CN117731692A - Copper sulfate dilution and preparation method and application thereof - Google Patents
Copper sulfate dilution and preparation method and application thereof Download PDFInfo
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- CN117731692A CN117731692A CN202311743702.4A CN202311743702A CN117731692A CN 117731692 A CN117731692 A CN 117731692A CN 202311743702 A CN202311743702 A CN 202311743702A CN 117731692 A CN117731692 A CN 117731692A
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- copper sulfate
- mixed solution
- maltodextrin
- sodium starch
- octenyl succinate
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- ARUVKPQLZAKDPS-UHFFFAOYSA-L copper(II) sulfate Chemical compound [Cu+2].[O-][S+2]([O-])([O-])[O-] ARUVKPQLZAKDPS-UHFFFAOYSA-L 0.000 title claims abstract description 62
- 229910000365 copper sulfate Inorganic materials 0.000 title claims abstract description 58
- 239000012895 dilution Substances 0.000 title claims abstract description 43
- 238000002360 preparation method Methods 0.000 title claims abstract description 25
- 238000003113 dilution method Methods 0.000 title description 2
- 239000011259 mixed solution Substances 0.000 claims abstract description 84
- 239000005913 Maltodextrin Substances 0.000 claims abstract description 57
- 229920002774 Maltodextrin Polymers 0.000 claims abstract description 57
- 229940035034 maltodextrin Drugs 0.000 claims abstract description 57
- GUOCOOQWZHQBJI-UHFFFAOYSA-N 4-oct-7-enoxy-4-oxobutanoic acid Chemical compound OC(=O)CCC(=O)OCCCCCCC=C GUOCOOQWZHQBJI-UHFFFAOYSA-N 0.000 claims abstract description 56
- 229940080313 sodium starch Drugs 0.000 claims abstract description 55
- 239000004227 calcium gluconate Substances 0.000 claims abstract description 53
- 229960004494 calcium gluconate Drugs 0.000 claims abstract description 53
- 235000013927 calcium gluconate Nutrition 0.000 claims abstract description 53
- NEEHYRZPVYRGPP-UHFFFAOYSA-L calcium;2,3,4,5,6-pentahydroxyhexanoate Chemical compound [Ca+2].OCC(O)C(O)C(O)C(O)C([O-])=O.OCC(O)C(O)C(O)C(O)C([O-])=O NEEHYRZPVYRGPP-UHFFFAOYSA-L 0.000 claims abstract description 53
- JZCCFEFSEZPSOG-UHFFFAOYSA-L copper(II) sulfate pentahydrate Chemical compound O.O.O.O.O.[Cu+2].[O-]S([O-])(=O)=O JZCCFEFSEZPSOG-UHFFFAOYSA-L 0.000 claims abstract description 47
- 239000000243 solution Substances 0.000 claims abstract description 45
- 238000010790 dilution Methods 0.000 claims abstract description 41
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 35
- 239000000843 powder Substances 0.000 claims abstract description 33
- 238000000034 method Methods 0.000 claims abstract description 28
- 238000001035 drying Methods 0.000 claims abstract description 10
- 239000003094 microcapsule Substances 0.000 claims abstract description 5
- 239000007787 solid Substances 0.000 claims abstract description 5
- 238000010298 pulverizing process Methods 0.000 claims abstract description 4
- 238000001694 spray drying Methods 0.000 claims description 29
- 239000000706 filtrate Substances 0.000 claims description 13
- 239000012528 membrane Substances 0.000 claims description 13
- 238000010008 shearing Methods 0.000 claims description 9
- 238000002156 mixing Methods 0.000 claims description 3
- 235000016709 nutrition Nutrition 0.000 claims description 3
- 239000011148 porous material Substances 0.000 claims description 3
- 230000000007 visual effect Effects 0.000 claims description 3
- 239000000825 pharmaceutical preparation Substances 0.000 claims description 2
- 229940127557 pharmaceutical product Drugs 0.000 claims description 2
- 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 2
- 238000004519 manufacturing process Methods 0.000 claims 1
- 230000008569 process Effects 0.000 abstract description 9
- 239000003085 diluting agent Substances 0.000 abstract description 6
- 239000003814 drug Substances 0.000 abstract description 4
- 238000004062 sedimentation Methods 0.000 abstract description 4
- 229940079593 drug Drugs 0.000 abstract description 3
- 230000000052 comparative effect Effects 0.000 description 23
- 239000000047 product Substances 0.000 description 22
- 239000000463 material Substances 0.000 description 21
- 238000012856 packing Methods 0.000 description 20
- 239000002994 raw material Substances 0.000 description 20
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 15
- 239000010949 copper Substances 0.000 description 15
- 229910052802 copper Inorganic materials 0.000 description 15
- 239000008213 purified water Substances 0.000 description 11
- 230000001276 controlling effect Effects 0.000 description 10
- 238000010438 heat treatment Methods 0.000 description 10
- 238000007689 inspection Methods 0.000 description 10
- 238000003756 stirring Methods 0.000 description 10
- 238000005303 weighing Methods 0.000 description 10
- 230000000694 effects Effects 0.000 description 8
- 239000002245 particle Substances 0.000 description 6
- 239000007921 spray Substances 0.000 description 4
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical group [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 3
- 238000010521 absorption reaction Methods 0.000 description 3
- 210000000988 bone and bone Anatomy 0.000 description 3
- 229960005069 calcium Drugs 0.000 description 3
- 239000011575 calcium Substances 0.000 description 3
- 229910052791 calcium Inorganic materials 0.000 description 3
- 230000001804 emulsifying effect Effects 0.000 description 3
- 235000013305 food Nutrition 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- JPVYNHNXODAKFH-UHFFFAOYSA-N Cu2+ Chemical compound [Cu+2] JPVYNHNXODAKFH-UHFFFAOYSA-N 0.000 description 2
- 102000004190 Enzymes Human genes 0.000 description 2
- 108090000790 Enzymes Proteins 0.000 description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- 229920002472 Starch Polymers 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 2
- 229910001431 copper ion Inorganic materials 0.000 description 2
- 235000005911 diet Nutrition 0.000 description 2
- 230000000378 dietary effect Effects 0.000 description 2
- 238000007865 diluting Methods 0.000 description 2
- 238000004090 dissolution Methods 0.000 description 2
- 239000000796 flavoring agent Substances 0.000 description 2
- 235000019634 flavors Nutrition 0.000 description 2
- 238000000265 homogenisation Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 229940032147 starch Drugs 0.000 description 2
- 235000019698 starch Nutrition 0.000 description 2
- 239000008107 starch Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000010998 test method Methods 0.000 description 2
- 239000011573 trace mineral Substances 0.000 description 2
- 235000013619 trace mineral Nutrition 0.000 description 2
- BHPQYMZQTOCNFJ-UHFFFAOYSA-N Calcium cation Chemical compound [Ca+2] BHPQYMZQTOCNFJ-UHFFFAOYSA-N 0.000 description 1
- QPLDLSVMHZLSFG-UHFFFAOYSA-N Copper oxide Chemical compound [Cu]=O QPLDLSVMHZLSFG-UHFFFAOYSA-N 0.000 description 1
- 208000018522 Gastrointestinal disease Diseases 0.000 description 1
- 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 description 1
- 208000012902 Nervous system disease Diseases 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- 206010047700 Vomiting Diseases 0.000 description 1
- 230000000844 anti-bacterial effect Effects 0.000 description 1
- 230000003078 antioxidant effect Effects 0.000 description 1
- 239000003899 bactericide agent Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 210000000941 bile Anatomy 0.000 description 1
- 238000013124 brewing process Methods 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000002738 chelating agent Substances 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000008395 clarifying agent Substances 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 230000002542 deteriorative effect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 235000015872 dietary supplement Nutrition 0.000 description 1
- 238000007907 direct compression Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 239000002612 dispersion medium Substances 0.000 description 1
- 235000013601 eggs Nutrition 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 238000011010 flushing procedure Methods 0.000 description 1
- 239000005452 food preservative Substances 0.000 description 1
- 235000019249 food preservative Nutrition 0.000 description 1
- 235000012055 fruits and vegetables Nutrition 0.000 description 1
- 230000011132 hemopoiesis Effects 0.000 description 1
- KCYQMQGPYWZZNJ-BQYQJAHWSA-N hydron;2-[(e)-oct-1-enyl]butanedioate Chemical compound CCCCCC\C=C\C(C(O)=O)CC(O)=O KCYQMQGPYWZZNJ-BQYQJAHWSA-N 0.000 description 1
- 230000036039 immunity Effects 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000001727 in vivo Methods 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 208000017169 kidney disease Diseases 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 210000004185 liver Anatomy 0.000 description 1
- 208000019423 liver disease Diseases 0.000 description 1
- 244000005700 microbiome Species 0.000 description 1
- 230000035764 nutrition Effects 0.000 description 1
- 239000007800 oxidant agent Substances 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000012216 screening Methods 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 229940083542 sodium Drugs 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 235000013826 starch sodium octenyl succinate Nutrition 0.000 description 1
- 239000001334 starch sodium octenyl succinate Substances 0.000 description 1
- 239000013589 supplement Substances 0.000 description 1
- 230000008673 vomiting Effects 0.000 description 1
Landscapes
- Medicinal Preparation (AREA)
Abstract
The invention relates to the field of biological medicine, and discloses a copper sulfate diluent, a preparation method and application thereof. A method for preparing a copper sulfate dilution comprising: drying and pulverizing the mixed solution with the solid content of 30-40% to obtain microcapsule powder; the mixed solution is a solution in which sodium starch octenyl succinate, maltodextrin, calcium gluconate and copper sulfate pentahydrate are dissolved, wherein the sodium starch octenyl succinate accounts for 20-50%, the maltodextrin accounts for 20-49%, the calcium gluconate accounts for 2-10%, and the copper sulfate pentahydrate accounts for 4-58%. The disclosed copper sulfate dilution is prepared by the preparation method. The diluted product prepared by the invention has fine powder, the 100 mesh passing rate is more than 99%, blue color points are not generated in the process of brewing, the water solubility is stronger, in addition, the product has excellent fluidity, the repose angle is less than 30, the diluted product can be uniformly dispersed in a medium, the advantage of unsuitable sedimentation is provided, and the diluted product can be applied to nourishments and medicines.
Description
Technical Field
The invention relates to the technical field of biological medicines, in particular to a copper sulfate diluent, a preparation method and application thereof.
Background
Copper is an important component of bones, and can promote the deposition of calcium and phosphorus on soft bones to improve bone firmness, and copper can also participate in hematopoiesis by affecting the absorption and release of iron. In addition, the scholars prove that trace element copper can enhance the immunity function of the organism through the in-vivo enzyme and the antioxidant property of the trace element copper. In addition, copper ions contained in the copper sulfate can react with an oxidant to prolong the shelf life of foods, and can be used as a food preservative to inhibit the enzyme activity and the microorganism growth in the foods, so that the foods are prevented from deteriorating, and the copper ions are also used as a bactericide in the fruit and vegetable industry.
In combination with dietary copper intake of residents in China, recommended dietary copper (RNI) of adults is 0.8mg/d, highest tolerable intake (UL) is 8mg/d, and high copper content in the body possibly causes gastrointestinal diseases, nervous system diseases, liver and kidney diseases and the like, so that the copper supplement is required to be diluted in order to improve application safety. In general, nutritional supplements are presented as powdered products, and would have a high economic value if a well-brewed, well-dispersed copper diluent could be prepared.
In view of this, the present invention has been made.
Disclosure of Invention
The invention aims to provide copper sulfate dilution and a preparation method and application thereof.
The invention is realized in the following way:
in a first aspect, the present invention provides a method for preparing a copper sulfate dilution comprising:
drying and pulverizing the mixed solution with the solid content of 30-40% to obtain microcapsule powder;
the mixed solution is a solution in which sodium starch octenyl succinate, maltodextrin, calcium gluconate and copper sulfate pentahydrate are dissolved, wherein the sodium starch octenyl succinate accounts for 20-50%, the maltodextrin accounts for 20-49%, the calcium gluconate accounts for 2-10%, and the copper sulfate pentahydrate accounts for 4-58%.
In an alternative embodiment, sodium starch octenyl succinate is preferably 25 to 47%, maltodextrin is preferably 15 to 40%, calcium gluconate is preferably 3 to 7%, and copper sulfate pentahydrate is preferably 12 to 48%.
In an alternative embodiment, the method further comprises preparing a mixed solution before spray drying, wherein the preparation method of the mixed solution comprises the following steps:
adding the copper sulfate pentahydrate into the high-temperature mixed solution, and shearing in a homogenizer until visual appearance to obtain a bright blue solution; the high-temperature mixed solution is mixed solution which consists of sodium starch octenyl succinate, maltodextrin, calcium gluconate and water and has the temperature of 80-100 ℃.
In an alternative embodiment, the high temperature mixed solution is prepared by adding sodium starch octenyl succinate, maltodextrin and calcium gluconate into water at 80-100 ℃; or uniformly mixing sodium starch octenyl succinate, maltodextrin, calcium gluconate and water, and then raising the temperature to 80-100 ℃.
In an alternative embodiment, the shear homogenizing speed is 1000-5000 r/min and the shear time is 5-10 min.
In an alternative embodiment, the shear homogenizing speed is 2000-4000 r/min.
In an alternative embodiment, the preparation of the bright blue solution further comprises passing the bright blue solution through a filter membrane with a pore diameter of 25 μm, and obtaining a filtrate to obtain a mixed solution.
In an alternative embodiment, the method of drying the powder is spray drying;
preferably, the air inlet temperature of spray drying is 150-165 ℃, and the air outlet temperature is 100-110 ℃.
In a second aspect, the invention provides a copper sulphate dilution made by a method according to any one of the preceding embodiments.
In a third aspect, the invention provides the use of a copper sulphate dilution as in the previous embodiments in a nutritional or pharmaceutical product.
The invention has the following beneficial effects:
according to the preparation method, the copper sulfate pentahydrate is used as a preparation raw material, the food-grade raw material maltodextrin is used for dilution, the mixed solution is emulsified by using excellent emulsifying property and film forming property of sodium starch octenyl succinate, so that the sodium starch octenyl succinate has an embedding effect on the copper sulfate pentahydrate in a spray drying process, calcium is introduced into calcium gluconate, strength and viscoelasticity of a film are enhanced, the embedded copper sulfate can resist stronger strain pressure, cracks caused by particle collision in the spray drying process are prevented, a better embedding effect is achieved, hygroscopicity of the copper sulfate is reduced, bad smell of a part of copper sulfate is covered, the proportion of each raw material is adjusted within a proper range, the preparation method is provided, after the solution is fully dissolved, the solution is dried, copper fishy smell of copper elements is improved, a diluted product prepared from the mixed solution with the substances is fine and smooth in powder passing rate of more than 99%, blue color is not generated in the process of flushing, the blue color is better in the process, the solution is better in the water-soluble liquid dispersion medium is better than 30, and the preparation method is excellent in sedimentation and sedimentation is easy.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings that are needed in the embodiments will be briefly described below, it being understood that the following drawings only illustrate some embodiments of the present invention and therefore should not be considered as limiting the scope, and other related drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
FIG. 1 is a graph of the diluted product obtained in example 1 and the solvent obtained after dissolution in water;
FIG. 2 is a graph of a direct compression tablet of the copper sulfate dilution of example 1;
FIG. 3 is a graph of storage stability analysis of a copper sulfate dilution.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention more clear, the technical solutions of the embodiments of the present invention will be clearly and completely described below. 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.
The copper sulfate dilution provided by the embodiment of the invention, and the preparation method and application thereof are specifically described below.
The preparation method of the copper sulfate dilution provided by the embodiment of the invention comprises the following steps:
drying and pulverizing the mixed solution with the mass concentration of 30-40% to obtain microcapsule powder;
the mixed solution is a solution in which sodium starch octenyl succinate, maltodextrin, calcium gluconate and copper sulfate pentahydrate are dissolved, wherein the sodium starch octenyl succinate accounts for 20-50%, the maltodextrin accounts for 20-49%, the calcium gluconate accounts for 2-10%, and the copper sulfate pentahydrate accounts for 4-58%.
Anhydrous copper sulfate and hydrated copper sulfate are the main forms of copper, but anhydrous copper sulfate is strong in harshness, deliquescent in humid air and easy to form black copper oxide at high temperature, and the obtained product has poor flavor and stability when being used as raw materials for preparing a copper sulfate dilution. Relatively, the water solubility and stability of the hydrated copper sulfate are improved, and the prepared copper sulfate diluted product has better flavor and application stability. In addition, the hydrated copper sulfate also has the effects of promoting vomiting, removing putrefaction, detoxifying and the like; the hydrated copper sulfate can be used as a clarifying agent and a chelating agent for processing wine and preserved eggs, and can also be used as a traditional Chinese medicinal material for increasing the flow of bile, so that the use safety is high.
The hydrated copper sulfate pure product has moisture absorption, and when the hydrated copper sulfate pure product is mixed with other base materials, the problems of difficult control of content and poor mixability exist due to small addition amount, so that the problem of poor mixability is needed to be overcome when the diluted copper sulfate product is prepared by taking the copper sulfate pentahydrate as a raw material.
According to the preparation method provided by the embodiment of the invention, the copper sulfate pentahydrate is used as a preparation raw material, the food-grade raw material maltodextrin is used for diluting the copper sulfate pentahydrate, the sodium starch octenyl succinate is used for playing an emulsifying effect and an embedding effect, calcium is introduced by using calcium gluconate, and the proportion of each raw material is adjusted within a proper range.
Preferably, the sodium starch octenyl succinate is 25-47%, the maltodextrin is 15-40%, the calcium gluconate is 3-7%, and the copper sulfate pentahydrate is 12-48%.
The proportion of the raw materials can further ensure that a diluent with better performance is prepared.
Optionally, the method further comprises preparing a mixed solution before spray drying, wherein the preparation method of the mixed solution comprises the following steps:
adding the copper sulfate pentahydrate into the high-temperature mixed solution, and shearing in a homogenizer until visual appearance to obtain a bright blue solution; the high-temperature mixed solution is a mixed solution which consists of sodium starch octenyl succinate, maltodextrin, calcium gluconate and water and has the temperature of 80-100 ℃ (for example, 80 ℃, 90 ℃ or 100 ℃).
Considering the subsequent absorption effect of the copper sulfate, it is important to control the uniform and proper particle size of the system, so that the uniform and completely dissolved solution of the system can be ensured by adopting high-temperature and shearing homogenization combination, and the particle size reaches a controllable range, so that the diluted copper sulfate with good performance is obtained through drying.
Preferably, in order to avoid undissolved particles in the solution, which affects the performance of the prepared dilution, the preparation of the bright blue solution further comprises passing the solution through a filter membrane with a pore diameter of 25 μm, and obtaining the filtrate as a mixed solution.
Preferably, the homogenization conditions to achieve solute dissolution are: the shearing homogenizing rotating speed is 1000-5000 r/min (for example 1000r/min, 1200r/min or 1500 r/min), and the shearing time is 5-10 min (for example 5min, 8min or 10 min); more preferably, the shear homogenizing speed is 2000-4000 r/min (e.g., 2000r/min, 3000r/min, or 4000 r/min).
Further, the high temperature mixed solution is prepared by adding starch sodium octenyl succinate, maltodextrin and calcium gluconate into water of 80-100deg.C (such as 80deg.C, 90deg.C or 100deg.C); or after uniformly mixing sodium starch octenyl succinate, maltodextrin, calcium gluconate and water, raising the temperature to 80-100 ℃ (for example 80 ℃, 90 ℃ or 100 ℃).
Preferably, the method of drying the powder is spray drying. The powder with uniform granularity and good particle dispersibility can be prepared by spray drying.
The copper sulfate dilution provided by the embodiment of the invention is prepared by adopting the preparation method provided by the embodiment of the application.
The embodiment of the invention also provides application of the copper sulfate dilution in nutrition or medicines.
The features and capabilities of the present invention are described in further detail below in connection with the examples.
Example 1
Weighing 500 kg of purified water in a batching tank, heating by opening steam to raise the temperature to above 80 ℃, sequentially adding 100kg of sodium starch octenyl succinate, 120.25kg of maltodextrin and 14kg of calcium gluconate into hot water, and uniformly stirring to obtain a mixed solution; placing the mixed solution in a homogenizer, adding 59.25kg of copper sulfate pentahydrate into the mixed solution, controlling the rotating speed of the homogenizer to 3000r/min, homogenizing for 8min to obtain a visually bright blue solution; the bright blue solution is filtered by a filter membrane with the diameter of 25 mu m, and the filtrate is taken to obtain a mixed solution; the mixed solution is spray dried to obtain 20% copper sulfate dilution (calculated by copper sulfate pentahydrate) powder, wherein the content of sodium starch octenyl succinate is about 34%, the content of maltodextrin is about 41% and the content of calcium gluconate is about 5%. The air inlet temperature of spray drying is 150 ℃, and the air outlet temperature is 100 ℃; after powder is collected, the materials are sieved by a 60-mesh sieve and then enter a packing room for packing, warehousing and sending inspection by a vertical blanking system.
The resulting dilutions were shown in figure 1, which showed no non-uniform blue spots, indicating good dispersion uniformity of the final product. The diluted product prepared in this example was dissolved in water to prepare aqueous solutions of different concentrations, as shown in the right diagram of fig. 1, and the aqueous solutions were uniform in color.
The obtained diluted product was made into tablets, as shown in fig. 2, and as can be seen from fig. 2, the morphology of the tablets was good.
Example 2
Weighing 500 kg of purified water in a batching tank, heating by opening steam to raise the temperature to more than 80 ℃, adding 100kg of sodium starch octenyl succinate, 61kg of maltodextrin and 14kg of calcium gluconate into hot water for a second time, and uniformly stirring to obtain a mixed solution; placing the mixed solution in a homogenizer, adding 118.5kg of copper sulfate pentahydrate into the mixed solution, controlling the rotating speed of the homogenizer to 3000r/min, homogenizing for 8min to obtain a visually bright blue solution; the bright blue solution is filtered by a filter membrane with the diameter of 25 mu m, and the filtrate is taken to obtain a mixed solution; the mixed solution is subjected to spray drying to obtain 40% copper sulfate dilution (calculated by copper sulfate pentahydrate) powder, wherein the content of sodium starch octenyl succinate is about 34%, the content of maltodextrin is about 21%, and the content of calcium gluconate is about 5%. The air inlet temperature of spray drying is 150 ℃, and the air outlet temperature is 100 ℃; after powder is collected, the materials are sieved by a 60-mesh sieve and then enter a packing room for packing, warehousing and sending inspection by a vertical blanking system.
Example 3
Weighing 500 kg of purified water in a batching tank, heating by opening steam to raise the temperature to more than 80 ℃, adding 100kg of sodium starch octenyl succinate, 38.5kg of maltodextrin and 14kg of calcium gluconate into hot water in sequence, and uniformly stirring to obtain a mixed solution; placing the mixed solution in a homogenizer, adding 141kg of copper sulfate pentahydrate into the mixed solution, controlling the rotating speed of the homogenizer to 3000r/min, homogenizing for 8min to obtain a visually bright blue solution; the bright blue solution is filtered by a filter membrane with the diameter of 25 mu m, and the filtrate is taken to obtain a mixed solution; the mixed solution is spray dried to obtain 48% copper sulfate dilution (calculated by copper sulfate pentahydrate) powder, wherein the content of sodium starch octenyl succinate is about 34%, the content of maltodextrin is about 13% and the content of calcium gluconate is about 5%. The air inlet temperature of spray drying is 150 ℃, and the air outlet temperature is 100 ℃; after powder is collected, the materials are sieved by a 60-mesh sieve and then enter a packing room for packing, warehousing and sending inspection by a vertical blanking system.
Example 4
Weighing 500 kg of purified water in a batching tank, heating by opening steam to raise the temperature to above 80 ℃, adding 80kg of sodium starch octenyl succinate, 58.5kg of maltodextrin and 14kg of calcium gluconate into hot water in sequence, and uniformly stirring to obtain a mixed solution; placing the mixed solution in a homogenizer, adding 141kg of copper sulfate pentahydrate into the mixed solution, controlling the rotating speed of the homogenizer to 3000r/min, homogenizing for 8min to obtain a visually bright blue solution; the bright blue solution is filtered by a filter membrane with the diameter of 25 mu m, and the filtrate is taken to obtain a mixed solution; the mixed solution is spray dried to obtain 48% copper sulfate dilution (calculated by copper sulfate pentahydrate) powder, wherein the content of sodium starch octenyl succinate is about 27%, the content of maltodextrin is about 20% and the content of calcium gluconate is about 5%. The air inlet temperature of spray drying is 150 ℃, and the air outlet temperature is 100 ℃; after powder is collected, the materials are sieved by a 60-mesh sieve and then enter a packing room for packing, warehousing and sending inspection by a vertical blanking system.
Example 5
Weighing 500 kg of purified water in a batching tank, heating by opening steam to raise the temperature to above 80 ℃, adding 126.2kg of sodium starch octenyl succinate, 118.3kg of maltodextrin and 14kg of calcium gluconate into hot water in sequence, and stirring uniformly to obtain a mixed solution; placing the mixed solution in a homogenizer, adding 35kg of copper sulfate pentahydrate into the mixed solution, controlling the rotating speed of the homogenizer to 3000r/min, homogenizing for 8min to obtain a visually bright blue solution; the bright blue solution is filtered by a filter membrane with the diameter of 25 mu m, and the filtrate is taken to obtain a mixed solution; the mixed solution is subjected to spray drying to obtain 12% copper sulfate dilution (calculated by copper sulfate pentahydrate) powder, wherein the content of sodium starch octenyl succinate is about 43%, the content of maltodextrin is about 40% and the content of calcium gluconate is about 5%. The air inlet temperature of spray drying is 150 ℃, and the air outlet temperature is 100 ℃; after powder is collected, the materials are sieved by a 60-mesh sieve and then enter a packing room for packing, warehousing and sending inspection by a vertical blanking system.
Example 6
This embodiment is substantially the same as embodiment 1, except that:
the raw materials are different in dosage, and the prepared diluted product comprises the following components in percentage by weight:
copper sulfate content 4%, sodium starch octenyl succinate 50%, maltodextrin 39% and calcium gluconate 7%.
Weighing 500 kg of purified water in a batching tank, heating by opening steam to raise the temperature to above 80 ℃, adding 146.8kg of sodium starch octenyl succinate, 114.5kg of maltodextrin and 20.5kg of calcium gluconate into hot water in sequence, and stirring uniformly to obtain a mixed solution; placing the mixed solution in a homogenizer, adding 11.7kg of copper sulfate pentahydrate into the mixed solution, controlling the rotating speed of the homogenizer to 3000r/min, homogenizing for 8min to obtain a visually bright blue solution; the bright blue solution is filtered by a filter membrane with the diameter of 25 mu m, and the filtrate is taken to obtain a mixed solution; the mixed solution is spray dried to obtain 4% copper sulfate dilution (calculated by copper sulfate pentahydrate) powder, wherein the content of sodium starch octenyl succinate is about 50%, the content of maltodextrin is about 39% and the content of calcium gluconate is about 7%. The air inlet temperature of spray drying is 150 ℃, and the air outlet temperature is 100 ℃; after powder is collected, the materials are sieved by a 60-mesh sieve and then enter a packing room for packing, warehousing and sending inspection by a vertical blanking system.
Example 7
This embodiment is substantially the same as embodiment 1, except that:
the raw materials are different in dosage, and the prepared diluted product comprises the following components in percentage by weight:
the copper sulfate content is 58%, sodium starch octenyl succinate 20%, maltodextrin 20% and calcium gluconate 2%.
Weighing 500 kg of purified water in a batching tank, heating by opening steam to raise the temperature to above 80 ℃, adding 58.7kg of sodium starch octenyl succinate, 58.7kg of maltodextrin and 5.87kg of calcium gluconate into hot water in sequence, and stirring uniformly to obtain a mixed solution; placing the mixed solution into a homogenizer, adding 170.2kg of copper sulfate pentahydrate into the mixed solution, controlling the rotating speed of the homogenizer to 3000r/min, homogenizing for 8min to obtain a visually bright blue solution; the bright blue solution is filtered by a filter membrane with the diameter of 25 mu m, and the filtrate is taken to obtain a mixed solution; the mixed solution is subjected to spray drying to obtain 58% copper sulfate dilution (calculated by copper sulfate pentahydrate) powder, wherein the content of sodium starch octenyl succinate is about 20%, the content of maltodextrin is about 20% and the content of calcium gluconate is about 2%. The air inlet temperature of spray drying is 150 ℃, and the air outlet temperature is 100 ℃; after powder is collected, the materials are sieved by a 60-mesh sieve and then enter a packing room for packing, warehousing and sending inspection by a vertical blanking system.
Example 8
This embodiment is substantially the same as embodiment 1, except that:
the raw materials are different in dosage, and the prepared diluted product comprises the following components in percentage by weight:
the copper sulfate content is 30%, sodium starch octenyl succinate 30%, maltodextrin 30% and calcium gluconate 10%.
Weighing 500 kg of purified water in a batching tank, heating by opening steam to raise the temperature to above 80 ℃, adding 88.1kg of sodium starch octenyl succinate, 88.1kg of maltodextrin and 29.4kg of calcium gluconate into hot water in sequence, and stirring uniformly to obtain a mixed solution; placing the mixed solution into a homogenizer, adding 88.1kg of copper sulfate pentahydrate into the mixed solution, controlling the rotating speed of the homogenizer to 3000r/min, homogenizing for 8min to obtain a visually bright blue solution; the bright blue solution is filtered by a filter membrane with the diameter of 25 mu m, and the filtrate is taken to obtain a mixed solution; the mixed solution is subjected to spray drying to obtain 30% copper sulfate dilution (calculated by copper sulfate pentahydrate) powder, wherein the content of sodium starch octenyl succinate is about 30%, the content of maltodextrin is about 30% and the content of calcium gluconate is about 10%. The air inlet temperature of spray drying is 150 ℃, and the air outlet temperature is 100 ℃; after powder is collected, the materials are sieved by a 60-mesh sieve and then enter a packing room for packing, warehousing and sending inspection by a vertical blanking system.
Example 9
This embodiment is substantially the same as embodiment 1, except that:
the raw materials are different in dosage, and the prepared diluted product comprises the following components in percentage by weight:
the copper sulfate content is 35%, the octenyl succinic acid starch sodium is 47%, the maltodextrin is 15% and the calcium gluconate is 3%.
Weighing 500 kg of purified water in a batching tank, heating by opening steam to raise the temperature to above 80 ℃, adding 137.9kg of sodium starch octenyl succinate, 44.0kg of maltodextrin and 8.8kg of calcium gluconate into hot water in sequence, and stirring uniformly to obtain a mixed solution; placing the mixed solution in a homogenizer, adding 102.7kg of copper sulfate pentahydrate into the mixed solution, controlling the rotating speed of the homogenizer to 3000r/min, homogenizing for 8min to obtain a visually bright blue solution; the bright blue solution is filtered by a filter membrane with the diameter of 25 mu m, and the filtrate is taken to obtain a mixed solution; the mixed solution is subjected to spray drying to obtain 35% copper sulfate dilution (calculated by copper sulfate pentahydrate) powder, wherein the content of sodium starch octenyl succinate is about 47%, the content of maltodextrin is about 15% and the content of calcium gluconate is about 3%. The air inlet temperature of spray drying is 150 ℃, and the air outlet temperature is 100 ℃; after powder is collected, the materials are sieved by a 60-mesh sieve and then enter a packing room for packing, warehousing and sending inspection by a vertical blanking system.
Example 10
This embodiment is substantially the same as embodiment 1, except that:
the raw materials are different in dosage, and the prepared diluted product comprises the following components in percentage by weight:
the copper sulfate content is 30%, sodium starch octenyl succinate is 25%, maltodextrin is 40% and calcium gluconate is 5%.
Weighing 500 kg of purified water in a batching tank, heating by opening steam to raise the temperature to above 80 ℃, adding 73.4kg of sodium starch octenyl succinate, 117.4kg of maltodextrin and 14.7kg of calcium gluconate into hot water in sequence, and stirring uniformly to obtain a mixed solution; placing the mixed solution into a homogenizer, adding 88.1kg of copper sulfate pentahydrate into the mixed solution, controlling the rotating speed of the homogenizer to 3000r/min, homogenizing for 8min to obtain a visually bright blue solution; the bright blue solution is filtered by a filter membrane with the diameter of 25 mu m, and the filtrate is taken to obtain a mixed solution; the mixed solution is subjected to spray drying to obtain 30% copper sulfate dilution (calculated by copper sulfate pentahydrate) powder, wherein the content of sodium starch octenyl succinate is about 25%, the content of maltodextrin is about 40% and the content of calcium gluconate is about 5%. The air inlet temperature of spray drying is 150 ℃, and the air outlet temperature is 100 ℃; after powder is collected, the materials are sieved by a 60-mesh sieve and then enter a packing room for packing, warehousing and sending inspection by a vertical blanking system.
Comparative example 1
This comparative example is substantially the same as example 1, except that: adding the addition amount of copper sulfate pentahydrate, namely 146.75g of copper sulfate pentahydrate and 32.75kg of maltodextrin; the resulting dilution had a copper sulfate content of about 63%. The flowability of the material is poor.
Comparative example 2
This comparative example is substantially the same as example 1, except that: the amount of deionized water was less than in example 1 and the solids content of the mixed solution was 50%.
The sodium starch octenyl succinate is incompletely dissolved, the solution is viscous, and the materials are difficult to completely dissolve. The product has low material collection, blue color points and uneven color.
Comparative example 3
This comparative example is substantially the same as example 1, except that: the added amount of calcium gluconate is increased, namely, the added amount of calcium gluconate is 35.22kg, and the added amount of maltodextrin is 99.03kg.
The addition amount of calcium gluconate is more, and the material fluidity is slightly poor.
Comparative example 4
This comparative example is essentially the same as example 1, except that calcium gluconate is replaced entirely with maltodextrin. The material flow property is slightly poor.
Comparative example 5
This comparative example is substantially the same as example 1, except that: the sodium starch octenyl succinate is replaced by maltodextrin. The flowability of the material is poor.
Comparative example 6
This comparative example is substantially the same as example 1, except that: the addition amount of sodium starch octenyl succinate is reduced, and the addition amount of maltodextrin is increased, namely 67.5kg of sodium starch octenyl succinate and 152.75kg of maltodextrin are added. The flowability of the material is slightly poor.
Comparative example 7
This comparative example is substantially the same as example 1, except that: the maltodextrin was replaced entirely with starch octenyl succinate. The materials are difficult to dissolve and have poor flowability.
Comparative example 8
This comparative example is substantially the same as example 1, except that: the addition amount of sodium starch octenyl succinate is partially increased, namely 161.4kg of sodium starch octenyl succinate and 58.9kg of maltodextrin. Is difficult to dissolve and has poor material fluidity.
Experimental example 1
Testing the fineness of the powder of the prepared copper sulfate dilution, wherein the testing method is a 100-mesh standard screening method;
the preparation performance of the prepared copper sulfate dilution is tested, the test method is that 5g of the sample is dissolved in 100g of purified water at the normal temperature of 25 ℃ and the color state is observed;
the fluidity of the prepared copper sulfate dilution is tested, and the test method is to measure the repose angle of the sample by adopting a fixed cone bottom method;
the test results are recorded in table 1.
Table 1 Properties of the copper sulfate dilutions made in the examples and comparative examples
From the table, the copper sulfate dilution prepared by each embodiment of the application has fine powder, the 100 mesh passing rate is over 99 percent, the copper sulfate dilution does not generate blue color point in the process of brewing, the water-soluble cavity has excellent fluidity and the repose angle is less than 30; by comparing the example 1 with the comparative example 1, the product prepared in the example 1 has better brewing performance, has no blue color point in the brewing process, and shows that the diluted product with better performance can be obtained by taking the copper sulfate pentahydrate with proper proportion as the raw material; comparing example 1 with comparative example 2, the diluent prepared in comparative example 2 has smaller repose angle and better flowability, which indicates that the solid content of the solution to be dried should not be too large, and the flowability of the diluent prepared by too large is poor; comparing comparative examples 3-8 with example 1, comparative examples 3-8 have poor flowability and the 100 mesh passing rate cannot reach more than 99%, which means that calcium gluconate, maltodextrin and sodium starch octenyl succinate added in the preparation raw materials should be within the proportion range defined in the application, and any excessive or insufficient raw materials can affect the performance of the prepared dilution.
Experimental example 2
The stability of the dilutions made in example 1 (dilution 1) and comparative examples 2 to 8 was tested, in particular: a certain amount of copper sulfate dilution (calculated by copper sulfate pentahydrate) microcapsule powder is weighed, placed in a constant temperature drying oven with constant temperature of 38 ℃ and relative humidity of 75%, placed for 1, 3, 5, 7 and 15 days, and the content change of copper element is measured according to GB 5009.13. The stability results were counted as shown in fig. 3.
As can be seen from fig. 3, the dilution provided in example 1 of the present application (copper sulfate pentahydrate 20%, copper content 5%) has significantly better stability than the respective examples.
In summary, the preparation method provided by the invention takes the copper sulfate pentahydrate as a preparation raw material, the food-grade raw material maltodextrin is used for diluting the copper sulfate pentahydrate, the mixed solution is emulsified by utilizing the excellent emulsifying property and film forming property of sodium starch octenyl succinate, the bad smell of copper sulfate is utilized, the sodium starch octenyl succinate plays an embedding effect on the copper sulfate pentahydrate in the spray drying process, calcium element is introduced by utilizing calcium gluconate, the strength and the viscoelasticity of a film are enhanced, the embedded copper sulfate can resist stronger strain pressure, cracks caused by particle collision in the spray drying process are prevented, thereby achieving a better embedding effect, the proportion of each raw material is regulated within a proper range, the preparation method is provided for fully dissolving various elements to obtain a solution, and then drying the solution, so that not only is the hygroscopicity of copper sulfate reduced, but also part of copper smell is covered, the diluted product prepared by the mixed solution dissolved with the various substances is fine and smooth, the 100-mesh passing rate is more than 99%, blue color is not generated in the process, the water-soluble powder-like flow angle sedimentation is better, and the sedimentation-free sedimentation-type product is easy, and the sedimentation-free from sedimentation-of the powder-type product is 30.
The above is only a preferred embodiment of the present invention, and is not intended to limit the present invention, but various modifications and variations can be made to the present invention by those skilled in the art. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. A method for preparing a copper sulfate dilution, comprising:
drying and pulverizing the mixed solution with the solid content of 30-40% to obtain microcapsule powder;
the mixed solution is a solution in which sodium starch octenyl succinate, maltodextrin, calcium gluconate and copper sulfate pentahydrate are dissolved, wherein the sodium starch octenyl succinate accounts for 20-50%, the maltodextrin accounts for 20-49%, the calcium gluconate accounts for 2-10%, and the copper sulfate pentahydrate accounts for 4-58%.
2. The method according to claim 1, wherein the sodium starch octenyl succinate is 25 to 47%, the maltodextrin is 15 to 40%, the calcium gluconate is 3 to 7%, and the copper sulfate pentahydrate is 12 to 48%.
3. The method of claim 1, further comprising preparing a mixed solution prior to performing spray drying, the method of preparing a mixed solution comprising:
adding the copper sulfate pentahydrate into the high-temperature mixed solution, and shearing in a homogenizer until visual appearance to obtain a bright blue solution; the high-temperature mixed solution is mixed solution which consists of sodium starch octenyl succinate, maltodextrin, calcium gluconate and water and has the temperature of 80-100 ℃.
4. The method according to claim 3, wherein the high-temperature mixed solution is prepared by adding sodium starch octenyl succinate, maltodextrin and calcium gluconate to water at 80-100 ℃; or after uniformly mixing the sodium starch octenyl succinate, the maltodextrin, the calcium gluconate and water, raising the temperature to 80-100 ℃.
5. The method according to claim 3, wherein the shearing homogenizing speed is 1000-5000 r/min and the shearing time is 5-10 min.
6. The method according to claim 5, wherein the shearing homogenizing speed is 2000-4000 r/min.
7. The method according to claim 3, wherein the preparation of the brilliant blue solution further comprises passing the brilliant blue solution through a filter membrane having a pore size of 25 μm, and collecting the filtrate to obtain the mixed solution.
8. The method of claim 1, wherein the method of drying the powder is spray drying;
preferably, the air inlet temperature of spray drying is 150-165 ℃, and the air outlet temperature is 100-110 ℃.
9. A copper sulphate dilution produced by the production method according to any one of claims 1 to 8.
10. Use of a copper sulphate dilution according to claim 9 in a nutritional or pharmaceutical product.
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