Copper sulfate diluent, its preparation method and application

CN117731692BActive Publication Date: 2026-08-14ZHENGZHOU RUIPU BIOLOGICAL ENG CO LTD
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Patent Information

Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2023-12-18
Publication Date
2026-08-14

AI Technical Summary

Benefits of technology

[0022]The preparation method described above uses copper sulfate pentahydrate as the raw material. It dilutes the copper sulfate pentahydrate with food-grade maltodextrin and emulsifies the solution using the excellent emulsifying and film-forming properties of sodium octenyl succinate starch. This allows the sodium octenyl succinate starch to encapsulate the copper sulfate pentahydrate during spray drying. Furthermore, calcium gluconate introduces calcium to enhance the film's strength and viscoelasticity, enabling the encapsulated copper sulfate to withstand stronger strain pressures and preventing cracks caused by particle collisions during spray drying, thus achieving a better encapsulation effect. This method not only reduces the hygroscopicity of copper sulfate but also masks some of its unpleasant odor. By adjusting the proportions of each raw material within a suitable range, it provides a preparation method that involves fully dissolving various elements to obtain a solution and then drying the solution. This not only improves the coppery odor of copper but also produces a fine powder from the mixed solution containing the above-mentioned substances, with a 100-mesh pass rate of over 99%. It does not produce blue spots during reconstitution, has stronger water solubility, and exhibits excellent flowability with an angle of repose of <30°, allowing it to be uniformly dispersed in the medium and possessing the advantage of not easily settling.

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Abstract

This invention relates to the field of biomedicine, disclosing a copper sulfate diluent, its preparation method, and its applications. The preparation method of the copper sulfate diluent includes: drying a mixed solution with a solid content of 30-40% to obtain microcapsule powder; the mixed solution is a solution containing sodium octenyl succinate starch, maltodextrin, calcium gluconate, and copper sulfate pentahydrate, wherein the proportions of sodium octenyl succinate starch are 20-50%, maltodextrin is 20-49%, calcium gluconate is 2-10%, and copper sulfate pentahydrate is 4-58%. The disclosed copper sulfate diluent is prepared using the above method. The diluent obtained by this invention has a fine powder with a 100-mesh pass rate of over 99%, does not produce blue spots during reconstitution, has stronger water solubility, and exhibits excellent flowability with an angle of repose <30°, allowing for uniform dispersion in a medium and preventing sedimentation. It can be used in nutritional products and pharmaceuticals.
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Description

Technical Field

[0001] This invention relates to the field of biomedical technology, and more specifically, to copper sulfate dilution, its preparation method, and its application. Background Technology

[0002] Copper, an important component of bones, promotes the deposition of calcium and phosphorus in cartilage, increasing bone density. Furthermore, copper participates in hematopoiesis by influencing iron absorption and release. Other researchers have demonstrated that trace element copper can enhance the body's immune function through enzymes and its own antioxidant properties. In addition, copper sulfate contains copper ions that not only react with oxidants to extend the shelf life of food, but also act as a food preservative, inhibiting enzyme activity and microbial growth in food, thus preventing spoilage. It is also used as a bactericide in the fruit and vegetable industry.

[0003] Based on the dietary copper intake of Chinese residents, the Chinese Nutrition Society recommends a daily intake (RNI) of 0.8 mg / day for adults and a tolerable upper intake level (UL) of 8 mg / day. High copper levels in the body may lead to gastrointestinal diseases, nervous system diseases, and liver and kidney diseases. Therefore, to improve the safety of use, it is necessary to dilute copper supplements. Generally, nutritional supplements are presented as powder products, and developing a copper diluent that is easy to dissolve and disperse would have significant economic value.

[0004] In view of this, the present invention is proposed. Summary of the Invention

[0005] The purpose of this invention is to provide copper sulfate dilution, its preparation method, and its application.

[0006] This invention is implemented as follows:

[0007] In a first aspect, the present invention provides a method for preparing a diluted copper sulfate product, comprising:

[0008] Microcapsule powder is obtained by drying a mixed solution with a solid content of 30-40%.

[0009] The mixed solution is a solution containing sodium octenyl succinate starch, maltodextrin, calcium gluconate, and copper sulfate pentahydrate. The sodium octenyl succinate starch accounts for 20-50%, maltodextrin accounts for 20-49%, calcium gluconate accounts for 2-10%, and copper sulfate pentahydrate accounts for 4-58%.

[0010] In optional embodiments, sodium octenyl succinate starch is preferably 25-47%, maltodextrin is preferably 15-40%, calcium gluconate is preferably 3-7%, and copper sulfate pentahydrate is preferably 12-48%.

[0011] In an optional embodiment, the preparation of a mixed solution is further included before spray drying, and the method for preparing the mixed solution includes:

[0012] Copper sulfate pentahydrate was added to a high-temperature mixture and sheared in a homogenizer until a bright blue solution was obtained visually. The high-temperature mixture was a mixture of sodium octenyl succinate starch, maltodextrin, calcium gluconate, and water at a temperature of 80–100°C.

[0013] In an optional embodiment, the high-temperature mixture is prepared by adding sodium octenyl succinate starch, maltodextrin, and calcium gluconate to water at 80–100°C; or by mixing sodium octenyl succinate starch, maltodextrin, calcium gluconate, and water evenly, and then raising the temperature to 80–100°C.

[0014] In an optional embodiment, the shearing and homogenization speed is 1000-5000 r / min, and the shearing time is 5-10 min.

[0015] In an optional embodiment, the shearing and homogenization rotation speed is 2000–4000 r / min.

[0016] In an optional embodiment, after obtaining the bright blue solution, the solution is further passed through a filter membrane with a pore size of 25 μm, and the filtrate is taken to obtain the mixed solution.

[0017] In an optional implementation, the drying and powdering method is spray drying;

[0018] Preferably, the inlet air temperature for spray drying is 150–165°C, and the outlet air temperature is 100–110°C.

[0019] Secondly, the present invention provides a copper sulfate dilution, which is prepared by any of the preparation methods described in the foregoing embodiments.

[0020] Thirdly, the present invention provides the use of copper sulfate dilutions as described above in nutritional products or pharmaceuticals.

[0021] The present invention has the following beneficial effects:

[0022] The preparation method described above uses copper sulfate pentahydrate as the raw material. It dilutes the copper sulfate pentahydrate with food-grade maltodextrin and emulsifies the solution using the excellent emulsifying and film-forming properties of sodium octenyl succinate starch. This allows the sodium octenyl succinate starch to encapsulate the copper sulfate pentahydrate during spray drying. Furthermore, calcium gluconate introduces calcium to enhance the film's strength and viscoelasticity, enabling the encapsulated copper sulfate to withstand stronger strain pressures and preventing cracks caused by particle collisions during spray drying, thus achieving a better encapsulation effect. This method not only reduces the hygroscopicity of copper sulfate but also masks some of its unpleasant odor. By adjusting the proportions of each raw material within a suitable range, it provides a preparation method that involves fully dissolving various elements to obtain a solution and then drying the solution. This not only improves the coppery odor of copper but also produces a fine powder from the mixed solution containing the above-mentioned substances, with a 100-mesh pass rate of over 99%. It does not produce blue spots during reconstitution, has stronger water solubility, and exhibits excellent flowability with an angle of repose of <30°, allowing it to be uniformly dispersed in the medium and possessing the advantage of not easily settling. Attached Figure Description

[0023] To more clearly illustrate the technical solutions of the embodiments of the present invention, the accompanying drawings used in the embodiments will be briefly introduced below. It should be understood that the following drawings only show some embodiments of the present invention and should not be regarded as a limitation on the scope. For those skilled in the art, other related drawings can be obtained based on these drawings without creative effort.

[0024] Figure 1 The images show the morphology of the diluted product obtained in Example 1 and the morphology of the solvent prepared by dissolving it in water.

[0025] Figure 2 This is a diagram of a directly compressed tablet of copper sulfate dilution from Example 1.

[0026] Figure 3 This is a graph showing the storage stability analysis of diluted copper sulfate. Detailed Implementation

[0027] To make the objectives, technical solutions, and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below. Where specific conditions are not specified in the embodiments, conventional conditions or conditions recommended by the manufacturer shall apply. Reagents or instruments whose manufacturers are not specified are all conventional products that can be purchased commercially.

[0028] The following provides a detailed description of the copper sulfate diluent, its preparation method, and its application provided in the embodiments of the present invention.

[0029] The method for preparing copper sulfate diluent provided in this embodiment of the invention includes:

[0030] The mixed solution with a mass concentration of 30-40% is dried and powdered to obtain microcapsule powder;

[0031] The mixed solution is a solution containing sodium octenyl succinate starch, maltodextrin, calcium gluconate, and copper sulfate pentahydrate, wherein the sodium octenyl succinate starch accounts for 20-50%, maltodextrin accounts for 20-49%, calcium gluconate accounts for 2-10%, and copper sulfate pentahydrate accounts for 4-58%.

[0032] Anhydrous copper sulfate and hydrated copper sulfate are the main forms of copper. However, anhydrous copper sulfate has a strong pungent odor, is easily deliquescent in humid air, and readily forms black copper oxide at high temperatures. Therefore, products prepared from anhydrous copper sulfate have poor flavor and stability. In contrast, hydrated copper sulfate has improved water solubility and stability, resulting in products with better flavor and application stability. Furthermore, hydrated copper sulfate also possesses emetic, desiccant, and detoxifying properties. It can also be used as a clarifying and chelating agent in wine and preserved egg processing, and as a traditional Chinese medicine to increase bile flow, with high safety profile.

[0033] Pure hydrated copper sulfate is hygroscopic. When mixed with other base materials, the content is difficult to control and the mixing is poor due to the small amount added. Therefore, the problem of poor mixing needs to be overcome in order to prepare copper sulfate dilution using pentahydrate copper sulfate as raw material.

[0034] The preparation method provided in this invention uses copper sulfate pentahydrate as the raw material. It dilutes the copper sulfate using food-grade maltodextrin, utilizes sodium octenyl succinate starch for emulsification and encapsulation, and introduces calcium using calcium gluconate. By adjusting the proportions of each raw material within a suitable range, this method provides a preparation method that fully dissolves various elements to obtain a solution, which is then dried. This method not only dilutes and encapsulates the copper sulfate using the emulsifying and film-forming properties of sodium octenyl succinate starch, but also introduces calcium using calcium gluconate, enhancing the film's strength and viscoelasticity, preventing cracks during spray drying, and improving the hygroscopicity and coppery odor of the copper sulfate. Furthermore, the diluted product obtained from the mixed solution containing the above substances is a fine powder with a 100-mesh pass rate of over 99%. It does not produce blue spots during reconstitution, exhibits stronger water solubility, and has excellent flowability with an angle of repose <30°, allowing for uniform dispersion in the medium and preventing sedimentation.

[0035] Preferably, the sodium octenyl succinate starch content is 25-47%, the maltodextrin content is 15-40%, the calcium gluconate content is 3-7%, and the copper sulfate pentahydrate content is 12-48%.

[0036] The above raw material ratio can further ensure the production of a diluent with better performance.

[0037] Optionally, the preparation of a mixed solution is included prior to spray drying, and the method for preparing the mixed solution includes:

[0038] Add copper sulfate pentahydrate to the high-temperature mixture and place it in a homogenizer for shearing until a bright blue solution is obtained visually; the high-temperature mixture is a mixture of sodium octenyl succinate starch, maltodextrin, calcium gluconate and water at a temperature of 80-100°C (e.g., 80°C, 90°C or 100°C).

[0039] Considering the subsequent absorption effect of copper sulfate, it is important to control the uniformity of the system and the appropriate particle size. Therefore, a combination of high temperature and shear homogenization is used to ensure that a homogeneous and completely dissolved solution can be obtained, and that the particle size is within a controllable range. This allows for the production of a high-performance copper sulfate dilution after drying.

[0040] Preferably, to avoid the presence of undissolved particles in the solution affecting the performance of the prepared diluted product, after obtaining the bright blue solution, the solution is further passed through a filter membrane with a pore size of 25 μm, and the filtrate is taken to obtain the mixed solution.

[0041] Preferably, the homogenization conditions for achieving solute dissolution are: a shear homogenization speed of 1000–5000 r / min (e.g., 1000 r / min, 1200 r / min, or 1500 r / min) and a shearing time of 5–10 min (e.g., 5 min, 8 min, or 10 min); more preferably, the shear homogenization speed is 2000–4000 r / min (e.g., 2000 r / min, 3000 r / min, or 4000 r / min).

[0042] Furthermore, the high-temperature mixture can be prepared by adding sodium octenyl succinate starch, maltodextrin, and calcium gluconate to water at 80–100°C (e.g., 80°C, 90°C, or 100°C); or by mixing sodium octenyl succinate starch, maltodextrin, calcium gluconate, and water evenly, and then raising the temperature to 80–100°C (e.g., 80°C, 90°C, or 100°C).

[0043] Preferably, the drying method is spray drying. Spray drying can produce powders with uniform particle size and good particle dispersibility.

[0044] The copper sulfate diluent provided in this embodiment of the invention is prepared using the preparation method provided in this application.

[0045] The present invention also provides the application of the above-mentioned copper sulfate dilution in nutritional products or pharmaceuticals.

[0046] The features and performance of the present invention will be further described in detail below with reference to embodiments.

[0047] Example 1

[0048] Weigh 500 kg of purified water into a mixing tank, turn on steam heating to raise the temperature to above 80℃, add 100 kg of sodium octenyl succinate starch, 120.25 kg of maltodextrin, and 14 kg of calcium gluconate to the hot water in sequence, and stir until homogeneous to obtain a mixed solution; place the mixed solution in a homogenizer, add 59.25 kg of copper sulfate pentahydrate to the mixed solution, control the homogenizer speed to 3000 r / min, homogenize for 8 min to obtain a solution that appears bright blue; filter the bright blue solution through a 25 μm filter membrane, and collect the filtrate to obtain the mixed solution; spray dry the mixed solution to obtain a 20% copper sulfate diluted product (calculated as copper sulfate pentahydrate) powder, in which the content of sodium octenyl succinate starch is approximately 34%, the content of maltodextrin is approximately 41%, and the content of calcium gluconate is approximately 5%. The inlet air temperature for spray drying is 150℃, and the outlet air temperature is 100℃. After powder collection, the material passes through a 60-mesh sieve and is then fed into the packaging room via a vertical feeding system for packaging, warehousing, and inspection.

[0049] The resulting diluted product, such as Figure 1 As shown, there are no unevenly distributed blue dots, indicating that the finished product has good dispersion uniformity. The diluted product obtained in this example was dissolved in water to prepare aqueous solutions of different concentrations, such as... Figure 1 As shown in the right figure, the aqueous solution has a uniform color.

[0050] The obtained diluted product is made into tablets, such as... Figure 2 As shown, from Figure 2 It can be seen that the tablets have a good morphology.

[0051] Example 2

[0052] Weigh 500 kg of purified water into a mixing tank, turn on steam heating to raise the temperature to above 80℃, add 100 kg of sodium octenyl succinate starch, 61 kg of maltodextrin, and 14 kg of calcium gluconate to the hot water in sequence, and stir until homogeneous to obtain a mixed solution; place the mixed solution in a homogenizer, add 118.5 kg of copper sulfate pentahydrate to the mixed solution, control the homogenizer speed to 3000 r / min, homogenize for 8 min to obtain a solution that appears bright blue; filter the bright blue solution through a 25 μm filter membrane, and collect the filtrate to obtain the mixed solution; spray dry the mixed solution to obtain a 40% copper sulfate diluted product (calculated as copper sulfate pentahydrate) powder, in which the content of sodium octenyl succinate starch is approximately 34%, the content of maltodextrin is approximately 21%, and the content of calcium gluconate is approximately 5%. The inlet air temperature for spray drying is 150℃, and the outlet air temperature is 100℃. After powder collection, the material passes through a 60-mesh sieve and is then fed into the packaging room via a vertical feeding system for packaging, warehousing, and inspection.

[0053] Example 3

[0054] Weigh 500 kg of purified water into a mixing tank, turn on steam heating to raise the temperature to above 80℃, and add 100 kg of sodium octenyl succinate starch, 38.5 kg of maltodextrin, and 14 kg of calcium gluconate to the hot water in sequence. Stir well to obtain a mixed solution. Place the mixed solution in a homogenizer, add 141 kg of copper sulfate pentahydrate to the mixed solution, control the homogenizer speed at 3000 r / min, and homogenize for 8 min to obtain a solution that appears bright blue. Filter the bright blue solution through a 25 μm filter membrane and collect the filtrate to obtain the mixed solution. Spray dry the mixed solution to obtain a 48% copper sulfate diluted product (calculated as copper sulfate pentahydrate) powder, in which the content of sodium octenyl succinate starch is approximately 34%, the content of maltodextrin is approximately 13%, and the content of calcium gluconate is approximately 5%. The inlet air temperature for spray drying is 150℃, and the outlet air temperature is 100℃. After powder collection, the material passes through a 60-mesh sieve and is then fed into the packaging room via a vertical feeding system for packaging, warehousing, and inspection.

[0055] Example 4

[0056] Weigh 500 kg of purified water into a mixing tank, turn on steam heating to raise the temperature to above 80℃, and add 80 kg of sodium octenyl succinate starch, 58.5 kg of maltodextrin, and 14 kg of calcium gluconate to the hot water in sequence, stirring until homogeneous to obtain a mixed solution. Place the mixed solution in a homogenizer, add 141 kg of copper sulfate pentahydrate to the mixed solution, control the homogenizer speed at 3000 r / min, and homogenize for 8 min to obtain a solution that appears bright blue. Filter the bright blue solution through a 25 μm filter membrane, and collect the filtrate to obtain the mixed solution. Spray dry the mixed solution to obtain a 48% copper sulfate diluted product (calculated as copper sulfate pentahydrate) powder, in which the content of sodium octenyl succinate starch is approximately 27%, the content of maltodextrin is approximately 20%, and the content of calcium gluconate is approximately 5%. The inlet air temperature of the spray dryer is 150℃, and the outlet air temperature is 100℃. After powder collection, the material is passed through a 60-mesh sieve and then fed into the packaging room via a vertical feeding system for packaging, warehousing, and inspection.

[0057] Example 5

[0058] Weigh 500 kg of purified water into a mixing tank, turn on steam heating to raise the temperature to above 80℃, and add 126.2 kg of sodium octenyl succinate starch, 118.3 kg of maltodextrin, and 14 kg of calcium gluconate to the hot water in sequence. Stir well to obtain a mixed solution. Place the mixed solution in a homogenizer, add 35 kg of copper sulfate pentahydrate to the mixed solution, control the homogenizer speed to 3000 r / min, and homogenize for 8 min to obtain a solution that appears bright blue. Filter the bright blue solution through a 25 μm filter membrane and collect the filtrate to obtain the mixed solution. Spray dry the mixed solution to obtain a 12% copper sulfate diluted product (calculated as copper sulfate pentahydrate) powder, in which the content of sodium octenyl succinate starch is approximately 43%, the content of maltodextrin is approximately 40%, and the content of calcium gluconate is approximately 5%. The inlet air temperature for spray drying is 150℃, and the outlet air temperature is 100℃. After powder collection, the material passes through a 60-mesh sieve and is then fed into the packaging room via a vertical feeding system for packaging, warehousing, and inspection.

[0059] Example 6

[0060] This embodiment is basically the same as Embodiment 1, except that:

[0061] The content of each component in the diluted product varies depending on the amount of each raw material used:

[0062] The contents are: copper sulfate 4%, sodium octenyl succinate starch 50%, maltodextrin 39%, and calcium gluconate 7%.

[0063] Weigh 500 kg of purified water into a mixing tank, turn on steam heating to raise the temperature to above 80℃, and add 146.8 kg of sodium octenyl succinate starch, 114.5 kg of maltodextrin, and 20.5 kg of calcium gluconate to the hot water in sequence. Stir well to obtain a mixed solution. Place the mixed solution in a homogenizer, add 11.7 kg of copper sulfate pentahydrate to the mixed solution, control the homogenizer speed at 3000 r / min, and homogenize for 8 min to obtain a solution that appears bright blue. Filter the bright blue solution through a 25 μm filter membrane and collect the filtrate to obtain the mixed solution. Spray dry the mixed solution to obtain a 4% copper sulfate diluted product (calculated as copper sulfate pentahydrate) powder, in which the content of sodium octenyl succinate starch is approximately 50%, the content of maltodextrin is approximately 39%, and the content of calcium gluconate is approximately 7%. The inlet air temperature for spray drying is 150℃, and the outlet air temperature is 100℃. After powder collection, the material passes through a 60-mesh sieve and is then fed into the packaging room via a vertical feeding system for packaging, warehousing, and inspection.

[0064] Example 7

[0065] This embodiment is basically the same as Embodiment 1, except that:

[0066] The content of each component in the diluted product varies depending on the amount of each raw material used:

[0067] The contents are: copper sulfate 58%, sodium octenyl succinate starch 20%, maltodextrin 20%, and calcium gluconate 2%.

[0068] Weigh 500 kg of purified water into a mixing tank, turn on steam heating to raise the temperature to above 80℃, and add 58.7 kg of sodium octenyl succinate starch, 58.7 kg of maltodextrin, and 5.87 kg of calcium gluconate to the hot water in sequence. Stir well to obtain a mixed solution. Place the mixed solution in a homogenizer, add 170.2 kg of copper sulfate pentahydrate to the mixed solution, control the homogenizer speed at 3000 r / min, and homogenize for 8 min to obtain a solution that appears bright blue. Filter the bright blue solution through a 25 μm filter membrane and collect the filtrate to obtain the mixed solution. Spray dry the mixed solution to obtain a 58% copper sulfate diluted product (calculated as copper sulfate pentahydrate) powder, in which the content of sodium octenyl succinate starch is approximately 20%, the content of maltodextrin is approximately 20%, and the content of calcium gluconate is approximately 2%. The inlet air temperature for spray drying is 150℃, and the outlet air temperature is 100℃. After powder collection, the material passes through a 60-mesh sieve and is then fed into the packaging room via a vertical feeding system for packaging, warehousing, and inspection.

[0069] Example 8

[0070] This embodiment is basically the same as Embodiment 1, except that:

[0071] The content of each component in the diluted product varies depending on the amount of each raw material used:

[0072] The contents are: copper sulfate 30%, sodium octenyl succinate starch 30%, maltodextrin 30%, and calcium gluconate 10%.

[0073] Weigh 500 kg of purified water into a mixing tank, turn on steam heating to raise the temperature to above 80℃, and add 88.1 kg of sodium octenyl succinate starch, 88.1 kg of maltodextrin, and 29.4 kg of calcium gluconate to the hot water in sequence. Stir well to obtain a mixed solution. Place the mixed solution in a homogenizer, add 88.1 kg of copper sulfate pentahydrate to the mixed solution, control the homogenizer speed at 3000 r / min, and homogenize for 8 min to obtain a solution that appears bright blue. Filter the bright blue solution through a 25 μm filter membrane and collect the filtrate to obtain the mixed solution. Spray dry the mixed solution to obtain a 30% copper sulfate diluted product (calculated as copper sulfate pentahydrate) powder, in which the content of sodium octenyl succinate starch is approximately 30%, the content of maltodextrin is approximately 30%, and the content of calcium gluconate is approximately 10%. The inlet air temperature for spray drying is 150℃, and the outlet air temperature is 100℃. After powder collection, the material passes through a 60-mesh sieve and is then fed into the packaging room via a vertical feeding system for packaging, warehousing, and inspection.

[0074] Example 9

[0075] This embodiment is basically the same as Embodiment 1, except that:

[0076] The content of each component in the diluted product varies depending on the amount of each raw material used:

[0077] The contents are: copper sulfate 35%, sodium octenyl succinate starch 47%, maltodextrin 15%, and calcium gluconate 3%.

[0078] Weigh 500 kg of purified water into a mixing tank, turn on steam heating to raise the temperature to above 80℃, and add 137.9 kg of sodium octenyl succinate starch, 44.0 kg of maltodextrin, and 8.8 kg of calcium gluconate to the hot water in sequence. After stirring evenly, a mixture is obtained. Place the mixture in a homogenizer, add 102.7 kg of copper sulfate pentahydrate to the mixture, control the homogenizer speed at 3000 r / min, and homogenize for 8 min to obtain a solution that appears bright blue. Filter the bright blue solution through a 25 μm filter membrane, and collect the filtrate to obtain the mixed solution. Spray dry the mixed solution to obtain a 35% copper sulfate diluted product (calculated as copper sulfate pentahydrate) powder, in which the content of sodium octenyl succinate starch is approximately 47%, the content of maltodextrin is approximately 15%, and the content of calcium gluconate is approximately 3%. The inlet air temperature for spray drying is 150℃, and the outlet air temperature is 100℃. After powder collection, the material passes through a 60-mesh sieve and is then fed into the packaging room via a vertical feeding system for packaging, warehousing, and inspection.

[0079] Example 10

[0080] This embodiment is basically the same as Embodiment 1, except that:

[0081] The content of each component in the diluted product varies depending on the amount of each raw material used:

[0082] The composition includes 30% copper sulfate, 25% sodium octenyl succinate starch, 40% maltodextrin, and 5% calcium gluconate.

[0083] Weigh 500 kg of purified water into a mixing tank, turn on steam heating to raise the temperature to above 80℃, and add 73.4 kg of sodium octenyl succinate starch, 117.4 kg of maltodextrin, and 14.7 kg of calcium gluconate to the hot water in sequence. Stir well to obtain a mixed solution. Place the mixed solution in a homogenizer, add 88.1 kg of copper sulfate pentahydrate to the mixed solution, control the homogenizer speed at 3000 r / min, and homogenize for 8 min to obtain a solution that appears bright blue. Filter the bright blue solution through a 25 μm filter membrane and collect the filtrate to obtain the mixed solution. Spray dry the mixed solution to obtain a 30% copper sulfate diluted product (calculated as copper sulfate pentahydrate) powder, in which the content of sodium octenyl succinate starch is approximately 25%, the content of maltodextrin is approximately 40%, and the content of calcium gluconate is approximately 5%. The inlet air temperature for spray drying is 150℃, and the outlet air temperature is 100℃. After powder collection, the material passes through a 60-mesh sieve and is then fed into the packaging room via a vertical feeding system for packaging, warehousing, and inspection.

[0084] Comparative Example 1

[0085] This comparative example is basically the same as Example 1, except that the amount of copper sulfate pentahydrate added is increased, that is, the amount of copper sulfate pentahydrate added is 146.75g, and the amount of maltodextrin added is 32.75kg; the copper sulfate content of the obtained diluted product is about 63%. The material has poor flowability.

[0086] Comparative Example 2

[0087] This comparative example is basically the same as Example 1, except that the amount of deionized water used is less than that in Example 1, and the solid content of the mixed solution is 50%.

[0088] Sodium octenyl succinate starch does not dissolve completely, resulting in a viscous solution that is difficult to fully dissolve. Product yield is low, and the material contains blue spots and exhibits uneven coloring.

[0089] Comparative Example 3

[0090] This comparative example is basically the same as Example 1, except that the amount of calcium gluconate added is increased, that is, the amount of calcium gluconate added is 35.22 kg and the amount of maltodextrin added is 99.03 kg.

[0091] The addition of calcium gluconate is relatively high, resulting in slightly poorer material flowability.

[0092] Comparative Example 4

[0093] This comparative example is basically the same as Example 1, except that calcium gluconate was completely replaced with maltodextrin. The material flowability is slightly worse.

[0094] Comparative Example 5

[0095] This comparative example is basically the same as Example 1, except that sodium octenyl succinate starch is completely replaced with maltodextrin. The material has poor flowability.

[0096] Comparative Example 6

[0097] This comparative example is basically the same as Example 1, except that the amount of sodium octenyl succinate starch added is reduced and the amount of maltodextrin added is increased. Specifically, the amount of sodium octenyl succinate starch added is 67.5 kg and the amount of maltodextrin added is 152.75 kg. The material flowability is slightly worse.

[0098] Comparative Example 7

[0099] This comparative example is basically the same as Example 1, except that all maltodextrin was replaced with octenyl succinic acid starch. The material is difficult to dissolve and has poor flowability.

[0100] Comparative Example 8

[0101] This comparative example is basically the same as Example 1, except that the amount of sodium octenyl succinate starch added is partially increased, that is, the amount of sodium octenyl succinate starch added is 161.4 kg, and the amount of maltodextrin added is 58.9 kg. It is difficult to dissolve and the material has poor flowability.

[0102] Experimental Example 1

[0103] The fineness of the prepared copper sulfate diluted product powder was tested by sieving through a 100-mesh standard sieve.

[0104] The reconstitution properties of the prepared copper sulfate dilution were tested by dissolving 5g of sample in 100g of purified water at 25℃ and observing the color and state.

[0105] The flowability of the prepared copper sulfate dilution was tested by measuring the angle of repose of the sample using the fixed cone base method.

[0106] Record the test results in Table 1.

[0107] Table 1. Performance of copper sulfate diluents prepared in each example and comparative example.

[0108]

[0109]

[0110] As can be seen from the table above, the copper sulfate diluents prepared in each embodiment of this application are finely powdered with a 100-mesh pass rate of over 99%. They do not produce blue spots during reconstitution, have excellent water solubility and flowability, and an angle of repose of <30°. Comparing Example 1 with Comparative Example 1, the product prepared in Example 1 has better reconstitution properties and no blue spots during reconstitution, indicating that using copper sulfate pentahydrate as a raw material in a suitable proportion can yield a better-performing diluent. Comparing Example 1 with Comparative Example 2, the diluent prepared in Comparative Example 2 has a smaller angle of repose and better flowability, indicating that the solid content of the solution used for drying should not be too high, as a high solid content will result in poor flowability of the diluent. Comparing Comparative Examples 3-8 with Example 1, Comparative Examples 3-8 have poor flowability and the 100-mesh pass rate cannot all reach over 99%, indicating that the calcium gluconate, maltodextrin, and sodium octenyl succinate starch added to the raw materials should be within the proportion range specified in this application. Too much or too little of any raw material will affect the performance of the prepared diluent.

[0111] Experimental Example 2

[0112] The stability of the diluents prepared in Example 1 (diluent 1) and Comparative Examples 2-8 was tested. The specific test method was as follows: A certain amount of 20% copper sulfate diluent (calculated as copper sulfate pentahydrate) microcapsule powder was weighed and placed in a constant temperature drying oven at 38℃ and 75% relative humidity for 1, 3, 5, 7, and 15 days. The change in copper content was determined according to GB 5009.13. The stability results were statistically analyzed, such as... Figure 3 As shown.

[0113] from Figure 3 It can be seen that the diluent provided in Example 1 of this application (20% copper sulfate pentahydrate and 5% copper content) has significantly better stability than the other examples.

[0114] In summary, the preparation method provided by this invention uses copper sulfate pentahydrate as the raw material. It dilutes the solution with food-grade maltodextrin, utilizes the excellent emulsifying and film-forming properties of sodium octenyl succinate starch to emulsify the mixed solution, and eliminates the unpleasant odor of copper sulfate. The sodium octenyl succinate starch then effectively encapsulates the copper sulfate pentahydrate during spray drying. Furthermore, calcium gluconate introduces calcium, enhancing the film's strength and viscoelasticity. This allows the encapsulated copper sulfate to withstand stronger strain pressures, preventing cracks caused by particle collisions during spray drying, thereby achieving… To achieve a better encapsulation effect and adjust the ratio of each raw material within a suitable range, a preparation method is provided that involves fully dissolving various elements to obtain a solution, and then drying the solution. This not only reduces the hygroscopicity of copper sulfate but also masks some of the coppery odor. Furthermore, the diluted product obtained from the mixed solution containing the above-mentioned substances is finely powdered with a 100-mesh pass rate of over 99%. It does not produce blue spots during reconstitution, has stronger water solubility, and exhibits excellent flowability with an angle of repose of <30°, allowing it to be uniformly dispersed in the medium and possessing the advantage of not easily settling.

[0115] The above are merely preferred embodiments of the present invention and are not intended to limit the invention. Various modifications and variations can be made to the present invention by those skilled in the art. Any modifications, equivalent substitutions, improvements, etc., made within the spirit and principles of the present invention should be included within the scope of protection of the present invention.

Claims

1. A method for preparing a diluted copper sulfate product, characterized in that, include: Microcapsule powder is obtained by drying a mixed solution with a solid content of 30-40%. The mixed solution is a solution containing sodium octenyl succinate starch, maltodextrin, calcium gluconate and copper sulfate pentahydrate. In the copper sulfate dilution, the sodium octenyl succinate starch accounts for 20-50%, maltodextrin accounts for 20-49%, calcium gluconate accounts for 2-10%, and copper sulfate pentahydrate accounts for 4-58%.

2. The preparation method according to claim 1, characterized in that, The sodium octenyl succinate starch content is 25-47%, the maltodextrin content is 15-40%, the calcium gluconate content is 3-7%, and the copper sulfate pentahydrate content is 12-48%.

3. The preparation method according to claim 1, characterized in that, The process includes preparing a mixed solution prior to drying and pulverizing, the method for preparing the mixed solution comprising: Copper sulfate pentahydrate was added to a high-temperature mixture and sheared in a homogenizer until a bright blue solution was obtained visually; the high-temperature mixture was a mixture of sodium octenyl succinate starch, maltodextrin, calcium gluconate and water at a temperature of 80~100℃.

4. The preparation method according to claim 3, characterized in that, The high-temperature mixture is prepared by adding sodium octenyl succinate starch, maltodextrin, and calcium gluconate to water at 80-100°C; or by mixing sodium octenyl succinate starch, maltodextrin, calcium gluconate, and water evenly, and then raising the temperature to 80-100°C.

5. The preparation method according to claim 3, characterized in that, The shearing speed is 1000~5000 r / min, and the shearing time is 5~10 min.

6. The preparation method according to claim 5, characterized in that, The shearing speed is 2000~4000 r / min.

7. The preparation method according to claim 3, characterized in that, After obtaining the bright blue solution, the process further includes passing it through a filter membrane with a pore size of 25 μm, and taking the filtrate to obtain the mixed solution.

8. The preparation method according to claim 1, characterized in that, The drying and powdering method is spray drying.

9. The preparation method according to claim 8, characterized in that, The inlet air temperature for spray drying is 150~165℃, and the outlet air temperature is 100~110℃.

10. A diluted copper sulfate product, characterized in that, It is prepared by the preparation method described in any one of claims 1 to 9.

11. The use of the copper sulfate dilution as described in claim 10 in the preparation of nutritional products or pharmaceuticals.

Citation Information

Patent Citations

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