CN113930086B - Preparation method for improving color and stability of edible lake of calcium carbonate - Google Patents
Preparation method for improving color and stability of edible lake of calcium carbonate Download PDFInfo
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- CN113930086B CN113930086B CN202111208947.8A CN202111208947A CN113930086B CN 113930086 B CN113930086 B CN 113930086B CN 202111208947 A CN202111208947 A CN 202111208947A CN 113930086 B CN113930086 B CN 113930086B
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- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 title claims abstract description 150
- 229910000019 calcium carbonate Inorganic materials 0.000 title claims abstract description 74
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 97
- 239000000049 pigment Substances 0.000 claims abstract description 61
- 239000000243 solution Substances 0.000 claims abstract description 41
- 239000011259 mixed solution Substances 0.000 claims abstract description 40
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 29
- 239000002244 precipitate Substances 0.000 claims abstract description 27
- 238000002156 mixing Methods 0.000 claims abstract description 25
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 claims abstract description 16
- 238000009210 therapy by ultrasound Methods 0.000 claims abstract description 12
- 159000000007 calcium salts Chemical class 0.000 claims abstract description 11
- 125000000129 anionic group Chemical group 0.000 claims abstract description 6
- 239000007864 aqueous solution Substances 0.000 claims abstract description 6
- 238000001035 drying Methods 0.000 claims abstract description 6
- 238000000227 grinding Methods 0.000 claims abstract description 4
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical group [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 60
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 30
- 238000000034 method Methods 0.000 claims description 14
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 claims description 11
- 239000001110 calcium chloride Substances 0.000 claims description 11
- 229910001628 calcium chloride Inorganic materials 0.000 claims description 11
- JMEVHYCNAPFOAB-UHFFFAOYSA-L 2-(3-hydroxy-5-sulfonato-1H-indol-2-yl)-3-oxoindole-5-sulfonate Chemical compound [O-]c1c([nH]c2ccc(cc12)S([O-])(=O)=O)C1=[NH+]c2ccc(cc2C1=O)S([O-])(=O)=O JMEVHYCNAPFOAB-UHFFFAOYSA-L 0.000 claims description 10
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 10
- 239000011734 sodium Substances 0.000 claims description 10
- 229910052708 sodium Inorganic materials 0.000 claims description 10
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Chemical compound [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 claims description 6
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 claims description 4
- 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 claims description 3
- 235000005979 Citrus limon Nutrition 0.000 claims description 3
- 244000131522 Citrus pyriformis Species 0.000 claims description 3
- NKWPZUCBCARRDP-UHFFFAOYSA-L calcium bicarbonate Chemical compound [Ca+2].OC([O-])=O.OC([O-])=O NKWPZUCBCARRDP-UHFFFAOYSA-L 0.000 claims description 3
- 229910000020 calcium bicarbonate Inorganic materials 0.000 claims description 3
- 229910000027 potassium carbonate Inorganic materials 0.000 claims description 3
- 235000009328 Amaranthus caudatus Nutrition 0.000 claims description 2
- 240000001592 Amaranthus caudatus Species 0.000 claims description 2
- LSNNMFCWUKXFEE-UHFFFAOYSA-M Bisulfite Chemical compound OS([O-])=O LSNNMFCWUKXFEE-UHFFFAOYSA-M 0.000 claims description 2
- 235000012735 amaranth Nutrition 0.000 claims description 2
- 239000004178 amaranth Substances 0.000 claims description 2
- 235000012730 carminic acid Nutrition 0.000 claims description 2
- IINNWAYUJNWZRM-UHFFFAOYSA-L erythrosin B Chemical group [Na+].[Na+].[O-]C(=O)C1=CC=CC=C1C1=C2C=C(I)C(=O)C(I)=C2OC2=C(I)C([O-])=C(I)C=C21 IINNWAYUJNWZRM-UHFFFAOYSA-L 0.000 claims description 2
- 125000000542 sulfonic acid group Chemical group 0.000 claims description 2
- 239000002932 luster Substances 0.000 claims 1
- 235000013373 food additive Nutrition 0.000 abstract description 3
- 239000002778 food additive Substances 0.000 abstract description 3
- 230000000052 comparative effect Effects 0.000 description 23
- 235000019441 ethanol Nutrition 0.000 description 23
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 20
- 238000001179 sorption measurement Methods 0.000 description 19
- 238000003756 stirring Methods 0.000 description 19
- 230000000694 effects Effects 0.000 description 6
- 238000012360 testing method Methods 0.000 description 6
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 5
- 230000008859 change Effects 0.000 description 4
- 239000011159 matrix material Substances 0.000 description 4
- 235000000177 Indigofera tinctoria Nutrition 0.000 description 3
- 235000013305 food Nutrition 0.000 description 3
- 238000005286 illumination Methods 0.000 description 3
- 230000006872 improvement Effects 0.000 description 3
- 229940097275 indigo Drugs 0.000 description 3
- COHYTHOBJLSHDF-UHFFFAOYSA-N indigo powder Natural products N1C2=CC=CC=C2C(=O)C1=C1C(=O)C2=CC=CC=C2N1 COHYTHOBJLSHDF-UHFFFAOYSA-N 0.000 description 3
- 239000006228 supernatant Substances 0.000 description 3
- 239000003463 adsorbent Substances 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- TYJJADVDDVDEDZ-UHFFFAOYSA-M potassium hydrogencarbonate Chemical compound [K+].OC([O-])=O TYJJADVDDVDEDZ-UHFFFAOYSA-M 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 239000000758 substrate Substances 0.000 description 2
- 208000024827 Alzheimer disease Diseases 0.000 description 1
- 239000000120 Artificial Saliva Substances 0.000 description 1
- 206010006187 Breast cancer Diseases 0.000 description 1
- 208000026310 Breast neoplasm Diseases 0.000 description 1
- 206010039966 Senile dementia Diseases 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- 229940069428 antacid Drugs 0.000 description 1
- 239000003159 antacid agent Substances 0.000 description 1
- 230000001458 anti-acid effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 210000000988 bone and bone Anatomy 0.000 description 1
- 229940069978 calcium supplement Drugs 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000003086 colorant Substances 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 235000002864 food coloring agent Nutrition 0.000 description 1
- 235000010855 food raising agent Nutrition 0.000 description 1
- KHLVKKOJDHCJMG-QDBORUFSSA-L indigo carmine Chemical compound [Na+].[Na+].N/1C2=CC=C(S([O-])(=O)=O)C=C2C(=O)C\1=C1/NC2=CC=C(S(=O)(=O)[O-])C=C2C1=O KHLVKKOJDHCJMG-QDBORUFSSA-L 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000003550 marker Substances 0.000 description 1
- 210000005036 nerve Anatomy 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 238000004088 simulation Methods 0.000 description 1
- 238000002798 spectrophotometry method Methods 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 230000001360 synchronised effect Effects 0.000 description 1
- 238000005406 washing Methods 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
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
- A23L5/00—Preparation or treatment of foods or foodstuffs, in general; Food or foodstuffs obtained thereby; Materials therefor
- A23L5/40—Colouring or decolouring of foods
- A23L5/42—Addition of dyes or pigments, e.g. in combination with optical brighteners
- A23L5/47—Addition of dyes or pigments, e.g. in combination with optical brighteners using synthetic organic dyes or pigments not covered by groups A23L5/43 - A23L5/46
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23V—INDEXING SCHEME RELATING TO FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES AND LACTIC OR PROPIONIC ACID BACTERIA USED IN FOODSTUFFS OR FOOD PREPARATION
- A23V2002/00—Food compositions, function of food ingredients or processes for food or foodstuffs
Landscapes
- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Nutrition Science (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Food Science & Technology (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Coloring Foods And Improving Nutritive Qualities (AREA)
Abstract
The invention relates to the technical field of food additives, and provides a preparation method for improving the color and stability of edible lakes of calcium carbonate, which comprises the following steps: s1, dissolving carbonate in water to prepare carbonate aqueous solution; s2, adding a water-soluble anionic pigment into the carbonate aqueous solution obtained in the step S1 to obtain a mixed solution; s3, adding ethanol into the S2 mixed solution, fully mixing, and adjusting the pH to 9-11; s4, dissolving calcium salt in water, adding ethanol, mixing uniformly, mixing into the solution obtained in the S3, carrying out ultrasonic treatment for 1-10 minutes, and centrifugally collecting calcium carbonate precipitate adsorbed with pigment; s5, drying and grinding the calcium carbonate precipitate adsorbed with the pigment obtained in the step S4 to obtain the edible lake based on calcium carbonate. By the technical scheme, the color and stability of the edible calcium carbonate lake are obviously improved.
Description
Technical Field
The invention relates to the technical field of food additives, in particular to a preparation method for improving the color and stability of edible lakes of calcium carbonate.
Background
The lake is a water-insoluble pigment product obtained by adsorbing a water-soluble pigment on a water-insoluble substrate, separating the pigment-adsorbed substrate, and drying. When the pigment, matrix and other reagents used are food grade, the resulting lake is an edible lake. In the preparation of edible lakes, aluminum hydroxide is the traditional adsorption matrix and is most widely used. Numerous studies have shown that excessive intake of aluminum may lead to senile dementia, increase the incidence of breast cancer, and possibly affect the development of bones and nerves of newborns, making the safety of aluminum hydroxide-based lakes questioned. At present, the search for a safe and reliable adsorption matrix to replace aluminum hydroxide for preparing lakes is an urgent goal in the food pigment industry. Current research indicates that the use of calcium carbonate instead of aluminum hydroxide is a very potential solution.
Calcium carbonate is a common food additive which has wide application and can be used as a calcium supplement, a colorant, a leavening agent, an antacid and the like. The calcium carbonate particles have significant surface charge and flexible surface modification properties and can be applied as adsorbents. It has been found that calcium carbonate exhibits good adsorptivity to a variety of water-soluble anionic food colors, and has the ability to prepare lakes.
The invention patent 'a preparation method of edible lake based on calcium carbonate' (application number 201910512968.5) discloses a novel lake preparation technology based on calcium carbonate: firstly adding pigment into carbonate solution to form mixed solution, then regulating pH value, adding calcium salt, then making ultrasonic treatment, centrifuging, drying and grinding so as to obtain the invented edible calcium carbonate lake. It is found that the adsorption between calcium carbonate and pigment is electrostatic adsorption or is mainly driven by electrostatic adsorption. However, unlike aluminum hydroxide, the use of calcium carbonate as an adsorbent and theoretical research are relatively lacking, and there is room for further improvement in the color and stability of calcium carbonate lakes, which has certain limitations in application, particularly in high-moisture foods, due to the lack of adsorption stability.
Disclosure of Invention
The invention provides a preparation method for improving the color and stability of an edible calcium carbonate lake, which solves the problems that the preparation method of the calcium carbonate lake in the prior art is to be improved in the aspects of color and stability of the lake and is limited in application.
The technical scheme of the invention is as follows:
a preparation method for improving the color and stability of calcium carbonate edible lakes, which comprises the following steps:
s1, dissolving carbonate in water to prepare carbonate aqueous solution;
s2, adding a water-soluble anionic pigment into the carbonate aqueous solution obtained in the step S1 to obtain a mixed solution;
s3, adding ethanol into the S2 mixed solution, fully mixing, and adjusting the pH to 9-11;
s4, dissolving calcium salt in water, adding ethanol, mixing uniformly, mixing into the solution obtained in the S3, carrying out ultrasonic treatment for 1-10 minutes, and centrifuging to collect calcium carbonate precipitate adsorbed with pigment.
As a further technical scheme, the method further comprises S5, and the edible lake based on calcium carbonate is obtained by drying and grinding the calcium carbonate precipitate obtained in the step S4.
As a further technical scheme, in the step S1, the carbonate is sodium carbonate or potassium carbonate.
As a further technical scheme, in the step S1, the mass concentration of the carbonate solution is 0.9% -1.2%.
As a further technical scheme, in the step S2, the water-soluble anionic pigment is a pigment containing sulfonic acid groups or a pigment containing carboxyl groups.
As a further technical scheme, the sulfonic acid-containing primary pigment comprises one or more of sodium indigotin disulfonate, brilliant blue, lemon yellow, sunset yellow, amaranth, neored, carmine and allure red, and the carboxyl-containing pigment is erythrosin.
As a further technical scheme, in the step S3, the ethanol accounts for 9% -11% of the total volume of the solution obtained after the ethanol is mixed with the S2 solution.
As a further technical scheme, in the step S4, the calcium salt is a water-soluble calcium salt selected from calcium chloride or calcium bicarbonate.
As a further technical scheme, in the step S4, the molar ratio of the added calcium salt to the carbonate is 1:1.
As a further technical scheme, in the step S4, the ultrasonic frequency is 25-100kHz.
The beneficial effects of the invention are as follows:
1. the invention uses CaCO 3 Based on the technology of novel lake production for the matrix, ethanol is added in the preparation process of the lake to further improve the color of the lake. Compared with the prior art without ethanol, the indigo lake blue prepared by the novel process has higher color value and brighter color.
2. The invention increases the use of ethanol in the lake preparation technology, and by adopting specific addition amount and addition sequence, compared with the prior method, the color stability of the lake is greatly improved. Compared with the prior art without ethanol, the indigo lake prepared by the novel process can still keep bright blue after long-time storage, and the color stability of the indigo lake is greatly improved.
3. According to the invention, through the use of ethanol, the relation between calcium carbonate crystallization and adsorption is adjusted, so that calcium carbonate forms a special microstructure, the combination effect between the calcium carbonate and pigment is obviously enhanced, the adsorption stability of the lake is improved, and the application range of the edible lake of the calcium carbonate is widened.
Detailed Description
The technical solutions of the embodiments of the present invention will be clearly and completely described below in conjunction with the embodiments of the present invention, and it is apparent that the described embodiments are only some embodiments of the present invention, not all embodiments. All other embodiments, which can be made by one of ordinary skill in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Example 1
2.0g of sodium carbonate is dissolved in 180mL of water to obtain sodium carbonate solution; adding 50.0mg of sodium indigo disulfonate into the sodium carbonate solution, and stirring fully to completely dissolve the pigment to obtain a mixed solution; adding 20mL of absolute ethyl alcohol into the mixed solution, fully mixing, adding a proper amount of hydrochloric acid, and adjusting the pH of the mixed solution to pH=10.5; dissolving 2.1g of calcium chloride in 22.5mL of water, adding 2.5mL of absolute ethyl alcohol, uniformly mixing, adding into a solution with pH of 10.5, stirring and carrying out ultrasonic treatment for 2min, wherein the ultrasonic frequency is 40kHz, and rapidly centrifuging and collecting a calcium carbonate precipitate adsorbed with pigment by using a centrifuge; the obtained calcium carbonate precipitate adsorbed with pigment is dried in a 60 ℃ oven and then ground to obtain the edible lake based on calcium carbonate.
Example 2
2.0g of sodium carbonate is dissolved in 180mL of water to obtain sodium carbonate solution; adding 80.0mg of brilliant blue into a sodium carbonate solution, and stirring thoroughly to dissolve the pigment completely to obtain a mixed solution; adding 20mL of absolute ethyl alcohol into the mixed solution, fully mixing, adding a proper amount of hydrochloric acid, and adjusting the pH of the mixed solution to pH=10; dissolving 2.1g of calcium chloride in 22.5mL of water, adding 2.5mL of absolute ethyl alcohol, uniformly mixing, adding into a solution with pH=10, stirring and carrying out ultrasonic treatment for 3min, wherein the ultrasonic frequency is 40kHz, and rapidly centrifuging and collecting calcium carbonate precipitates adsorbed with pigment by using a centrifuge; the obtained pigment-adsorbed calcium carbonate precipitate is dried in a 50 ℃ oven and then ground to obtain the edible lake based on calcium carbonate.
Example 3
2.0g of sodium carbonate is dissolved in 180mL of water to obtain sodium carbonate solution; adding 50.0mg of sodium indigo disulfonate into the sodium carbonate solution, and stirring fully to completely dissolve the pigment to obtain a mixed solution; adding 20mL of absolute ethyl alcohol into the mixed solution, fully mixing, adding a proper amount of hydrochloric acid, and adjusting the pH of the mixed solution to pH=10.5; dissolving 3.0g of calcium bicarbonate in 22.5mL of water, adding 2.5mL of absolute ethyl alcohol, uniformly mixing, adding into a solution with pH of 10.5, stirring and carrying out ultrasonic treatment for 1min, wherein the ultrasonic frequency is 40kHz, and rapidly centrifuging and collecting a calcium carbonate precipitate adsorbed with pigment by using a centrifuge; the obtained calcium carbonate precipitate adsorbed with pigment is dried in a 60 ℃ oven and then ground to obtain the edible lake based on calcium carbonate.
Example 4
2.0g of sodium carbonate is dissolved in 180mL of water to obtain sodium carbonate solution; stirring 57.0mg of lemon Huang Jiaru sodium carbonate solution fully to completely dissolve pigment to obtain a mixed solution; adding 20mL of absolute ethyl alcohol into the mixed solution, fully mixing, adding a proper amount of hydrochloric acid, and adjusting the pH of the mixed solution to pH=10.5; dissolving 2.1g of calcium chloride in 22.5mL of water, adding 2.5mL of absolute ethyl alcohol, uniformly mixing, adding into a solution with pH of 10.5, stirring and carrying out ultrasonic treatment for 3min, wherein the ultrasonic frequency is 60kHz, and rapidly centrifuging and collecting a calcium carbonate precipitate adsorbed with pigment by using a centrifuge; the obtained calcium carbonate precipitate adsorbed with pigment is dried in an oven at 80 ℃ and then ground to obtain the edible lake based on calcium carbonate.
Example 5
2.0g of sodium carbonate was dissolved in 190mL of water to obtain a sodium carbonate solution; adding 50.0mg of sodium indigo disulfonate into the sodium carbonate solution, and stirring fully to completely dissolve the pigment to obtain a mixed solution; adding 25mL of absolute ethyl alcohol into the mixed solution, fully mixing, adding a proper amount of hydrochloric acid, and adjusting the pH of the mixed solution to pH=10; dissolving 2.1g of calcium chloride in 22.5mL of water, adding 2.5mL of absolute ethyl alcohol, uniformly mixing, adding into a solution with pH=10, stirring and carrying out ultrasonic treatment for 3min, wherein the ultrasonic frequency is 80kHz, and rapidly centrifuging and collecting calcium carbonate precipitates adsorbed with pigment by using a centrifuge; the obtained calcium carbonate precipitate adsorbed with pigment is dried in a 60 ℃ oven and then ground to obtain the edible lake based on calcium carbonate.
Example 6
2.0g of potassium carbonate was dissolved in 180mL of water to obtain a potassium carbonate solution; adding 50.0mg of sodium indigo disulfonate into the potassium carbonate solution, and stirring fully to completely dissolve the pigment to obtain a mixed solution; adding 20mL of absolute ethyl alcohol into the mixed solution, fully mixing, adding a proper amount of hydrochloric acid, and adjusting the pH of the mixed solution to pH=10; dissolving 1.6g of calcium chloride in 22.5mL of water, adding 2.5mL of absolute ethyl alcohol, uniformly mixing, adding into a solution with pH=10, stirring and carrying out ultrasonic treatment for 2.5min, wherein the ultrasonic frequency is 60kHz, and rapidly centrifuging and collecting a calcium carbonate precipitate adsorbed with pigment by using a centrifuge; the obtained calcium carbonate precipitate adsorbed with pigment is dried in a 60 ℃ oven and then ground to obtain the edible lake based on calcium carbonate.
Comparative example 1
2.0g of sodium carbonate was dissolved in 200mL of water to obtain a sodium carbonate solution; adding 50.0mg of sodium indigo disulfonate into the sodium carbonate solution, and stirring fully to completely dissolve the pigment to obtain a mixed solution; adding a proper amount of hydrochloric acid into the mixed solution, and adjusting the pH of the mixed solution to pH=10.5; 2.1g of calcium chloride is dissolved in 25mL of water and added to the solution with pH=10.5, stirred and sonicated for 2min at an ultrasonic frequency of 40kHz, and the calcium carbonate precipitate adsorbed with pigment is rapidly centrifuged and collected using a centrifuge; the obtained calcium carbonate precipitate adsorbed with pigment is dried in a 60 ℃ oven and then ground to obtain the edible lake based on calcium carbonate.
Comparative example 2
2.0g of sodium carbonate is dissolved in a mixed solution of 180mL of water and 20mL of ethanol to obtain a sodium carbonate/ethanol/water solution; adding 50.0mg of sodium indigo disulfonate into the sodium carbonate/ethanol/water solution, and stirring thoroughly to dissolve the pigment completely to obtain a mixed solution; adding a proper amount of hydrochloric acid into the mixed solution, and adjusting the pH of the mixed solution to pH=10.5; 2.1g of calcium chloride is dissolved in a mixed solution of 22.5mL of water and 2.5mL of ethanol, then added into the solution with pH=10.5, stirred and sonicated for 2min, the ultrasonic frequency is 40kHz, and the calcium carbonate precipitate adsorbed with pigment is rapidly centrifuged and collected by using a centrifuge; the obtained calcium carbonate precipitate adsorbed with pigment is dried in a 60 ℃ oven and then ground to obtain the edible lake based on calcium carbonate.
Comparative example 3
2.0g of sodium carbonate was dissolved in 140mL of water to obtain a sodium carbonate solution; adding 50.0mg of sodium indigo disulfonate into the sodium carbonate solution, and stirring fully to completely dissolve the pigment to obtain a mixed solution; adding 60mL of absolute ethyl alcohol into the mixed solution, fully mixing, adding a proper amount of hydrochloric acid, and adjusting the pH of the mixed solution to pH=10.5; dissolving 2.1g of calcium chloride in 17.5mL of water, adding 7.5mL of absolute ethyl alcohol, uniformly mixing, adding into the solution with pH of 10.5, stirring and carrying out ultrasonic treatment for 2min, wherein the ultrasonic frequency is 40kHz, and rapidly centrifuging and collecting the calcium carbonate precipitate adsorbed with pigment by using a centrifuge; the obtained calcium carbonate precipitate adsorbed with pigment is dried in a 60 ℃ oven and then ground to obtain the edible lake based on calcium carbonate.
Comparative example 4
2.0g of sodium carbonate is dissolved in 100mL of water to obtain sodium carbonate solution; adding 50.0mg of sodium indigo disulfonate into the sodium carbonate solution, and stirring fully to completely dissolve the pigment to obtain a mixed solution; adding 100mL of absolute ethyl alcohol into the mixed solution, fully mixing, adding a proper amount of hydrochloric acid, and adjusting the pH of the mixed solution to pH=10.5; dissolving 2.1g of calcium chloride in 12.5mL of water, adding 12.5mL of absolute ethyl alcohol, uniformly mixing, adding into the solution with pH of 10.5, stirring and carrying out ultrasonic treatment for 2min, wherein the ultrasonic frequency is 40kHz, and rapidly centrifuging and collecting the calcium carbonate precipitate adsorbed with pigment by using a centrifuge; the obtained calcium carbonate precipitate adsorbed with pigment is dried in a 60 ℃ oven and then ground to obtain the edible lake based on calcium carbonate.
The detection method comprises the following steps:
pigment adsorption rate: in the preparation of the sample, 4mL of the supernatant was collected by a syringe and filtered through a 0.22 μm filter after centrifugation, and the content of sodium indigo disulfonate in the supernatant was measured by spectrophotometry to calculate the adsorption rate a (%) of the pigment.
The color is as follows: 150mg of the sample was weighed and placed in a No. 0 self-sealing bag, which was then flattened to obtain a flat lake surface. The L, a and b values of the resulting lakes of the examples and comparative examples were measured using color difference, respectively. Blue lakes compare b values, with lower b values indicating a darker blue shade.
Color stability of lakes under light conditions: the sample prepared in the color performance test was placed in an illumination incubator with an illumination intensity of 12000LX and an illumination temperature of 25 ℃. Detecting the change of the color lake value b with time, and changing the change delta b of the blue color value b after 48 hours 1 Δb as a marker for color stability of lakes 1 Smaller absolute values of (c) indicate higher color stability.
Adsorption stability of pigments in lakes: 200mg of lake was weighed into a No. 0 sealed bag, and then flattened to obtain a flat lake surface. The b values of the samples obtained in the examples and comparative examples were measured using a color difference meter, respectively, and were recorded as b 1 . Transferring the lake in the seal bag into 100mL artificial saliva Simulation Solution (SSF), magnetically stirring at 37 ℃ for 2min at 100rpm, centrifuging (5000 rpm,15 min) in a 50mL centrifuge tube, discarding supernatant, drying the centrifuged precipitate in an oven to obtain new lake sample, flattening in a No. 0 seal film, detecting the b value of the sample with a color difference meter, and recording as b 2 . Change of lake b value Δb 2 (b 2 -b 1 ) As a measure of adsorption stability, the smaller the change in b value (Δb 2 Smaller absolute value) indicates higher adsorption stability.
The test results are set forth in table 1.
Table 1 performance testing of example 1 and comparative lakes
Example 1 is a sample prepared according to the present invention; comparative example 1 is a sample prepared according to the existing calcium carbonate edible lake preparation patent; comparative example 2 is to explore the effect of the order of addition of ethanol on lake properties; comparative examples 3 and 4 are to investigate the effect of different ethanol addition amounts on lake properties. Wherein, the ethanol addition amount of example 1 was 10% (v/v), the ethanol addition amount of comparative example 3 was 30% (v/v), and the ethanol addition amount of comparative example 4 was 50% (v/v).
As can be seen from the test results in the table, example 1 was compared with comparative examples 1 and 2, and example 1 showed a color stability (. DELTA.b) at the pigment adsorption rate (A), the color (b) 1 ) Adsorption stability (Δb) 2 ) And color after rinsing (b) 2 ) The method realizes synchronous optimization and promotion, improves the practicability of the edible lake of the calcium carbonate, and proves that the key steps of adding the ethanol in the lake preparation technology and the key steps of adding the ethanol in the order of adding the ethanol, which are required to be protected by the invention, have practical effects after the sodium carbonate and the pigment are completely dissolved in water.
Example 1 was compared with comparative examples 3 and 4, and comparative examples 3 and 4 were found to be stable only in the adsorption stability index (. DELTA.b) 2 ) The above is dominant, and this is probably due to their significantly lower pigment adsorption rate. Example 1 in other criteria, including pigment adsorption (A), color (b), color stability (Δb) 1 ) And color after rinsing (b) 2 ) The improvement is high. The pigment adsorption ratio of example 1 was about 1.5 to 1.9 times that of comparative example 3 and comparative example 4, the color index was about 1.8 to 5.5 times that of comparative example 3 and comparative example 4, the color stability was about 1.7 to 1.8 times that of comparative example 3 and comparative example 4, and the color b after washing was found 2 About 1.7 to 45.6 times of comparative example 3 and comparative example 4, it was confirmed that the content of ethanol in the present invention also has a significant effect on the color and stability of the lake, and it was demonstrated that the addition amount of ethanol in the present invention is a key step, having a practical effect.
Table 1 presents only the results of the study of example 1, and the tests described above were also performed for the other examples, the test results being similar to those of example 1 and omitted, the test results showing the general applicability of the technical solutions protected by this patent.
Experimental results show that the preparation method for improving the color and the stability of the edible calcium carbonate lake provided by the invention reserves the safety advantage of the existing preparation technology of the edible calcium carbonate lake on one hand, greatly improves the stability and the color performance of the edible calcium carbonate lake on the other hand, has the advantages of simplicity, easiness, convenience in operation and lower cost, widens the application range of the edible calcium carbonate lake, and has great market value.
The foregoing description of the preferred embodiments of the invention is not intended to be limiting, but rather is intended to cover all modifications, equivalents, alternatives, and improvements that fall within the spirit and scope of the invention.
Claims (10)
1. A preparation method for improving the color and stability of an edible lake of calcium carbonate, which is characterized by comprising the following steps:
s1, dissolving carbonate in water to prepare carbonate aqueous solution;
s2, adding a water-soluble anionic pigment into the carbonate aqueous solution obtained in the step S1 to obtain a mixed solution;
s3, adding ethanol into the mixed solution obtained in the step S2, fully mixing, and adjusting the pH to 9-11;
s4, dissolving calcium salt in water, adding ethanol, mixing uniformly, mixing into the solution obtained in the S3, carrying out ultrasonic treatment for 1-10 minutes, and centrifuging to collect calcium carbonate precipitate adsorbed with pigment;
in the step S3, the ethanol accounts for 9% -11% of the total volume of the solution obtained after the ethanol is mixed with the mixed solution obtained in the step S2.
2. The method for preparing the edible lake color and stability of calcium carbonate according to claim 1, wherein the step S4 is further followed by the step S5 of drying and grinding the calcium carbonate precipitate obtained in the step S4 to obtain the edible lake based on calcium carbonate.
3. The method for preparing the edible lake color and stability of calcium carbonate according to claim 1, wherein in the step S1, the carbonate is sodium carbonate or potassium carbonate.
4. The method for preparing the calcium carbonate edible lake color and stability according to claim 1, wherein the mass concentration of the carbonate solution in the step S1 is 0.9% -1.2%.
5. The method for improving the color and luster and stability of an edible lake of calcium carbonate according to claim 1, wherein in the step S2, the water-soluble anionic pigment is a sulfonic acid group-containing pigment or a carboxyl group-containing pigment.
6. The method of claim 5, wherein the primary sulfonic acid-containing pigment comprises one or more of sodium indigo disulfonate, brilliant blue, lemon yellow, sunset yellow, amaranth, neo-red, carmine, and allure red, and the carboxyl-containing pigment is erythrosin.
7. The method for improving the color and stability of an edible lake of calcium carbonate according to claim 1, wherein in the step S4, the calcium salt is a water-soluble calcium salt.
8. The method of claim 7, wherein the water-soluble calcium salt is selected from the group consisting of calcium chloride and calcium bicarbonate.
9. The method for preparing the edible lake color and stability of calcium carbonate according to claim 1, wherein in the step S4, the molar ratio of the added calcium salt to the carbonate is 1:1.
10. The method for preparing the edible lake color and stability of calcium carbonate according to claim 1, wherein the ultrasonic frequency used in the step S4 is 25-100kHz.
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| CN1044671A (en) * | 1990-02-28 | 1990-08-15 | 孙博南 | Manufacturing method of fluorescent ink |
| CN108795096A (en) * | 2018-05-18 | 2018-11-13 | 山东中惠生物科技股份有限公司 | Natural plants color lake and preparation method thereof |
| CN110183873A (en) * | 2019-06-14 | 2019-08-30 | 北京工商大学 | A kind of preparation method of the edible color lake based on calcium carbonate |
| CN110194906A (en) * | 2019-06-17 | 2019-09-03 | 广州素旺生物科技有限公司 | A kind of food grade shellac mixed liquor and preparation method thereof |
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| CN1044671A (en) * | 1990-02-28 | 1990-08-15 | 孙博南 | Manufacturing method of fluorescent ink |
| CN108795096A (en) * | 2018-05-18 | 2018-11-13 | 山东中惠生物科技股份有限公司 | Natural plants color lake and preparation method thereof |
| CN110183873A (en) * | 2019-06-14 | 2019-08-30 | 北京工商大学 | A kind of preparation method of the edible color lake based on calcium carbonate |
| CN110194906A (en) * | 2019-06-17 | 2019-09-03 | 广州素旺生物科技有限公司 | A kind of food grade shellac mixed liquor and preparation method thereof |
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