CN113293602A - Preparation method of fluorescent whitening agent - Google Patents
Preparation method of fluorescent whitening agent Download PDFInfo
- Publication number
- CN113293602A CN113293602A CN202110496254.7A CN202110496254A CN113293602A CN 113293602 A CN113293602 A CN 113293602A CN 202110496254 A CN202110496254 A CN 202110496254A CN 113293602 A CN113293602 A CN 113293602A
- Authority
- CN
- China
- Prior art keywords
- fluorescent whitening
- whitening agent
- preparation
- heating
- phthalimide
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Images
Classifications
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06L—DRY-CLEANING, WASHING OR BLEACHING FIBRES, FILAMENTS, THREADS, YARNS, FABRICS, FEATHERS OR MADE-UP FIBROUS GOODS; BLEACHING LEATHER OR FURS
- D06L4/00—Bleaching fibres, filaments, threads, yarns, fabrics, feathers or made-up fibrous goods; Bleaching leather or furs
- D06L4/60—Optical bleaching or brightening
- D06L4/614—Optical bleaching or brightening in aqueous solvents
Landscapes
- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Detergent Compositions (AREA)
Abstract
The invention discloses a preparation method of a fluorescent whitening agent, which comprises the following steps of mixing phthalic anhydride and ammonium carbonate according to a molar ratio of 1: 1.2, mixing, crushing by a crusher, putting into a reaction kettle, heating for about 4 hours to 180 ℃, and then slightly and rapidly heating to 290-300 ℃; discharging the obtained melt to be crystallized, cooling, solidifying and crushing to obtain phthalimide; putting phthalimide into a reaction kettle, heating to 80-90 ℃ for melting, then adding glacial acetic acid, an emulsifier, a preservative and water, continuing stirring until the temperature is reduced to about 50 ℃, adding a proper amount of salt, and finally obtaining a solution after the reaction; and (5) carrying out suction filtration on the solution by using a sand core, circulating for 3-5 times, drying, packaging and warehousing. The invention is suitable for whitening and dyeing auxiliary of cloth, has good whitening effect, and the dyed cloth has enough color whiteness, uniform and beautiful color and practical value.
Description
Technical Field
The invention relates to the technical field of textile auxiliary agents, in particular to a preparation method of a fluorescent whitening agent.
Background
Fluorescent whitening agents (fluorescents) are a fluorescent dye, otherwise known as white dyes, and are also complex organic compounds. Its characteristic is that it can excite incident ray to produce fluorescence, so that the dyed material can obtain the scintillation effect similar to fluorite, and the material seen by naked eye is very white. The rapid development of fluorescent whitening agents has led to the emergence of this group of reactive dyes and organic pigments DPP as three major achievements in the dye world in the late 20 th century. Many industries have begun to use optical brighteners such as: paper, plastic, leather, detergent. Optical brighteners are also used in many high-tech fields, for example: fluorescent detection, dye lasers, security printing, and the like, and even high sensitivity films for high-altitude photography use fluorescent whitening agents to increase the sensitivity of the photosensitive latex.
Because the color whiteness of the fabrics dyed by the conventional fluorescent whitening agent is not enough and the color is not uniform, the product quality of the fluorescent whitening agent needs to be further improved, and therefore, a preparation method of the fluorescent whitening agent is provided.
Disclosure of Invention
Aiming at the defects in the prior art, the invention aims to provide a preparation method of a fluorescent whitening agent.
The technical scheme adopted by the invention for realizing the purpose is as follows: a method for preparing a fluorescent whitening agent, wherein the fluorescent whitening agent is prepared from the following ingredients:
35-40% of phthalic anhydride;
25-30% of ammonium carbonate;
5-10% of glacial acetic acid;
1-3% of an emulsifier;
1-3% of a preservative;
15-20% of water;
proper amount of salt;
the sum of the percentages of the components is 100%.
A process for the preparation of a fluorescent whitening agent comprising the steps of:
in the step (1): phthalic anhydride and ammonium carbonate were mixed in a molar ratio of 1: 1.2, mixing, crushing by a crusher, putting into a reaction kettle, heating for about 4 hours to 180 ℃, and then slightly and rapidly heating to 290-300 ℃;
in the step (2): discharging the melt obtained in the step (1) to be crystallized, cooling, solidifying and crushing to obtain phthalimide;
in the step (3): putting the phthalimide obtained in the step (2) into a reaction kettle, heating to 80-90 ℃ for melting, then adding glacial acetic acid, an emulsifier, a preservative and water, continuing stirring until the temperature is reduced to about 50 ℃, adding a proper amount of salt, and finally obtaining a solution after the reaction is finished
In the step (4): and (4) carrying out suction filtration on the solution in the step (3) by using a sand core, circulating for 3-5 times, drying, packaging and warehousing.
The preparation method of the fluorescent whitening agent is characterized by comprising the following steps: the emulsifier is one or more of glyceryl monostearate, butyl stearate, stearyl alcohol, sucrose ester and soybean lecithin.
The preparation method of the fluorescent whitening agent is characterized by comprising the following steps: the preservative is one or more of sodium benzoate, potassium sorbate, dehydroacetic acid and butyl hydroxybenzoate.
The preparation method of the fluorescent whitening agent is characterized by comprising the following steps: the water is deionized water.
The preparation method of the fluorescent whitening agent is characterized by comprising the following steps: in the step (2) or the step (3), the yield of the phthalimide is 95% or more.
The invention has the beneficial effects that: the preparation method of the fluorescent whitening agent is suitable for whitening and dyeing-assisting of cloth, has a good whitening effect, enables the dyed cloth to have sufficient color whiteness and uniform and attractive color, and has practical value.
Drawings
FIG. 1 is a schematic view of the structure of the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in 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.
Referring to fig. 1, a method for preparing fluorescent whitening agent comprises the following steps:
35-40% of phthalic anhydride;
25-30% of ammonium carbonate;
5-10% of glacial acetic acid;
1-3% of an emulsifier;
1-3% of a preservative;
15-20% of water;
proper amount of salt;
the sum of the percentages of the components is 100%.
A process for the preparation of a fluorescent whitening agent comprising the steps of:
in the step (1): phthalic anhydride and ammonium carbonate were mixed in a molar ratio of 1: 1.2, mixing, crushing by a crusher, putting into a reaction kettle, heating for about 4 hours to 180 ℃, and then slightly and rapidly heating to 290-300 ℃;
in the step (2): discharging the melt obtained in the step (1) to be crystallized, cooling, solidifying and crushing to obtain phthalimide;
in the step (3): putting the phthalimide obtained in the step (2) into a reaction kettle, heating to 80-90 ℃ for melting, then adding glacial acetic acid, an emulsifier, a preservative and water, continuing stirring until the temperature is reduced to about 50 ℃, adding a proper amount of salt, and finally obtaining a solution after the reaction is finished
In the step (4): and (4) carrying out suction filtration on the solution in the step (3) by using a sand core, circulating for 3-5 times, drying, packaging and warehousing.
In the invention:
as a preferred technical scheme of the invention: the emulsifier is one or more of glyceryl monostearate, butyl stearate, stearyl alcohol, sucrose ester and soybean lecithin.
As a preferred technical scheme of the invention: the preservative is one or more of sodium benzoate, potassium sorbate, dehydroacetic acid and butyl hydroxybenzoate.
As a preferred technical scheme of the invention: the water is deionized water.
As a preferred technical scheme of the invention: in the step (2) or the step (3), the yield of phthalimide is 95% or more
Specific example 1:
phthalic anhydride and ammonium carbonate were mixed in a molar ratio of 1: 1.2, mixing, crushing by a crusher, putting into a reaction kettle, heating for about 4 hours to 180 ℃, and then heating to 300 ℃ at a slight speed; discharging the obtained melt to be crystallized, cooling, solidifying and crushing to obtain phthalimide; putting phthalimide into a reaction kettle, heating to 90 ℃ for melting, then adding glacial acetic acid, butyl stearate, potassium sorbate and deionized water, continuing stirring until the temperature is reduced to about 45 ℃, adding a proper amount of salt, and finally obtaining a solution after the reaction; and (5) carrying out suction filtration on the solution by using a sand core, circulating for 5 times, drying, packaging and warehousing.
Specific example 2:
phthalic anhydride and ammonium carbonate were mixed in a molar ratio of 1: 1.2, mixing, crushing by a crusher, putting into a reaction kettle, heating for about 4 hours to 180 ℃, and then heating to 290 ℃ at a slightly rapid speed; discharging the obtained melt to be crystallized, cooling, solidifying and crushing to obtain phthalimide; putting phthalimide into a reaction kettle, heating to 80 ℃ for melting, then adding glacial acetic acid, glyceryl monostearate, sodium benzoate and deionized water, continuing stirring until the temperature is reduced to 55 ℃, adding a proper amount of salt, and finally obtaining a solution after the reaction is finished; and (5) carrying out suction filtration on the solution by using a sand core, circulating for 3 times, drying, packaging and warehousing.
The invention is suitable for whitening and dyeing auxiliary of cloth, has good whitening effect, and the dyed cloth has enough color whiteness, uniform and beautiful color and practical value.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential attributes thereof. The present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein. Any reference sign in a claim should not be construed as limiting the claim concerned.
Furthermore, it should be understood that although the present description refers to embodiments, not every embodiment may contain only a single embodiment, and such description is for clarity only, and those skilled in the art should integrate the description, and the embodiments may be combined as appropriate to form other embodiments understood by those skilled in the art.
Claims (6)
1. The fluorescent whitening agent is characterized by being prepared from the following ingredients:
35-40% of phthalic anhydride;
25-30% of ammonium carbonate;
5-10% of glacial acetic acid;
1-3% of an emulsifier;
1-3% of a preservative;
15-20% of water;
proper amount of salt;
the sum of the percentages of the components is 100%.
2. A process for the preparation of a fluorescent whitening agent according to claim 1, comprising the steps of:
in the step (1): phthalic anhydride and ammonium carbonate were mixed in a molar ratio of 1: 1.2, mixing, crushing by a crusher, putting into a reaction kettle, heating for about 4 hours to 180 ℃, and then slightly and rapidly heating to 290-300 ℃;
in the step (2): discharging the melt obtained in the step (1) to be crystallized, cooling, solidifying and crushing to obtain phthalimide;
in the step (3): putting the phthalimide obtained in the step (2) into a reaction kettle, heating to 80-90 ℃ for melting, then adding glacial acetic acid, an emulsifier, a preservative and water, continuing stirring until the temperature is reduced to about 50 ℃, adding a proper amount of salt, and finally obtaining a solution after the reaction is finished
In the step (4): and (4) carrying out suction filtration on the solution in the step (3) by using a sand core, circulating for 3-5 times, drying, packaging and warehousing.
3. A process for the preparation of a fluorescent whitening agent according to claims 1-2, characterized in that: the emulsifier is one or more of glyceryl monostearate, butyl stearate, stearyl alcohol, sucrose ester and soybean lecithin.
4. A process for the preparation of a fluorescent whitening agent according to claims 1-2, characterized in that: the preservative is one or more of sodium benzoate, potassium sorbate, dehydroacetic acid and butyl hydroxybenzoate.
5. A process for the preparation of a fluorescent whitening agent according to claim 2, characterized in that: the water is deionized water.
6. A process for the preparation of a fluorescent whitening agent according to claim 2, characterized in that: in the step (2) or the step (3), the yield of the phthalimide is 95% or more.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110496254.7A CN113293602A (en) | 2021-05-07 | 2021-05-07 | Preparation method of fluorescent whitening agent |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110496254.7A CN113293602A (en) | 2021-05-07 | 2021-05-07 | Preparation method of fluorescent whitening agent |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN113293602A true CN113293602A (en) | 2021-08-24 |
Family
ID=77321861
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202110496254.7A Pending CN113293602A (en) | 2021-05-07 | 2021-05-07 | Preparation method of fluorescent whitening agent |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN113293602A (en) |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| SU481607A1 (en) * | 1972-03-10 | 1975-08-25 | Уманский Витаминный Завод | Phalimide Preparation Method |
| JPH05339221A (en) * | 1992-06-11 | 1993-12-21 | Neos Co Ltd | Fluorine-containing aminobenzoic acid derivative |
| JP2001122858A (en) * | 1999-10-22 | 2001-05-08 | Kawasaki Kasei Chem Ltd | Production of phthalimide compound |
| CN1835933A (en) * | 2003-08-21 | 2006-09-20 | 西巴特殊化学品控股有限公司 | Optical brighteners |
| CN105113293A (en) * | 2015-08-20 | 2015-12-02 | 浙江百德纺织有限公司 | Fluorescent textile dye |
| CN110804011A (en) * | 2019-11-12 | 2020-02-18 | 内蒙古科迈化工有限公司 | Method for synthesizing phthalimide |
-
2021
- 2021-05-07 CN CN202110496254.7A patent/CN113293602A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| SU481607A1 (en) * | 1972-03-10 | 1975-08-25 | Уманский Витаминный Завод | Phalimide Preparation Method |
| JPH05339221A (en) * | 1992-06-11 | 1993-12-21 | Neos Co Ltd | Fluorine-containing aminobenzoic acid derivative |
| JP2001122858A (en) * | 1999-10-22 | 2001-05-08 | Kawasaki Kasei Chem Ltd | Production of phthalimide compound |
| CN1835933A (en) * | 2003-08-21 | 2006-09-20 | 西巴特殊化学品控股有限公司 | Optical brighteners |
| CN105113293A (en) * | 2015-08-20 | 2015-12-02 | 浙江百德纺织有限公司 | Fluorescent textile dye |
| CN110804011A (en) * | 2019-11-12 | 2020-02-18 | 内蒙古科迈化工有限公司 | Method for synthesizing phthalimide |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| EP0207003B1 (en) | Graft polymer soluble or dispersible in water, its preparation and use | |
| US4306875A (en) | Salts of basic dyes, preparation and uses of same | |
| EP0210129B1 (en) | Graft polymer soluble or dispersible in water, its preparation and use | |
| US4281999A (en) | Aqueous dye preparations of dyes difficultly soluble in water | |
| CN113293602A (en) | Preparation method of fluorescent whitening agent | |
| EP0074569B1 (en) | Cationic methine dyes, process for their preparation and their use, in dyeing textile materials and other substrates | |
| US2643197A (en) | Fluorescent alkoxy benzoyl derivatives of 4,4' diamino stilbene-2,2' disulfonic acidand detergent compositions containing same | |
| US2168348A (en) | Cellulosic composition and method of preparing same | |
| KR20190047797A (en) | Novel fluorescent dye having good dyeability and solubility and preparation method for the same | |
| US2043069A (en) | Preparation of dyed filaments and films | |
| CN106398307A (en) | Preparation process of phthalocyanine blue for PU inkjet printing | |
| KR101474326B1 (en) | Liquid alkali buffer for reactive dye and method for making the same | |
| CN112174947A (en) | Plastic whitening agent OB and preparation method thereof | |
| US2890092A (en) | Dyeing synthetic fibers with vat dyestuffs | |
| CN108559334A (en) | A method of improving fluorescent dye tinctorial property on timber | |
| JP2007182525A (en) | Dyeing method for indigo-dyed goods | |
| US2515723A (en) | Dibenzanthrone dyestuff | |
| CN115162034B (en) | Acetic acid printed fabric washing anti-overlapping reagent and use method thereof | |
| US4474577A (en) | Modified acid dyestuff | |
| US2817667A (en) | Red vat dyestuffs of the pyrazol-anthrone series | |
| Park et al. | Dye and fibre discoveries of the twentieth century. Part 1: From the magic of electric light to the nightmare of world war | |
| US2343928A (en) | Production of colored film-forming materials | |
| US2911415A (en) | Optical whitener | |
| EP0431906A2 (en) | Cotton rope-dyeing methods | |
| DE1644404A1 (en) | New anthraquinone colors and intermediates |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20210824 |