CN115960474B - Preparation method of high-solid-content liquid brilliant blue - Google Patents
Preparation method of high-solid-content liquid brilliant blue Download PDFInfo
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- CN115960474B CN115960474B CN202211661391.2A CN202211661391A CN115960474B CN 115960474 B CN115960474 B CN 115960474B CN 202211661391 A CN202211661391 A CN 202211661391A CN 115960474 B CN115960474 B CN 115960474B
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- SGHZXLIDFTYFHQ-UHFFFAOYSA-L Brilliant Blue Chemical compound [Na+].[Na+].C=1C=C(C(=C2C=CC(C=C2)=[N+](CC)CC=2C=C(C=CC=2)S([O-])(=O)=O)C=2C(=CC=CC=2)S([O-])(=O)=O)C=CC=1N(CC)CC1=CC=CC(S([O-])(=O)=O)=C1 SGHZXLIDFTYFHQ-UHFFFAOYSA-L 0.000 title claims abstract description 103
- 239000007788 liquid Substances 0.000 title claims abstract description 70
- 238000002360 preparation method Methods 0.000 title claims abstract description 31
- IXPNQXFRVYWDDI-UHFFFAOYSA-N 1-methyl-2,4-dioxo-1,3-diazinane-5-carboximidamide Chemical compound CN1CC(C(N)=N)C(=O)NC1=O IXPNQXFRVYWDDI-UHFFFAOYSA-N 0.000 claims abstract description 75
- 235000010413 sodium alginate Nutrition 0.000 claims abstract description 75
- 229940005550 sodium alginate Drugs 0.000 claims abstract description 75
- 239000000661 sodium alginate Substances 0.000 claims abstract description 75
- 239000004952 Polyamide Substances 0.000 claims abstract description 26
- 229920002647 polyamide Polymers 0.000 claims abstract description 26
- 238000000034 method Methods 0.000 claims abstract description 20
- 239000007787 solid Substances 0.000 claims abstract description 17
- 239000002904 solvent Substances 0.000 claims abstract description 6
- 238000002156 mixing Methods 0.000 claims abstract description 5
- 239000007864 aqueous solution Substances 0.000 claims abstract description 3
- 239000000243 solution Substances 0.000 claims description 47
- JQWHASGSAFIOCM-UHFFFAOYSA-M sodium periodate Chemical compound [Na+].[O-]I(=O)(=O)=O JQWHASGSAFIOCM-UHFFFAOYSA-M 0.000 claims description 24
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 19
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 13
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 13
- 238000007254 oxidation reaction Methods 0.000 claims description 12
- 238000003756 stirring Methods 0.000 claims description 10
- 238000006243 chemical reaction Methods 0.000 claims description 4
- 230000003647 oxidation Effects 0.000 claims description 3
- 238000001035 drying Methods 0.000 claims description 2
- 238000012869 ethanol precipitation Methods 0.000 claims description 2
- 238000000746 purification Methods 0.000 claims description 2
- 239000002537 cosmetic Substances 0.000 abstract description 3
- 229940079593 drug Drugs 0.000 abstract description 3
- 239000003814 drug Substances 0.000 abstract description 3
- 235000013305 food Nutrition 0.000 abstract description 3
- 239000002994 raw material Substances 0.000 abstract description 3
- 239000000843 powder Substances 0.000 description 26
- 230000000052 comparative effect Effects 0.000 description 17
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 14
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 14
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 14
- 230000000694 effects Effects 0.000 description 9
- 230000014759 maintenance of location Effects 0.000 description 9
- 239000000049 pigment Substances 0.000 description 9
- 230000001590 oxidative effect Effects 0.000 description 8
- 238000005303 weighing Methods 0.000 description 8
- 238000001914 filtration Methods 0.000 description 7
- 238000004108 freeze drying Methods 0.000 description 7
- 238000010438 heat treatment Methods 0.000 description 7
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 description 7
- 239000011780 sodium chloride Substances 0.000 description 7
- 238000012360 testing method Methods 0.000 description 5
- 230000009286 beneficial effect Effects 0.000 description 4
- 239000002245 particle Substances 0.000 description 4
- 238000002835 absorbance Methods 0.000 description 3
- 238000001514 detection method Methods 0.000 description 3
- 238000013112 stability test Methods 0.000 description 3
- 239000003086 colorant Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000004062 sedimentation Methods 0.000 description 2
- 230000000087 stabilizing effect Effects 0.000 description 2
- SHHKMWMIKILKQW-UHFFFAOYSA-N 2-formylbenzenesulfonic acid Chemical compound OS(=O)(=O)C1=CC=CC=C1C=O SHHKMWMIKILKQW-UHFFFAOYSA-N 0.000 description 1
- BQGRVFPPZJPWPB-UHFFFAOYSA-N 3-[(n-ethylanilino)methyl]benzenesulfonic acid Chemical compound C=1C=CC=CC=1N(CC)CC1=CC=CC(S(O)(=O)=O)=C1 BQGRVFPPZJPWPB-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 125000003368 amide group Chemical group 0.000 description 1
- 239000001055 blue pigment Substances 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 230000032798 delamination Effects 0.000 description 1
- 238000003795 desorption Methods 0.000 description 1
- 238000010790 dilution Methods 0.000 description 1
- 239000012895 dilution Substances 0.000 description 1
- 239000000975 dye Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 239000001052 yellow pigment Substances 0.000 description 1
Classifications
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W90/00—Enabling technologies or technologies with a potential or indirect contribution to greenhouse gas [GHG] emissions mitigation
- Y02W90/10—Bio-packaging, e.g. packing containers made from renewable resources or bio-plastics
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- Cosmetics (AREA)
Abstract
The invention discloses a preparation method of high-solid-content liquid brilliant blue. The preparation method of the high-solid-content liquid brilliant blue comprises the following steps: adding oxidized sodium alginate, hyperbranched polyamide and brilliant blue into a solvent at the temperature of 90-120 ℃ and mixing to obtain the aqueous solution; wherein, the high-solid content liquid brilliant blue comprises 30 to 60 percent of brilliant blue, 5 to 12 percent of hyperbranched polyamide and 4 to 8 percent of oxidized sodium alginate according to mass percent. The high-solid-content liquid brilliant blue prepared by the method has excellent color stability and storage stability, is relatively safe in preparation raw materials, and can be widely applied to industries such as food, medicines, cosmetics and the like.
Description
Technical Field
The invention relates to the technical field of dyes, in particular to a preparation method of high-solid-content liquid brilliant blue.
Background
Brilliant blue, acid blue NO.9 or edible yellow pigment 1, its molecular formula is C 37 H 34 N 2 Na 2 O 9 S 2 The water-soluble non-azo colorant is prepared by condensing and oxidizing benzaldehyde o-sulfonic acid and N-ethyl-N- (3-sulfobenzyl) -aniline. Brilliant blue is an important colorant and is widely applied in the industries of foods, medicines, cosmetics and the like.
In the related art, in order to avoid the defects of caking of powdery brilliant blue, inaccurate liquid preparation weighing and the like, the powdery brilliant blue is prepared into liquid brilliant blue. However, in practical application, although powder pollution caused by powdery brilliant blue is reduced to a certain extent after the powdery brilliant blue is prepared into the liquid brilliant blue, and the preparation is promoted to be more uniform, the powdery brilliant blue has limited solubility in a solvent (such as 18.7g/100mL in water at 21 ℃), and when the solid content in the liquid brilliant blue is lower, the transportation cost is high, so that the enterprise is not beneficial to saving the cost; when the solid content in the liquid brilliant blue is higher, the brilliant blue particles are easy to settle, and the stability of the liquid brilliant blue is seriously affected.
Therefore, there is a need for a method for preparing high solid content liquid brilliant blue, which not only can increase the solid content of liquid brilliant blue, but also can prepare liquid brilliant blue with excellent stability.
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 the preparation method of the high-solid-content liquid brilliant blue, which can effectively improve the pigment stability and the storage stability of the liquid brilliant blue.
The invention discloses a preparation method of high-solid-content liquid brilliant blue, which comprises the following steps: adding oxidized sodium alginate, hyperbranched polyamide and brilliant blue into a solvent at the temperature of 90-120 ℃ and mixing to obtain the aqueous solution;
wherein, the high-solid content liquid brilliant blue comprises 30 to 60 percent of brilliant blue, 5 to 12 percent of hyperbranched polyamide and 4 to 8 percent of oxidized sodium alginate according to mass percent.
The preparation method provided by the embodiment of the invention has at least the following beneficial effects:
(1) In the high-solid-content liquid brilliant blue, the stability of the liquid brilliant blue is effectively improved by reasonably matching oxidized sodium alginate, hyperbranched polyamide and brilliant blue, and the color retention rate of the brilliant blue can be improved to a certain extent.
(2) In a high-solid-content liquid brilliant blue system, the hyperbranched structure of the hyperbranched polyamide has an excellent wrapping effect on brilliant blue particles, can effectively relieve sedimentation of brilliant blue pigment, and further, oxidized sodium alginate is added in the system, the hyperbranched polyamide can be grafted on the oxidized sodium alginate, and the hyperbranched polyamide and the oxidized sodium alginate are matched for use, so that the hyperbranched polyamide has an excellent effect of promoting stability in a solution.
(3) The preparation method of the high-solid-content liquid brilliant blue is simple and has high raw material safety.
In some embodiments of the invention, polyvinyl alcohol is also added to the high solids liquid brilliant blue.
In some embodiments of the present invention, the polyvinyl alcohol is added in an amount of 2 to 4% by mass.
In some embodiments of the invention, the solvent is water.
In some embodiments of the present invention, the high solids liquid brilliant blue comprises, in mass percent, 50 to 60% brilliant blue, 8 to 12% hyperbranched polyamide, 4 to 5% oxidized sodium alginate, and 2 to 4% polyvinyl alcohol.
In some embodiments of the invention, the stirring speed of the mixing process is 400 to 600rpm.
In some embodiments of the present invention, the preparation method of oxidized sodium alginate specifically includes the following steps:
adding sodium periodate into the sodium alginate solution for oxidation reaction, and purifying and drying after the reaction is finished.
In some embodiments of the invention, the sodium alginate solution contains 1-3% sodium alginate by mass.
In some embodiments of the invention, the final concentration of sodium periodate is from 0.05 to 0.1mol/L.
Too high a concentration of sodium periodate increases the degree of decrease in the molecular weight of sodium alginate, thereby affecting the stabilizing effect on the brilliant blue of the liquid.
In some embodiments of the invention, the time of oxidation is from 6 to 12 hours.
In some embodiments of the invention, the purification employs an ethanol precipitation process.
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 preparation method of the high-solid-content liquid brilliant blue comprises the following preparation steps:
step S1, weighing 10g of sodium alginate powder, adding water to prepare a 2% sodium alginate solution, adding a sodium periodate solution with the final concentration of 0.1mol/L, oxidizing for 6 hours in a dark place, and adding 1mL of glycol to terminate the oxidation reaction to obtain an oxidized sodium alginate solution;
s2, adding 3g of NaCl and 2 times of ethanol into the oxidized sodium alginate solution to precipitate oxidized sodium alginate in the solution, filtering, and freeze-drying to obtain oxidized sodium alginate powder;
and step S3, adding 55g of brilliant blue, 5g of hyperbranched polyamide and 5g of oxidized sodium alginate powder into water under the conditions that the stirring speed is 500rmp and the heating temperature is 100 ℃, and then fixing the volume to 100mL to obtain the high-solid-content liquid brilliant blue.
Example 2
The preparation method of the high-solid-content liquid brilliant blue comprises the following preparation steps:
step S1, weighing 10g of sodium alginate powder, adding water to prepare a 2% sodium alginate solution, adding a sodium periodate solution with the final concentration of 0.1mol/L, oxidizing for 6 hours in a dark place, and adding 1mL of glycol to terminate the oxidation reaction to obtain an oxidized sodium alginate solution;
s2, adding 3g of NaCl and 2 times of ethanol into the oxidized sodium alginate solution to precipitate oxidized sodium alginate in the solution, filtering, and freeze-drying to obtain oxidized sodium alginate powder;
and step S3, adding 55g of brilliant blue, 5g of hyperbranched polyamide, 5g of oxidized sodium alginate powder and 2g of polyvinyl alcohol into water under the conditions that the stirring speed is 500rmp and the heating temperature is 100 ℃, and then fixing the volume to 100mL to obtain the high-solid-content liquid brilliant blue.
Example 3
The preparation method of the high-solid-content liquid brilliant blue comprises the following preparation steps:
step S1, weighing 10g of sodium alginate powder, adding water to prepare a 2% sodium alginate solution, adding a sodium periodate solution with the final concentration of 0.1mol/L, oxidizing for 6 hours in a dark place, and adding 1mL of glycol to terminate the oxidation reaction to obtain an oxidized sodium alginate solution;
s2, adding 3g of NaCl and 2 times of ethanol into the oxidized sodium alginate solution to precipitate oxidized sodium alginate in the solution, filtering, and freeze-drying to obtain oxidized sodium alginate powder;
and step S3, adding 55g of brilliant blue, 8g of hyperbranched polyamide, 5g of oxidized sodium alginate powder and 2g of polyvinyl alcohol into water under the conditions that the stirring speed is 500rmp and the heating temperature is 100 ℃, and then fixing the volume to 100mL to obtain the high-solid-content liquid brilliant blue.
Example 4
The preparation method of the high-solid-content liquid brilliant blue comprises the following preparation steps:
step S1, weighing 10g of sodium alginate powder, adding water to prepare a 2% sodium alginate solution, adding a sodium periodate solution with the final concentration of 0.1mol/L, oxidizing for 6 hours in a dark place, and adding 1mL of glycol to terminate the oxidation reaction to obtain an oxidized sodium alginate solution;
s2, adding 3g of NaCl and 2 times of ethanol into the oxidized sodium alginate solution to precipitate oxidized sodium alginate in the solution, filtering, and freeze-drying to obtain oxidized sodium alginate powder;
and step S3, adding 55g of brilliant blue, 12g of hyperbranched polyamide, 5g of oxidized sodium alginate powder and 2g of polyvinyl alcohol into water under the conditions that the stirring speed is 500rmp and the heating temperature is 100 ℃, and then fixing the volume to 100mL to obtain the high-solid-content liquid brilliant blue.
Example 5
The preparation method of the high-solid-content liquid brilliant blue comprises the following preparation steps:
step S1, weighing 10g of sodium alginate powder, adding water to prepare a 2% sodium alginate solution, adding a sodium periodate solution with the final concentration of 0.1mol/L, oxidizing for 6 hours in a dark place, and adding 1mL of glycol to terminate the oxidation reaction to obtain an oxidized sodium alginate solution;
s2, adding 3g of NaCl and 2 times of ethanol into the oxidized sodium alginate solution to precipitate oxidized sodium alginate in the solution, filtering, and freeze-drying to obtain oxidized sodium alginate powder;
and step S3, adding 45g of brilliant blue, 8g of hyperbranched polyamide, 5g of oxidized sodium alginate powder and 2g of polyvinyl alcohol into water under the conditions that the stirring speed is 500rmp and the heating temperature is 100 ℃, and then fixing the volume to 100mL to obtain the high-solid-content liquid brilliant blue.
Example 6
The preparation method of the high-solid-content liquid brilliant blue comprises the following preparation steps:
step S1, weighing 10g of sodium alginate powder, adding water to prepare a 2% sodium alginate solution, adding a sodium periodate solution with the final concentration of 0.1mol/L, oxidizing for 6 hours in a dark place, and adding 1mL of glycol to terminate the oxidation reaction to obtain an oxidized sodium alginate solution;
s2, adding 3g of NaCl and 2 times of ethanol into the oxidized sodium alginate solution to precipitate oxidized sodium alginate in the solution, filtering, and freeze-drying to obtain oxidized sodium alginate powder;
and S3, adding 60g of brilliant blue, 8g of hyperbranched polyamide, 5g of oxidized sodium alginate powder and 2g of polyvinyl alcohol into water under the conditions that the stirring speed is 500rmp and the heating temperature is 100 ℃, and then fixing the volume to 100mL to obtain the high-solid-content liquid brilliant blue.
Comparative example 1
The preparation method of the high-solid-content liquid brilliant blue comprises the following preparation steps:
step S1, weighing 10g of sodium alginate powder, adding water to prepare a 2% sodium alginate solution, adding a sodium periodate solution with the final concentration of 0.1mol/L, oxidizing for 6 hours in a dark place, and adding 1mL of glycol to terminate the oxidation reaction to obtain an oxidized sodium alginate solution;
s2, adding 3g of NaCl and 2 times of ethanol into the oxidized sodium alginate solution to precipitate oxidized sodium alginate in the solution, filtering, and freeze-drying to obtain oxidized sodium alginate powder;
and S3, adding 65g of brilliant blue, 8g of hyperbranched polyamide, 5g of oxidized sodium alginate powder and 2g of polyvinyl alcohol into water under the conditions that the stirring speed is 500rmp and the heating temperature is 100 ℃, and then fixing the volume to 100mL to obtain the high-solid-content liquid brilliant blue.
Comparative example 2
The difference between this comparative example and example 3 is that: the sodium alginate powder in the prepared high-solid-content liquid brilliant blue is not subjected to oxidation treatment.
Comparative example 3
The difference between this comparative example and example 3 is that: the prepared high-solid-content liquid brilliant blue powder is not added with oxidized sodium alginate.
Comparative example 4
The difference between this comparative example and example 3 is that: the prepared high-solid liquid brilliant blue is free of hyperbranched polyamide.
Comparative example 5
The difference between this comparative example and example 3 is that: the reaction in step S3 is carried out at normal temperature (28.+ -. 2 ℃ C.).
Test case
The present test example was conducted to examine the color stability (i.e., pigment retention) and storage stability of the high-solid content liquid brilliant blue obtained in examples 1 to 6 and comparative examples 1 to 5, respectively.
(1) The color stability (pigment retention) test method is as follows: respectively taking 1mL of the prepared high-solid-content liquid brilliant blue, adding 1000mL of deionized water for dilution, uniformly stirring, taking a small amount of brilliant blue solution, detecting absorbance at 629nm, and marking as A 0 The method comprises the steps of carrying out a first treatment on the surface of the Then, after 10 days of standing at 37 ℃ under illumination, a small amount of brilliant blue solution is taken and the absorbance at 629nm is detected and designated A 1 The method comprises the steps of carrying out a first treatment on the surface of the And finally, calculating the pigment retention rate through absorbance before and after treatment, and judging the color stability. The method for calculating the pigment retention rate comprises the following steps:
pigment retention = a 0 /A 1 ×100％。
(2) The storage stability test method is as follows: the high solids liquid brilliant blue prepared above was allowed to stand at 25℃respectively, visually observed for the occurrence of significant precipitation, and the time when delamination occurred for the first time was counted.
The pigment retention and storage stability test results are shown in the following table:
table 1: pigment retention and storage stability test results
From the above test results, it can be seen that the high solid content liquid brilliant blue prepared by the method of the present invention has excellent color stability and storage stability. Wherein:
the test results of example 1 and example 2 show that: the addition of a certain amount of polyvinyl alcohol to the high-solid-content liquid brilliant blue solution of the invention is beneficial to improving the stability of the liquid brilliant blue.
The detection results of example 2, example 3, example 4 and comparative example 4 show that: the hyperbranched polyamide can improve the storage stability and pigment retention rate of the brilliant blue of the liquid to a certain extent, mainly because the hyperbranched polyamide has a hydrogen bond effect between an amide group and the brilliant blue after being dissolved in water, and the hyperbranched structure can have a wrapping effect on the brilliant blue, thereby avoiding sedimentation of brilliant blue particles and improving the stability of the brilliant blue of the liquid. When hyperbranched polyamide is not added into the system (as shown in comparative example 4), the bright blue particles are easy to separate out and generate layering phenomenon due to the loss of the clamping effect.
The detection results of example 5, example 6 and comparative example 1 show that: in the high-solid content liquid brilliant blue solution system of the present invention, the solid content of brilliant blue can reach 60%, whereas when it is higher than 60%, as shown in comparative example 1, the storage stability is lowered and desorption easily occurs.
The detection results of example 3, comparative example 2 and comparative example 3 show that: the oxidized sodium alginate powder is beneficial to improving the stability of a liquid brilliant blue solution system, and is mainly because the oxidized sodium alginate can generate a grafting effect with hyperbranched polyamide, so that the solution system is more stable.
The test results of example 3 and comparative example 5 show that: when the high-solid-content liquid brilliant blue solution is prepared, the reaction temperature is increased, so that the adsorption effect of hyperbranched polyamide and oxidized sodium alginate powder on brilliant blue can be effectively improved, and the stabilizing effect is further improved.
In summary, the invention provides a preparation method of high-solid-content liquid brilliant blue, which has excellent color stability and storage stability, 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 (11)
1. The preparation method of the high-solid-content liquid brilliant blue is characterized by comprising the following steps of: adding oxidized sodium alginate, hyperbranched polyamide and brilliant blue into a solvent at the temperature of 90-120 ℃ and mixing to obtain the aqueous solution;
wherein, the high-solid content liquid brilliant blue comprises 30 to 60 percent of brilliant blue, 5 to 12 percent of hyperbranched polyamide and 4 to 8 percent of oxidized sodium alginate according to mass percent.
2. The method for preparing high-solid-content liquid brilliant blue according to claim 1, wherein polyvinyl alcohol is further added to the high-solid-content liquid brilliant blue.
3. The method for preparing high-solid-content liquid brilliant blue according to claim 2, wherein the added amount of the polyvinyl alcohol is 2-4% by mass.
4. The method for preparing high-solid liquid brilliant blue according to claim 1, wherein the solvent is water.
5. The method for preparing high-solid-content liquid brilliant blue according to claim 3, wherein the high-solid-content liquid brilliant blue comprises 50-60% of brilliant blue, 8-12% of hyperbranched polyamide, 4-5% of oxidized sodium alginate and 2-4% of polyvinyl alcohol according to mass percentage.
6. The method for preparing high solid content liquid brilliant blue according to claim 1, wherein the stirring rotation speed in the mixing process is 400-600 rpm.
7. The method for preparing high-solid-content liquid brilliant blue according to any one of claims 1 to 6, wherein the method for preparing oxidized sodium alginate specifically comprises the following steps:
adding sodium periodate into the sodium alginate solution for oxidation reaction, and purifying and drying after the reaction is finished.
8. The preparation method of high-solid-content liquid brilliant blue according to claim 7, wherein the mass fraction of sodium alginate in the sodium alginate solution is 1-3%.
9. The method for preparing high-solid-content liquid brilliant blue according to claim 7, wherein the final concentration of sodium periodate is 0.05-0.1 mol/L.
10. The method for preparing high-solid-content liquid brilliant blue according to claim 7, wherein the time of the oxidation is 6 to 12 hours.
11. The method for preparing high-solid-content liquid brilliant blue according to claim 7, wherein the purification is performed by ethanol precipitation.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CH648584A5 (en) * | 1981-09-15 | 1985-03-29 | Ciba Geigy Ag | Process for preparing concentrated aqueous formulations of anionic dyes |
| GB0315617D0 (en) * | 2003-07-03 | 2003-08-13 | Burke Michael H | Process for preparing a stable anthelmintic suspension formulation |
| CN105521496A (en) * | 2015-12-28 | 2016-04-27 | 合肥工业大学 | A preparing method of injectable hydrogel of a chemically bonded anticancer medicine |
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- 2022-12-23 CN CN202211661391.2A patent/CN115960474B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CH648584A5 (en) * | 1981-09-15 | 1985-03-29 | Ciba Geigy Ag | Process for preparing concentrated aqueous formulations of anionic dyes |
| GB0315617D0 (en) * | 2003-07-03 | 2003-08-13 | Burke Michael H | Process for preparing a stable anthelmintic suspension formulation |
| CN105521496A (en) * | 2015-12-28 | 2016-04-27 | 合肥工业大学 | A preparing method of injectable hydrogel of a chemically bonded anticancer medicine |
Non-Patent Citations (1)
| Title |
|---|
| 海藻酸钠改性材料的研究进展;柴雍等;现代化工;第38卷(第7期);57-61, 63 * |
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