CN116355437A - Preparation method for improving saturation of bromofluorescein lake - Google Patents
Preparation method for improving saturation of bromofluorescein lake Download PDFInfo
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- CN116355437A CN116355437A CN202310236968.3A CN202310236968A CN116355437A CN 116355437 A CN116355437 A CN 116355437A CN 202310236968 A CN202310236968 A CN 202310236968A CN 116355437 A CN116355437 A CN 116355437A
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- 229960001483 eosin Drugs 0.000 title claims abstract description 43
- 238000002360 preparation method Methods 0.000 title claims abstract description 31
- SEACYXSIPDVVMV-UHFFFAOYSA-L eosin Y Chemical compound [Na+].[Na+].[O-]C(=O)C1=CC=CC=C1C1=C2C=C(Br)C(=O)C(Br)=C2OC2=C(Br)C([O-])=C(Br)C=C21 SEACYXSIPDVVMV-UHFFFAOYSA-L 0.000 title abstract 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 46
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims abstract description 36
- 239000011259 mixed solution Substances 0.000 claims abstract description 35
- 239000000243 solution Substances 0.000 claims abstract description 32
- 229910000019 calcium carbonate Inorganic materials 0.000 claims abstract description 18
- 239000000049 pigment Substances 0.000 claims abstract description 10
- 238000002156 mixing Methods 0.000 claims abstract description 9
- 230000001105 regulatory effect Effects 0.000 claims abstract description 8
- 239000000975 dye Substances 0.000 claims abstract description 7
- 239000000976 ink Substances 0.000 claims abstract description 7
- 239000002537 cosmetic Substances 0.000 claims abstract description 6
- 239000003814 drug Substances 0.000 claims abstract description 6
- 235000013305 food Nutrition 0.000 claims abstract description 6
- 239000007788 liquid Substances 0.000 claims abstract description 4
- 238000000926 separation method Methods 0.000 claims abstract description 4
- 239000007790 solid phase Substances 0.000 claims abstract description 3
- DBZJJPROPLPMSN-UHFFFAOYSA-N bromoeosin Chemical compound O1C(=O)C2=CC=CC=C2C21C1=CC(Br)=C(O)C(Br)=C1OC1=C(Br)C(O)=C(Br)C=C21 DBZJJPROPLPMSN-UHFFFAOYSA-N 0.000 claims description 39
- ZDTNHRWWURISAA-UHFFFAOYSA-N 4',5'-dibromo-3',6'-dihydroxyspiro[2-benzofuran-3,9'-xanthene]-1-one Chemical compound O1C(=O)C2=CC=CC=C2C21C1=CC=C(O)C(Br)=C1OC1=C(Br)C(O)=CC=C21 ZDTNHRWWURISAA-UHFFFAOYSA-N 0.000 claims description 19
- 230000002378 acidificating effect Effects 0.000 claims description 18
- 238000000034 method Methods 0.000 claims description 17
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 14
- 238000003756 stirring Methods 0.000 claims description 14
- 239000007864 aqueous solution Substances 0.000 claims description 8
- 230000001376 precipitating effect Effects 0.000 claims description 8
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 6
- 239000003795 chemical substances by application Substances 0.000 claims description 3
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 2
- JGDITNMASUZKPW-UHFFFAOYSA-K aluminium trichloride hexahydrate Chemical compound O.O.O.O.O.O.Cl[Al](Cl)Cl JGDITNMASUZKPW-UHFFFAOYSA-K 0.000 claims description 2
- 229940009861 aluminum chloride hexahydrate Drugs 0.000 claims description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-N ammonia Natural products N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 2
- VSGNNIFQASZAOI-UHFFFAOYSA-L calcium acetate Chemical compound [Ca+2].CC([O-])=O.CC([O-])=O VSGNNIFQASZAOI-UHFFFAOYSA-L 0.000 claims description 2
- 239000001639 calcium acetate Substances 0.000 claims description 2
- 229960005147 calcium acetate Drugs 0.000 claims description 2
- 235000011092 calcium acetate Nutrition 0.000 claims description 2
- 229960003563 calcium carbonate Drugs 0.000 claims description 2
- ZYIBVBKZZZDFOY-UHFFFAOYSA-N phloxine O Chemical compound O1C(=O)C(C(=C(Cl)C(Cl)=C2Cl)Cl)=C2C21C1=CC(Br)=C(O)C(Br)=C1OC1=C(Br)C(O)=C(Br)C=C21 ZYIBVBKZZZDFOY-UHFFFAOYSA-N 0.000 claims description 2
- 238000000527 sonication Methods 0.000 claims description 2
- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 abstract description 5
- 229940079593 drug Drugs 0.000 abstract description 4
- 239000002253 acid Substances 0.000 abstract description 2
- 239000012535 impurity Substances 0.000 abstract description 2
- 238000005119 centrifugation Methods 0.000 description 17
- 230000000052 comparative effect Effects 0.000 description 16
- 239000002244 precipitate Substances 0.000 description 10
- 238000001035 drying Methods 0.000 description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 6
- 238000004140 cleaning Methods 0.000 description 5
- 238000000227 grinding Methods 0.000 description 5
- 238000009210 therapy by ultrasound Methods 0.000 description 5
- 230000000694 effects Effects 0.000 description 3
- 238000005286 illumination Methods 0.000 description 3
- 238000001179 sorption measurement Methods 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- 239000000463 material Substances 0.000 description 2
- 238000011056 performance test Methods 0.000 description 2
- 239000006228 supernatant Substances 0.000 description 2
- 238000002604 ultrasonography Methods 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 1
- 150000007513 acids Chemical class 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000004108 freeze drying Methods 0.000 description 1
- 239000002932 luster Substances 0.000 description 1
- 239000012860 organic pigment Substances 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 210000003296 saliva Anatomy 0.000 description 1
- 238000004088 simulation Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- 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
- C09B63/00—Lakes
-
- C—CHEMISTRY; METALLURGY
- 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
- C09B67/00—Influencing the physical, e.g. the dyeing or printing properties of dyestuffs without chemical reactions, e.g. by treating with solvents grinding or grinding assistants, coating of pigments or dyes; Process features in the making of dyestuff preparations; Dyestuff preparations of a special physical nature, e.g. tablets, films
- C09B67/0096—Purification; Precipitation; Filtration
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Coloring Foods And Improving Nutritive Qualities (AREA)
Abstract
The invention discloses a preparation method for improving the saturation of bromofluorescein lakes. The preparation method for improving the saturation of bromofluorescein lakes comprises the following steps: mixing bromofluorescein with 60-85% acid ethanol water solution to remove ethanol and obtain mixed solution; adding a precipitant into the mixed solution, regulating the pH value of the solution to 7-9, carrying out solid-liquid separation, and collecting a solid phase, namely the bromofluorescein lake. The preparation method for improving the saturation of the bromofluorescein lake is simple, convenient to operate, and the lake is prepared by calcium carbonate, so that the prepared lake has high tinting strength, few impurities, high purity and high saturation, and can be effectively used in the fields of dyes, printing ink, pigments, ink, medicines, cosmetics or foods and the like.
Description
Technical Field
The invention relates to the technical field of dyes, in particular to a preparation method for improving the saturation of bromofluorescein lakes.
Background
Lakes are non-water-soluble colored substances precipitated from water-soluble dyes by the action of different types of precipitants, and are generally used in the fields of dyes, inks, pigments, inks, medicines, cosmetics, foods, etc. The above applications generally require that the lakes have vivid color, good hiding power, water insolubility, stability to acids, bases, heat, etc., and good light fastness.
The saturation of a color refers to the vividness of the color, also known as purity. Under the HSV color model, saturation is one of three important attributes of color. The high saturation pigment has brightness and vividness comparable to those of organic pigments.
The preparation methods of the lakes are many, but the lakes prepared by the existing preparation process of the lakes are not ideal in saturation, stability and the like.
Disclosure of Invention
The present invention aims to solve at least one of the technical problems existing in the prior art. Therefore, the invention provides a preparation method for improving the saturation of bromofluorescein lakes.
The invention also provides the bromofluorescein lake prepared by the preparation method.
The invention also provides application of the bromofluorescein lake.
In a first aspect of the present invention, a method for improving the saturation of a bromofluorescein lake is presented, the method comprising the steps of:
s1, mixing bromofluorescein with an acidic ethanol aqueous solution with the volume concentration of 60-85%, and removing ethanol to obtain a mixed solution;
s2, adding a precipitant into the mixed solution, regulating the pH value of the solution to 7-9, carrying out solid-liquid separation, and collecting a solid phase, namely the bromofluorescein lake.
In some embodiments of the invention, the bromofluorescein comprises at least one of 4',5' -dibromofluorescein, 2',4',5',7' -tetrabromofluorescein, 2',4',5',7' -tetrabromo-4, 7-dichlorofluorescein, and 2',4',5',7' -tetrabromo-4, 5,6, 7-tetrachlorofluorescein.
In some embodiments of the invention, the acidic ethanol solution has a pH of 1 to 5.
In some embodiments of the invention, the pH is adjusted with acetic acid, hydrochloric acid, or aqueous ammonia.
In some embodiments of the invention, the mass to volume ratio of the bromofluorescein to the acidic ethanol solution is 1g (4-12) mL.
In some embodiments of the invention, the removing ethanol is performed using reduced pressure concentration.
In some embodiments of the invention, the reduced pressure concentration is at a temperature of 50 to 70 ℃.
In some embodiments of the present invention, the volume ratio of the mixed solution to the precipitant is (1-3): 1.
in some embodiments of the invention, the mixing solution and the precipitant are added in a volume ratio of (1.5-3): 1.
in some embodiments of the invention, the precipitant comprises aluminum chloride hexahydrate, calcium carbonate, or calcium acetate solution.
In some embodiments of the invention, the precipitant is 40-60% by mass.
In some embodiments of the invention, the precipitant is present in an amount of 50 to 55% by mass.
In some embodiments of the invention, the precipitating agent further comprises the steps of stirring and sonication after the precipitating agent is added.
In some embodiments of the invention, the power of the ultrasound is 140-170W, the temperature is 25-30 ℃, and the ultrasound time is 6-10 min.
In some embodiments of the invention, the step of stirring is further included after adjusting the pH of the solution, the stirring time being 30-60 minutes.
In some embodiments of the invention, the step of standing for 12-18 hours is further included after adjusting the pH of the solution.
In some embodiments of the present invention, the solid-liquid separation in step S2 is performed by centrifugation under conditions of 3000 to 5000g at 22 to 28 ℃ for 8 to 12min.
In some embodiments of the invention, the method further comprises the step of drying the bromofluorescein-based lake.
In some embodiments of the invention, the drying is freeze-drying or heat-drying.
In some embodiments of the invention, the temperature of the heat drying is 40-60 ℃.
According to a second aspect of the present invention, a bromofluorescein lake prepared by the above preparation method is provided.
According to a third aspect of the present invention, there is provided the use of a bromofluorescein-based lake as described above in dyes, inks, pigments, in the preparation of pharmaceuticals, cosmetics or food.
The preparation method provided by the embodiment of the invention has at least the following beneficial effects: the preparation method for improving the saturation of the bromofluorescein lake is simple, convenient to operate, and the lake is prepared by calcium carbonate, so that the prepared lake has high tinting strength, few impurities, high purity and high saturation, and can be effectively used in the fields of dyes, printing ink, pigments, medicines, cosmetics or foods and the like.
Additional features and advantages of the invention will be set forth in the description which follows, and in part will be obvious from the description, or may be learned by practice of the invention.
Detailed Description
The conception and the technical effects produced by the present invention will be clearly and completely described in conjunction with the embodiments below to fully understand the objects, features and effects of the present invention. It is apparent that the described embodiments are only some embodiments of the present invention, but not all embodiments, and that other embodiments obtained by those skilled in the art without inventive effort are within the scope of the present invention based on the embodiments of the present invention.
In the description of the present invention, the descriptions of the terms "one embodiment," "some embodiments," "illustrative embodiments," "examples," "specific examples," or "some examples," etc., mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the present invention. In this specification, schematic representations of the above terms do not necessarily refer to the same embodiments or examples. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.
The specific conditions are not noted in the examples and are carried out according to conventional conditions or conditions recommended by the manufacturer. The reagents or apparatus used were conventional products commercially available without the manufacturer's attention.
Example 1
The embodiment provides a preparation method of bromofluorescein lake saturation, which comprises the following preparation steps:
(1) Mixing 4',5' -dibromofluorescein with an acidic ethanol aqueous solution with the volume concentration of 80% (the pH value is adjusted to 2.0 by adopting hydrochloric acid) to obtain a first mixed solution, wherein the adding mass volume ratio of the 4',5' -dibromofluorescein to the acidic ethanol aqueous solution is 1:10 (g/mL);
(2) Concentrating the first mixed solution at 60 ℃ under reduced pressure, and removing ethanol to obtain a second mixed solution;
(3) Adding 55% calcium carbonate solution (the adding volume ratio of the second mixed solution to the calcium carbonate solution is 1.8:1) into the second mixed solution, stirring and carrying out ultrasonic treatment for 20min (the ultrasonic power is 150W, the temperature is 28 ℃), regulating the pH value to 8, continuing stirring for 40min, and standing and precipitating for 15 h;
(4) The precipitate was collected by centrifugation (centrifugation conditions: 4000g, centrifugation at 25 ℃ C. For 10 min);
(5) Adding 3 times of pure water into the precipitate, repeatedly cleaning for 3 times, drying in a 60 ℃ oven, and performing superfine grinding.
Example 2
The embodiment provides a preparation method of bromofluorescein lake saturation, which comprises the following preparation steps:
(1) Mixing 4',5' -dibromofluorescein with an acidic ethanol aqueous solution with a volume concentration of 75% (the pH value is adjusted to 2.0 by adopting hydrochloric acid) to obtain a first mixed solution, wherein the adding mass volume ratio of the 4',5' -dibromofluorescein to the acidic ethanol aqueous solution is 1:10 (g/mL);
(2) Concentrating the first mixed solution at 60 ℃ under reduced pressure, and removing ethanol to obtain a second mixed solution;
(3) Adding 55% calcium carbonate solution (the adding volume ratio of the second mixed solution to the calcium carbonate solution is 2:1) into the second mixed solution, stirring and carrying out ultrasonic treatment for 30min (the ultrasonic power is 150W, the temperature is 28 ℃), regulating the pH value to 8, continuing stirring for 40min, and standing and precipitating for 15 h;
(4) The precipitate was collected by centrifugation (centrifugation conditions: 4000g, centrifugation at 25 ℃ C. For 10 min);
(5) Adding 3 times of pure water into the precipitate, repeatedly cleaning for 3 times, drying in a 60 ℃ oven, and performing superfine grinding.
Example 3
The embodiment provides a preparation method of bromofluorescein lake saturation, which comprises the following preparation steps:
(1) Mixing 4',5' -dibromofluorescein with an acidic ethanol water solution with a volume concentration of 85% (the pH value is adjusted to 3.0 by adopting hydrochloric acid) to obtain a first mixed solution, wherein the adding mass volume ratio of the 4',5' -dibromofluorescein to the acidic ethanol water solution is 1:10 (g/mL);
(2) Concentrating the first mixed solution at 60 ℃ under reduced pressure, and removing ethanol to obtain a second mixed solution;
(3) Adding 55% calcium carbonate solution (the adding volume ratio of the second mixed solution to the calcium carbonate solution is 1.8:1) into the second mixed solution, stirring and carrying out ultrasonic treatment for 20min (the ultrasonic power is 150W, the temperature is 28 ℃), regulating the pH value to 8, continuing stirring for 40min, and standing and precipitating for 15 h;
(4) The precipitate was collected by centrifugation (centrifugation conditions: 4000g, centrifugation at 25 ℃ C. For 10 min);
(5) Adding 3 times of pure water into the precipitate, repeatedly cleaning for 3 times, drying in a 60 ℃ oven, and performing superfine grinding.
Example 4
The embodiment provides a preparation method of bromofluorescein lake saturation, which comprises the following preparation steps:
(1) Mixing 4',5' -dibromofluorescein with an acidic ethanol aqueous solution with the volume concentration of 80% (the pH value is adjusted to 2.0 by adopting hydrochloric acid) to obtain a first mixed solution, wherein the adding mass volume ratio of the 4',5' -dibromofluorescein to the acidic ethanol aqueous solution is 1:10 (g/mL);
(2) Concentrating the first mixed solution at 60 ℃ under reduced pressure, and removing ethanol to obtain a second mixed solution;
(3) Adding 50% calcium carbonate solution (the adding volume ratio of the second mixed solution to the calcium carbonate solution is 2:1) into the second mixed solution, stirring and carrying out ultrasonic treatment for 20min (the ultrasonic power is 150W, the temperature is 28 ℃), regulating the pH value to 8, continuing stirring for 40min, and standing and precipitating for 15 h;
(4) The precipitate was collected by centrifugation (centrifugation conditions: 4000g, centrifugation at 25 ℃ C. For 10 min);
(5) Adding 3 times of pure water into the precipitate, repeatedly cleaning for 3 times, drying in a 60 ℃ oven, and performing superfine grinding.
Example 5
The embodiment provides a preparation method of bromofluorescein lake saturation, which comprises the following preparation steps:
(1) Mixing 4',5' -dibromofluorescein with an acidic ethanol water solution with a volume concentration of 85% (the pH value is adjusted to 1.0 by adopting hydrochloric acid) to obtain a first mixed solution, wherein the adding mass volume ratio of the 4',5' -dibromofluorescein to the acidic ethanol water solution is 1:10 (g/mL);
(2) Concentrating the first mixed solution at 60 ℃ under reduced pressure, and removing ethanol to obtain a second mixed solution;
(3) Adding 55% calcium carbonate solution (the adding volume ratio of the second mixed solution to the calcium carbonate solution is 1.8:1) into the second mixed solution, stirring and carrying out ultrasonic treatment for 20min (the ultrasonic power is 150W, the temperature is 28 ℃), regulating the pH value to 8, continuing stirring for 40min, and standing and precipitating for 15 h;
(4) The precipitate was collected by centrifugation (centrifugation conditions: 4000g, centrifugation at 25 ℃ C. For 10 min);
(5) Adding 3 times of pure water into the precipitate, repeatedly cleaning for 3 times, drying in a 60 ℃ oven, and performing superfine grinding.
Comparative example 1
This comparative example presents a method for preparing bromofluorescein lake saturation, which differs from example 1 in that: the volume concentration of the acidic aqueous ethanol solution was 50%.
Comparative example 2
This comparative example presents a method for preparing bromofluorescein lake saturation, which differs from example 1 in that: the volume concentration of the acidic aqueous ethanol solution was 90%.
Comparative example 3
This comparative example presents a method for preparing bromofluorescein lake saturation, which differs from example 1 in that: in the step (3), the adding volume ratio of the second mixed solution to the calcium carbonate solution is 1:1.
comparative example 4
This comparative example presents a method for preparing bromofluorescein lake saturation, which differs from example 1 in that: in the step (3), the adding volume ratio of the second mixed solution to the calcium carbonate solution is 1:2.3.
comparative example 5
This comparative example presents a method for preparing bromofluorescein lake saturation, which differs from example 1 in that: the mass concentration of the calcium carbonate is 45%.
Comparative example 6
This comparative example presents a method for preparing bromofluorescein lake saturation, which differs from example 1 in that: the mass concentration of the calcium carbonate is 60%.
Test examples
The following performance tests were performed on the bromofluorescein-based lakes prepared in examples 1 to 5 and comparative examples 1 to 6:
1. laked adsorption quantity
In the preparation process of the bromofluorescein lake, collecting the supernatant after centrifugation in the step (4), measuring the content of 4',5' -dibromofluorescein in the supernatant, and calculating the pigment adsorption quantity (mg/g).
2. Color and luster of
The b values of the 4',5' -dibromofluorescein lakes prepared in examples 1 to 5 and comparative examples 1 to 6 were respectively measured using color difference values. Lakes compare the b values, with lower b values indicating darker shades, higher concentrations, and higher saturation.
3. Laked adsorption stability
50mg of the 4',5' -dibromofluorescein lakes prepared in examples 1 to 5 and comparative examples 1 to 6 were weighed, transferred to 100mL of saliva simulation (pH 7), stirred at a speed of 100rpm, and after 2min, the content of pigment released from the solution was detected, and the content of pigment remaining in the lakes was calculated as a percentage, with the more pigment remaining and the more stable the lake.
4. Color stability of lakes
The 4',5' -dibromofluorescein lakes prepared in examples 1 to 5 and comparative examples 1 to 6 were placed in an illumination incubator, respectively, with the illumination intensity set at 15000LX and the illumination temperature at 28 ℃. The change of the color value of the color lake with time is detected, and the decrease of the chromaticity (the increase of the b value) after 48 hours is taken as a sign for measuring the color stability of the color lake, wherein the smaller the change of the b value is, the higher the color stability is.
TABLE 1
The results are shown in Table 1, and it can be seen from Table 1 that the effect of the lake prepared by the inventive example is good, the absorption amount of the lake is high, the purity and stability are higher, and the saturation degree is significantly improved.
The table only shows the research results taking 4',5' -dibromo fluorescein lake as an object, and for other bromofluorescein lakes, the preparation method and performance test experiments are consistent with those of the 4',5' -dibromo fluorescein lake, the test results are similar to those of the 4',5' -dibromo fluorescein lake, and the test results show the general applicability of the technical scheme protected by the patent.
In summary, the invention provides a preparation method of bromofluorescein lake saturation, and the bromofluorescein lake prepared by the method has excellent color stability, storage stability, high purity and high saturation, is relatively safe in preparation raw materials, and can be widely applied to industries such as food, medicines, cosmetics and the like.
While the embodiments of the present invention have been described in detail, the present invention is not limited to the above embodiments, and various changes can be made without departing from the spirit of the present invention within the knowledge of those skilled in the art. Furthermore, embodiments of the invention and features of the embodiments may be combined with each other without conflict.
Claims (10)
1. A method for improving the saturation of bromofluorescein lakes, comprising the steps of:
s1, mixing bromofluorescein with an acidic ethanol aqueous solution with the volume concentration of 60-85%, and removing ethanol to obtain a mixed solution;
s2, adding a precipitant into the mixed solution, regulating the pH value of the solution to 7-9, carrying out solid-liquid separation, and collecting a solid phase, namely the bromofluorescein lake.
2. The method of claim 1, wherein the bromofluorescein comprises at least one of 4',5' -dibromofluorescein, 2',4',5',7' -tetrabromofluorescein, 2',4',5',7' -tetrabromo-4, 7-dichlorofluorescein, and 2',4',5',7' -tetrabromo-4, 5,6, 7-tetrachlorofluorescein.
3. The method according to claim 1, wherein the acidic aqueous ethanol solution has a pH of 1 to 5.
4. The method according to claim 1, wherein the pH is adjusted with acetic acid, hydrochloric acid or aqueous ammonia.
5. The preparation method of claim 1, wherein the mass-volume ratio of the bromofluorescein to the acidic ethanol solution is 1g (4-12) mL.
6. The method of claim 1, wherein the precipitant comprises aluminum chloride hexahydrate, calcium carbonate, or calcium acetate solution; preferably, the mass fraction of the precipitant is 40-60%.
7. The preparation method according to claim 1, wherein the addition volume ratio of the mixed solution to the precipitant is (1-3): 1.
8. the method of claim 1, further comprising the steps of stirring and sonication after the precipitating agent is added; preferably, the power of the ultrasonic wave is 140-170W, the temperature is 25-30 ℃, and the ultrasonic wave time is 6-10 min.
9. A bromofluorescein lake prepared by the method of any one of claims 1-8.
10. Use of a bromofluorescein-based lake according to claim 9 in dyes, inks, pigments, for the preparation of medicaments, cosmetics or food.
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| CN202310236968.3A CN116355437A (en) | 2023-03-13 | 2023-03-13 | Preparation method for improving saturation of bromofluorescein lake |
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| CN202310236968.3A CN116355437A (en) | 2023-03-13 | 2023-03-13 | Preparation method for improving saturation of bromofluorescein lake |
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|---|---|---|---|---|
| US2157667A (en) * | 1938-06-15 | 1939-05-09 | Max Factor & Co | Dyestuff and method of making the same |
| CN1884389A (en) * | 2005-06-21 | 2006-12-27 | 福建农林大学 | Monascus color color lake and preparation method thereof |
| CN107936607A (en) * | 2017-12-04 | 2018-04-20 | 上海染料研究所有限公司 | A kind of preparation method of bromo fluoresceins cosmetic dyes |
| CN113563360A (en) * | 2021-08-16 | 2021-10-29 | 中国科学技术大学 | Amphiphilic fluorescent dye and synthetic method and application thereof |
-
2023
- 2023-03-13 CN CN202310236968.3A patent/CN116355437A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US2157667A (en) * | 1938-06-15 | 1939-05-09 | Max Factor & Co | Dyestuff and method of making the same |
| CN1884389A (en) * | 2005-06-21 | 2006-12-27 | 福建农林大学 | Monascus color color lake and preparation method thereof |
| CN107936607A (en) * | 2017-12-04 | 2018-04-20 | 上海染料研究所有限公司 | A kind of preparation method of bromo fluoresceins cosmetic dyes |
| CN113563360A (en) * | 2021-08-16 | 2021-10-29 | 中国科学技术大学 | Amphiphilic fluorescent dye and synthetic method and application thereof |
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