CN105885039A - Preparation method of high-performance daylight type fluorescent pigment for powder coating - Google Patents
Preparation method of high-performance daylight type fluorescent pigment for powder coating Download PDFInfo
- Publication number
- CN105885039A CN105885039A CN201610421619.9A CN201610421619A CN105885039A CN 105885039 A CN105885039 A CN 105885039A CN 201610421619 A CN201610421619 A CN 201610421619A CN 105885039 A CN105885039 A CN 105885039A
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- CN
- China
- Prior art keywords
- preparation
- acid
- polyamine
- polyalcohol
- fluorescent pigment
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- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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Classifications
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G69/00—Macromolecular compounds obtained by reactions forming a carboxylic amide link in the main chain of the macromolecule
- C08G69/44—Polyester-amides
-
- 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
- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/03—Powdery paints
- C09D5/033—Powdery paints characterised by the additives
- C09D5/035—Coloring agents, e.g. 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
- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/22—Luminous paints
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/06—Luminescent, e.g. electroluminescent, chemiluminescent materials containing organic luminescent materials
Abstract
The invention relates to a preparation method of a high-performance daylight type fluorescent pigment for a powder coating. The preparation method comprises the following steps that 1, polyamine and polyatomic alcohol are put into a reaction kettle and stirred, and the temperature is slowly increased; 2, an antioxidant and a catalyst are added; 3, polyatomic acid is added in twice, the temperature is increased, and reacting under heat preservation is conducted; 4, fluorescent dye is added, stirring is conducted at high speed, and the materials are discharged and cooled; 5, cooled materials are subjected to coarse crushing and airflow crushing, and then the high-performance daylight type fluorescent pigment is obtained. According to the preparation method, polyamine, polyatomic alcohol and polyatomic acid react with one another to generate polyester-polyamide copolymer resin, the properties of the polyester-polyamide copolymer resin are controlled by controlling the varieties and the adding proportion of the raw materials, the high-performance daylight type fluorescent pigment which is high in fluorescence intensity and good in high-temperature-resistant roasting property and is used for powder coating is prepared by replacing single polyester resin in existing products with the polyester-polyamide copolymer resin to serve as carrier resin of the fluorescent pigment, and therefore the various properties of the existing fluorescent pigment for the powder coating are improved.
Description
Technical field
The present invention relates to the preparation method of a kind of high-performance sunlight-type fluorescent pigment used for powder coating, be specifically related to a kind of powder
The coating preparation method of high-performance sunlight-type fluorescent pigment.
Background technology
Sunlight-type fluorescent pigment is mainly made up of vector resin, fluorescent dye and auxiliary agent, and wherein vector resin contributes to fluorescence
Dyestuff color development, protection fluorescent dye, beneficially product are better dispersed in the effect of downstream product system.
The vector resin of the sunlight-type fluorescent pigment being presently used for powdery paints mainly has two kinds:
A kind of is the polyester resin of small-molecular-weight, and this resinoid is good with the affinity of powder paint substrate, and product fluorescence is good,
But, this series products in use exists clearly disadvantageous:
(1) heat resistance of product is the best, it is impossible to meet the requirement of long-time high-temperature baking.The temperature tolerance of product can only
Reach about 190 DEG C, and can not be the most high temperature resistant.But the baking condition of powdery paints requires to reach 200 DEG C, 15min,
Existing product uses with this understanding, colour-darkening, and fluorescence is deteriorated.
(2) softening point of product is on the low side, causes powder coating product easily to lump in storage process, and mobility is bad, on
Powder rate is on the low side, easily produces powder ball, unstable product quality.
Another kind is heat cured melamine resinoid, and temperature tolerance and the softening point of this series products are the most no problem, but, by
Containing formaldehyde in product, have formaldehyde gas to release when high-temperature baking, severe contamination production environment, to Workshop Production personnel
Healthy the most unfavorable, use and be very limited.
Therefore, the preparation method of high-performance sunlight-type fluorescent pigment used for powder coating exists further to improve and optimize needs
Asking, this is also one of the study hotspot in this technical field and emphasis, the present invention is accomplished especially power and starting point
Place.
Summary of the invention
For the above-mentioned technical problem overcoming prior art to exist, the present inventor after having carried out substantial amounts of further investigation,
Thus complete the present invention.
The present invention is achieved through the following technical solutions, in particular to a kind of high-performance daylight type fluorescence used for powder coating
The preparation method of pigment, comprises the steps:
Step one, puts in reactor by polyamine, polyalcohol, opens stirring, slowly heat up；
Step 2, adds antioxidant, catalyst；
Step 3, adds polyacid at twice, heats up, and insulation is reacted；
Step 4, adds fluorescent dye, high-speed stirred, and quickly discharging cools down；
Step 5, carries out coarse crushing and air-flow crushing by the material after cooling, to obtain final product.
Preferably, described polyamine, described polyalcohol, the weight ratio of described polyacid be 15～42 10～30 25～
45；More preferably 25～40 20～30 30～40；Can be such as 23.9 28.6 41.5 or 34.6 20.5
38.9 or 41.5 19.7 32.8.
Preferably, described polyamine is hexamethylene diamine, aniline, m-xylene diamine, isophorone diamine, cyclohexylamine, second two
At least one in amine, monoethanolamine, diethanol amine.
Preferably, described polyalcohol be ethanol, ethylene glycol, glycerine, trimethylolpropane, pentaerythrite, new penta 2
At least one in alcohol, phenmethylol.
Preferably, described polyacid be hexanedioic acid, benzoic acid, phthalic acid, M-phthalic acid, terephthalic acid (TPA),
At least one in phthalic anhydride, trimellitic anhydride, trimesic acid.
Preferably, the weight of described antioxidant is 1:94 with described polyamine, polyalcohol, the ratio of polyacid three's gross weight,
Described antioxidant is at least one in antioxidant 1010, irgasfos 168, antioxidant 546, triphenyl phosphite.
Preferably, the weight of described catalyst is 1:94 with described polyamine, polyalcohol, the ratio of polyacid three's gross weight,
Described catalyst is at least one in sulfuric acid, phosphoric acid, hydrochloric acid, butyl tin dilaurate.
Preferably, the weight of described fluorescent dye with described polyamine, polyalcohol, the ratio of polyacid three's gross weight is
4:94。
Preferably, in step one, slowly it is warmed up to 160 DEG C；In step 3, it is warmed up to 250 DEG C, is incubated at 250 DEG C
React 20 minutes；In step 4, high-speed stirred 5 minutes.
Compared with prior art, beneficial effects of the present invention is as follows: the present invention utilizes polyamine, polyalcohol anti-with polyacid
Polyester-polyamide copolymer resins should be generated, and control polyester-polyamide by controlling raw-material kind and adding proportion
The performance of copolymer resins, replaces in existing product using single polyester resin as fluorescence with this polyester-polyamide copolymer resins
The vector resin of pigment, improves the properties of existing fluorescent pigment used for powder coating.First, polyester-polyamide tree
The degree of crystallinity of fat is low, and the transparency is good, and the fluorescence of fluorescent pigment is high；Secondly, the phase of polyester-polyamide resin and dyestuff
Capacitive is good, has more preferable protectiveness to dyestuff, improves the heat-resisting quantity of fluorescent pigment；Again, polyester-polyamide tree
The softening point of fat is high, does not results in powdery paints and produces agglomeration problems in storage process；It addition, polyester-polyamide tree
Fat is good with the compatibility of base-material in powdery paints, and the gloss of powder coating product is high, and levelling is good.The present invention is by carrier
The modification of resin, has not only prepared the fluorescent pigment that fluorescence is high, and has improved the temperature of fluorescent pigment used for powder coating
The degree scope of application, improves the phenomenon of the product caking in use run into.
Detailed description of the invention
Below in conjunction with specific embodiment, the present invention is described in detail.Following example will assist in those skilled in the art
Member is further appreciated by the present invention, but limits the present invention the most in any form.It should be pointed out that, the common skill to this area
For art personnel, without departing from the inventive concept of the premise, it is also possible to make some deformation and improvement.These broadly fall into
Protection scope of the present invention.
Embodiment 1
The present embodiment relates to the preparation method of a kind of sunlight-type fluorescent pigment used for powder coating, comprises the steps of:
Step one, puts in reactor by polyamine, polyalcohol, opens stirring, be slowly warmed up to 160 DEG C；
Step 2, adds antioxidant, catalyst；
Step 3, adds polyacid at twice, is warmed up to 250 DEG C, and at 250 DEG C, insulation carries out reacting 20 minutes；
Step 4, adds fluorescent dye, high-speed stirred 5 minutes, and quickly discharging cools down；
Step 5, carries out coarse crushing and air-flow crushing by the material after cooling, to obtain final product.
Embodiment 2
The present embodiment relates to a kind of preparation method being molded and using sunlight-type fluorescent pigment, comprises the steps of:
Step one, puts in reactor by polyamine, polyalcohol, opens stirring, be slowly warmed up to 160 DEG C；
Step 2, adds antioxidant, catalyst；
Step 3, adds polyacid at twice, is warmed up to 250 DEG C, and at 250 DEG C, insulation carries out reacting 20 minutes；
Step 4, adds fluorescent dye, high-speed stirred 5 minutes, and quickly discharging cools down；
Step 5, carries out coarse crushing and air-flow crushing by the material after cooling, to obtain final product.
Embodiment 3
The present embodiment relates to a kind of preparation method being molded and using sunlight-type fluorescent pigment, comprises the steps of:
Step one, puts in reactor by polyamine, polyalcohol, opens stirring, be slowly warmed up to 160 DEG C；
Step 2, adds antioxidant, catalyst；
Step 3, adds polyacid at twice, is warmed up to 250 DEG C, and at 250 DEG C, insulation carries out reacting 20 minutes；
Step 4, adds fluorescent dye, high-speed stirred 5 minutes, and quickly discharging cools down；
Step 5, carries out coarse crushing and air-flow crushing by the material after cooling, to obtain final product.
Comparative example 1
This comparative example relates to the preparation method of a kind of sunlight-type fluorescent pigment used for powder coating, comprises the steps of:
Step one, puts in reactor by polyamine, polyalcohol, opens stirring, be slowly warmed up to 160 DEG C；
Step 2, adds antioxidant, catalyst；
Step 3, adds polyacid at twice, is warmed up to 250 DEG C, and at 250 DEG C, insulation carries out reacting 20 minutes；
Step 4, adds fluorescent dye, high-speed stirred 5 minutes, and quickly discharging cools down；
Step 5, carries out coarse crushing and air-flow crushing by the material after cooling, to obtain final product.
Each embodiment of table 1 and comparative example raw material dosage (unit g)
| Material name | Comparative example 1 | Embodiment 1 | Embodiment 2 | Embodiment 3 |
| Propane diols | / | / | 2 | 7.9 |
| Neopentyl glycol | 13.4 | 20.8 | / | / |
| Glycerine | 12.3 | 2.6 | / | |
| Pentaerythrite | / | 7.8 | 15.9 | 11.8 |
| Terephthalic acid (TPA) | 4.6 | 30.2 | / | / |
| M-phthalic acid | / | / | 30 | 11.6 |
| Benzoic acid | 33.7 | 11.3 | 8.9 | 21.2 |
| Hexamethylene diamine | 20.6 | 30.1 | ||
| Cyclohexylamine | 9.6 | 2.4 | 11.4 | |
| Isophorone diamine | 9.4 | 14.3 | 32.2 | / |
| Catalyst | 1 | 1 | 1 | 1 |
| Antioxidant | 1 | 1 | 1 | 1 |
| Fluorescent dye | 4 | 4 | 4 | 4 |
The testing result of the product of table 2 embodiment and comparative example
| Project name | Comparative example 1 | Embodiment 1 | Embodiment 2 | Embodiment 3 |
| Average grain diameter (D50), um | 12.7 | 11.3 | 11.6 | 13.4 |
| Softening point, DEG C | 102 | 125 | 131 | 130 |
| Aberration (with standard items ratio) | 1.17 | 0.86 | 0.44 | 0.77 |
| Intensity (with standard items ratio), % | 99.53 | 100.21 | 103.43 | 101.62 |
| 105 DEG C of volatile matters, % | 3.25 | 2.37 | 2.72 | 2.66 |
| Oil absorption, gram/100 grams | 60.4 | 61.2 | 61.4 | 62.4 |
| Temperature tolerance (△ E≤3), DEG C | 195 | 235 | 230 | 235 |
Table 3 present invention obtains the main performance index of product
| Project name | Index | Project name | Index |
| Average grain diameter (D50), um | ≤15 | 105 DEG C of volatile matters, % | ≤3 |
| Softening point, DEG C | ≥120 | Oil absorption, gram/100 grams | ≤65 |
| Aberration (with standard items ratio) | △E≤1 | Temperature tolerance (△ E≤3), DEG C | ≥210 |
| Intensity (with standard items ratio), % | 100±5 |
By table 2 and table 3 it can be seen that the softening point of fluorescent pigment product of present invention acquisition, heat resistance significantly improve.
Above the specific embodiment of the present invention is described.It is to be appreciated that the invention is not limited in above-mentioned spy
Determining embodiment, those skilled in the art can make various deformation or amendment within the scope of the claims, this not shadow
Ring the flesh and blood of the present invention.
Claims (10)
1. the preparation method of a high-performance sunlight-type fluorescent pigment used for powder coating, it is characterised in that comprise the steps:
Step one, puts in reactor by polyamine, polyalcohol, opens stirring, slowly heat up；
Step 2, adds antioxidant, catalyst；
Step 3, adds polyacid at twice, heats up, and insulation is reacted；
Step 4, adds fluorescent dye, high-speed stirred, and quickly discharging cools down；
Step 5, carries out coarse crushing and air-flow crushing by the material after cooling, to obtain final product.
2. preparation method as claimed in claim 1, it is characterised in that described polyamine, described polyalcohol, described many
The weight ratio of unit's acid is 15～42 10～30 25～45.
3. preparation method as claimed in claim 2, it is characterised in that described polyamine, described polyalcohol, described many
The weight ratio of unit's acid is 25～40 20～30 30～40.
4. preparation method as claimed in claim 1, it is characterised in that described polyamine is hexamethylene diamine, aniline, isophthalic
At least one in dimethylamine, isophorone diamine, cyclohexylamine, ethylenediamine, monoethanolamine, diethanol amine.
5. preparation method as claimed in claim 1, it is characterised in that described polyalcohol be ethanol, ethylene glycol, the third three
At least one in alcohol, trimethylolpropane, pentaerythrite, neopentyl glycol, phenmethylol.
6. preparation method as claimed in claim 1, it is characterised in that described polyacid is hexanedioic acid, benzoic acid, neighbour
At least one in phthalic acid, M-phthalic acid, terephthalic acid (TPA), phthalic anhydride, trimellitic anhydride, trimesic acid.
7. preparation method as claimed in claim 1, it is characterised in that the weight of described antioxidant and described polyamine,
Polyalcohol, the ratio of polyacid three's gross weight are 1:94, and described antioxidant is antioxidant 1010, irgasfos 168, antioxygen
At least one in agent 546, triphenyl phosphite.
8. preparation method as claimed in claim 1, it is characterised in that the weight of described catalyst and described polyamine,
Polyalcohol, the ratio of polyacid three's gross weight are 1:94, and described catalyst is sulfuric acid, phosphoric acid, hydrochloric acid, tin dilaurate fourth
At least one in base tin.
9. preparation method as claimed in claim 1, it is characterised in that the weight of described fluorescent dye and described polyamine,
Polyalcohol, the ratio of polyacid three's gross weight are 4:94.
10. preparation method as claimed in claim 1, it is characterised in that in step one, be slowly warmed up to 160 DEG C；
In step 3, it is warmed up to 250 DEG C, insulation reaction 20 minutes at 250 DEG C；In step 4, high-speed stirred 5 minutes.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610421619.9A CN105885039A (en) | 2016-06-07 | 2016-06-07 | Preparation method of high-performance daylight type fluorescent pigment for powder coating |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610421619.9A CN105885039A (en) | 2016-06-07 | 2016-06-07 | Preparation method of high-performance daylight type fluorescent pigment for powder coating |
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| CN105885039A true CN105885039A (en) | 2016-08-24 |
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| CN201610421619.9A Pending CN105885039A (en) | 2016-06-07 | 2016-06-07 | Preparation method of high-performance daylight type fluorescent pigment for powder coating |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109054305A (en) * | 2018-08-31 | 2018-12-21 | 湖南博隽生物医药有限公司 | Effective material of a kind of three chambers, two capsule and preparation method thereof |
| CN109251516A (en) * | 2017-07-10 | 2019-01-22 | 合肥杰事杰新材料股份有限公司 | A kind of automobile-used nylon fluorescence interior trim strip material and preparation method thereof |
| CN109705701A (en) * | 2018-12-28 | 2019-05-03 | 安徽神剑新材料股份有限公司 | A kind of preparation method of fluorescent powder coating and preparation method thereof and the polyester resin and fluorescent pigment that use |
| CN110819077A (en) * | 2019-10-28 | 2020-02-21 | 黄山加佳荧光材料有限公司 | Non-stick screw type fluorescent pigment for low-temperature injection molding and preparation method thereof |
| CN111205446A (en) * | 2020-02-28 | 2020-05-29 | 衡阳山泰化工有限公司 | High-temperature-resistant organic amine modified polyester resin and preparation method and application thereof |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4975220A (en) * | 1989-11-09 | 1990-12-04 | Nalco Chemical Company | Polyamide-polyester fluorescent pigments |
| JP2000239376A (en) * | 1999-02-19 | 2000-09-05 | Dainippon Toryo Co Ltd | Production of pigment dispersant for aqueous paint |
| TW200909521A (en) * | 2007-07-27 | 2009-03-01 | Chisso Corp | Composition comprising polyester amide acid and ink-jet composition using the composition |
| CN105062014A (en) * | 2015-08-10 | 2015-11-18 | 黄山加佳荧光材料有限公司 | Daylight fluorescent pigment with dissoluble color concentrate and preparation method of daylight fluorescent pigment |
-
2016
- 2016-06-07 CN CN201610421619.9A patent/CN105885039A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4975220A (en) * | 1989-11-09 | 1990-12-04 | Nalco Chemical Company | Polyamide-polyester fluorescent pigments |
| JP2000239376A (en) * | 1999-02-19 | 2000-09-05 | Dainippon Toryo Co Ltd | Production of pigment dispersant for aqueous paint |
| TW200909521A (en) * | 2007-07-27 | 2009-03-01 | Chisso Corp | Composition comprising polyester amide acid and ink-jet composition using the composition |
| CN105062014A (en) * | 2015-08-10 | 2015-11-18 | 黄山加佳荧光材料有限公司 | Daylight fluorescent pigment with dissoluble color concentrate and preparation method of daylight fluorescent pigment |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109251516A (en) * | 2017-07-10 | 2019-01-22 | 合肥杰事杰新材料股份有限公司 | A kind of automobile-used nylon fluorescence interior trim strip material and preparation method thereof |
| CN109054305A (en) * | 2018-08-31 | 2018-12-21 | 湖南博隽生物医药有限公司 | Effective material of a kind of three chambers, two capsule and preparation method thereof |
| CN109705701A (en) * | 2018-12-28 | 2019-05-03 | 安徽神剑新材料股份有限公司 | A kind of preparation method of fluorescent powder coating and preparation method thereof and the polyester resin and fluorescent pigment that use |
| CN110819077A (en) * | 2019-10-28 | 2020-02-21 | 黄山加佳荧光材料有限公司 | Non-stick screw type fluorescent pigment for low-temperature injection molding and preparation method thereof |
| CN110819077B (en) * | 2019-10-28 | 2022-04-12 | 黄山加佳荧光材料有限公司 | Non-stick screw type fluorescent pigment for low-temperature injection molding and preparation method thereof |
| CN111205446A (en) * | 2020-02-28 | 2020-05-29 | 衡阳山泰化工有限公司 | High-temperature-resistant organic amine modified polyester resin and preparation method and application thereof |
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Application publication date: 20160824 |