CN113424855B - Preparation method of temperature-sensitive sorbic acid microcapsule - Google Patents
Preparation method of temperature-sensitive sorbic acid microcapsule Download PDFInfo
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- CN113424855B CN113424855B CN202110427062.0A CN202110427062A CN113424855B CN 113424855 B CN113424855 B CN 113424855B CN 202110427062 A CN202110427062 A CN 202110427062A CN 113424855 B CN113424855 B CN 113424855B
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- A21—BAKING; EDIBLE DOUGHS
- A21D—TREATMENT, e.g. PRESERVATION, OF FLOUR OR DOUGH, e.g. BY ADDITION OF MATERIALS; BAKING; BAKERY PRODUCTS; PRESERVATION THEREOF
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Abstract
The invention discloses a preparation method of a temperature-sensitive sorbic acid microcapsule, which comprises the following steps: preparing a core material: pulverizing sorbic acid; preparing a wall material: melting the oily substance; mixing core materials and wall materials: uniformly mixing and mixing the crushed sorbic acid and the melted oil to obtain a sorbic acid embedding solution; preparing microcapsules: pumping the prepared sorbic acid embedding liquid, spraying and condensing under high pressure to prepare the sorbic acid microcapsule. The invention provides a sorbic acid product suitable for wheaten food fermentation.
Description
Technical Field
The invention belongs to the technical field of baked food, and particularly relates to a preparation method of a temperature-sensitive sorbic acid microcapsule.
Background
The microcapsule technology is a microcapsule technology for storing solid, liquid and gas by wrapping trace substances in a polymer film. The microcapsule has different sizes of 5-200 μm and various shapes, and can change the state of substance, protect sensitive components, isolate the interaction between materials, reduce volatility, control release, mix insoluble components, reduce the toxicity of some chemical additives, prolong storage time, store heat energy, etc. Microcapsules made with a particular wall material selected can function to release the encapsulated core material in a particular environment by being destroyed in a particular external environment, such as a particular temperature, pH, pressure, and the like.
Sorbic acid and potassium sorbate are the most widely used preservatives internationally, have higher antibacterial performance, inhibit the growth and propagation of mould, inhibit the growth of microorganism and play a role in antisepsis by inhibiting dehydrogenase systems in microorganisms, have the inhibiting effect on mould, saccharomycetes and part of aerobic bacteria, and are widely used for antisepsis of various cheese products such as cheese and yoghurt, bread and snack products, beverages, fruit juice, jam, pickles, fish products and other foods.
Sorbic acid (molecular weight 112.13) is slightly soluble in water and is inconvenient to use, and the baking industry commonly uses a water-soluble potassium salt, namely potassium sorbate (molecular weight 150.22). In application, the application effect of the sorbic acid superfine powder in a product is better than that of potassium sorbate, but the superfine powder has large surface area and is easy to absorb moisture and agglomerate, and after microcapsule treatment is carried out by using a proper wall material (such as molecular distillation monoglyceride, hydrogenated vegetable oil, refined beef tallow and the like), the sorbic acid superfine powder has good fluidity and does not agglomerate under the condition of fine granularity. In addition, the sorbic acid has strong inhibition on yeast, so the sorbic acid cannot be directly added into bread ingredients, the problem can be solved by the embedded sorbic acid, and the sorbic acid is released only in the baking stage after the bread is put into a furnace, so the later bacteriostatic and fresh-keeping effects are achieved.
Disclosure of Invention
This section is for the purpose of summarizing some aspects of embodiments of the invention and to briefly introduce some preferred embodiments. In this section, as well as in the abstract and title of the application, simplifications or omissions may be made to avoid obscuring the purpose of the section, the abstract and the title, and such simplifications or omissions are not intended to limit the scope of the invention.
The present invention has been made in view of the above and/or problems occurring in the prior sorbic acid microcapsule products.
Therefore, one of the purposes of the invention is to overcome the defects of the existing sorbic acid microcapsule product and provide a preparation method of the temperature-sensitive sorbic acid microcapsule.
To solve the above technical problem, according to an aspect of the present invention, the present invention provides the following technical solutions: a preparation method of a thermo-sensitive sorbic acid microcapsule is characterized by comprising the following steps: the method comprises the following steps:
preparing a core material: pulverizing sorbic acid;
preparing a wall material: melting the oily substance;
mixing core materials and wall materials: uniformly mixing and mixing the crushed sorbic acid and the melted oil to obtain sorbic acid embedding liquid;
preparing microcapsules: pumping the prepared sorbic acid embedding liquid, spraying and condensing under high pressure to prepare the sorbic acid microcapsule.
As a preferable embodiment of the preparation method of the temperature-sensitive sorbic acid microcapsule of the invention, wherein: in the wall material preparation, the oily substance comprises hydrogenated vegetable oil and molecular distillation monoglyceride, and the mass ratio of the hydrogenated vegetable oil to the molecular distillation monoglyceride is 4:1-1: 4.
As a preferable embodiment of the preparation method of the temperature-sensitive sorbic acid microcapsule of the invention, wherein: in the preparation of the wall material, the type of the oily substance is preferably hydrogenated vegetable oil or molecular distillation monoglyceride.
As a preferable embodiment of the preparation method of the temperature-sensitive sorbic acid microcapsule of the invention, wherein: in preparing the wall material, the type of the oily substance is preferably hydrogenated vegetable oil.
As a preferable embodiment of the preparation method of the temperature-sensitive sorbic acid microcapsule of the invention, wherein: in the wall material preparation, the mass between the hydrogenated vegetable oil and the molecular distillation monoglyceride is 1-3: 1 to 3.
As a preferable embodiment of the preparation method of the thermo-sensitive sorbic acid microcapsule of the invention, wherein: in the wall material preparation, the mass ratio of the hydrogenated vegetable oil to the molecular distillation monoglyceride is 1:1.
As a preferable embodiment of the preparation method of the thermo-sensitive sorbic acid microcapsule of the invention, wherein: in the preparation of the microcapsule, the spraying pressure of high-pressure spraying condensation is 0.2-0.6 MPa.
As a preferable embodiment of the preparation method of the temperature-sensitive sorbic acid microcapsule of the invention, wherein: in the preparation of the microcapsules, the spraying pressure of the high-pressure cooling spray was 0.4 MPa.
As a preferable embodiment of the preparation method of the thermo-sensitive sorbic acid microcapsule of the invention, wherein: in the mixed core material and wall material, the mass ratio of the sorbic acid serving as the core material to the wall material is 1: 1-4.
As a preferable embodiment of the preparation method of the temperature-sensitive sorbic acid microcapsule of the invention, wherein: in the mixed core material and wall material, the mass ratio of the sorbic acid serving as the core material to the wall material is 1: 1.5.
The temperature-sensitive sorbic acid microcapsule prepared by the invention is solid powder at room temperature, the particle size is more than 80 meshes, when the temperature reaches more than 70 ℃, the wall material is dissolved to release sorbic acid, the anti-corrosion effect of the sorbic acid can be greatly improved, and the adverse effect of the sorbic acid on group fermentation is reduced, so that the flavor and the appearance of baked food are improved, and the shelf life of the baked food are prolonged.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings required to be used in the description of the embodiments are briefly introduced below, and it is obvious that the drawings in the description below are only some embodiments of the present invention, and it is obvious for those skilled in the art that other drawings can be obtained according to the drawings without inventive labor. Wherein:
FIG. 1 is a standard sorbic acid concentration curve obtained in example 16 of the present invention;
FIG. 2 is a diagram showing a sample of thermo-sensitive sorbic acid microcapsules in example 1;
the left picture in the figure is a sample sieved by 80-120 meshes, and the right picture is a sample sieved by more than 120 meshes;
FIG. 3 is a three-dimensional microscope picture of thermo-sensitive sorbic acid in the examples 1 to 3 with super depth of field;
in the figure, a and b are microscope pictures of the product prepared in example 1; c. d is a microscope picture of the product obtained in example 2; e. f is a microscope picture of the product prepared in example 3;
FIG. 4 is a three-dimensional microscope picture of thermo-sensitive sorbic acid in the examples 4 to 6 with super depth of field;
in the figure, a and b represent the core-wall ratio of 1:1.5 microcapsule microscopy pictures; c. d is the core-wall ratio of 1:2 microcapsule microscopic picture; e. f is the core-wall ratio of 1:3 microcapsule microscopic picture;
FIG. 5 is a super-depth of field three-dimensional microscope picture of thermo-sensitive sorbic acid in examples 7-8;
in the figure, a and b represent hydrogenated vegetable oil in example 7: molecular distillation monoglyceride ═ 3:1 is microcapsule microscopic picture of wall material; c. d is the oil obtained in example 8 as hydrogenated vegetable oil: molecular distillation monoglyceride ═ 1:3 is microcapsule microscopic picture of wall material;
FIG. 6 is a super-depth-of-field three-dimensional microscopic picture of thermo-sensitive sorbic acid in example 10;
FIG. 7 is a super-depth of field three-dimensional microscope picture of thermo-sensitive sorbic acid in example 12;
FIG. 8 is a super-depth of field three-dimensional microscope picture of thermo-sensitive sorbic acid in example 15;
FIG. 9 shows the variation of heat flux with temperature variation in the temperature-sensitive capsules prepared in example 1
Detailed Description
In order to make the aforementioned objects, features and advantages of the present invention more comprehensible, specific embodiments thereof are described in detail below with reference to examples of the specification.
In the following description, numerous specific details are set forth in order to provide a thorough understanding of the present invention, but the present invention may be practiced in other ways than those specifically described and will be readily apparent to those of ordinary skill in the art without departing from the spirit of the present invention, and therefore the present invention is not limited to the specific embodiments disclosed below.
Furthermore, reference herein to "one embodiment" or "an embodiment" means that a particular feature, structure, or characteristic described in connection with the embodiment is included in at least one implementation of the invention. The appearances of the phrase "in one embodiment" in various places in the specification are not necessarily all referring to the same embodiment, nor are separate or alternative embodiments mutually exclusive of other embodiments.
Example 1
Weighing a certain amount of ester wall materials according to a proportion, placing the ester wall materials in a water bath kettle at 85 ℃ for melting, adding sorbic acid powder into the ester wall material solution, stirring for 5-8min under the stirring condition of 9000 plus 10000rpm to ensure that sorbic acid is well and uniformly dispersed to obtain a high-concentration sorbic acid embedding solution, wherein the concentration of sorbic acid in the sorbic acid embedding solution is 0.001 mg/mL; wherein, the molecular weight of the sorbic acid is 112.13, the wall material is mixed fat of equal amount of hydrogenated vegetable oil and molecular distillation monoglyceride, and the mass ratio of the core material to the wall material is 1: 4; a high-pressure spray gun and the like are preheated by using hot water originally, and then the sorbic acid embedding liquid is pumped into a cavity of the spray gun by a peristaltic pump for granulation. The spraying conditions are as follows: the materials are kept warm in a water bath at 85 ℃, the rotating speed of a peristaltic pump is 25mL/min, the spraying pressure is 0.4MPa, and the condensation temperature is 25 ℃; after that, the obtained sorbic acid microcapsule particles were sieved with a 80-mesh sieve to obtain sorbic acid microcapsules.
Example 2
Weighing a certain amount of ester wall materials according to a proportion, placing the ester wall materials in a water bath kettle at 85 ℃ for melting, adding sorbic acid powder into the ester wall material solution, stirring for 5-8min under the stirring condition of 9000 plus 10000rpm to ensure that sorbic acid is well and uniformly dispersed to obtain a high-concentration sorbic acid embedding solution, wherein the concentration of sorbic acid in the sorbic acid embedding solution is 0.001 mg/mL; wherein, the molecular weight of the sorbic acid is 112.13, and the wall material is molecular distillation monoglyceride; a high-pressure spray gun and the like are preheated by using hot water in the prior art, and then a sorbic acid embedding solution is pumped into a cavity of the spray gun by a peristaltic pump for granulation. The spraying conditions are as follows: the materials are kept warm in a water bath at 85 ℃, the rotating speed of a peristaltic pump is 25mL/min, the spraying pressure is 0.4MPa, and the condensation temperature is 25 ℃; after that, the obtained sorbic acid microcapsule particles were sieved with a 80-mesh sieve to obtain sorbic acid microcapsules.
Example 3
Weighing a certain amount of ester wall materials according to a proportion, placing the ester wall materials in a water bath kettle at 85 ℃ for melting, adding sorbic acid powder into the ester wall material solution, stirring for 5-8min under the stirring condition of 9000 plus 10000rpm to ensure that sorbic acid is well and uniformly dispersed to obtain a high-concentration sorbic acid embedding solution, wherein the concentration of sorbic acid in the sorbic acid embedding solution is 0.001 mg/mL; wherein, the sorbic acid has a molecular weight of 112.13, and the wall material is hydrogenated vegetable oil; a high-pressure spray gun and the like are preheated by using hot water originally, and then the sorbic acid embedding liquid is pumped into a cavity of the spray gun by a peristaltic pump for granulation. The spraying conditions are as follows: the materials are kept warm in a water bath at 85 ℃, the rotating speed of a peristaltic pump is 25mL/min, the spraying pressure is 0.4MPa, and the condensation temperature is 25 ℃; after that, the obtained sorbic acid microcapsule particles were sieved with a 80-mesh sieve to obtain sorbic acid microcapsules.
Example 4
Weighing a certain amount of ester wall materials according to a proportion, placing the ester wall materials in a water bath kettle at 85 ℃ for melting, adding sorbic acid powder into the ester wall material solution, stirring for 5-8min under the stirring condition of 9000 plus 10000rpm to ensure that sorbic acid is well and uniformly dispersed to obtain a high-concentration sorbic acid embedding solution, wherein the concentration of sorbic acid in the sorbic acid embedding solution is 0.001 mg/mL; wherein, the molecular weight of sorbic acid is 112.13, the wall material is mixed grease of hydrogenated vegetable oil and molecular distillation monoglyceride, and the mass ratio of the core material to the wall material is 1: 1.5; a high-pressure spray gun and the like are preheated by using hot water originally, and then the sorbic acid embedding liquid is pumped into a cavity of the spray gun by a peristaltic pump for granulation. The spraying conditions are as follows: the materials are kept warm in a water bath at 85 ℃, the rotating speed of a peristaltic pump is 25mL/min, the spraying pressure is 0.4MPa, and the condensation temperature is 25 ℃; after that, the obtained sorbic acid microcapsule particles were sieved with a 80-mesh sieve to obtain sorbic acid microcapsules.
Example 5
Weighing a certain amount of ester wall materials according to a proportion, placing the ester wall materials in a water bath kettle at 85 ℃ for melting, adding sorbic acid powder into the ester wall material solution, stirring for 5-8min under the stirring condition of 9000 plus 10000rpm to ensure that sorbic acid is well and uniformly dispersed to obtain a high-concentration sorbic acid embedding solution, wherein the concentration of sorbic acid in the sorbic acid embedding solution is 0.001 mg/mL; wherein, the molecular weight of the sorbic acid is 112.13, the wall material is mixed fat of hydrogenated vegetable oil and molecular distillation monoglyceride, and the mass ratio of the core material to the wall material is 1: 2; a high-pressure spray gun and the like are preheated by using hot water in the prior art, and then a sorbic acid embedding solution is pumped into a cavity of the spray gun by a peristaltic pump for granulation. The spraying conditions are as follows: the materials are kept warm in a water bath at 85 ℃, the rotating speed of a peristaltic pump is 25mL/min, the spraying pressure is 0.4MPa, and the condensation temperature is 25 ℃; after that, the obtained sorbic acid microcapsule particles were sieved with a 80-mesh sieve to obtain sorbic acid microcapsules.
Example 6
Weighing a certain amount of ester wall materials according to a proportion, placing the ester wall materials in a water bath kettle at 85 ℃ for melting, adding sorbic acid powder into the ester wall material solution, stirring for 5-8min under the stirring condition of 9000 plus 10000rpm to ensure that sorbic acid is well and uniformly dispersed to obtain a high-concentration sorbic acid embedding solution, wherein the concentration of sorbic acid in the sorbic acid embedding solution is 0.001 mg/mL; wherein, the molecular weight of sorbic acid is 112.13, the wall material is mixed grease of hydrogenated vegetable oil and molecular distillation monoglyceride, and the mass ratio of the core material to the wall material is 1: 3; a high-pressure spray gun and the like are preheated by using hot water originally, and then the sorbic acid embedding liquid is pumped into a cavity of the spray gun by a peristaltic pump for granulation. The spraying conditions are as follows: the materials are kept warm in a water bath at 85 ℃, the rotating speed of a peristaltic pump is 25mL/min, the spraying pressure is 0.4MPa, and the condensation temperature is 25 ℃; after the completion of the treatment, the obtained sorbic acid microcapsule particles were sieved with a 80-mesh sieve to obtain sorbic acid microcapsules.
Example 7
Weighing a certain amount of ester wall materials according to a proportion, placing the ester wall materials in a water bath kettle at 85 ℃ for melting, adding sorbic acid powder into the ester wall material solution, stirring for 5-8min under the stirring condition of 9000-10000rpm to ensure that the sorbic acid is well and uniformly dispersed to obtain a high-concentration sorbic acid embedding solution, wherein the concentration of the sorbic acid in the sorbic acid embedding solution is 0.001 mg/mL; wherein, the molecular weight of the sorbic acid is 112.13, the wall material is mixed fat of hydrogenated vegetable oil and molecular distillation monoglyceride, the mass ratio of the hydrogenated vegetable oil to the molecular distillation monoglyceride in the wall material is 3:1, and the mass ratio of the core material to the wall material is 1: 4; a high-pressure spray gun and the like are preheated by using hot water originally, and then the sorbic acid embedding liquid is pumped into a cavity of the spray gun by a peristaltic pump for granulation. The spraying conditions are as follows: the materials are kept warm in a water bath at 85 ℃, the rotating speed of a peristaltic pump is 25mL/min, the spraying pressure is 0.4MPa, and the condensation temperature is 25 ℃; after that, the obtained sorbic acid microcapsule particles were sieved with a 80-mesh sieve to obtain sorbic acid microcapsules.
Example 8
Weighing a certain amount of ester wall materials according to a proportion, placing the ester wall materials in a water bath kettle at 85 ℃ for melting, adding sorbic acid powder into the ester wall material solution, stirring for 5-8min under the stirring condition of 9000 plus 10000rpm to ensure that sorbic acid is well and uniformly dispersed to obtain a high-concentration sorbic acid embedding solution, wherein the concentration of sorbic acid in the sorbic acid embedding solution is 0.001 mg/mL; wherein, the molecular weight of the sorbic acid is 112.13, the wall material is mixed fat of hydrogenated vegetable oil and molecular distillation monoglyceride, the mass ratio of the hydrogenated vegetable oil to the molecular distillation monoglyceride in the wall material is 1:3, and the mass ratio of the core material to the wall material is 1: 4; a high-pressure spray gun and the like are preheated by using hot water in the prior art, and then a sorbic acid embedding solution is pumped into a cavity of the spray gun by a peristaltic pump for granulation. The spraying conditions are as follows: the materials are kept warm in a water bath at 85 ℃, the rotating speed of a peristaltic pump is 25mL/min, the spraying pressure is 0.4MPa, and the condensation temperature is 25 ℃; after that, the obtained sorbic acid microcapsule particles were sieved with a 80-mesh sieve to obtain sorbic acid microcapsules.
Example 9
Weighing a certain amount of ester wall materials according to a proportion, placing the ester wall materials in a water bath kettle at 85 ℃ for melting, adding sorbic acid powder into the ester wall material solution, stirring for 5-8min under the stirring condition of 9000-10000rpm to ensure that the sorbic acid is well and uniformly dispersed to obtain a high-concentration sorbic acid embedding solution, wherein the concentration of the sorbic acid in the sorbic acid embedding solution is 0.001 mg/mL; wherein, the molecular weight of the sorbic acid is 112.13, the wall material is monoglyceride UPB SG, and the mass ratio of the core material to the wall material is 1: 1.5; a high-pressure spray gun and the like are preheated by using hot water originally, and then the sorbic acid embedding liquid is pumped into a cavity of the spray gun by a peristaltic pump for granulation. The spraying conditions are as follows: the materials are kept warm in a water bath at 85 ℃, the rotating speed of a peristaltic pump is 25mL/min, the spraying pressure is 0.4MPa, and the condensation temperature is 25 ℃; after that, the obtained sorbic acid microcapsule particles were sieved with a 80-mesh sieve to obtain sorbic acid microcapsules.
Example 10
Weighing a certain amount of ester wall materials according to a proportion, placing the ester wall materials in a water bath kettle at 85 ℃ for melting, adding sorbic acid powder into the ester wall material solution, stirring for 5-8min under the stirring condition of 9000 plus 10000rpm to ensure that sorbic acid is well and uniformly dispersed to obtain a high-concentration sorbic acid embedding solution, wherein the concentration of sorbic acid in the sorbic acid embedding solution is 0.001 mg/mL; wherein, the molecular weight of the sorbic acid is 112.13, the wall material is monoglyceride HS-C, and the mass ratio of the core material to the wall material is 1: 1.5; a high-pressure spray gun and the like are preheated by using hot water in the prior art, and then a sorbic acid embedding solution is pumped into a cavity of the spray gun by a peristaltic pump for granulation. The spraying conditions are as follows: the materials are kept warm in a water bath at 85 ℃, the rotating speed of a peristaltic pump is 25mL/min, the spraying pressure is 0.4MPa, and the condensation temperature is 25 ℃; after that, the obtained sorbic acid microcapsule particles were sieved with a 80-mesh sieve to obtain sorbic acid microcapsules.
Example 11
Weighing a certain amount of ester wall materials according to a proportion, placing the ester wall materials in a water bath kettle at 85 ℃ for melting, adding sorbic acid powder into the ester wall material solution, stirring for 5-8min under the stirring condition of 9000-10000rpm to ensure that the sorbic acid is well and uniformly dispersed to obtain a high-concentration sorbic acid embedding solution, wherein the concentration of the sorbic acid in the sorbic acid embedding solution is 0.001 mg/mL; wherein, the molecular weight of the sorbic acid is 112.13, the wall material is PGE 55-M (polyglycerol fatty acid ester), and the mass ratio of the core material to the wall material is 1: 1.5; a high-pressure spray gun and the like are preheated by using hot water originally, and then the sorbic acid embedding liquid is pumped into a cavity of the spray gun by a peristaltic pump for granulation. The spraying conditions are as follows: the materials are kept warm in a water bath at 85 ℃, the rotating speed of a peristaltic pump is 25mL/min, the spraying pressure is 0.4MPa, and the condensation temperature is 25 ℃; after that, the obtained sorbic acid microcapsule particles were sieved with a 80-mesh sieve to obtain sorbic acid microcapsules.
Example 12
Weighing a certain amount of ester wall materials according to a proportion, placing the ester wall materials in a water bath kettle at 85 ℃ for melting, adding sorbic acid powder into the ester wall material solution, stirring for 5-8min under the stirring condition of 9000 plus 10000rpm to ensure that sorbic acid is well and uniformly dispersed to obtain a high-concentration sorbic acid embedding solution, wherein the concentration of sorbic acid in the sorbic acid embedding solution is 0.001 mg/mL; wherein, the molecular weight of sorbic acid is 112.13, the wall material is SSL (sodium stearoyl lactylate), and the mass ratio of the core material to the wall material is 1: 1.5; a high-pressure spray gun and the like are preheated by using hot water originally, and then the sorbic acid embedding liquid is pumped into a cavity of the spray gun by a peristaltic pump for granulation. The spraying conditions are as follows: the materials are kept warm in a water bath at 85 ℃, the rotating speed of a peristaltic pump is 25mL/min, the spraying pressure is 0.4MPa, and the condensation temperature is 25 ℃; after that, the obtained sorbic acid microcapsule particles were sieved with a 80-mesh sieve to obtain sorbic acid microcapsules.
Example 13
Weighing a certain amount of ester wall materials according to a proportion, placing the ester wall materials in a water bath kettle at 85 ℃ for melting, adding sorbic acid powder into the ester wall material solution, stirring for 5-8min under the stirring condition of 9000 plus 10000rpm to ensure that sorbic acid is well and uniformly dispersed to obtain a high-concentration sorbic acid embedding solution, wherein the concentration of sorbic acid in the sorbic acid embedding solution is 0.001 mg/mL; wherein, the molecular weight of sorbic acid is 112.13, the wall material is mixed grease of hydrogenated vegetable oil and molecular distillation monoglyceride, and the mass ratio of the core material to the wall material is 1: 1.5; a high-pressure spray gun and the like are preheated by using hot water in the prior art, and then a sorbic acid embedding solution is pumped into a cavity of the spray gun by a peristaltic pump for granulation. The spraying conditions are as follows: the materials are kept warm in a water bath at 85 ℃, the rotating speed of a peristaltic pump is 25mL/min, the spraying pressure is 0.6MPa, and the condensation temperature is 25 ℃; after that, the obtained sorbic acid microcapsule particles were sieved with a 80-mesh sieve to obtain sorbic acid microcapsules.
Example 14
Weighing a certain amount of ester wall materials according to a proportion, placing the ester wall materials in a water bath kettle at 85 ℃ for melting, adding sorbic acid powder into the ester wall material solution, stirring for 5-8min under the stirring condition of 9000 plus 10000rpm to ensure that sorbic acid is well and uniformly dispersed to obtain a high-concentration sorbic acid embedding solution, wherein the concentration of sorbic acid in the sorbic acid embedding solution is 0.001 mg/mL; wherein, the molecular weight of sorbic acid is 112.13, the wall material is mixed grease of hydrogenated vegetable oil and molecular distillation monoglyceride, and the mass ratio of the core material to the wall material is 1: 1.5; a high-pressure spray gun and the like are preheated by using hot water originally, and then the sorbic acid embedding liquid is pumped into a cavity of the spray gun by a peristaltic pump for granulation. The spraying conditions are as follows: the materials are kept warm in a water bath at 85 ℃, the rotating speed of a peristaltic pump is 25mL/min, the spraying pressure is 0.2MPa, and the condensation temperature is 25 ℃; after that, the obtained sorbic acid microcapsule particles were sieved with a 80-mesh sieve to obtain sorbic acid microcapsules.
Example 15
Weighing a certain amount of ester wall materials according to a proportion, placing the ester wall materials in a water bath kettle at 85 ℃ for melting, adding sorbic acid powder into the ester wall material solution, stirring for 5-8min under the stirring condition of 9000-10000rpm to ensure that the sorbic acid is well and uniformly dispersed to obtain a high-concentration sorbic acid embedding solution, wherein the concentration of the sorbic acid in the sorbic acid embedding solution is 0.001 mg/mL; wherein, the molecular weight of the sorbic acid is 112.13, the wall material is mixed fat of hydrogenated vegetable oil and molecular distillation monoglyceride, and the mass ratio of the core material to the wall material is 1: 1.5; placing the obtained embedding solution in a refrigerator at the temperature of-20 ℃, quickly freezing for 1h, and grinding by a grinder to obtain sorbic acid microcapsule powder; after the completion of the treatment, the obtained sorbic acid microcapsule particles were sieved with a 80-mesh sieve to obtain sorbic acid microcapsules.
Comparative example 1
Weighing a certain amount of ester wall materials according to a proportion, placing the ester wall materials in a water bath kettle at 85 ℃ for melting, adding sorbic acid powder into the ester wall material solution, stirring for 5-8min under the stirring condition of 9000-10000rpm to ensure that the sorbic acid is well and uniformly dispersed to obtain a high-concentration sorbic acid embedding solution, wherein the concentration of the sorbic acid in the sorbic acid embedding solution is 0.001 mg/mL; wherein, the molecular weight of the sorbic acid is 112.13, the wall material is mixed fat of equal amount of hydrogenated vegetable oil and molecular distillation monoglyceride, and the mass ratio of the core material to the wall material is 1: 1; a high-pressure spray gun and the like are preheated by using hot water originally, and then the sorbic acid embedding liquid is pumped into a cavity of the spray gun by a peristaltic pump for granulation. The spraying conditions are as follows: the materials are kept warm in a water bath at 85 ℃, the rotating speed of a peristaltic pump is 25mL/min, the spraying pressure is 0.4MPa, and the condensation temperature is 25 ℃; after the completion of the treatment, the obtained sorbic acid microcapsule particles were sieved with a 80-mesh sieve to obtain sorbic acid microcapsules.
Example 16
Weighing a certain amount of ester wall materials according to a proportion, placing the ester wall materials in a water bath kettle at 85 ℃ for melting, adding sorbic acid powder into the ester wall material solution, stirring for 5-8min under the stirring condition of 9000 plus 10000rpm to ensure that sorbic acid is well and uniformly dispersed to obtain a high-concentration sorbic acid embedding solution, wherein the concentration of sorbic acid in the sorbic acid embedding solution is 0.001 mg/mL; wherein, the molecular weight of the sorbic acid is 112.13, the wall material is mixed fat of equal amount of hydrogenated vegetable oil and molecular distillation monoglyceride, and the mass ratio of the core material to the wall material is 1: 4; a high-pressure spray gun and the like are preheated by using hot water originally, and then the sorbic acid embedding liquid is pumped into a cavity of the spray gun by a peristaltic pump for granulation. The spraying conditions are as follows: the materials are kept warm in water bath at 85 ℃, the rotating speed of a peristaltic pump is 25mL/min, and the mixture is sprayedThe fog pressure is 0.4MPa, and the condensation temperature is 25 ℃; after that, the obtained sorbic acid microcapsule particles were sieved with a 80-mesh sieve to obtain sorbic acid microcapsules. Measuring at 254nm by ultraviolet spectrophotometer, and weighing 25.203g NaHCO 3 Adding water to dissolve, transferring into a 1000mL volumetric flask, and fixing the volume (NaHCO) 3 The concentration was 0.3 mol/L). Then, sorbic acid was prepared into standard solutions of 0, 1, 2, 3, 4 and 5mg/mL, and the absorbances were measured at 254nm wavelength. The concentration was plotted on the abscissa and the absorbance on the ordinate to obtain Table 1.
TABLE 1 data for sorbic acid concentration and absorbance
FIG. 1, R in FIG. 1, was prepared according to Table 1 2 Not less than 0.99 percent, reliable standard curve and establishment of the relation between the absorbance and the sorbic acid concentration.
Example 17
The sorbic acid microcapsules prepared in examples 1 to 15 and comparative example 1 were measured for absorbance at 254nm using an ultraviolet spectrophotometer, and the sorbic acid concentration and the encapsulation efficiency were further calculated from the relationship between the absorbance and the sorbic acid concentration, wherein the calculation formula between the encapsulation efficiency and the sorbic acid concentration was as follows:
sorbic acid encapsulation efficiency%
Wherein A is the absorbance of the weighed sorbic acid microcapsule;
a is the sorbic acid wall-core ratio;
m is the mass of the weighed sorbic acid microcapsule, and the unit is mg;
n is a coefficient multiple.
The data obtained are shown in table 2:
TABLE 2 encapsulation efficiency of sorbic acid microcapsules prepared in examples 1 to 15
As can be seen from table 2, the encapsulation efficiency data of the sorbic acid microcapsules produced in examples 1, 4, 5 and 6 and comparative example 1 can be found, and when the mass of the core material wall material is 1:1.5, the encapsulation efficiency is higher at a ratio of 1:1.5, but in the actual utilization rate and the actual utilization amount of sorbic acid used, the sorbic acid is more sufficiently utilized in example 1, and when the mass ratio of the core material wall material is changed to 1:1, the sorbic acid is pumped into the spray gun and is often clogged, and defects of finished products cannot be obtained, so that the mass ratio of the core material wall material preferred in the present invention is 1: 1.5.
From the encapsulation efficiency data of the sorbic acid microcapsules in examples 1, 2, 3, 7 and 8 in table 2, the sorbic acid encapsulation efficiency of the product is highest when the mass ratio of the hydrogenated vegetable oil and the molecular distillation monoglyceride used as the wall material is 1:1, and the mass ratio of the hydrogenated vegetable oil and the molecular distillation monoglyceride preferred in the present invention is 1:1.
According to the encapsulation efficiency data of the sorbic acid microcapsules in the examples 1, 9, 10, 11 and 12 in the table 2, when the oily raw material of the wall material is changed, the encapsulation efficiency of the product is changed, the encapsulation efficiency in the example 1 is the highest, the preferable oily raw material of the wall material is hydrogenated vegetable oil, wherein the difference of the encapsulation efficiency in the examples 1, 9 and 10 is presumed to be that the melting point of the oily raw material is not proper, the melting point of the wall material mailbox raw material monoglyceride UPB SG adopted in the example 9 is 45 ℃, the melting point is lower, and the sorbic acid microcapsules prepared by spraying are adhered to influence the encapsulation effect; the monoglyceride HS-C used in example 10 has a higher melting point and a higher temperature required for the reaction process, and it is difficult to achieve a better encapsulation effect under normal temperature settings.
The encapsulation efficiency data of the sorbic acid microcapsules obtained in examples 8, 13 and 14 in table 2 show that the encapsulation efficiency of the finished product obtained in example 8 is the highest, and the spray pressure in the spray granulation in the present invention is preferably 0.4 MPa.
According to the encapsulation efficiency data of the sorbic acid microcapsule prepared in example 15 and other examples, the performance of the product prepared by the freeze-crushing granulation adopted in example 15 is poorer than that of the spray granulation adopted in other examples, and the preferred granulation mode of the invention is the spray granulation.
For microscopic imaging of the sorbic acid microcapsule prepared in the embodiment of the invention, a sample is observed by adopting a super-depth-of-field three-dimensional microscope (model: VHX-1000C), and a light source is a lower light source, so that figures 2-9 are obtained.
Example 18
The sorbic acid microcapsule obtained in example 1 was measured for melting point by DSC8500 at a temperature rise rate of 10 ℃/min in the range of 20 to 90 ℃ to give FIG. 9.
As can be seen from fig. 9, the sorbic acid microcapsule prepared in example 1 of the present invention gradually melts as the temperature increases.
It should be noted that the above-mentioned embodiments are only for illustrating the technical solutions of the present invention and not for limiting, and although the present invention has been described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications or equivalent substitutions may be made on the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention, which should be covered by the claims of the present invention.
Claims (1)
1. A preparation method of temperature-sensitive sorbic acid microcapsules is characterized by comprising the following steps: weighing ester wall materials, placing the ester wall materials in a water bath kettle at 85 ℃ for melting, adding core material sorbic acid powder into an ester wall material solution, stirring for 5-8min under the stirring condition of 9000 plus 10000rpm to ensure that sorbic acid is well and uniformly dispersed to obtain a high-concentration sorbic acid embedding solution, wherein the concentration of sorbic acid in the sorbic acid embedding solution is 0.001mg/mL, the ester wall materials are mixed fat of hydrogenated vegetable oil and molecular distillation monoglyceride in a mass ratio of 1:1, and the mass ratio of the core materials to the wall materials is 1: 4; preheating a high-pressure spray gun by using hot water, pumping a sorbic acid embedding liquid into a spray gun cavity by using a peristaltic pump, and granulating under the spraying conditions that: the materials are kept warm in a water bath at 85 ℃, the rotating speed of a peristaltic pump is 25mL/min, the spraying pressure is 0.4MPa, and the condensation temperature is 25 ℃; after that, the obtained sorbic acid microcapsule particles were sieved with a 80-mesh sieve to obtain sorbic acid microcapsules.
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