CN111286233A - Preparation method of fluorescent pigment gel - Google Patents
Preparation method of fluorescent pigment gel Download PDFInfo
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- CN111286233A CN111286233A CN202010048937.1A CN202010048937A CN111286233A CN 111286233 A CN111286233 A CN 111286233A CN 202010048937 A CN202010048937 A CN 202010048937A CN 111286233 A CN111286233 A CN 111286233A
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- gel
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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
- 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
- C09D17/00—Pigment pastes, e.g. for mixing in paints
- C09D17/003—Pigment pastes, e.g. for mixing in paints containing an organic pigment
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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
- C09B67/0001—Post-treatment of organic pigments or dyes
- C09B67/0004—Coated particulate pigments or dyes
- C09B67/0008—Coated particulate pigments or dyes with organic coatings
- C09B67/0013—Coated particulate pigments or dyes with organic coatings with polymeric coatings
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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
- 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
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Abstract
The invention relates to the technical field of fluorescent pigment preparation, and discloses a gel preparation method of a fluorescent pigment, which comprises the following steps: (1) mixing and grinding inorganic silicate and fluorescent dye to obtain mixed powder; (2) adding sodium alginate into water, stirring until the sodium alginate is completely dissolved, adding the mixed powder, and uniformly stirring to obtain mixed slurry; (3) adding anhydrous calcium chloride into the mixed slurry, and uniformly stirring to obtain a gel intermediate; (4) and adding sodium carbonate into the gel intermediate, uniformly stirring, precipitating, washing the obtained product until no color floating exists, and drying to obtain the fluorescent pigment. According to the invention, the sodium alginate gel is used for adsorbing fluorescent dye molecules, and the gel layer is converted into the inorganic salt protective layer, so that the fluorescent pigment is not easy to bleed, has good acid and alkali resistance, and is more stable.
Description
Technical Field
The invention relates to the technical field of fluorescent pigment preparation, in particular to a gel preparation method of a fluorescent pigment.
Background
After absorbing visible light and ultraviolet light, the fluorescent pigment can convert the original ultraviolet light which can not be felt by human eyes into visible light with a certain color, and the visible light is superposed with light reflected conventionally, so that the total reflected light intensity is higher than that of common pigments, and a very bright color is formed. These fluorescent pigments themselves often have inherent deficiencies in light resistance, solvent resistance, etc. and are therefore generally fused to the framework of polymeric materials by chemical or physical means and further processed into pigments.
At present, the domestic environment-friendly fluorescent liquid pigment is generally produced by adopting an emulsion polymerization method, for example, the publication No. CN103555069A of 'a preparation method of water-based fluorescent pigment color paste' disclosed in Chinese patent documents comprises the steps of preparation of a dispersion system, preparation of a pre-emulsion, reaction and reaction by adding an oxidation reduction initiation system to obtain the water-based fluorescent pigment color paste.
However, the fluorescent pigment prepared by the emulsion polymerization method has strong hydrophilicity on the surface of a polymer in the printing and dyeing and coating application processes, the resin and the dye in the polymer are mutually attracted by limited van der Waals force, and the dye in the polymer is easily dissolved in water or other media, so that the performance of the product is influenced, such as problems of soaping, temperature resistance, bleeding and the like, and a large amount of waste water is also generated to cause water pollution.
Disclosure of Invention
The invention provides a preparation method of fluorescent pigment gel, aiming at overcoming the problems that the surface of a polymer of the fluorescent pigment prepared by an emulsion polymerization method in the prior art has strong hydrophilicity in the printing and dyeing and coating application processes, and the dye in the polymer is easy to dissolve in water or other media, thereby affecting the performance of a product and easily causing color bleeding.
In order to achieve the purpose, the invention adopts the following technical scheme:
a preparation method of fluorescent pigment gel is characterized by comprising the following steps:
(1) mixing and grinding inorganic silicate and fluorescent dye to obtain mixed powder;
(2) adding sodium alginate into water, stirring until the sodium alginate is completely dissolved, adding the mixed powder, and uniformly stirring to obtain mixed slurry;
(3) adding anhydrous calcium chloride into the mixed slurry, and uniformly stirring to obtain a gel intermediate;
(4) and adding sodium carbonate into the gel intermediate, uniformly stirring, precipitating, washing the obtained product until no color floating exists, and drying to obtain the fluorescent pigment.
Preferably, the inorganic silicate in the step (1) is one or more of smectite, illite and feldspar.
Preferably, the fluorescent dye described in step (1) is a commercial rhodamine or solvent-based dye.
Preferably, the fluorescent dye is added in the step (1) in an amount of 0.1 to 5wt% based on the inorganic silicate.
Preferably, the mass ratio of the sodium alginate to the mixed powder in the step (2) is 1: (2-6.5).
Preferably, the dissolving temperature of the sodium alginate in the step (2) is 40-80 ℃, and the stirring time is 1-5 h.
Preferably, the mass ratio of the anhydrous calcium chloride to the sodium alginate added in the step (3) is 1: (0.5-2.5).
Preferably, the mass ratio of the sodium carbonate to the anhydrous calcium chloride added in the step (4) is 1: (1.1-1.3).
The invention adsorbs fluorescent dye molecules through environment-friendly sodium alginate gel, has stronger adsorption force, and fixes the dye molecules in a gel network; and then the gel layer is converted into an inorganic salt protective layer, so that on one hand, dye molecules are further coated, and on the other hand, the inorganic salt protective layer can enable the fluorescent pigment to have good acid and alkali resistance and to be more stable.
The sodium alginate is prepared from (1,4) - β -D-mannuronic acid (M) and (1,4) - α -LTwo monomers of guluronic acid (G) are unbranched block copolymers composed of glycosidic linkages, the chain structures of these two uronic acids are very similar and only differ from the positions of the hydroxyl groups thereon, but the spatial structure of the chain formed by further polymerization after ring formation is very different, thus determining the difference in their physicochemical properties. When the two monomers are connected in different ways, three different fragments can be formed: a polymannuronic acid block (MM), a polyguluronic acid block (GG), and a mannuronic acid-guluronic acid block (MG). When sodium alginate is mixed with Ca containing divalent cation2+When the solution is contacted, divalent cations occupy the hydrophilic spaces, a plurality of oxygen atoms carried by carboxyl and hydroxyl on GG polyguluronic acid blocks in the sodium alginate attract the divalent cations mutually, the generated chelation enables the molecular chains to be tightly combined, the synergistic effect is enhanced, the divalent cations and G blocks form an 'eg-box' structure, and finally, hydrogel with a three-dimensional network structure is formed, wherein calcium chloride serves as a calcium source and serves as a cross-linking agent. After the hydrogel is formed, sodium carbonate is added, calcium ions attract carbonate ions to generate nano amorphous calcium carbonate in situ, and the amorphous nano calcium carbonate ions are connected by the gel to form an inorganic salt coating layer.
Therefore, the beneficial effects of the invention are as follows: fluorescent dye molecules are adsorbed by sodium alginate gel, and the gel layer is converted into an inorganic salt protective layer, so that the fluorescent pigment is not easy to bleed, has good acid and alkali resistance, and is more stable.
Drawings
FIG. 1 is a diagram of the fluorescent pigment prepared in example 1 of the present invention under natural light source and ultraviolet light source (natural light source on the left, ultraviolet light source on the right).
FIG. 2 shows the dye adsorption rates at different initial dye concentrations.
Fig. 3 is a graph of the fluorescence intensity of example 1 and comparative example 1 treated for 12h at pH 5.
Detailed Description
The invention is further described with reference to the following detailed description and accompanying drawings.
Example 1:
a preparation method of a fluorescent pigment gel comprises the following steps:
(1) mixing and grinding 50g of smectite and 0.2g of rhodamine B to obtain mixed powder;
(2) dissolving 10g of sodium alginate in 200mL of 50 ℃ warm water, stirring at a high speed until no blocky aggregate exists in the liquid, adding the mixed powder into the slurry, and continuously stirring uniformly for 2h to obtain mixed slurry;
(3) adding 5.5g of anhydrous calcium chloride into the mixed slurry while stirring, so that gel floc rapidly appears in the slurry, and continuously stirring until the floc disappears to form uniform gel to obtain a gel intermediate;
(4) and adding 5g of sodium carbonate into the gel intermediate, changing the color of the solution, stirring until the color is uniform and unchanged, precipitating, washing the obtained product until no floating color exists, centrifugally drying, and grinding into powder to obtain the fluorescent pigment.
Example 2:
a preparation method of a fluorescent pigment gel comprises the following steps:
(1) mixing and grinding 50g of kaolinite and 0.5g of solvent yellow 172 to obtain mixed powder;
(2) dissolving 20g of sodium alginate in 200mL of 50 ℃ warm water, stirring at a high speed until no blocky aggregate exists in the liquid, adding the mixed powder into the slurry, and continuously stirring uniformly for 1h to obtain mixed slurry;
(3) adding 11g of anhydrous calcium chloride into the mixed slurry while stirring, so that gel floccules rapidly appear in the slurry, and continuously stirring until the floccules disappear to form uniform gel to obtain a gel intermediate;
(4) and adding 10g of sodium carbonate into the gel intermediate, changing the color of the solution, stirring until the color is uniform and unchanged, precipitating, washing the obtained product until no floating color exists, centrifugally drying, and grinding into powder to obtain the fluorescent pigment.
Example 3:
a preparation method of a fluorescent pigment gel comprises the following steps:
(1) mixing and grinding 15G of soapstone, 35G of montmorillonite and 0.15G of rhodamine 6G to obtain mixed powder;
(2) dissolving 25g of sodium alginate in 350mL of 40 ℃ warm water, stirring at a high speed until no blocky aggregate exists in the liquid, adding the mixed powder into the slurry, and continuously stirring uniformly for 1h to obtain mixed slurry;
(3) adding 6.5g of anhydrous calcium chloride into the mixed slurry while stirring, so that gel floc rapidly appears in the slurry, and continuously stirring until the floc disappears to form uniform gel to obtain a gel intermediate;
(4) and adding 6g of sodium carbonate into the gel intermediate, changing the color of the solution, stirring until the color is uniform and unchanged, precipitating, washing the obtained product until no floating color exists, centrifugally drying, and grinding into powder to obtain the fluorescent pigment.
Example 4:
a preparation method of a fluorescent pigment gel comprises the following steps:
(1) mixing and grinding 50g of smectite and 2.5g of rhodamine B to obtain mixed powder;
(2) dissolving 10g of sodium alginate in 200mL of 80 ℃ warm water, stirring at a high speed until no blocky aggregate exists in the liquid, adding the mixed powder into the slurry, and continuously stirring uniformly for 1h to obtain mixed slurry;
(3) adding 5.5g of anhydrous calcium chloride into the mixed slurry while stirring, so that gel floc rapidly appears in the slurry, and continuously stirring until the floc disappears to form uniform gel to obtain a gel intermediate;
(4) and adding 5g of sodium carbonate into the gel intermediate, changing the color of the solution, stirring until the color is uniform and unchanged, precipitating, washing the obtained product until no floating color exists, centrifugally drying, and grinding into powder to obtain the fluorescent pigment.
Example 5:
a preparation method of a fluorescent pigment gel comprises the following steps:
(1) mixing and grinding 25G of soapstone, 25G of montmorillonite and 0.15G of rhodamine 6G to obtain mixed powder;
(2) dissolving 25g of sodium alginate in 350mL of 50 ℃ warm water, stirring at a high speed until no blocky aggregate exists in the liquid, adding the mixed powder into the slurry, and continuously stirring uniformly for 5 hours to obtain mixed slurry;
(3) adding 62.5g of anhydrous calcium chloride into the mixed slurry while stirring, so that gel floc rapidly appears in the slurry, and continuously stirring until the floc disappears to form uniform gel to obtain a gel intermediate;
(4) and adding 60g of sodium carbonate into the gel intermediate, changing the color of the solution, stirring until the color is uniform and unchanged, precipitating, washing the obtained product until no floating color exists, centrifugally drying, and grinding into powder to obtain the fluorescent pigment.
Example 6:
a preparation method of a fluorescent pigment gel comprises the following steps:
(1) mixing and grinding 50g of kaolinite and 0.5g of solvent yellow 172 to obtain mixed powder;
(2) dissolving 0.8g of sodium alginate in 500mL of 50 ℃ warm water, stirring at a high speed until no blocky aggregate exists in the liquid, adding the mixed powder into the slurry, and continuously stirring uniformly for 3h to obtain mixed slurry;
(3) adding 1.6g of anhydrous calcium chloride into the mixed slurry while stirring, so that gel floc rapidly appears in the slurry, and continuously stirring until the floc disappears to form uniform gel to obtain a gel intermediate;
(4) and adding 1.5g of sodium carbonate into the gel intermediate, changing the color of the solution, stirring until the color is uniform and unchanged, precipitating, washing the obtained product until no floating color exists, centrifugally drying, and grinding into powder to obtain the fluorescent pigment.
Example 7:
example 7 differs from example 6 in that the mass of solvent yellow 172 was 1.5g, the mass of sodium alginate was 1.32g, and the rest was the same as in example 6.
Example 8:
example 8 differs from example 6 in that the fluorescent dye in example 6 is 2.38g of rhodamine B, and the rest is the same as in example 6.
Comparative example 1:
solvent yellow 172 fluorescent pigment is commercially available.
The adsorption rate (adsorption time 6 hours) of the dye in the above examples was measured, and the results are shown in table 1 and fig. 2.
Table 1: the adsorption rate of the dye.
| Example 1 | Example 2 | Example 3 | Example 4 | Example 5 | Example 6 | Example 7 | Example 8 | |
| Dye adsorption Rate (%) | 88.3％ | 93.1％ | 90.5％ | 90.3％ | 95.6％ | 94.2％ | 89.9％ | 92％ |
As can be seen from Table 1 and FIG. 2, the fluorescent pigment prepared by the method of the present invention has good adsorption property to the dye, and the lower the initial concentration of the dye is, the higher the adsorption rate is. The reason is that the higher the initial concentration of the dye is, the more easily an aggregation phenomenon occurs, and the aggregates after aggregation are less likely to enter between layers because they are sterically hindered and are less likely to dissociate.
The change in fluorescence intensity of the commercially available fluorescent pigments of example 1 and comparative example 1 after 12 hours of treatment at pH 5 was measured and the results are shown in fig. 3. As can be seen from FIG. 3, the acid and alkali resistance of the fluorescent pigment prepared by the method of the present invention is significantly improved compared to the conventional fluorescent pigment.
Claims (8)
1. A preparation method of fluorescent pigment gel is characterized by comprising the following steps:
(1) mixing and grinding inorganic silicate and fluorescent dye to obtain mixed powder;
(2) adding sodium alginate into water, stirring until the sodium alginate is completely dissolved, adding the mixed powder, and uniformly stirring to obtain mixed slurry;
(3) adding anhydrous calcium chloride into the mixed slurry, and uniformly stirring to obtain a gel intermediate;
(4) and adding sodium carbonate into the gel intermediate, uniformly stirring, precipitating, washing the obtained product until no color floating exists, and drying to obtain the fluorescent pigment.
2. The method for preparing a fluorescent pigment gel according to claim 1, wherein the inorganic silicate in the step (1) is one or more of smectite, illite and feldspar.
3. The method for preparing a fluorescent pigment gel as set forth in claim 1, wherein the fluorescent dye in the step (1) is a commercial rhodamine or solvent type dye.
4. The method for preparing a fluorescent pigment gel as claimed in claim 1, 2 or 3, wherein the fluorescent dye is added in an amount of 0.1 to 5wt% based on the inorganic silicate in the step (1).
5. The method for preparing fluorescent pigment gel as claimed in claim 1, wherein the mass ratio of the sodium alginate to the mixed powder in the step (2) is 1: (2-6.5).
6. The method for preparing fluorescent pigment gel according to claim 1 or 5, wherein the dissolving temperature of the sodium alginate in the step (2) is 40-80 ℃, and the stirring time is 1-5 h.
7. The method for preparing fluorescent pigment gel according to claim 1, wherein the mass ratio of the anhydrous calcium chloride to the sodium alginate added in the step (3) is 1: (0.5-2.5).
8. The method for preparing fluorescent pigment gel according to claim 1, wherein the mass ratio of the sodium carbonate to the anhydrous calcium chloride added in the step (4) is 1: (1.1-1.3).
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112159623A (en) * | 2020-09-28 | 2021-01-01 | 成都玉龙化工有限公司 | High-temperature-resistant coating and preparation method thereof |
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| CN104666250A (en) * | 2015-03-06 | 2015-06-03 | 华南农业大学 | Preparation method of chlortetracycline sustained-release microspheres |
| CN107998462A (en) * | 2017-11-10 | 2018-05-08 | 西安交通大学医学院第附属医院 | A kind of magnetic gel, its preparation and its application system for being used for mucous membrane under endoscope and peeling off operation |
| CN109894096A (en) * | 2019-04-03 | 2019-06-18 | 深圳市清研环境科技有限公司 | Adsorb the microballoon and preparation method thereof of dyestuff composite hydrogel |
| CN110499665A (en) * | 2019-08-13 | 2019-11-26 | 湖南省南盾防伪技术实业有限公司 | Calcium carbonate wraps up DNA- fluorescent dye composite Nano gel Double anti-counterfeit preparation method for coating |
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- 2020-01-16 CN CN202010048937.1A patent/CN111286233A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104666250A (en) * | 2015-03-06 | 2015-06-03 | 华南农业大学 | Preparation method of chlortetracycline sustained-release microspheres |
| CN107998462A (en) * | 2017-11-10 | 2018-05-08 | 西安交通大学医学院第附属医院 | A kind of magnetic gel, its preparation and its application system for being used for mucous membrane under endoscope and peeling off operation |
| CN109894096A (en) * | 2019-04-03 | 2019-06-18 | 深圳市清研环境科技有限公司 | Adsorb the microballoon and preparation method thereof of dyestuff composite hydrogel |
| CN110499665A (en) * | 2019-08-13 | 2019-11-26 | 湖南省南盾防伪技术实业有限公司 | Calcium carbonate wraps up DNA- fluorescent dye composite Nano gel Double anti-counterfeit preparation method for coating |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112159623A (en) * | 2020-09-28 | 2021-01-01 | 成都玉龙化工有限公司 | High-temperature-resistant coating and preparation method thereof |
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