Preparation method of quick-dry fluorescent ink

Abstract

The invention discloses a preparation method of quick-dry fluorescent ink, which comprises the following steps: taking a three-neck flask 1 with a mechanical stirring device and a condensing tube, adding phloroglucinol, acetyl ethyl acetate, 1, 4-dioxane and concentrated H2SO4 into the three-neck flask 1, and uniformly mixing; according to the preparation method of the quick-dry fluorescent ink, a fluorescent agent c and modified resin f are mixed, then a modified mixed base material is added, graphene subjected to oxidation treatment and a silver citrate complexing solution are mixed to prepare the modified mixed base material, and the prepared fluorescent ink is sintered to obtain the quick-dry fluorescent ink. The thermal treatment process is optimized, the conductivity of the fluorescent ink can be obviously improved, the ink prepared from the modified mixed base material has good stability, only a small amount of black precipitates appear at the bottom of a bottle after the ink is stored at room temperature for 60 days, the precipitates completely disappear after the ink is stirred again, and the prepared thin film is small in resistivity change and good in stability. The quality of the fluorescent ink is improved.

Description

technical field

[0001] The invention relates to the technical field of fine chemicals, in particular to a method for preparing a quick-drying fluorescent ink. Background technique

[0002] With the rise of digital printing, digital anti-counterfeiting technology is also constantly developing. Fluorescent inkjet ink is currently the most widely used digital anti-counterfeiting technology abroad. It is made by adding corresponding visible fluorescent compounds to inkjet inks. The printed matter can excite fluorescence under the action of ultraviolet rays, and has the characteristics of simple implementation, low cost, good concealment, bright colors, and convenient inspection.

[0003] There are certain defects in the stability of existing fluorescent inks, which lead to a large amount of precipitation of fluorescent inks after storage for a period of time, resulting in the problem of partial failure of fluorescent inks. In order to solve the above problems, those skilled in...

Examples

Embodiment 1

[0029] A method for preparing a quick-drying fluorescent ink, specifically comprising the following steps:

[0030] Step 1, take a three-necked flask 1 with a mechanical stirring device and a condenser tube, add phloroglucinol, acetyl ethyl acetate, 1,4-dioxane and concentrated H in the three-necked flask 1 2 SO 4 Mix evenly, use a mechanical stirring device to continue stirring, and at the same time heat the water bath to 60 ° C, keep warm and reflux for 2 hours, then pour the reaction solution into an ice-water bath for cooling, precipitate crystals, filter with suction, and wash twice with distilled water to obtain substance a , dissolve substance a in 5% NaOH solution by mass fraction and filter, add mass fraction 10% H to the filtrate 2 SO 4 Solution, the filtered precipitate was washed with cold water first, and then recrystallized with ethanol to obtain fluorescent base b, phloroglucinol, acetyl ethyl acetate, 1,4-dioxane and concentrated H 2 SO 4 The consumption ra...

Embodiment 2

[0040] A method for preparing a quick-drying fluorescent ink, specifically comprising the following steps:

[0041] Step 1, take a three-necked flask 1 with a mechanical stirring device and a condenser tube, add phloroglucinol, acetyl ethyl acetate, 1,4-dioxane and concentrated H in the three-necked flask 1 2 SO 4 Mix evenly, use a mechanical stirring device to continuously stir, and at the same time heat the water bath to 75 ° C, keep warm and reflux for 2 hours, then pour the reaction solution into an ice-water bath for cooling, precipitate the crystals, filter with suction, wash with distilled water 3 times, and obtain substance a , dissolve substance a in 5% NaOH solution by mass fraction and filter, add mass fraction 10% H to the filtrate 2 SO 4 solution, the filtered precipitate was washed with cold water, and then recrystallized with ethanol to obtain fluorescent base b, phloroglucinol, acetyl ethyl acetate, 1,4-dioxane and concentrated H 2 SO 4 The consumption rati...

Embodiment 3

[0051] A method for preparing a quick-drying fluorescent ink, specifically comprising the following steps:

[0052] Step 1, take a three-necked flask 1 with a mechanical stirring device and a condenser tube, add phloroglucinol, acetyl ethyl acetate, 1,4-dioxane and concentrated H in the three-necked flask 1 2 SO 4Mix evenly, use a mechanical stirring device to continue stirring, and at the same time heat the water bath to 70 ° C, keep warm and reflux for 2 hours, then pour the reaction solution into an ice-water bath for cooling, precipitate crystals, filter with suction, and wash with distilled water 3 times to obtain substance a , dissolve substance a in 5% NaOH solution by mass fraction and filter, add mass fraction 10% H to the filtrate 2 SO 4 solution, the filtered precipitate was washed with cold water, and then recrystallized with ethanol to obtain fluorescent base b, phloroglucinol, acetyl ethyl acetate, 1,4-dioxane and concentrated H 2 SO 4 The consumption ratio i...

technical field

[0001] The invention relates to the technical field of fine chemicals, in particular to a method for preparing a quick-drying fluorescent ink. Background technique

[0002] With the rise of digital printing, digital anti-counterfeiting technology is also constantly developing. Fluorescent inkjet ink is currently the most widely used digital anti-counterfeiting technology abroad. It is made by adding corresponding visible fluorescent compounds to inkjet inks. The printed matter can excite fluorescence under the action of ultraviolet rays, and has the characteristics of simple implementation, low cost, good concealment, bright colors, and convenient inspection.

[0003] There are certain defects in the stability of existing fluorescent inks, which lead to a large amount of precipitation of fluorescent inks after storage for a period of time, resulting in the problem of partial failure of fluorescent inks. In order to solve the above problems, those skilled in...

Examples

Embodiment 1

[0029] A method for preparing a quick-drying fluorescent ink, specifically comprising the following steps:

[0030] Step 1, take a three-necked flask 1 with a mechanical stirring device and a condenser tube, add phloroglucinol, acetyl ethyl acetate, 1,4-dioxane and concentrated H in the three-necked flask 1 2 SO 4 Mix evenly, use a mechanical stirring device to continue stirring, and at the same time heat the water bath to 60 ° C, keep warm and reflux for 2 hours, then pour the reaction solution into an ice-water bath for cooling, precipitate crystals, filter with suction, and wash twice with distilled water to obtain substance a , dissolve substance a in 5% NaOH solution by mass fraction and filter, add mass fraction 10% H to the filtrate 2 SO 4 Solution, the filtered precipitate was washed with cold water first, and then recrystallized with ethanol to obtain fluorescent base b, phloroglucinol, acetyl ethyl acetate, 1,4-dioxane and concentrated H 2 SO 4 The consumption ra...

Embodiment 2

[0040] A method for preparing a quick-drying fluorescent ink, specifically comprising the following steps:

[0041] Step 1, take a three-necked flask 1 with a mechanical stirring device and a condenser tube, add phloroglucinol, acetyl ethyl acetate, 1,4-dioxane and concentrated H in the three-necked flask 1 2 SO 4 Mix evenly, use a mechanical stirring device to continuously stir, and at the same time heat the water bath to 75 ° C, keep warm and reflux for 2 hours, then pour the reaction solution into an ice-water bath for cooling, precipitate the crystals, filter with suction, wash with distilled water 3 times, and obtain substance a , dissolve substance a in 5% NaOH solution by mass fraction and filter, add mass fraction 10% H to the filtrate 2 SO 4 solution, the filtered precipitate was washed with cold water, and then recrystallized with ethanol to obtain fluorescent base b, phloroglucinol, acetyl ethyl acetate, 1,4-dioxane and concentrated H 2 SO 4 The consumption rati...

Embodiment 3

[0051] A method for preparing a quick-drying fluorescent ink, specifically comprising the following steps:

[0052] Step 1, take a three-necked flask 1 with a mechanical stirring device and a condenser tube, add phloroglucinol, acetyl ethyl acetate, 1,4-dioxane and concentrated H in the three-necked flask 1 2 SO 4Mix evenly, use a mechanical stirring device to continue stirring, and at the same time heat the water bath to 70 ° C, keep warm and reflux for 2 hours, then pour the reaction solution into an ice-water bath for cooling, precipitate crystals, filter with suction, and wash with distilled water 3 times to obtain substance a , dissolve substance a in 5% NaOH solution by mass fraction and filter, add mass fraction 10% H to the filtrate 2 SO 4 solution, the filtered precipitate was washed with cold water, and then recrystallized with ethanol to obtain fluorescent base b, phloroglucinol, acetyl ethyl acetate, 1,4-dioxane and concentrated H 2 SO 4 The consumption ratio i...