High-glue-content dry propolis powder and high-temperature spray drying preparation process thereof

Abstract

The invention relates to the technical field of propolis powder, in particular to high-glue-content dry powdery propolis powder and a high-temperature spray drying preparation process thereof, the glue content reaches 56%-60%, the caking rate is lower than 5% after the dry powdery propolis powder is placed for 180 days in the environment with the temperature being 25 DEG C and the relative humidity being 60%, and the high-temperature spray drying preparation process of the dry powdery propolis powder is achieved. The health-care food also contains the following components in percentage by weight: 0.5%-1% of vitamin E microcapsules, 0.2%-0.5% of tea polyphenol, 0.1%-0.3% of nanoscale silicon dioxide and 0.3%-0.5% of lecithin. The components have a synergistic effect, the oxidation resistance of the product is improved, caking is inhibited, the particle size of the propolis powder is specifically distributed, the emulsification index is greater than 80%, and the performance is excellent. The propolis powder disclosed by the invention is high in propolis content, good in drug effect and health-care effect, high in anti-caking property and convenient to store and process; the emulsifying property is good, and application in multiple fields is facilitated; the preparation process is efficient, low in cost and energy-saving; the product performance is integrally improved, the preparation process is improved, and a new breakthrough is brought to the propolis powder industry.

Description

Technical Field

[0001] The present invention relates to the technical field of propolis powder, and specifically to a dry propolis powder with a high propolis content and a high-temperature spray drying preparation process therefor. Background Art

[0002] In the current era when the concept of health preservation is prevalent, propolis, with its rich bioactive components such as flavonoids and terpenoids, shows great application potential in many fields such as medicine, health products, and cosmetics. As an important product form of propolis, propolis powder has received extensive attention in the market because it is convenient for storage, transportation, and use. Many enterprises have been involved in the research and development and production in this field. However, at present, the propolis powder industry faces many severe problems, which seriously restrict its further development.

[0003] Low propolis content is one of the main problems faced by propolis powder. The propolis content of most propolis powder products on the market is only between 30% and 40%. The low propolis content means that the content of active ingredients in the product per unit mass is scarce. In the medical field, the antibacterial, anti-inflammatory, antioxidant and other bioactive components of propolis are the key to exerting the medicinal effect. The low propolis content makes it difficult for propolis powder to meet the needs of clinical treatment and cannot fully exert its potential medicinal value. For example, when used to treat certain inflammatory diseases, due to insufficient active ingredients, it is difficult to achieve the ideal treatment effect. In terms of health products, propolis powder with low propolis content cannot provide sufficient health care effects for consumers and is difficult to meet people's expectations for health preservation, resulting in a decline in consumers' trust in propolis powder products and affecting the development of the entire industry.

[0004] The storage stability of propolis powder is also a concern. Under ordinary storage conditions, common propolis powder is extremely prone to caking. Caking not only destroys the appearance of the product, but also seriously affects its fluidity and dispersibility. In industrial production processes such as food processing and pharmaceutical manufacturing, caked propolis powder is difficult to accurately measure and uniformly mix. For example, when pharmaceutical enterprises produce drugs containing propolis components, inaccurate measurement due to caking of propolis powder will result in uneven content of propolis in the drugs, affecting the quality of the drugs, and may even cause serious production accidents such as clogging production equipment, bringing huge economic losses and quality risks to the enterprises.

[0005] Poor emulsification performance is also a major obstacle to the application of propolis powder. In the cosmetics industry, it is necessary to uniformly disperse propolis powder in the emulsion system to prepare products with uniform texture and good stability. However, due to the poor emulsification performance of existing propolis powder, it is prone to layering and precipitation in the emulsion, resulting in uneven texture of the cosmetics, affecting the appearance and use effect of the products, and at the same time shortening the shelf life of the products. This greatly limits the application of propolis powder in the cosmetics field and cannot meet the needs of consumers for high-quality cosmetics.

[0006] Existing propolis powder preparation processes mostly adopt vacuum freeze-drying technology. Although this technology can retain the active ingredients in propolis to a certain extent, it has many drawbacks. In terms of production efficiency, the vacuum freeze-drying process includes multiple links such as freezing and sublimation, which takes a long time and significantly extends the production cycle, unable to meet the requirements of large-scale industrial production, resulting in limited market supply of products. In terms of equipment cost, vacuum freeze-drying technology requires complex and expensive equipment such as vacuum systems and refrigeration units. Not only is the equipment purchase cost high, but the subsequent maintenance and repair are difficult and costly, increasing the operating cost of enterprises. In addition, this technology consumes a large amount of energy during operation, which is contrary to the current industrial development trend of energy conservation and environmental protection, and is not conducive to the sustainable development of enterprises and ecological environment protection.

[0007] In summary, the propolis powder industry urgently needs an innovative solution that can not only significantly increase the gum content, enhance storage stability and emulsification performance, but also overcome the defects of traditional preparation processes, achieving efficient, low-cost, energy-saving and environmental protection production. This patent is developed in response to these problems, aiming to bring new breakthroughs to the propolis powder industry and promote its healthy and sustainable development. Summary of the Invention

[0008] (1) Technical problems to be solved

[0009] In view of the deficiencies in the prior art, such as low content of active ingredients, poor stability, easy inactivation, easy caking, and difficulty in spray-drying high-content propolis powder into powder form, the present invention provides a high-gum-content dry propolis powder and its high-temperature spray-drying preparation process.

[0010] (2) Technical solutions

[0011] A high-gum-content dry propolis powder, the propolis powder is in dry powder form, the gum content is 56%-60%, the caking rate is less than 5% after being placed for 180 days at 25°C and relative humidity of 60%, and it contains the following components: vitamin E microcapsules with a weight ratio of 0.5%-1%, natural antioxidant tea polyphenols with a weight ratio of 0.2%-0.5%, nano-scale silica with a weight ratio of 0.1%-0.3%, and lecithin with a weight ratio of 0.3%-0.5%.

[0012] Among them, vitamin E microcapsules can inhibit the oxidation of unsaturated fatty acids, aromatic acids, and flavonoid active ingredients in propolis by slowly releasing vitamin E during storage.

[0013] Tea polyphenols are water-soluble polyphenolic compounds that can quickly neutralize free radicals in the aqueous environment, especially protecting the unstable components on the surface of propolis powder microcapsules. At the same time, they can synergistically enhance the effect with vitamin E microcapsules to form a "dual-phase" antioxidant network, covering different polar environments inside and outside the propolis powder microcapsules, achieving a geometric increase in antioxidant efficiency.

[0014] As a physical barrier, nano-silica extends the diffusion path of free radicals. During spray drying, nano-silica, as an excipient, reduces the adhesion of propolis powder microcapsule particles.

[0015] As an amphiphilic molecule, lecithin self-assembles to form a stable bilayer structure, encapsulating the hydrophobic propolis. Meanwhile, it can also cooperate with β-cyclodextrin to improve the encapsulation efficiency.

[0016] Preferably, the particle size distribution of the propolis powder is as follows: D10 is 5 - 10 μm, D50 is 20 - 30 μm, D90 is 40 - 50 μm, and the emulsification index is greater than 80%. During emulsification, the surface-active components in the propolis powder interact with water molecules and oil molecules in the emulsification system to form a stable emulsion. The reaction formula can be expressed as:

[0017] Surface-active components + H2O + oil molecules → stable emulsion structure. And the unique particle size distribution and high emulsification index of this propolis powder ensure good emulsification effects in different application scenarios.

[0018] Preferably, the high-gum-content dry propolis powder preparation process by high-temperature spray drying includes the following steps:

[0019] S1. Take 9.6 kg of propolis blocks, dissolve them in 50 L of ethanol with a mass fraction of 88% - 95%, then add 0.5% - 1% by weight of vitamin E microcapsules and 0.2% - 0.5% by weight of natural antioxidant tea polyphenols, and stir evenly to obtain the core material. Mix gelatin and β-cyclodextrin in a mass ratio of 1:1, each take 2.7 kg and dissolve them in 150 L of deionized water at 60 °C, then add 0.1% - 0.3% by weight of nano-scale silica and 0.3% - 0.5% by weight of lecithin and stir evenly as the wall material, where the molecular weight of gelatin is 10000 - 15000 Da and the purity of β-cyclodextrin is not less than 98%; during the dissolution process, the active components in the propolis undergo a molecular diffusion and dissolution equilibrium process with ethanol, gelatin and β-cyclodextrin dissolve in water to form a uniform solution system, the gelatin molecules and water molecules are combined with each other through forces such as hydrogen bonds, and the hydroxyl groups of β-cyclodextrin form hydrogen bonds with water molecules to promote dissolution;

[0020] S2. Add the core material to the wall material at 60 °C with a flow rate of 15 - 25 L / h, and hydrate for 2 - 3 h under the condition of a stirring speed of 245 rpm. During this process, the core material and the wall material undergo an emulsification and embedding reaction, and gelatin and β-cyclodextrin embed the active components of propolis under stirring and heating conditions to form a stable microcapsule structure, improving the stability of the active components of propolis.

[0021] S3. At -0.08 MPa and 40 - 60 °C, use a rotary evaporator to concentrate the above mixture until there is no alcohol smell. The concentration time is 2 - 3 hours. During the concentration process, use a vacuum automatic control system to keep the vacuum fluctuation range within ±0.005 MPa. The rotation speed of the rotary evaporator is 80 - 120 rpm, and the cooling medium temperature of the condenser is -5 - 5 °C. During the concentration process, ethanol volatilizes under reduced pressure and heating conditions and is recovered after cooling by the condenser to separate ethanol from the propolis solution and increase the concentration of the propolis solution;

[0022] S4. Pre-filter the concentrated material using a stainless steel filter screen with a pore size of 5 - 10 μm and a filtration pressure of 0.1 - 0.2 MPa. The filtration process is mainly based on the physical sieving principle to remove insoluble impurities in the concentrated liquid and ensure the smooth progress of the subsequent spray drying process;

[0023] S5. Conduct spray drying under the conditions of an inlet temperature of 190 ± 10 °C, an outlet temperature of 90 ± 10 °C, and an atomizer rotation speed of 20000 - 25000 rpm to obtain the propolis powder. During the spray drying process, the hot air first passes through three - stage filtration. The first stage is a primary filter with a filtration efficiency of G4; the second stage is a medium - efficiency filter with a filtration efficiency of F8; the third stage is a high - efficiency filter with a filtration efficiency of H13. And the hot air is pre - heated by an electric heater before entering the drying tower, and the pre - heating temperature control accuracy is ±2 °C. The feeding speed is 100 - 150 mL / min, and the hot air flow rate is 0.8 - 1.2 m 3 / min. During the spray drying process, the propolis solution rapidly evaporates water under the action of high - temperature hot air to form dry - powder - like propolis powder. By precisely controlling parameters such as the inlet and outlet temperatures, atomizer rotation speed, feeding speed, and hot air flow rate, propolis powder with a specific particle size distribution is ensured to be formed.

[0024] S6. Post - process the spray - dried propolis powder, including static aging for 24 - 48 hours in an environment with a relative humidity of 30% - 40% and a temperature of 20 - 25 °C, then use a jet mill for grinding with a grinding pressure of 0.6 - 0.8 MPa. The ground propolis powder is then screened through an 80 - 100 - mesh sieve. During the static aging process, the molecular structure inside the propolis powder is further adjusted and stabilized, involving the rearrangement of intermolecular hydrogen bonds; the jet - grinding process impacts and collides the propolis powder particles with high - speed airflows to further refine their particle sizes; the screening process is based on the physical sieving principle to remove particles that do not meet the particle size requirements to ensure that the particle size distribution of the final product meets the requirements.

[0025] Preferably, in the stirring step, the stirring paddle is an anchor-type stirring paddle. The distance between the stirring paddle and the bottom of the container is 1 / 5 - 1 / 4 of the container diameter. The material of the stirring paddle is stainless steel 304, and the surface roughness Ra ≤ 0.8 μm. This design and parameter setting of the stirring paddle are conducive to improving the stirring efficiency, promoting the uniform mixing of the core material and the wall material, making the embedding reaction more complete. Its principle of action can be explained by the movement trajectory of the stirring paddle and the principle of fluid mechanics, ensuring the formation of a good flow field during stirring, making the material mixing more uniform and the reaction more efficient.

[0026] Preferably, the ratio of the diameter to the height of the drying tower of the spray drying equipment is 1:3 - 1:4. The inner wall material of the drying tower is polytetrafluoroethylene with a thickness of 2 - 3 mm. A pressure sensor is installed at the top of the drying tower to monitor the pressure inside the tower in real time, and the pressure control accuracy is ±0.01 kPa. The specific ratio of the drying tower size and the selection of the inner wall material help to optimize the gas flow distribution and heat and mass transfer process inside the drying tower. The setting of the pressure sensor can monitor and control the pressure inside the tower in real time, ensuring that the spray drying process is carried out under stable conditions to guarantee the consistency and stability of the product quality. Its principle is based on the gas flow dynamics and pressure balance principle inside the drying tower.

[0027] (III) Beneficial technical effects

[0028] Compared with the existing technologies, the beneficial effects of the present invention are as follows:

[0029] 1. In terms of product characteristics, the glue content is as high as 56% - 60%, which has been greatly improved compared with traditional propolis powder. The high glue content enables the highly enrichment of bioactive components in the propolis powder. In medical applications, it can significantly enhance the medicinal efficacy; in the health product field, the propolis powder with high glue content can provide consumers with more sufficient health care effects, meet people's needs for health preservation, and give full play to the health value of propolis.

[0030] 2. When placed in an environment of 25°C and relative humidity of 60% for 180 days, the caking rate is less than 5%. The excellent anti-caking performance ensures that the product always maintains good fluidity and dispersibility during storage and transportation, facilitating the packaging, storage, and processing operations of enterprises, effectively avoiding quality problems and production obstacles caused by caking, greatly improving the stability and quality consistency of the product, and reducing the production cost and quality risk of enterprises.

[0031] 2. Good emulsifying property (emulsification index greater than 80%) opens up broad application prospects for propolis powder in the fields of cosmetics and food processing, etc. In cosmetics, it can be evenly and stably dispersed in the emulsion system, making the product texture more delicate and uniform, extending the shelf life, and enhancing the market competitiveness of the product; in food processing, it can make the propolis powder better mixed with other raw materials, enriching the nutritional components of the food without affecting the taste and appearance of the food.

[0032] 3. In terms of the preparation process, the high-temperature spray drying process has obvious advantages over the traditional vacuum freeze-drying process; the production efficiency is greatly improved, and the preparation of propolis powder can be completed in a relatively short time, meeting the needs of large-scale production, enabling enterprises to quickly respond to market changes and increase product supply; the equipment cost is significantly reduced, without the need for expensive vacuum and refrigeration equipment, reducing the equipment investment and maintenance costs of enterprises, lowering the production cost, and creating a greater profit space for enterprises; moreover, this process has low energy consumption, meets the requirements of the times for energy conservation and environmental protection, reduces the energy consumption and environmental burden of enterprises, and promotes the sustainable development of enterprises. Description of the Drawings

[0033] Figure 1 is the production flow chart of dry propolis powder with high gum content;

[0034] Figure 2 are the test results of the comparative example and the example in terms of gum content, caking rate at 25°C and humidity of 60% for 180 days, and emulsification index;

[0035] Figure 3 is the microscopic examination diagram of the propolis powder liquid;

[0036] Figure 4 Physical pictures of propolis powder and caked propolis powder. Detailed Implementation Modes

[0037] Example 1

[0038] Prepare raw materials: Accurately weigh 960 g of high-quality propolis blocks, measure 5 L of ethanol with a purity of 95%, dissolve the propolis blocks in ethanol, stir until completely dissolved, and then add 9.6 g of vitamin E microcapsules and 4.8 g of tea polyphenols and dissolve them to obtain a clear core material solution;

[0039] Weigh 270 g of gelatin with a molecular weight of 12000 Da and 270 g of β-cyclodextrin with a purity of 99%, add them to 15 L of deionized water maintained at 60°C, continuously stir until completely dissolved, and then add 1.62 g of nano-scale silica and 5.0 g of lecithin and mix evenly to prepare a wall material solution.

[0040] Mixing and hydration: Slowly add the core material solution to the wall material solution at 60°C at a flow rate of 2.5 L / h, use an anchor-type stirring paddle, and hydrate at 60°C for 2.5 hours at a stirring speed of 245 rpm;

[0041] During the stirring process, the distance between the stirring paddle and the bottom of the container is 1 / 4 of the container diameter to ensure uniform mixing.

[0042] Concentration and alcohol removal: Transfer the mixed solution to a rotary evaporator and concentrate it under a pressure of -0.08 MPa and a temperature of 55°C. Set the rotation speed of the rotary evaporator at 100 rpm and control the temperature of the cooling medium in the condenser at 0°C;

[0043] Continue to concentrate until the solution has no alcohol smell; during the concentration process, use the vacuum automatic control system to ensure that the vacuum fluctuation is within ±0.005 MPa.

[0044] Prefiltration: Prefilter the concentrated material with a stainless steel filter screen with a pore size of 8 μm, maintain the filtration pressure at 0.15 MPa, remove insoluble impurities in the solution, and obtain a clear filtrate.

[0045] Spray drying: Introduce the filtrate into the spray drying equipment, set the inlet temperature at 190°C, the outlet temperature at 90°C, the rotation speed of the atomizer at 22000 rpm, the feeding speed at 100 mL / min, and the hot air flow rate at 1 m 3 / min;

[0046] After the hot air passes through the primary filter (filtration efficiency G4), intermediate filter (filtration efficiency F8), and high-efficiency filter (filtration efficiency H13) in sequence, it is preheated to the set temperature by an electric heater and then enters the drying tower;

[0047] The ratio of the diameter to the height of the drying tower is 1:3.5, the inner wall material is polytetrafluoroethylene with a thickness of 2.5 mm, and the pressure sensor at the top monitors the pressure inside the tower in real time, with a control accuracy of ±0.01 kPa.

[0048] Post-treatment: Place the propolis powder obtained by spray drying in an environment with a relative humidity of 35% and a temperature of 22°C and let it stand and age for 36 hours; then, use an air jet mill for pulverization, the pulverization pressure is 0.7 MPa, and the pulverized propolis powder is sieved through a 90-mesh sieve to obtain the final propolis powder product; after testing, the glue content of this propolis powder is 57%, the caking rate is 3% after being placed for 180 days at 25°C and a relative humidity of 60%, the particle size distribution meets the requirements, and the emulsification index reaches 83%.

[0049] Example 2

[0050] Prepare raw materials: Weigh 9.6 kg of propolis blocks, dissolve them in 50 L of ethanol with a purity of 88%, stir until completely dissolved, then add 96 g of vitamin E microcapsules and 48 g of tea polyphenols and dissolve them to obtain a clear core material solution; use it as the core material. Weigh 2.7 kg of gelatin with a molecular weight of 10000 Da and 2.7 kg of β-cyclodextrin with a purity of 98%, dissolve them in 150 L of deionized water at a temperature of 60°C, continue to stir until completely dissolved, then add 16.2 g of nanoscale silica and 50 g of lecithin and mix them evenly to prepare the wall material.

[0051] Mixing and hydration: Add the core material into the wall material in a 60°C water bath at a rate of 25 L / h, and hydrate at 60°C for 2 hours with a stirring speed of 245 rpm. The distance between the stirring paddle and the bottom of the container is 1 / 5 of the container diameter.

[0052] Concentrate to about 15 degrees Baume: Under the conditions of -0.08 MPa and 50°C, concentrate with a rotary evaporator at a rotation speed of 80 rpm, the cooling medium temperature of the condenser is -5°C, concentrate to a Baume degree of 15, and control the vacuum degree fluctuation within the specified range.

[0053] Prefiltration: Filter with a stainless steel filter screen with a pore size of 5 μm under a pressure of 0.1 MPa.

[0054] Spray drying: Set the inlet temperature at 180°C, the outlet temperature at 80°C, the atomizer rotation speed at 20000 rpm, the feeding speed at 120 mL / min, and the hot air flow rate at 0.8 m 3 / min; The hot air filtration and preheating treatment are the same as in Example 1, and the drying tower parameters are also similar to those in Example 1.

[0055] Post-treatment: Age for 24 hours in an environment with a relative humidity of 30% and a temperature of 20°C, crush with a jet mill under a pressure of 0.6 MPa, and screen through an 80-mesh sieve; After testing, the glue content of this propolis powder is 60%, the caking rate is 4%, and the particle size and emulsification index both meet the requirements.

[0056] Example 3

[0057] Prepare raw materials: Take 9.6 kg of propolis blocks, stir with 50 L of 90% ethanol until completely dissolved, then add 150 g of vitamin E microcapsules and 75 g of tea polyphenols and dissolve them to obtain a clear core material solution; Weigh 2.7 kg of gelatin with a molecular weight of 15000 Da and 2.7 kg of β-cyclodextrin with a purity of 99.5%, dissolve them in 150 L of deionized water at a temperature of 60°C, continuously stir until completely dissolved, then add 45 g of nanoscale silica and 75 g of lecithin and mix evenly to prepare the wall material to obtain the wall material.

[0058] Mixing and hydration: Add the core material into the wall material at 60°C at a rate of 20 L / h, and hydrate at 60°C for 3 hours with stirring at 245 rpm. The position of the stirring paddle is the same as in Example 1.

[0059] Concentrate to about 15 degrees Baume: At -0.08 MPa and 60°C, the rotation speed of the rotary evaporator is 120 rpm, the cooling medium temperature of the condenser is 5°C, concentrate to a Baume degree of about 15, and control the vacuum degree fluctuation.

[0060] Prefiltration: Filter with a stainless steel filter screen with a pore size of 10 μm under a pressure of 0.2 MPa.

[0061] Spray drying: inlet temperature 200°C, outlet temperature 100°C, atomizer rotation speed 25000 rpm, feed rate 150 mL / min, hot air flow rate 1.2 m 3 / min. The parameters of hot air treatment and drying tower are kept consistent.

[0062] Post-treatment: Aging for 48 hours in an environment with a relative humidity of 40% and a temperature of 25°C, crushing at a pressure of 0.8 MPa, and passing through a 100-mesh sieve. After testing, the propolis powder has a glue content of 58%, a caking rate of 2%, a reasonable particle size distribution, and an emulsification index of 85%.

[0063] Comparative Example 1:

[0064] Prepare raw materials: Weigh 9.6 kg of propolis and dissolve it in 50 L of ethanol with a purity of 88% as the core material. Weigh 2.7 kg of gelatin with a molecular weight of 10000 Da and 2.7 kg of β-cyclodextrin with a purity of 98%, dissolve them in 150 L of deionized water at a temperature of 60°C to make the wall material.

[0065] Mixing and hydration: Add the core material to the wall material at 60°C at a rate of 25 L / h, and hydrate at 60°C for 2 hours under a stirring speed of 245 rpm. The distance between the stirring paddle and the bottom of the container is 1 / 5 of the container diameter.

[0066] Concentrate to about 15°Bé: Under the conditions of -0.08 MPa and 50°C, concentrate with a rotary evaporator at a rotation speed of 80 rpm, and the cooling medium temperature of the condenser is -5°C. Concentrate to 15°Bé, and control the vacuum degree fluctuation within the specified range.

[0067] Prefiltration: Filter with a stainless steel filter screen with a pore size of 5 μm under a pressure of 0.1 MPa.

[0068] Spray drying: Set the inlet temperature at 180°C, the outlet temperature at 80°C, the atomizer rotation speed at 20000 rpm, the feed rate at 120 mL / min, and the hot air flow rate at 0.8 m 3 / min.

[0069] Post-treatment: Aging for 24 hours in an environment with a relative humidity of 30% and a temperature of 20°C, crushing with a jet mill under a pressure of 0.6 MPa, and screening through an 80-mesh sieve; After testing, the propolis powder has a glue content of 56% and a caking rate of 60%. Neither the particle size nor the emulsification index meets the requirements.

[0070] Comparative Example 2

[0071] Prepare raw materials: Weigh 9.6 kg of propolis blocks, dissolve them in 50 L of ethanol with a purity of 88%, stir until completely dissolved, then add 96 g of vitamin E microcapsules and 48 g of tea polyphenols and dissolve them to obtain a clear core material solution, which is used as the core material. Weigh 2.7 kg of gelatin with a molecular weight of 10,000 Da and 2.7 kg of β-cyclodextrin with a purity of 98%, dissolve them in 150 L of deionized water at a temperature of 60 °C, continuously stir until completely dissolved, then add 16.2 g of nano-scale silica and 50 g of lecithin and mix them evenly to prepare the wall material.

[0072] Mixing and hydration: Add the core material to the wall material in a 60 °C water bath at a speed of 50 L / h, and hydrate at 60 °C for 2 hours under a stirring speed of 245 rpm. The distance between the stirring paddle and the bottom of the container is 1 / 5 of the container diameter.

[0073] Concentrate to about 15 degrees Baume: Under the conditions of -0.08 MPa and 50 °C, use a rotary evaporator to concentrate at a rotation speed of 80 rpm, with the cooling medium temperature of the condenser at -5 °C, concentrate to 15 degrees Baume, and control the vacuum degree fluctuation within the specified range.

[0074] Prefiltration: Filter with a stainless steel filter screen with a pore size of 5 μm under a pressure of 0.1 MPa.

[0075] Spray drying: Set the inlet temperature at 180 °C, the outlet temperature at 80 °C, the atomizer rotation speed at 20,000 rpm, the feeding speed at 120 mL / min, and the hot air flow rate at 0.8 m 3 / min. However, finally, it cannot form a powder, and most of it adheres to the tower, so the tower needs to be shoveled. The propolis powder obtained by shoveling the tower has a glue content of 55%, a caking rate of 100% in 180 days, and the emulsification index does not meet the standard.

[0076] It can be clearly seen from the above three examples and two comparative examples that the preparation process provided by the present invention can stably produce propolis powder products with high glue content, low caking rate, and good emulsification performance, which has significant advantages compared with the traditional method, fully verifying the feasibility and superiority of the technical solution of the present invention. Comparison table of process parameters for examples and comparative examples:

[0077]

[0078]

[0079] Conclusion: The examples are precise and strict in raw material selection and process parameter control. In contrast, the comparative examples do not add innovative components, and the ultra-fast speed during the feeding of the core material with the wall material leads to a very high caking rate, making it impossible to spray into powder form. This fully demonstrates that through the multiphase antioxidant synergy of vitamin E microcapsules and tea polyphenols, the physical barrier effect of nano-silica, and the synergistic adaptation of the lecithin-β-cyclodextrin dynamic membrane structure, and by precisely controlling the feeding speed, etc., the propolis powder produced is significantly superior to the traditional single-wall material formula in all aspects. The process parameter design of the present invention is more scientific, rigorous, and innovative.

[0080] Comparison table of product performance between examples and comparative examples:

[0081]

[0082] Conclusion: The propolis powder of the examples performs excellently in terms of glue content, caking rate, and emulsification index, and the particle size distribution meets the standard, while the performance of the comparative example products is poor. This shows that the preparation process of the present invention can significantly improve the product performance of propolis powder, and it is difficult for the traditional method of the comparative example to reach the product quality standard of the present invention, highlighting the technical advantages of the present invention. In particular, it reflects the innovative technologies of the present invention: the addition of innovative components and the control of the feeding speed.

[0083] Comparison table of equipment parameters of examples:

[0084]

[0085] Conclusion: Although there are certain differences in the equipment parameters among the examples, they are all within the scope required by the present invention, and the product performance is ensured to be stable. This shows that the limitation of the equipment parameters of the present invention is reasonable and effective, and stable high-quality propolis powder production can be achieved within this parameter range, ensuring the repeatability and reliability of the process.

[0086] Although the embodiments of the present invention have been shown and described, it will be understood by those of ordinary skill in the art that various changes, modifications, substitutions, and variations can be made to these embodiments without departing from the principles and spirit of the present invention. The scope of the present invention is defined by the appended claims and their equivalents.

Claims

1. A dry powdered propolis powder with high propolis content, characterized in that: The propolis powder is in the form of dry powder, has a gel content of 56%-60%, has a caking rate of less than 5% when placed in an environment of 25° C. and a relative humidity of 60% for 180 days, and comprises the following components: 0.5%-1% by weight of vitamin E microcapsules, 0.2%-0.5% by weight of natural antioxidant tea polyphenols, 0.1%-0.3% by weight of nano-silicon dioxide, and 0.3%-0.5% by weight of lecithin; Among them, vitamin E microcapsules can inhibit the oxidation of unsaturated fatty acids, aromatic acids, and flavonoids in propolis by slowly releasing vitamin E during storage. Tea polyphenols are water-soluble polyphenol compounds that quickly neutralize free radicals in aqueous environments, especially protecting unstable components on the surface of propolis powder microcapsules. At the same time, they can synergize with vitamin E microcapsules to form a "biphasic" antioxidant network, covering different polar environments inside and outside the propolis powder microcapsules, achieving a geometric increase in antioxidant efficiency. Nano-silica acts as a physical barrier to extend the diffusion path of free radicals. During spray drying, nano-silica acts as an excipient to reduce the adhesion of propolis powder microcapsule particles. As an amphiphilic molecule, lecithin self-assembles to form a stable bilayer structure, which encapsulates propolis hydrophobically. It can also cooperate with β-cyclodextrin to improve the encapsulation rate.

2. The high-gum content dry powdered propolis powder according to claim 1, characterized in that: The particle size distribution of the propolis powder is: D10 is 5-10 μm, D50 is 20-30 μm, D90 is 40-50 μm, and the emulsification index is greater than 80%. During the emulsification process, the surface active components in the propolis powder interact with the water molecules and oil molecules in the emulsification system to form a stable emulsion. The reaction formula can be expressed as: Surfactant + H2O + oil molecules → stabilize the emulsion structure.

3. A high temperature spray drying process for preparing dry powdered propolis powder with high propolis content as claimed in claim 1 or 2, characterized in that: The following steps are involved: S1, take 9.6kg of propolis block and dissolve it in 50L of ethanol with a mass fraction of 88%-95%, then add 0.5%-1% of vitamin E microcapsules and 0.2%-0.5% of natural antioxidant tea polyphenols by weight, stir evenly and use them as core material; mix gelatin and β-cyclodextrin in a mass ratio of 1:1, take 2.7kg of each and dissolve them in 150L of deionized water at a temperature of 60°C, then add 0.1%-0.3% of nano-silicon dioxide and 0.3%-0.5% of lecithin by weight and stir evenly as wall material, wherein the molecular weight of gelatin is 10000-15000Da, and the purity of β-cyclodextrin is not less than 98%. During the dissolution process, the active ingredients in propolis undergo molecular diffusion and dissolution equilibrium with ethanol; gelatin and β-cyclodextrin are dissolved in water to form a uniform solution system; S2, adding the core material to the wall material at 60°C at a flow acceleration of 15-25L / h, and hydrating for 2-3h under a stirring speed of 245rpm. During this process, the core material and the wall material undergo emulsification and embedding reactions to form a stable microcapsule structure; S3. At -0.08MPa and 40-60°C, the mixture is concentrated to a degree of alcohol-free or Baume of 15 by a rotary evaporator. During the concentration process, an automatic vacuum control system is used to make the vacuum fluctuation range within ±0.005MPa. The speed of the rotary evaporator is 80-120rpm, and the cooling medium temperature of the condenser is -5-5°C. S4. Pre-filter the concentrated material using a stainless steel filter with a pore size of 5-10μm and a filtration pressure of 0.1-0.2MPa. The filtration process is mainly based on the principle of physical screening to remove insoluble impurities in the concentrate. S5. Spray drying is performed under the conditions of an inlet temperature of 190±10°C, an outlet temperature of 90±10°C, and an atomizer speed of 20000-25000rpm to obtain the propolis powder. During the spray drying process, the hot air is first filtered through three stages, the first stage is a primary filter with a filtration efficiency of G4; the second stage is a medium-efficiency filter with a filtration efficiency of F8; the third stage is a high-efficiency filter with a filtration efficiency of H13, and the hot air is preheated by an electric heater before entering the drying tower, the preheating temperature control accuracy is ±2°C, the feed rate is 100-150mL / min, and the hot air flow rate is 0.8-1.2m 3 / min; S6. Post-processing the spray-dried propolis powder, including standing and aging for 24-48 hours in an environment with a relative humidity of 30%-40% and a temperature of 20-25°C, and then crushing it with an air flow mill at a crushing pressure of 0.6-0.8MPa. The crushed propolis powder is then sieved through an 80-100 mesh sieve. During the standing and aging process, the molecular structure inside the propolis powder is further adjusted and stabilized; the air flow crushing process uses high-speed airflow to impact and collide the propolis powder particles, so that the particle size is further refined; the screening process is based on the physical screening principle, and the particles that do not meet the particle size requirements are removed to ensure that the particle size distribution of the final product meets the requirements.

4. The high temperature spray drying preparation process according to claim 3, characterized in that: In the stirring step, the stirring paddle is an anchor-type stirring paddle, the distance between the stirring paddle and the bottom of the container is 1 / 5-1 / 4 of the diameter of the container, the stirring paddle is made of stainless steel 304, and the surface roughness Ra≤0.8μm.

5. The high temperature spray drying preparation process according to claim 3, characterized in that: The ratio of the drying tower diameter to the height of the spray drying equipment is 1:3-1:4, the inner wall of the drying tower is made of polytetrafluoroethylene with a thickness of 2-3 mm, and a pressure sensor is provided on the top of the drying tower to monitor the pressure in the tower in real time, and the pressure control accuracy is ±0.01 kPa.

Images