiment 6:
Take by weighing 0.1g alkalescence purple (0.00025mol) and be dissolved in 8ml H
2O adds 0.2N alum liquor 10ml, water glass (SiO successively
2: 2.8836N, Na
2O:0.8587N) after 7ml, mixture evenly stir 30 minutes, the stainless steel still of packing into sealing, 120 ℃ were heated three days.Take out, suction filtration, the dyestuff of removing surface adhesion with ethanol, distilled water repetitive scrubbing is colourless to washings, 100 ℃ of oven dry.The gained composite pigment is a lavender.
Embodiment 7:
Take by weighing 0.2g magenta (0.0005mol) and be dissolved in 8ml H
2O adds 0.2N alum liquor 10ml, water glass (SiO successively
2: 2.8836N, Na
2O:0.8587N) after 7ml, mixture evenly stir 30 minutes, the stainless steel still of packing into sealing, 100 ℃ were heated four days.Take out, suction filtration, the dyestuff of removing surface adhesion with ethanol, distilled water repetitive scrubbing is colourless to washings, 100 ℃ of oven dry.The gained composite pigment is a garnet.
Embodiment 8:
Take by weighing 0.2g magenta (0.0005mol) and be dissolved in 8ml H
2O adds water glass (SiO successively
2: 2.8836N, Na
2O:0.8587N) after 7ml, mixture evenly stir 30 minutes, the stainless steel still of packing into sealing, 100 ℃ were heated four days.Take out, suction filtration, the dyestuff of removing surface adhesion with ethanol, distilled water repetitive scrubbing is colourless to washings, 100 ℃ of oven dry.The gained composite pigment is a bright red.
Embodiment 9:
Take by weighing 0.2g alkalescent light green (0.00054mol) and be dissolved in 8ml H
2O adds water glass (SiO successively
2: 2.8836N, Na
2O:0.8587N) after 7ml, mixture evenly stir 30 minutes, the stainless steel still of packing into sealing, 100 ℃ were heated four days.Take out, suction filtration, the dyestuff of removing surface adhesion with ethanol, distilled water repetitive scrubbing is colourless to washings, 100 ℃ of oven dry.The gained composite pigment is blackish green.
Embodiment 10:
Take by weighing 0.2g alkalescent light green (0.00054mol) and be dissolved in 8ml H
2O adds 0.2N alum liquor 10ml, water glass (SiO successively
2: 2.8836N, Na
2O:0.8587N) after 7ml, mixture evenly stir 30 minutes, the stainless steel still of packing into sealing, 95 ℃ were heated three days.Take out, suction filtration, the dyestuff of removing surface adhesion with ethanol, distilled water repetitive scrubbing is colourless to washings, 100 ℃ of oven dry.The gained composite pigment is a light green.
Claims (3)
1, a kind of organic dye/silicon carrier composite pigment, it is to be made of inorganic carrier and organic dye coloring agent object; Wherein the organic dye weight percentage is 5-10%, and the inorganic carrier weight percentage is 90-95%; It is characterized in that described inorganic carrier is soft silica or amorphous aluminosilicate; Described organic dye is basic dyestuff or cationic dyestuff;
Described basic dyestuff is alkaline bright yellow O, 2 basic orange 2, Basic Violet 5BN, basic rhodamine, magenta, alkali green, or their mixture;
Described cationic dyestuff is cationic red GTL, the emerald green blue X-GB of positively charged ion or their mixture.
2, according to the described organic dye of claim 1/silicon carrier composite pigment, it is characterized in that described amorphous aluminosilicate is a sodium silicoaluminate, wherein, SiO
2: Al
2O
3=5～20: 1.
3, a kind of method for preparing the described organic dye of claim 1/silicon carrier composite pigment is characterized in that it comprises the steps:
1) press metering with reactant feed water glass or water glass and Tai-Ace S 150, organic dye cationic dyestuff or basic dyestuff, water mixes, and stirs 15-60 minute under the room temperature;
2) pack into and seal in the stainless steel still, 80～120 degrees centigrade of heating 2～4 days;
3) take out product, use ethanol, the distilled water repetitive scrubbing is with the dyestuff of removal surface attachment, suction filtration, and 80～100 ℃ of oven dry get final product;
Described water glass is that the mole proportioning of the reactant of raw material is: Na
2O: SiO
2: organic dye: H
2O=3: 5～20: 0.2～1.5: 1100;
Described water glass and Tai-Ace S 150 are that the mole proportioning of the reactant of raw material is: Na
2O: SiO
2: Al
2O
3: organic dye: H
2O=3: 5～20: 1: 0.2～1.5: 1100.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200310107589 CN1283727C (en) | 2003-12-18 | 2003-12-18 | Organic dye/silicon carrier compound pigment and preparing method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200310107589 CN1283727C (en) | 2003-12-18 | 2003-12-18 | Organic dye/silicon carrier compound pigment and preparing method thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1552770A CN1552770A (en) | 2004-12-08 |
| CN1283727C true CN1283727C (en) | 2006-11-08 |
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ID=34334399
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 200310107589 Expired - Fee Related CN1283727C (en) | 2003-12-18 | 2003-12-18 | Organic dye/silicon carrier compound pigment and preparing method thereof |
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Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103756361B (en) * | 2014-01-20 | 2015-05-13 | 山西大学 | Silicon-based modified fadable pigment and preparation method thereof |
| CN110541314A (en) * | 2018-05-28 | 2019-12-06 | 句容市华冠服帽厂 | Carrier for attaching dye |
| CN109096820A (en) * | 2018-07-18 | 2018-12-28 | 辽宁鸿港化工有限公司 | A kind of Organic-inorganic composite pigment and preparation method thereof |
| CN111019406B (en) * | 2019-12-16 | 2021-06-15 | 安徽大学 | Method for coloring aluminum pigment by utilizing mercapto coordination |
| CN114316945B (en) * | 2021-12-14 | 2024-03-26 | 华南师范大学 | Luminescent material and preparation method and application thereof |
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2003
- 2003-12-18 CN CN 200310107589 patent/CN1283727C/en not_active Expired - Fee Related
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| Publication number | Publication date |
|---|---|
| CN1552770A (en) | 2004-12-08 |
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