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Preparation method of fluorescent invisible ink based on hydroxyapatite nanocrystalline

A hydroxyapatite and invisible ink technology, applied in inks, household appliances, applications, etc., can solve the problems of unsatisfactory preparation cost, biocompatibility angle, few fluorescent hydroxyapatite nanocrystals, etc. The effect of implementation, good dispersion, and easy availability

Inactive Publication Date: 2019-03-29
HUBEI UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Since hydroxyapatite itself is non-fluorescent, currently it is mainly realized by replacing it with expensive rare earth elements europium or terbium, which is not satisfactory in terms of preparation cost or biocompatibility.
[0006] So far, there are very few cases of fluorescent hydroxyapatite nanocrystals that do not rely on rare earth doping, especially the hydroxyapatite fluorescent ink that can be applied to inkjet printing has not been reported

Method used

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  • Preparation method of fluorescent invisible ink based on hydroxyapatite nanocrystalline
  • Preparation method of fluorescent invisible ink based on hydroxyapatite nanocrystalline
  • Preparation method of fluorescent invisible ink based on hydroxyapatite nanocrystalline

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] 1) 0.01 mol of calcium chloride was dissolved in 10 grams of deionized water to form solution A;

[0036] 2) 0.015mol sodium citrate and 0.007mol arginine were dissolved in 10 grams of deionized water to form solution B;

[0037] 3) 0.006mol disodium hydrogen phosphate is dissolved in 15 grams of deionized water to form solution C;

[0038] 4) Add solution B obtained in step 2) dropwise to solution A obtained in step 1) at room temperature, and fully stir for 15 min to form mixed solution 1;

[0039] 5) adding solution C obtained in step 3) dropwise to mixed solution 1 obtained in step 4) at room temperature, and fully stirring for 15 min to form mixed solution 2;

[0040] 6) Transfer the obtained mixed solution 2 of step 5) into a closed hydrothermal reactor, react at 190° C. for 3 hours, and then naturally cool to room temperature to obtain a reaction solution;

[0041] 7) The reaction solution obtained in step 6) is centrifuged with a high-speed centrifuge to obtai...

Embodiment 2

[0045] Embodiment 2: with embodiment 1, the difference is,

[0046] 1) 0.01 mol of calcium nitrate was dissolved in 10 grams of deionized water to form solution A;

[0047] 2) dissolve 0.003mol potassium citrate and 0.001mol norleucine in 10 grams of deionized water to form solution B;

[0048] 3) 0.006mol potassium phosphate is dissolved in 15 grams of deionized water to form solution C;

[0049] 6) Transfer the obtained mixed solution 2 of step 5) into a closed hydrothermal reactor, react at 120° C. for 12 hours, and naturally cool to room temperature to obtain a reaction solution;

[0050]7) Use a high-speed centrifuge to centrifuge the reaction solution in step 6) to obtain a precipitate. The precipitate is alternately centrifuged and washed three times with deionized water and absolute ethanol to remove excess electrolyte in the system, and then redispersed in deionized water. The particle mass concentration of the dispersion liquid is 0.1 wt%, and the pH of the dispers...

Embodiment 3

[0051] Embodiment 3, with embodiment 1, difference is,

[0052] 2) 0.006mol sodium citrate and 0.003mol arginine were dissolved in 10 grams of deionized water to form solution B;

[0053] 3) Dissolve 0.006 mol of dipotassium hydrogen phosphate in 15 grams of deionized water to form solution C;

[0054] 6) Transfer the mixed solution 2 obtained in step 5) to a closed hydrothermal reactor, react at 150° C. for 9 hours, and then naturally cool to room temperature to obtain a reaction solution;

[0055] 7) Use a high-speed centrifuge to centrifuge the reaction solution obtained in step 6) to obtain a precipitate. The precipitate is alternately centrifuged and washed three times with deionized water and absolute ethanol to remove excess electrolyte in the system, and then redispersed in deionized water , adjusting the particle mass concentration of the dispersion to 5 wt%, and adjusting the pH of the dispersion to 8.5 with 0.1M sodium hydroxide solution to obtain the hydroxyapatit...

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Abstract

The invention relates to a preparation method of fluorescent invisible ink based on hydroxyapatite nanocrystalline. The method comprises the following steps: dissolving soluble calcium salt in deionized water to form a solution A; dissolving soluble citrate and amino acid in deionized water to form a solution B; dissolving soluble phosphate in deionized water to form a solution C; dropwise addingthe solution B into the solution A, and stirring to form a mixed solution I; dropwise adding the solution C into the mixed solution I, and stirring to form a mixed solution II; performing a heating reaction on the mixed solution II, cooling and then performing centrifugal separation, and performing centrifugal washing alternately on precipitate with deionized water and absolute ethanol, and dispersing in the deionized water again to obtain water-soluble hydroxyapatite fluorescent nanocrystalline dispersion liquid; and adjusting the mass fraction and pH value of the water-soluble hydroxyapatitefluorescent nanocrystalline particles in the dispersion liquid to obtain the fluorescent invisible ink. The preparation method involved in the invention is rich in raw material sources and simple insynthetic process; a product is colorless under natural light; and the fluorescent invisible ink emits visible light under ultraviolet light, and is suitable for writing, inkjet printing, seal mint-mark and the like.

Description

technical field [0001] The invention relates to the field of colorless fluorescent invisible ink, in particular to a preparation method of an ultraviolet fluorescent invisible ink based on hydroxyapatite nanoparticles. Background technique [0002] Anti-counterfeiting ink is an ink for printing invisible anti-counterfeiting marks, text, images and other contents for the needs of product anti-counterfeiting and important document anti-counterfeiting. Fluorescent invisible ink has the characteristics of simple implementation process, low cost, good concealment, strong reproducibility, and easy detection. [0003] At present, there are certain research results on fluorescent invisible inks in China, but organic fluorescent dyes or organic rare-earth metal fluorescent complexes are mostly used as fluorescent luminescent agents, which have certain toxicity, low environmental protection index, and adverse effects on human body. However, domestic research on fluorescent inks suita...

Claims

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Application Information

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IPC IPC(8): C09D11/50
CPCC09D11/50
Inventor 谭军军程诚方雅俊王金桃刘洋熊焰
Owner HUBEI UNIV OF TECH
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