CN111349349A - High-light-resistance fluorescent whitening agent and preparation method thereof - Google Patents
High-light-resistance fluorescent whitening agent and preparation method thereof Download PDFInfo
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- 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
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Abstract
The invention discloses a high-light-resistance fluorescent whitening agent and a preparation method thereof, and relates to the technical field of fluorescent whitening agents. The composite material comprises the following raw materials in parts by weight: 70-80 parts of deionized water, 3-6 parts of diethylenetriamine, 5-8 parts of adipic acid, 4-6 parts of cyanuric chloride, 1-3 parts of diaminostilbene disulfonic acid, 1-3 parts of sulfanilic acid, 0.6-0.8 part of aniline, 1-3 parts of inorganic base, 5-8 parts of hydrochloric acid, 0.5-0.8 part of emulsifier, 1-1.2 parts of catalyst and 1-2 parts of 3-phenyl-2-acrylic acid. According to the preparation method of the high-light-resistance fluorescent whitening agent, the catalyst and the emulsifier used in the preparation process are easy to obtain, the temperature in the preparation process is convenient to control, the stability of the fluorescent whitening agent in the use process is favorably ensured by adding diaminostilbene disulfonic acid and sulfanilic acid, and the fluorescent whitening agent has the advantages of very strong light resistance and heat resistance, difficulty in yellowing and good dispersibility, and the faint scent and fragrance of the fluorescent whitening agent in the use process are favorably increased by adding 3-phenyl-2-acrylic acid, so that the fluorescent whitening agent has good market popularization value.
Description
Technical Field
The invention belongs to the technical field of fluorescent whitening agents, relates to a high-light-resistance fluorescent whitening agent, and further relates to a preparation method of the high-light-resistance fluorescent whitening agent.
Background
The brightening agent is an organic compound capable of raising whiteness of fibre fabric and paper, also called optical brightening agent and fluorescent brightening agent, the fabric is often yellow due to containing coloured impurity, and in the past, it is decoloured by adopting chemical bleaching method, and the brightening agent is added into the product, and the fluorescent brightening agent is a fluorescent dye, also called white dye or complex organic compound, and its property is that it can excite incident light to produce fluorescence, so that the dyed material can obtain the flash-light effect similar to fluorite, and the material seen by naked eye is very white, and the fluorescent brightening agent possesses high light quantum yield, and can effectively whiten and brighten the treated substrate, and the fluorescent brightening agent can be extensively used in various fields of paper-making, textile, detergent, plastics, printing ink, leather, UV absorbent, developing agent, ABS, organic glass card, name card and high-grade paper, etc., the market demand is huge.
In the using process of the fluorescent whitening agent in the prior art, the thermal stability is poor, the fluorescent whitening agent is easy to decompose in a high-temperature environment, the light resistance is poor, the using range of the fluorescent whitening agent is reduced, and therefore the application of the fluorescent whitening agent is limited.
Disclosure of Invention
The invention aims to provide a high-light-resistance fluorescent whitening agent to solve the problem of poor thermal stability in the prior art.
The second object of the present invention is to provide a process for the preparation of the above highly light-fast fluorescent whitening agent.
The invention provides the following technical scheme: a high light-resistant fluorescent whitening agent comprises the following raw materials in parts by weight: 70-80 parts of deionized water, 3-6 parts of diethylenetriamine, 5-8 parts of adipic acid, 4-6 parts of cyanuric chloride, 1-3 parts of diaminostilbene disulfonic acid, 1-3 parts of sulfanilic acid, 0.6-0.8 part of aniline, 1-3 parts of inorganic base, 5-8 parts of hydrochloric acid, 0.5-0.8 part of emulsifier, 1-1.2 parts of catalyst and 1-2 parts of 3-phenyl-2-acrylic acid.
A preparation method of a high-light-resistance fluorescent whitening agent comprises the following steps:
s1, preparation of solution I: adding diethylenetriamine and distilled water into a four-neck flask, mixing and stirring at the temperature of 60-70 ℃, then adding an adipic acid solution, stirring, and cooling to obtain a solution I for later use;
s2, preparation of a mixed solution I: sequentially adding diaminostilbene disulfonic acid and cyanuric chloride into the solution I obtained in the step S1, heating and uniformly stirring, and cooling for reaction for 1-2 hours to obtain a mixed solution I for later use;
s3, preparing a mixed solution II: adding sulfanilic acid, aniline, a catalyst and 3-phenyl-2-acrylic acid into the mixed solution in the step S2, heating, raising the temperature, stirring and reacting for 1-1.5h, and uniformly stirring to obtain a mixed solution II for later use;
s4, treatment of the mixed liquid II: adjusting the pH value of the mixed solution II in the step S3 to 8-9, and reacting at the temperature of 20-30 ℃ for 20-30min for later use;
s5, preparation of emulsion: adding an emulsifier into the mixed solution II subjected to cooling treatment in the step S4, stirring at a high speed for 5-10min, and putting the obtained mixture into an emulsifying barrel for later use;
s6, acid precipitation treatment: adding 400-600ml of deionized water into the emulsification barrel in the step S5, and adding hydrochloric acid into the emulsion after high-speed emulsification for acid precipitation treatment;
s7, obtaining of high-light-resistance fluorescent whitening agent: and (5) adding inorganic base into the mixture subjected to acid precipitation in the step S6 for neutralization reaction, drying the mixture in a dryer for 40-60min after the neutralization reaction, and crushing the dried material into powder to obtain the required high-light-resistance fluorescent whitening agent.
Further optimizing the technical scheme, the four-neck flask in the step S1 is a four-neck flask provided with a reflux condenser, a thermometer and a stirrer, and the temperature of the first solution in the step S1 is 30-40 ℃.
Further optimizing the technical scheme, the catalyst in the step S3 is one of stannous octoate and dibutyltin dilaurate.
Further optimizing the technical scheme, the heating temperature in the step S2 is 70-80 ℃, the reaction time in the step S2 is 1.5h, and the cooling temperature in the step S2 is 30-40 ℃.
Further optimizing the technical scheme, the heating temperature in the step S3 is 80-90 ℃, and the reaction time is 1 h.
Further optimizing the technical scheme, the high-speed stirring time in the step S5 is 7min, and the emulsion in the step S6 is acidified to a pH value of 2.0-3.
Further optimizing the technical scheme, the neutralization reaction in the step S7 is carried out until the pH value is 8-8.5, the drying time is 50min, and the powder in the step S7 passes through a screening net with 100 meshes and 120 meshes for screening treatment.
Further optimizing the technical scheme, the emulsifier in the step S5 is one of nonylphenol polyoxyethylene ether, octylphenol polyoxyethylene ether, polyoxyethylene fatty alcohol ether and polyethylene glycol 400.
Further optimizing the technical scheme, the inorganic base in step S7 is one or a mixture of sodium hydroxide, sodium carbonate, sodium bicarbonate and potassium hydroxide.
Advantageous effects
Compared with the prior art, the invention provides a high-light-resistance fluorescent whitening agent and a preparation method thereof, and the fluorescent whitening agent has the following beneficial effects:
1. the high-light-resistance fluorescent whitening agent provided by the invention is synthesized by adding cyanuric chloride, diethylenetriamine and adipic acid and performing catalytic reaction under the action of a catalyst, and has the characteristics of safe operation, high product yield, no toxicity and environmental friendliness.
2. According to the preparation method of the high light-resistant fluorescent whitening agent, the catalyst and the emulsifier used in the preparation process are easy to obtain, the temperature in the preparation process is convenient to control, the stability of the fluorescent whitening agent in the use process is favorably ensured by adding the diaminostilbene disulfonic acid and the sulfanilic acid, and the fluorescent whitening agent has the advantages of very strong light resistance and heat resistance, difficulty in yellowing and good dispersibility, and the 3-phenyl-2-acrylic acid is added, so that the fragrant smell of the fluorescent whitening agent in the use process is favorably increased, and the preparation method has good market popularization value.
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FIG. 1 is a flow chart of a preparation method of a high-light-resistance fluorescent whitening agent provided by the invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the 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.
The first embodiment is as follows: referring to fig. 1, a high light-resistant fluorescent whitening agent comprises the following raw materials in parts by weight: 70 parts of deionized water, 3 parts of diethylenetriamine, 5 parts of adipic acid, 4 parts of cyanuric chloride, 1 part of diaminostilbene disulfonic acid, 1 part of sulfanilic acid, 0.6 part of aniline, 1 part of inorganic base, 5 parts of hydrochloric acid, 0.5 part of emulsifier, 1 part of catalyst and 1 part of 3-phenyl-2-acrylic acid.
The preparation method of the high-light-resistance fluorescent whitening agent comprises the following steps:
s1, preparation of solution I: adding diethylenetriamine and distilled water into a four-neck flask, mixing and stirring at the temperature of 60-70 ℃, then adding an adipic acid solution, stirring, and cooling to obtain a solution I for later use;
s2, preparation of a mixed solution I: sequentially adding diaminostilbene disulfonic acid and cyanuric chloride into the solution I obtained in the step S1, heating and uniformly stirring, and cooling for reaction for 1-2 hours to obtain a mixed solution I for later use;
s3, preparing a mixed solution II: adding sulfanilic acid, aniline, a catalyst and 3-phenyl-2-acrylic acid into the mixed solution in the step S2, heating, raising the temperature, stirring and reacting for 1-1.5h, and uniformly stirring to obtain a mixed solution II for later use;
s4, treatment of the mixed liquid II: adjusting the pH value of the mixed solution II in the step S3 to 8-9, and reacting at the temperature of 20-30 ℃ for 20-30min for later use;
s5, preparation of emulsion: adding an emulsifier into the mixed solution II subjected to cooling treatment in the step S4, stirring at a high speed for 5-10min, and putting the obtained mixture into an emulsifying barrel for later use;
s6, acid precipitation treatment: adding 400ml of deionized water into the emulsifying barrel in the step S5, and adding hydrochloric acid into the emulsion after high-speed emulsification for acid precipitation;
s7, obtaining of high-light-resistance fluorescent whitening agent: and (5) adding inorganic base into the mixture subjected to acid precipitation in the step S6 for neutralization reaction, drying the mixture in a dryer for 40-60min after the neutralization reaction, and crushing the dried material into powder to obtain the required high-light-resistance fluorescent whitening agent.
As a specific optimization scheme of this example, the four-neck flask in step S1 is a four-neck flask equipped with a reflux condenser, a thermometer and a stirrer, and the first solution in step S1 has a temperature lowering temperature of 30 ℃.
As a specific optimization scheme of this embodiment, the catalyst in step S3 is one of stannous octoate and dibutyltin dilaurate.
As a specific optimization scheme of this embodiment, the temperature for heating and temperature increasing in step S2 is 70 ℃, the reaction time in step S2 is 1h, and the temperature for temperature decreasing in step S2 is 30 ℃.
As a specific optimization scheme of this embodiment, the temperature of the heating and temperature increasing in step S3 is 80 ℃, and the reaction time is 1 h.
As a specific optimization scheme of the embodiment, the high-speed stirring time in the step S5 is 5min, and the emulsion in the step S6 is acidified to a pH value of 2.0.
As a specific optimization scheme of this embodiment, the neutralization reaction in step S7 is performed until the pH value is 8, the drying time is 40min, and the powder in step S7 is screened through a 100-mesh screen.
As a specific optimization scheme of this embodiment, the emulsifier in step S5 is one of nonylphenol polyoxyethylene ether, octylphenol polyoxyethylene ether, polyoxyethylene fatty alcohol ether, and polyethylene glycol 400.
As a specific optimization scheme of this embodiment, the inorganic base in step S7 is a mixture of sodium hydroxide and sodium carbonate.
Example two: referring to fig. 1, a high light-resistant fluorescent whitening agent comprises the following raw materials in parts by weight: 75 parts of deionized water, 4 parts of diethylenetriamine, 6 parts of adipic acid, 5 parts of cyanuric chloride, 2 parts of diaminostilbene disulfonic acid, 2 parts of sulfanilic acid, 0.7 part of aniline, 2 parts of inorganic alkali, 6 parts of hydrochloric acid, 0.7 part of emulsifier, 1.1 part of catalyst and 1.1 part of 3-phenyl-2-acrylic acid.
The preparation method of the high-light-resistance fluorescent whitening agent comprises the following steps:
s1, preparation of solution I: adding diethylenetriamine and distilled water into a four-neck flask, mixing and stirring at the temperature of 60-70 ℃, then adding an adipic acid solution, stirring, and cooling to obtain a solution I for later use;
s2, preparation of a mixed solution I: sequentially adding diaminostilbene disulfonic acid and cyanuric chloride into the solution I obtained in the step S1, heating and uniformly stirring, and cooling for reaction for 1-2 hours to obtain a mixed solution I for later use;
s3, preparing a mixed solution II: adding sulfanilic acid, aniline, a catalyst and 3-phenyl-2-acrylic acid into the mixed solution in the step S2, heating, raising the temperature, stirring and reacting for 1-1.5h, and uniformly stirring to obtain a mixed solution II for later use;
s4, treatment of the mixed liquid II: adjusting the pH value of the mixed solution II in the step S3 to 8-9, and reacting at the temperature of 20-30 ℃ for 20-30min for later use;
s5, preparation of emulsion: adding an emulsifier into the mixed solution II subjected to cooling treatment in the step S4, stirring at a high speed for 5-10min, and putting the obtained mixture into an emulsifying barrel for later use;
s6, acid precipitation treatment: adding 500ml of deionized water into the emulsifying barrel in the step S5, and adding hydrochloric acid into the emulsion after high-speed emulsification for acid precipitation;
s7, obtaining of high-light-resistance fluorescent whitening agent: and (5) adding inorganic base into the mixture subjected to acid precipitation in the step S6 for neutralization reaction, drying the mixture in a dryer for 40-60min after the neutralization reaction, and crushing the dried material into powder to obtain the required high-light-resistance fluorescent whitening agent.
As a specific optimization scheme of this embodiment, the four-neck flask in step S1 is a four-neck flask equipped with a reflux condenser, a thermometer and a stirrer, and the first solution in step S1 has a temperature reduction temperature of 35 ℃.
As a specific optimization scheme of this embodiment, the catalyst in step S3 is stannous octoate.
As a specific optimization scheme of this embodiment, the temperature for heating and temperature increasing in step S2 is 75 ℃, the reaction time in step S2 is 1.5h, and the temperature for temperature decreasing in step S2 is 35 ℃.
As a specific optimization scheme of this embodiment, the temperature of the heating and temperature increasing in step S3 is 85 ℃, and the reaction time is 1.2 h.
As a specific optimization scheme of the embodiment, the high-speed stirring time in the step S5 is 8min, and the emulsion in the step S6 is acidified to a pH value of 2.0.
As a specific optimization scheme of this embodiment, the neutralization reaction in step S7 is performed until the pH value is 8, the drying time is 50min, and the powder in step S7 is screened through a 100-mesh screen.
As a specific optimization scheme of this embodiment, the emulsifier in step S5 is one of nonylphenol polyoxyethylene ether, octylphenol polyoxyethylene ether, polyoxyethylene fatty alcohol ether, and polyethylene glycol 400.
As a specific optimization scheme of this embodiment, the inorganic base in step S7 is a mixture of sodium carbonate and sodium bicarbonate.
Example three: referring to fig. 1, a high light-resistant fluorescent whitening agent comprises the following raw materials in parts by weight: 80 parts of deionized water, 6 parts of diethylenetriamine, 8 parts of adipic acid, 6 parts of cyanuric chloride, 3 parts of diaminostilbene disulfonic acid, 3 parts of sulfanilic acid, 0.8 part of aniline, 3 parts of inorganic base, 8 parts of hydrochloric acid, 0.8 part of emulsifier, 1.2 parts of catalyst and 2 parts of 3-phenyl-2-acrylic acid.
The preparation method of the high-light-resistance fluorescent whitening agent comprises the following steps:
s1, preparation of solution I: adding diethylenetriamine and distilled water into a four-neck flask, mixing and stirring at the temperature of 60-70 ℃, then adding an adipic acid solution, stirring, and cooling to obtain a solution I for later use;
s2, preparation of a mixed solution I: sequentially adding diaminostilbene disulfonic acid and cyanuric chloride into the solution I obtained in the step S1, heating and uniformly stirring, and cooling for reaction for 1-2 hours to obtain a mixed solution I for later use;
s3, preparing a mixed solution II: adding sulfanilic acid, aniline, a catalyst and 3-phenyl-2-acrylic acid into the mixed solution in the step S2, heating, raising the temperature, stirring and reacting for 1-1.5h, and uniformly stirring to obtain a mixed solution II for later use;
s4, treatment of the mixed liquid II: adjusting the pH value of the mixed solution II in the step S3 to 8-9, and reacting at the temperature of 20-30 ℃ for 20-30min for later use;
s5, preparation of emulsion: adding an emulsifier into the mixed solution II subjected to cooling treatment in the step S4, stirring at a high speed for 5-10min, and putting the obtained mixture into an emulsifying barrel for later use;
s6, acid precipitation treatment: adding 600ml of deionized water into the emulsifying barrel in the step S5, and adding hydrochloric acid into the emulsion after high-speed emulsification for acid precipitation;
s7, obtaining of high-light-resistance fluorescent whitening agent: and (5) adding inorganic base into the mixture subjected to acid precipitation in the step S6 for neutralization reaction, drying the mixture in a dryer for 40-60min after the neutralization reaction, and crushing the dried material into powder to obtain the required high-light-resistance fluorescent whitening agent.
As a specific optimization scheme of this example, the four-neck flask in step S1 is a four-neck flask equipped with a reflux condenser, a thermometer and a stirrer, and the first solution in step S1 has a temperature reduction temperature of 40 ℃.
As a specific optimization scheme of this embodiment, the catalyst in step S3 is dibutyltin dilaurate.
As a specific optimization scheme of this embodiment, the temperature for heating and temperature increasing in step S2 is 80 ℃, the reaction time in step S2 is 2h, and the temperature for temperature decreasing in step S2 is 40 ℃.
As a specific optimization scheme of this embodiment, the temperature of the heating and temperature increasing in step S3 is 90 ℃, and the reaction time is 1.5 h.
As a specific optimization scheme of this example, the high-speed stirring time in the step S5 is 10min, and the emulsion in the step S6 is acidified to a pH value of 2.0.
As a specific optimization scheme of this embodiment, the neutralization reaction in step S7 is performed until the pH value is 8, the drying time is 60min, and the powder in step S7 is screened through a 100-mesh screen.
As a specific optimization scheme of this embodiment, the emulsifier in step S5 is one of nonylphenol polyoxyethylene ether, octylphenol polyoxyethylene ether, polyoxyethylene fatty alcohol ether, and polyethylene glycol 400.
As a specific optimization scheme of this embodiment, the inorganic base in step S7 is a mixture of sodium bicarbonate and potassium hydroxide.
The high-light-resistance fluorescent whitening agent is synthesized by adding cyanuric chloride, diethylenetriamine and adipic acid and performing catalytic reaction under the action of a catalyst, and has the characteristics of safe operation, high product yield, no toxicity and environmental protection.
The high light-resistant fluorescent whitening agent and the preparation method thereof have the advantages that cyanuric chloride, diethylenetriamine and adipic acid are added to perform catalytic reaction under the action of a catalyst to synthesize the fluorescent whitening agent, the operation is safe, the product yield is high, the fluorescent whitening agent has the characteristics of no toxicity and environmental protection in the using process, the catalyst and the emulsifier used in the preparation process are easy to obtain, the temperature in the preparation process is convenient to control, the stability of the fluorescent whitening agent in the using process is favorably ensured by adding diaminostilbene disulfonic acid and sulfanilic acid, meanwhile, the fluorescent whitening agent has the advantages of very strong light resistance and heat resistance, difficult yellowing and good dispersibility, the 3-phenyl-2-acrylic acid is added to favorably increase the faint scent and fragrance of the fluorescent whitening agent in the using process, and the fluorescent whitening agent has good market popularization value.
Claims (10)
1. The high-light-resistance fluorescent whitening agent is characterized by comprising the following raw materials in parts by weight: 70-80 parts of deionized water, 3-6 parts of diethylenetriamine, 5-8 parts of adipic acid, 4-6 parts of cyanuric chloride, 1-3 parts of diaminostilbene disulfonic acid, 1-3 parts of sulfanilic acid, 0.6-0.8 part of aniline, 1-3 parts of inorganic base, 5-8 parts of hydrochloric acid, 0.5-0.8 part of emulsifier, 1-1.2 parts of catalyst and 1-2 parts of 3-phenyl-2-acrylic acid.
2. The process for the preparation of highly lightfast fluorescent whitening agent according to claim 1, characterized by the following steps:
s1, preparation of solution I: adding diethylenetriamine and distilled water into a four-neck flask, mixing and stirring at the temperature of 60-70 ℃, then adding an adipic acid solution, stirring, and cooling to obtain a solution I for later use;
s2, preparation of a mixed solution I: sequentially adding diaminostilbene disulfonic acid and cyanuric chloride into the solution I obtained in the step S1, heating, raising the temperature, uniformly stirring, and cooling for reacting for 1-2 hours to obtain a mixed solution I for later use;
s3, preparing a mixed solution II: adding sulfanilic acid, aniline, a catalyst and 3-phenyl-2-acrylic acid into the mixed solution in the step S2, heating, raising the temperature, stirring and reacting for 1-1.5h, and uniformly stirring to obtain a mixed solution II for later use;
s4, treatment of the mixed liquid II: adjusting the pH value of the mixed solution II in the step S3 to 8-9, and reacting at the temperature of 20-30 ℃ for 20-30min for later use;
s5, preparation of emulsion: adding an emulsifier into the mixed solution II subjected to cooling treatment in the step S4, stirring at a high speed for 5-10min, and putting the obtained mixture into an emulsifying barrel for later use;
s6, acid precipitation treatment: adding 400-600ml of deionized water into the emulsification barrel in the step S5, and adding hydrochloric acid into the emulsion after high-speed emulsification for acid precipitation treatment;
s7, obtaining of high-light-resistance fluorescent whitening agent: and (5) adding inorganic base into the mixture subjected to acid precipitation in the step S6 for neutralization reaction, drying the mixture in a dryer for 40-60min after the neutralization reaction, and crushing the dried material into powder to obtain the required high-light-resistance fluorescent whitening agent.
3. The method for preparing a highly light-resistant fluorescent whitening agent according to claim 2, wherein the four-necked flask of step S1 is a four-necked flask equipped with a reflux condenser, a thermometer and a stirrer, and the first solution of step S1 has a reduced temperature of 30-40 ℃.
4. The method for preparing a fluorescent whitening agent with high light fastness according to claim 2, wherein the catalyst in step S3 is one of stannous octoate and dibutyltin dilaurate.
5. The method for preparing a fluorescent brightener with high light fastness according to claim 2, wherein the temperature for heating and raising the temperature in step S2 is 70-80 ℃, the reaction time in step S2 is 1.5h, and the temperature for lowering the temperature in step S2 is 30-40 ℃.
6. The method for preparing a fluorescent whitening agent with high light fastness according to claim 2, wherein the heating temperature in the step S3 is 80-90 ℃, and the reaction time is 1 h.
7. The method for preparing a fluorescent whitening agent with high light fastness according to claim 2, wherein the stirring at high speed in step S5 is carried out for 7min, and the emulsion in step S6 is acidified to pH value of 2.0-3.
8. The method as claimed in claim 2, wherein the neutralization reaction in step S7 is carried out to pH 8-8.5, the drying time is 50min, and the powder in step S7 is screened through a screen of 100-120 mesh.
9. The method for preparing a highly light-resistant fluorescent whitening agent according to claim 2, wherein the emulsifier in step S5 is one of nonylphenol polyoxyethylene ether, octylphenol polyoxyethylene ether, polyoxyethylene fatty alcohol ether, and polyethylene glycol 400.
10. The method of claim 2, wherein the inorganic base in step S7 is one or more selected from sodium hydroxide, sodium carbonate, sodium bicarbonate, and potassium hydroxide.
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CN114316622A (en) * | 2021-12-20 | 2022-04-12 | 江苏格罗瑞化学有限公司 | High-light-resistance anti-yellowing fluorescent whitening agent and preparation method thereof |
Citations (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN1589352A (en) * | 2001-11-21 | 2005-03-02 | 克莱里安特财务(Bvi)有限公司 | Improvements relating to optical brighteners |
CN105885001A (en) * | 2016-06-07 | 2016-08-24 | 安徽建筑大学 | Polyurethane based fluorescent whitening agent and preparation method thereof |
CN106634013A (en) * | 2016-12-16 | 2017-05-10 | 山西青山化工有限公司 | Device for preparing toluylene bis(triazinyl) particular fluorescent whitening agent and preparation method thereof |
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 |
CN108203553A (en) * | 2016-12-19 | 2018-06-26 | 江苏格罗瑞化学有限公司 | A kind of modified fluorescent whitening agent and its processing technology |
-
2020
- 2020-04-13 CN CN202010284453.7A patent/CN111349349A/en active Pending
Patent Citations (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN1589352A (en) * | 2001-11-21 | 2005-03-02 | 克莱里安特财务(Bvi)有限公司 | Improvements relating to optical brighteners |
CN105885001A (en) * | 2016-06-07 | 2016-08-24 | 安徽建筑大学 | Polyurethane based fluorescent whitening agent and preparation method thereof |
CN106634013A (en) * | 2016-12-16 | 2017-05-10 | 山西青山化工有限公司 | Device for preparing toluylene bis(triazinyl) particular fluorescent whitening agent and preparation method thereof |
CN108203553A (en) * | 2016-12-19 | 2018-06-26 | 江苏格罗瑞化学有限公司 | A kind of modified fluorescent whitening agent and its processing technology |
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 |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN114316622A (en) * | 2021-12-20 | 2022-04-12 | 江苏格罗瑞化学有限公司 | High-light-resistance anti-yellowing fluorescent whitening agent and preparation method thereof |
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