CN114316622A - High-light-resistance anti-yellowing fluorescent whitening agent and preparation method thereof - Google Patents

High-light-resistance anti-yellowing fluorescent whitening agent and preparation method thereof Download PDF

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CN114316622A
CN114316622A CN202111560156.1A CN202111560156A CN114316622A CN 114316622 A CN114316622 A CN 114316622A CN 202111560156 A CN202111560156 A CN 202111560156A CN 114316622 A CN114316622 A CN 114316622A
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acid
whitening agent
yellowing
stirring
fluorescent whitening
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葛仁华
张凌
杨成凤
王云龙
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Jiangsu Glory Chemical Co ltd
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Jiangsu Glory Chemical Co ltd
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Abstract

The invention discloses a high-light-resistance anti-yellowing fluorescent whitening agent, which consists of the following raw materials in percentage by mass: 70-80% of deionized water, 3-6% of diethylenetriamine, 4-6% of cyanuric chloride, 0.6-0.8% of aniline, 1-3% of inorganic base, 5-8% of hydrochloric acid, 0.5-0.8% of emulsifier, 3-5% of organic acid, 3-5% of inorganic acid, 1-3% of corn modified starch and 1-3% of polyvinyl alcohol, wherein the processing technology comprises the following steps: preparing a solution, preparing a mixed solution, preparing an emulsion, carrying out acid precipitation treatment, and obtaining a whitening agent; the processing technology adopted by the invention is raw materials specified by national standards, the high-light-resistance anti-yellowing fluorescent whitening agent prepared by the invention is greatly improved, chemical components such as corn modified starch, polyvinyl alcohol and the like are added into the whitening agent, the whitening agent is mixed and produced according to a certain proportion, and the reaction time and the reaction temperature are strictly controlled, so that the light resistance and the yellowing resistance of the whitening agent can be greatly improved, and the fluorescent whitening agent has the characteristics of no toxicity and environmental protection in the using process.

Description

High-light-resistance anti-yellowing fluorescent whitening agent and preparation method thereof
Technical Field
The invention relates to the technical field of composite fabric processing, in particular to a high-light-resistance anti-yellowing fluorescent whitening agent and a preparation method thereof.
Background
Whitening agents are a class of organic compounds that enhance the whiteness of fabrics and paper and the like. Also known as optical brighteners and fluorescent brighteners. Fabrics and the like are often yellow due to colored impurities, and in the past, chemical bleaching methods are used for decolorization, and whitening agents are added into products.
The whitening agent on the market at present is easy to be decomposed by the change of temperature in the using process, thereby affecting the normal use, has poor light resistance, and is easy to generate the phenomenon of yellowing after long-term use. Based on the above statement, the invention provides a fluorescent whitening agent with high light resistance and yellowing resistance and a preparation method thereof.
Disclosure of Invention
The invention aims to provide a fluorescent whitening agent with high light resistance and yellowing resistance and a preparation method thereof, so as to solve the problems in the background technology.
In order to achieve the purpose, the invention provides the following technical scheme: a fluorescent whitening agent with high light resistance and yellowing resistance is composed of the following raw materials in percentage by mass: 70-80% of deionized water, 3-6% of diethylenetriamine, 4-6% of cyanuric chloride, 0.6-0.8% of aniline, 1-3% of inorganic base, 5-8% of hydrochloric acid, 0.5-0.8% of emulsifier, 3-5% of organic acid, 3-5% of inorganic acid, 1-3% of corn modified starch and 1-3% of polyvinyl alcohol.
Preferably, the organic acid is a monocarboxylic acid, a dicarboxylic acid or a tricarboxylic acid having 1 to 12 carbon atoms.
Preferably, the inorganic acid is carbonic acid, phosphoric acid, sulfuric acid, hydrochloric acid or nitric acid.
Preferably, the inorganic base is one or more of sodium hydroxide, sodium carbonate, sodium bicarbonate and potassium hydroxide.
Preferably, the emulsifier is one of nonylphenol polyoxyethylene ether, octylphenol polyoxyethylene ether and polyoxyethylene fatty alcohol ether.
Preferably, the inorganic base is caustic soda, potassium hydroxide, calcium hydroxide, aluminum hydroxide, magnesium hydroxide, copper hydroxide, ferric hydroxide and the like.
A method for preparing the fluorescent whitening agent with high light resistance and yellowing resistance, which comprises the following steps:
s1: preparing a solution, namely adding diethylenetriamine and distilled water into a four-neck flask provided with a reflux condenser pipe, a thermometer and a stirrer for mixing, heating the four-neck flask to 50-70 ℃ and carrying out corresponding stirring, adding an adipic acid solution after stirring, continuing stirring, heating and stirring for reaction after automatic heat release is finished, and continuing adding distilled water after the reaction temperature is reduced to obtain a self-made polyamide solution for later use;
s2: preparing a mixed solution, namely adding diaminostilbene disulfonic acid and cyanuric chloride into the solution I obtained in the step S1 in sequence, heating, raising the temperature, uniformly stirring, controlling the temperature, adding organic acid and inorganic acid to control the pH value of the reaction solution to be 7-9, heating, raising the temperature, adding a proper amount of aniline, continuously heating, standing for 2-3 hours after the reaction is finished to obtain a mixed solution I for later use;
s3: preparing emulsion, namely mixing the corn modified starch and the polyvinyl alcohol according to the proportion of 4:3, adding a proper amount of emulsifier after stirring and mixing, then stirring at a high speed for 15-25 minutes, and putting the obtained mixture into an emulsifying bottle for later use;
s4: acid precipitation, namely mixing the mixed solution obtained in the step S3 with the mixed solution obtained in the step S2, adding 400 ml of deionized water after mixing, stirring, and adding a proper amount of hydrochloric acid after stirring for acid precipitation;
s5: and (4) obtaining a whitening agent, namely adding inorganic base into the mixed solution obtained in the step S4 for neutralization reaction, after the reaction is finished, drying the mixed solution in a dryer for 60 minutes, and after the drying, crushing the dried mixed solution in a crusher to enable the materials to become powder, thus obtaining the required high-light-resistance anti-yellowing fluorescent whitening agent.
Compared with the prior art, the invention has the beneficial effects that: the processing technology adopted by the invention is raw materials specified by national standards, the high-light-resistance anti-yellowing fluorescent whitening agent prepared by the invention is greatly improved, chemical components such as corn modified starch, polyvinyl alcohol and the like are added into the whitening agent, the whitening agent is mixed and produced according to a certain proportion, and the reaction time and the reaction temperature are strictly controlled, so that the light resistance and the yellowing resistance of the whitening agent can be greatly improved, and the fluorescent whitening agent has the characteristics of no toxicity and environmental protection in the using process.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example one
The invention provides a technical scheme that: a fluorescent whitening agent with high light resistance and yellowing resistance is composed of the following raw materials in percentage by mass: 70-80% of deionized water, 3-6% of diethylenetriamine, 4-6% of cyanuric chloride, 0.6-0.8% of aniline, 1-3% of inorganic base, 5-8% of hydrochloric acid, 0.5-0.8% of emulsifier, 3-5% of organic acid, 3-5% of inorganic acid, 1-3% of corn modified starch and 1-3% of polyvinyl alcohol.
A method for preparing the fluorescent whitening agent with high light resistance and yellowing resistance, which comprises the following steps:
s1: preparing a solution, namely adding diethylenetriamine and distilled water into a four-neck flask provided with a reflux condenser pipe, a thermometer and a stirrer for mixing, heating the four-neck flask to 50 ℃ and carrying out corresponding stirring, adding an adipic acid solution after stirring, continuing stirring, heating and stirring for reaction after automatic heat release is finished, and continuing adding distilled water after the reaction temperature is reduced to obtain a self-made polyamide solution for later use;
s2: preparing a mixed solution, namely adding diaminostilbene disulfonic acid and cyanuric chloride into the solution I obtained in the step S1 in sequence, heating, raising the temperature, uniformly stirring, controlling the temperature, adding organic acid and inorganic acid to control the pH value of the reaction solution to be 7-9, heating, raising the temperature, adding a proper amount of aniline, continuously heating, standing for 2 hours after the reaction is finished to obtain a mixed solution I for later use;
s3: preparing emulsion, namely mixing the corn modified starch and the polyvinyl alcohol according to the proportion of 4:3, adding a proper amount of emulsifier after stirring and mixing, then stirring at a high speed for 15 minutes, and putting the obtained mixture into an emulsion bottle for later use;
s4: acid precipitation, namely mixing the mixed solution obtained in the step S3 with the mixed solution obtained in the step S2, adding 400 ml of deionized water after mixing, stirring, and adding a proper amount of hydrochloric acid after stirring for acid precipitation;
s5: and (4) obtaining a whitening agent, namely adding inorganic base into the mixed solution obtained in the step S4 for neutralization reaction, after the reaction is finished, drying the mixed solution in a dryer for 60 minutes, and after the drying, crushing the dried mixed solution in a crusher to enable the materials to become powder, thus obtaining the required high-light-resistance anti-yellowing fluorescent whitening agent.
Example two
The invention provides a technical scheme that: a fluorescent whitening agent with high light resistance and yellowing resistance is composed of the following raw materials in percentage by mass: 70-80% of deionized water, 3-6% of diethylenetriamine, 4-6% of cyanuric chloride, 0.6-0.8% of aniline, 1-3% of inorganic base, 5-8% of hydrochloric acid, 0.5-0.8% of emulsifier, 3-5% of organic acid, 3-5% of inorganic acid, 1-3% of corn modified starch and 1-3% of polyvinyl alcohol.
A method for preparing the fluorescent whitening agent with high light resistance and yellowing resistance, which comprises the following steps:
s1: preparing a solution, namely adding diethylenetriamine and distilled water into a four-neck flask provided with a reflux condenser pipe, a thermometer and a stirrer for mixing, heating the four-neck flask to 60 ℃ and carrying out corresponding stirring, adding an adipic acid solution after stirring, continuing stirring, heating and stirring for reaction after automatic heat release is finished, and continuing adding distilled water after the reaction temperature is reduced to obtain a self-made polyamide solution for later use;
s2: preparing a mixed solution, namely adding diaminostilbene disulfonic acid and cyanuric chloride into the solution I obtained in the step S1 in sequence, heating, raising the temperature, uniformly stirring, controlling the temperature, adding organic acid and inorganic acid to control the pH value of the reaction solution to be 7-9, heating, raising the temperature, adding a proper amount of aniline, continuously heating, standing for 2 hours after the reaction is finished to obtain a mixed solution I for later use;
s3: preparing emulsion, namely mixing the corn modified starch and the polyvinyl alcohol according to the proportion of 4:3, adding a proper amount of emulsifier after stirring and mixing, then stirring at a high speed for 20 minutes, and putting the obtained mixture into an emulsion bottle for later use;
s4: acid precipitation, namely mixing the mixed solution obtained in the step S3 with the mixed solution obtained in the step S2, adding 400 ml of deionized water after mixing, stirring, and adding a proper amount of hydrochloric acid after stirring for acid precipitation;
s5: and (4) obtaining a whitening agent, namely adding inorganic base into the mixed solution obtained in the step S4 for neutralization reaction, after the reaction is finished, drying the mixed solution in a dryer for 60 minutes, and after the drying, crushing the dried mixed solution in a crusher to enable the materials to become powder, thus obtaining the required high-light-resistance anti-yellowing fluorescent whitening agent.
EXAMPLE III
The invention provides a technical scheme that: a fluorescent whitening agent with high light resistance and yellowing resistance is composed of the following raw materials in percentage by mass: 70-80% of deionized water, 3-6% of diethylenetriamine, 4-6% of cyanuric chloride, 0.6-0.8% of aniline, 1-3% of inorganic base, 5-8% of hydrochloric acid, 0.5-0.8% of emulsifier, 3-5% of organic acid, 3-5% of inorganic acid, 1-3% of corn modified starch and 1-3% of polyvinyl alcohol.
A method for preparing the fluorescent whitening agent with high light resistance and yellowing resistance, which comprises the following steps:
s1: preparing a solution, namely adding diethylenetriamine and distilled water into a four-neck flask provided with a reflux condenser pipe, a thermometer and a stirrer for mixing, heating the four-neck flask to 70 ℃ and carrying out corresponding stirring, adding an adipic acid solution after stirring, continuing stirring, heating and stirring for reaction after automatic heat release is finished, and continuing adding distilled water after the reaction temperature is reduced to obtain a self-made polyamide solution for later use;
s2: preparing a mixed solution, namely adding diaminostilbene disulfonic acid and cyanuric chloride into the solution I obtained in the step S1 in sequence, heating, raising the temperature, uniformly stirring, controlling the temperature, adding organic acid and inorganic acid to control the pH value of the reaction solution to be 7-9, heating, raising the temperature, adding a proper amount of aniline, continuously heating, standing for 2 hours after the reaction is finished to obtain a mixed solution I for later use;
s3: preparing emulsion, namely mixing the corn modified starch and the polyvinyl alcohol according to the proportion of 4:3, adding a proper amount of emulsifier after stirring and mixing, then stirring at a high speed for 20 minutes, and putting the obtained mixture into an emulsion bottle for later use;
s4: acid precipitation, namely mixing the mixed solution obtained in the step S3 with the mixed solution obtained in the step S2, adding 400 ml of deionized water after mixing, stirring, and adding a proper amount of hydrochloric acid after stirring for acid precipitation;
s5: and (4) obtaining a whitening agent, namely adding inorganic base into the mixed solution obtained in the step S4 for neutralization reaction, after the reaction is finished, drying the mixed solution in a dryer for 60 minutes, and after the drying, crushing the dried mixed solution in a crusher to enable the materials to become powder, thus obtaining the required high-light-resistance anti-yellowing fluorescent whitening agent.
By performing component detection on three groups of examples, the detection results are as follows:
Figure BDA0003420420150000061
from the experimental data in the above table, it can be seen that in the present embodiment, when the heating temperature of the four-neck flask is 50 ℃ and the stirring time of the emulsion is 15 minutes, the light-resistant effect and the anti-yellowing effect are general, when the heating temperature of the four-neck flask is 60 ℃ and the stirring time of the emulsion is 20 minutes, the light-resistant effect and the anti-yellowing effect are good, and when the heating temperature of the four-neck flask is 70 ℃ and the stirring time of the emulsion is 25 minutes, the light-resistant effect and the anti-yellowing effect are good, so that when the heating temperature of the four-neck flask is higher and the stirring time of the emulsion is longer, the light-resistant effect and the anti-yellowing effect are better.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.

Claims (7)

1. A high light-resistant anti-yellowing fluorescent whitening agent is characterized in that; the composite material consists of the following raw materials in percentage by mass: 70-80% of deionized water, 3-6% of diethylenetriamine, 4-6% of cyanuric chloride, 0.6-0.8% of aniline, 1-3% of inorganic base, 5-8% of hydrochloric acid, 0.5-0.8% of emulsifier, 3-5% of organic acid, 3-5% of inorganic acid, 1-3% of corn modified starch and 1-3% of polyvinyl alcohol.
2. A high light resistance anti-yellowing fluorescent whitening agent according to claim 1, characterized in that: the organic acid is a monocarboxylic acid, a dicarboxylic acid or a tricarboxylic acid having 1-12 carbon atoms.
3. A high light resistance anti-yellowing fluorescent whitening agent according to claim 1, characterized in that: the inorganic acid is carbonic acid, phosphoric acid, sulfuric acid, hydrochloric acid or nitric acid and the like.
4. A high light resistance anti-yellowing fluorescent whitening agent according to claim 1, characterized in that: the inorganic alkali is one or a mixture of sodium hydroxide, sodium carbonate, sodium bicarbonate and potassium hydroxide.
5. A high light resistance anti-yellowing fluorescent whitening agent according to claim 1, characterized in that: the emulsifier is one of nonylphenol polyoxyethylene ether, octylphenol polyoxyethylene ether and polyoxyethylene fatty alcohol ether.
6. A high light resistance anti-yellowing fluorescent whitening agent according to claim 5, characterized in that: the inorganic alkali is similar alkali such as caustic soda, potassium hydroxide, calcium hydroxide, aluminum hydroxide, magnesium hydroxide, copper hydroxide, ferric hydroxide and the like.
7. A process for the preparation of a highly light-fast and anti-yellowing fluorescent whitening agent according to any of claims 1 to 6, characterized in that: the preparation method comprises the following steps:
s1: preparing a solution, namely adding diethylenetriamine and distilled water into a four-neck flask provided with a reflux condenser pipe, a thermometer and a stirrer for mixing, heating the four-neck flask to 50-70 ℃ and carrying out corresponding stirring, adding an adipic acid solution after stirring, continuing stirring, heating and stirring for reaction after automatic heat release is finished, and continuing adding distilled water after the reaction temperature is reduced to obtain a self-made polyamide solution for later use;
s2: preparing a mixed solution, namely adding diaminostilbene disulfonic acid and cyanuric chloride into the solution I obtained in the step S1 in sequence, heating, raising the temperature, uniformly stirring, controlling the temperature, adding organic acid and inorganic acid to control the pH value of the reaction solution to be 7-9, heating, raising the temperature, adding a proper amount of aniline, continuously heating, standing for 2-3 hours after the reaction is finished to obtain a mixed solution I for later use;
s3: preparing emulsion, namely mixing the corn modified starch and the polyvinyl alcohol according to the proportion of 4:3, adding a proper amount of emulsifier after stirring and mixing, then stirring at a high speed for 15-25 minutes, and putting the obtained mixture into an emulsifying bottle for later use;
s4: acid precipitation, namely mixing the mixed solution obtained in the step S3 with the mixed solution obtained in the step S2, adding 400 ml of deionized water after mixing, stirring, and adding a proper amount of hydrochloric acid after stirring for acid precipitation;
s5: and (4) obtaining a whitening agent, namely adding inorganic base into the mixed solution obtained in the step S4 for neutralization reaction, after the reaction is finished, drying the mixed solution in a dryer for 60 minutes, and after the drying, crushing the dried mixed solution in a crusher to enable the materials to become powder, thus obtaining the required high-light-resistance anti-yellowing fluorescent whitening agent.
CN202111560156.1A 2021-12-20 2021-12-20 High-light-resistance anti-yellowing fluorescent whitening agent and preparation method thereof Pending CN114316622A (en)

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Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107674670A (en) * 2017-10-16 2018-02-09 王若梅 A kind of preparation method of the high fluorescent whitening agent of resistance to light type
CN111349349A (en) * 2020-04-13 2020-06-30 南京旭美化工有限公司 High-light-resistance fluorescent whitening agent and preparation method thereof

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107674670A (en) * 2017-10-16 2018-02-09 王若梅 A kind of preparation method of the high fluorescent whitening agent of resistance to light type
CN111349349A (en) * 2020-04-13 2020-06-30 南京旭美化工有限公司 High-light-resistance fluorescent whitening agent and preparation method thereof

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Application publication date: 20220412