CN116786046A - A kind of instant microcapsule and its preparation method - Google Patents
A kind of instant microcapsule and its preparation method Download PDFInfo
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Abstract
本发明提供了一种速溶型微胶囊及其制备方法。该微胶囊的制备方法包括如下步骤:1)将乳液使用压力喷雾进行干燥,得到潮粉;2)步骤1)得到的潮粉落入内置流化床中,经过干燥热空气进行处理,得到二次干燥的产品;所述处理的时间为5‑10min;3)将步骤2)得到二次干燥的产品加入振动流化床中,在造粒段通过气流喷雾粘合剂再进行湿造粒;所述粘合剂的喷出量为产品中总原料的2‑3wt%;所述乳液中包括脂溶性芯材。本发明提供的制备方法可以得到松散葡萄型产品,具有极好的溶解性,同时细粉由于未经过反复干燥,感官良好。
The invention provides a quick-dissolving microcapsule and a preparation method thereof. The preparation method of the microcapsules includes the following steps: 1) dry the emulsion using pressure spray to obtain tide powder; 2) the tide powder obtained in step 1) falls into the built-in fluidized bed and is processed by dry hot air to obtain the second The second-dried product; the processing time is 5-10 minutes; 3) Add the second-dried product obtained in step 2) into the vibrating fluidized bed, spray the binder through airflow in the granulation section, and then perform wet granulation; The spray amount of the adhesive is 2-3wt% of the total raw materials in the product; the emulsion includes a fat-soluble core material. The preparation method provided by the invention can obtain a loose grape-type product with excellent solubility. At the same time, the fine powder has good sensory properties because it has not been repeatedly dried.
Description
技术领域Technical field
本发明涉及微胶囊的技术领域,更具体地,涉及一种速溶型微胶囊及其制备方法。The present invention relates to the technical field of microcapsules, and more specifically, to a quick-dissolving microcapsule and a preparation method thereof.
背景技术Background technique
多不饱和脂肪酸油脂,例如花生四烯酸油脂,二十二碳六烯酸油脂等在生物系统中具有广泛的生物学功能,能够调节机体的脂类代谢和免疫,具有抗癌、预防和治疗心血管疾病、促进机体生长发育以及调控基因的表达等功能,多不饱和脂肪酸具备的诸多功能性特点已被消费者广泛理解。花生四烯酸油脂、二十二碳六烯酸油脂等由于自身结构易被氧化并产生令人不愉悦的气味,同时影响油脂的功能,通常采用微胶囊技术利用包裹材料对花生四烯酸油脂、二十二碳六烯酸油脂等多不饱和脂肪酸油脂进行保护,提高其稳定性和风味。Polyunsaturated fatty acid oils, such as arachidonic acid oil, docosahexaenoic acid oil, etc., have a wide range of biological functions in biological systems, can regulate the body's lipid metabolism and immunity, and have anti-cancer, prevention and treatment properties. The many functional characteristics of polyunsaturated fatty acids have been widely understood by consumers such as cardiovascular diseases, promoting body growth and development, and regulating gene expression. Arachidonic acid oil, docosahexaenoic acid oil, etc. are easily oxidized due to their own structure and produce unpleasant odors, and at the same time affect the function of the oil. Microcapsule technology is usually used to use packaging materials to treat arachidonic acid oil. , docosahexaenoic acid oil and other polyunsaturated fatty acid oils to protect it and improve its stability and flavor.
目前的多不饱和脂肪酸微胶囊产品在奶粉等冲调产品中能够表现出与整体物料一致的冲调性,但是随着终端产品的多样化需求和应用解决方案的拓展,当前的微胶囊产品较为难以满足在直饮粉、速溶粉等对溶解速度要求较高的产品中的应用。现有的解决微囊粉速溶性的方案基本都是围绕组分展开的,包括加入亲水性胶体、各种寡糖的复配、乳化剂的替换,等等,但鲜少有从制备工艺角度展开研究的方案。The current polyunsaturated fatty acid microcapsule products can show the same reconstitution properties as the overall materials in reconstituted products such as milk powder. However, with the diversified needs of end products and the expansion of application solutions, the current microcapsule products are relatively It is difficult to meet the application in products that require high dissolution speed, such as direct-drink powder and instant powder. Existing solutions to solve the problem of instant solubility of microencapsulated powders basically revolve around components, including adding hydrophilic colloids, compounding various oligosaccharides, replacing emulsifiers, etc., but few start from the preparation process. perspective research plan.
微胶囊制备过程主要包括物料剪切、混合、均质、喷雾干燥等工序。其中干燥工段是得到各种不同形态产品的核心工序之一,其关键控制点最多,对芯材影响较高,调控难度最高。The microcapsule preparation process mainly includes material shearing, mixing, homogenization, spray drying and other processes. Among them, the drying section is one of the core processes for obtaining products of various shapes. It has the most critical control points, has a high impact on the core material, and is the most difficult to control.
现有技术中喷雾干燥工段中的喷雾方式根据雾化机理的不同有压力喷雾、离心喷雾、气流喷雾等,其区别主要在于料液喷出的动力方式不同,同时雾化机理的不同导致喷雾塔中的进风出风方式也有较大区别。其中气流喷雾能耗较大、压力喷雾相较于离心喷雾干燥具有热效高,维护成本低,产品质量好的优点,其设备进出风方式为上进风上出风。喷雾干燥中干燥的主要工艺有:申请人首创的CN201010199030.1二次包埋工艺,液滴喷入到沸腾干燥装置中,被装置内鼓起的粉末所包裹;CN201310217380.X、CN201711419628.5等文献中的喷雾干燥工艺,要点在于旋风分离器收集的细粉从塔顶回塔附聚,细粉经过了二次加热;冷冻喷雾干燥是将乳化液雾化成液滴喷入装有冷冻液的冷冻仓中,冷冻液的温度低于乳化液的共晶点;将冷冻得到的物料进行真空冷冻干燥即得到多不饱和脂肪酸油脂微胶囊。另外现有技术中对于喷雾干燥方法的优化主要集中在进料的浓度、喷头的压力、进风出风的温度等,很少有提出新的喷雾干燥工艺。In the existing technology, the spray methods in the spray drying section include pressure spray, centrifugal spray, air flow spray, etc. depending on the atomization mechanism. The difference mainly lies in the different power modes of the material liquid spraying. At the same time, the different atomization mechanisms cause the spray tower to The air inlet and outlet methods are also quite different. Among them, airflow spray consumes a lot of energy, and pressure spray has the advantages of high thermal efficiency, low maintenance cost and good product quality compared to centrifugal spray drying. The air inlet and outlet mode of the equipment is upper air inlet and upper air outlet. The main drying processes in spray drying include: the CN201010199030.1 secondary embedding process pioneered by the applicant, in which droplets are sprayed into the boiling drying device and wrapped by the powder bulging in the device; CN201310217380.X, CN201711419628.5, etc. The key point of the spray drying process in the literature is that the fine powder collected by the cyclone separator returns to the tower from the top of the tower to agglomerate, and the fine powder has been heated twice; freeze spray drying is to atomize the emulsion into droplets and spray it into a tank filled with freezing liquid. In the freezing chamber, the temperature of the frozen liquid is lower than the eutectic point of the emulsion; the frozen material is vacuum freeze-dried to obtain polyunsaturated fatty acid oil microcapsules. In addition, the optimization of spray drying methods in the existing technology mainly focuses on the concentration of the feed material, the pressure of the nozzle, the temperature of the inlet and outlet air, etc., and few new spray drying processes have been proposed.
发明内容Contents of the invention
本发明的第一目的在于提供一种微胶囊的制备方法,使用该制备方法得到的微胶囊有更好的速溶效果和良好的感官性能。The first object of the present invention is to provide a method for preparing microcapsules. The microcapsules obtained by using the preparation method have better instant dissolving effect and good sensory properties.
本发明提供的微胶囊的制备方法,包括如下步骤:The preparation method of microcapsules provided by the invention includes the following steps:
1)将乳液使用压力喷雾进行干燥,得到潮粉;1) Use pressure spray to dry the emulsion to obtain moist powder;
2)步骤1)得到的潮粉落入内置流化床中,经过干燥热空气进行处理,得到二次干燥的产品;所述处理的时间为5-10min;2) The tide powder obtained in step 1) falls into the built-in fluidized bed and is processed by dry hot air to obtain a secondary dried product; the processing time is 5-10 minutes;
3)将步骤2)得到二次干燥的产品加入振动流化床中,在造粒段通过气流喷雾粘合剂再进行湿造粒;所述粘合剂的喷出量为产品中总原料的2-3wt%;3) Add the twice-dried product obtained in step 2) into the vibrating fluidized bed, spray the adhesive through airflow in the granulation section and then perform wet granulation; the spray amount of the adhesive is 1% of the total raw materials in the product. 2-3wt%;
所述乳液中包括脂溶性芯材。The emulsion includes a fat-soluble core material.
在现有技术中,常规的工艺会采用喷雾-塔内附聚工艺,其中一种工艺过程为气流喷雾下,细粉进入内置流化床内在60-70℃的环境下进行黏附1-5小时,使用该工艺制备含有脂溶性芯材的微胶囊,对脂溶性芯材特别是多不饱和脂肪酸是不友好的,影响感观;另一种工艺过程采用压力喷雾,细粉在塔顶回塔附聚,附聚时间虽然相对缩短,但细粉经过二次加热,且该工艺得到的微胶囊难以达到直饮粉或其他特殊领域的速溶要求。In the existing technology, the conventional process uses a spray-tower agglomeration process. One process is that under air spray, the fine powder enters the built-in fluidized bed and adheres in an environment of 60-70°C for 1-5 hours. , using this process to prepare microcapsules containing fat-soluble core materials, is unfriendly to fat-soluble core materials, especially polyunsaturated fatty acids, and affects the senses; another process uses pressure spray, and the fine powder is returned to the tower at the top Agglomeration, although the agglomeration time is relatively shortened, the fine powder undergoes secondary heating, and the microcapsules obtained by this process are difficult to meet the instant requirements of direct drinking powder or other special fields.
在本发明一个优选实施方式中,脂溶性芯材包括易氧化的物质,优选包括多不饱和脂肪酸油脂,例如DHA油脂、ARA油脂等。在本发明的具体实施方式中,本领域技术人员可以根据需要向乳液中加入常见的添加剂,包括但不限于,乳化剂、填充剂、抗氧化剂、拮抗剂、pH调节剂等等,乳化剂可以为变性淀粉、酪蛋白酸钠、乳清蛋白、阿拉伯胶、单双甘油酯中的一种或多种,填充剂可以为麦芽糊精、玉米糖浆、葡萄糖、乳糖中的一种或多种,抗氧化剂可以为抗坏血酸及其盐或衍生物、维生素E、磷脂等,拮抗剂可以为磷酸三钙、磷酸氢钙。本领域技术人员可以根据具体微胶囊的需求来选择加入的添加剂的种类和重量份。In a preferred embodiment of the present invention, the fat-soluble core material includes easily oxidized substances, preferably polyunsaturated fatty acid oils, such as DHA oils, ARA oils, etc. In specific embodiments of the present invention, those skilled in the art can add common additives to the emulsion as needed, including but not limited to, emulsifiers, fillers, antioxidants, antagonists, pH adjusters, etc., and the emulsifiers can It is one or more of modified starch, sodium caseinate, whey protein, arabic gum, monoglycerides and diglycerides, and the filler can be one or more of maltodextrin, corn syrup, glucose, and lactose. Antioxidants can be ascorbic acid and its salts or derivatives, vitamin E, phospholipids, etc., and antagonists can be tricalcium phosphate and hydrogen calcium phosphate. Those skilled in the art can select the type and weight of additives to be added according to the needs of specific microcapsules.
本发明中的乳液可以使用本领域中常用的制备方法制得,本发明的具体实施方式中,乳液的制备方法包括将油相加入水相,剪切均质,即得。其中水相的制备方法包括将粉剂(或是除了油相以外的微胶囊原料成分)与水混合,充分溶解,得到水相。粉剂即包括上述的添加剂。油相为易氧化的物质,例如多不饱和脂肪酸油脂。The emulsion in the present invention can be prepared using preparation methods commonly used in this field. In the specific embodiment of the present invention, the preparation method of the emulsion includes adding the oil phase to the water phase and shearing to homogenize. The preparation method of the water phase includes mixing the powder (or microcapsule raw material components except the oil phase) with water and fully dissolving to obtain the water phase. Powders include the above-mentioned additives. The oil phase is a substance that is easily oxidized, such as polyunsaturated fatty acid oils.
和现有技术相比,本发明提供的微胶囊的制备方法,使用压力喷雾干燥,在内置流化床中仅处理5-10min后,在振动流化床(也称外置流化床)通过气流喷雾特定浓度的粘合剂,喷洒在物料上再湿造粒,使用这样的制备方法可以得到松散的附聚产品,得到的产品具有更好的速溶效果。并且,虽然附聚时间不长,但由于整个工艺中脂溶性芯材经历的高温时间短,依然能够保证微胶囊产品的质量,具备良好的感官特性。Compared with the existing technology, the preparation method of microcapsules provided by the present invention uses pressure spray drying. After only processing for 5-10 minutes in a built-in fluidized bed, it is passed through a vibrating fluidized bed (also called an external fluidized bed). The adhesive with a specific concentration is sprayed by airflow, sprayed on the material and then wet and granulated. Using this preparation method, a loose agglomerated product can be obtained, and the obtained product has a better instant-dissolving effect. Moreover, although the agglomeration time is not long, due to the short high-temperature time experienced by the fat-soluble core material in the entire process, the quality of the microcapsule product can still be ensured and it has good sensory properties.
在本发明一个优选实施方式中,步骤1)中的压力喷雾可以为多级压力喷雾。在本发明具体实施方式中,压力喷雾是在压力喷雾干燥塔中进行。即将乳液泵至压力喷雾干燥塔(压力喷雾干燥塔)中,从压力喷雾塔上端通入干燥热空气,进行喷雾干燥,得到潮粉,干燥热空气从压力喷雾干燥塔上端排出。在本发明的具体实施方式中,喷雾压力可以为100-200bar。In a preferred embodiment of the present invention, the pressure spray in step 1) can be a multi-stage pressure spray. In a specific embodiment of the present invention, pressure spraying is performed in a pressure spray drying tower. That is, the emulsion is pumped into a pressure spray drying tower (pressure spray drying tower), dry hot air is introduced from the upper end of the pressure spray tower, and spray drying is performed to obtain moist powder. The dry hot air is discharged from the upper end of the pressure spray drying tower. In specific embodiments of the invention, the spray pressure may be 100-200 bar.
在现有技术如CN201310217380.X、CN201711419628.5中所给出的工艺流程中,虽然同样采用了压力喷雾,但是采用了“塔内附聚,即细粉从塔顶回塔附聚的工艺特点”,细粉经过二次加热,且产品溶解冲无法直接实现直饮粉或其他特殊领域的速溶要求。在本发明的具体实施方式中,步骤2)中的内置流化床是设置在压力喷雾干燥塔中,内置流化床通常是设在压力喷雾干燥塔的下部,使步骤1)得到的潮粉落入内置流化床中。当步骤1)得到的潮粉落入内置流化床中后,往内置流化床中通入干燥热空气对潮粉进行进一步处理,处理的时间为5-10min,得到二次干燥产品。处理完后,此处的热空气从压力喷雾干燥塔的上端排出。在本发明一个优选实施方式中,压力喷雾干燥塔中上进风温度140-200℃,上出风温度60-100℃。内置流化床中的进风温度可以为60-70℃。In the process flow given in the existing technologies such as CN201310217380. "The fine powder has been heated twice, and the product dissolution cannot directly meet the instant requirements of drinking powder or other special fields. In a specific embodiment of the present invention, the built-in fluidized bed in step 2) is arranged in a pressure spray drying tower. The built-in fluidized bed is usually located at the lower part of the pressure spray drying tower, so that the moist powder obtained in step 1) Fall into the built-in fluidized bed. When the wet powder obtained in step 1) falls into the built-in fluidized bed, dry hot air is passed into the built-in fluidized bed to further process the wet powder. The processing time is 5-10 minutes to obtain a secondary dry product. After treatment, the hot air here is discharged from the upper end of the pressure spray drying tower. In a preferred embodiment of the present invention, the upper air inlet temperature in the pressure spray drying tower is 140-200°C, and the upper air outlet temperature is 60-100°C. The inlet air temperature in the built-in fluidized bed can be 60-70°C.
在本发明中,在振动流化床进行气流喷雾的粘合剂的喷出量是核心之一,过高会有塌床现象,过低会导致粘合度不够,产品无法附聚,影响速溶性。在本发明一个优选实施方式中,粘合剂可以为水、磷脂溶液、包含乳化剂的水溶液、所述步骤1)中乳液中的一种或多种,其中溶液按照需求可选择为乳液或者油溶液,在一些具体的应用中可选择磷脂油溶液或者微胶囊制备时得到的变性淀粉配方乳液、蛋白配方乳液,也可以是直接含有变性淀粉或者蛋白的水溶液,溶液中粘合剂的含量可根据需要和工艺需求进行调整,在此不做过多限定。In the present invention, the ejection amount of the adhesive that is air-sprayed in the vibrating fluidized bed is one of the core. If it is too high, the bed will collapse. If it is too low, the adhesion will be insufficient and the product will not agglomerate, affecting the instant dissolution. sex. In a preferred embodiment of the present invention, the binder can be one or more of water, a phospholipid solution, an aqueous solution containing an emulsifier, and the emulsion in step 1), wherein the solution can be selected as an emulsion or oil as required. Solution, in some specific applications, you can choose phospholipid oil solution or modified starch formula emulsion or protein formula emulsion obtained during the preparation of microcapsules, or it can also be an aqueous solution directly containing modified starch or protein. The content of the binder in the solution can be determined according to It needs to be adjusted according to the process requirements and will not be too limited here.
在本发明的具体实施方式中,可以将振动流化床设置在压力喷雾干燥塔的下方,以使步骤2)得到的二次干燥的产品落入振动流化床中。在本发明一个优选实施方式中,可以在振动流化床的造粒段设有气流喷雾装置,该气流喷雾装置用于通过气流喷雾粘合剂在所述振动流化床上对所述二次干燥的产品进行湿造粒。其中,振动流化床造粒段的进风温度可以为60-70℃,需要强调的是,该工段虽然进风温度为60-70℃,但该工段是在喷雾溶液的条件下进行沾湿黏附,与常规的干燥附聚相比,芯材受到的热损伤更小。在本发明具体的实施方式中,还包括将湿造粒得到的产品进行干燥和/或冷却,得到成品。在本发明具体实施方式中,振动流化床上可以是兼具振动和鼓风功能,通过控制风的温度实现干燥和冷却。其中干燥段的时间可以为5-15min。其中,干燥段进风温度可以为45-55℃,冷却段进风温度可以为15-25℃。在本发明具体实施方式中,振动流化床可以依次包括造粒段、干燥段和冷却段,三个工段再流化床中是连续的,同时进行的。在振动流化床段,干燥热空气和冷却空气从振动流化床的上端排出。In a specific embodiment of the present invention, the vibrating fluidized bed can be arranged below the pressure spray drying tower, so that the secondary dried product obtained in step 2) falls into the vibrating fluidized bed. In a preferred embodiment of the present invention, an airflow spray device can be provided in the granulation section of the vibrating fluidized bed. The airflow spraying device is used to spray the adhesive on the vibrating fluidized bed through airflow to spray the secondary adhesive on the vibrating fluidized bed. The dried product is wet granulated. Among them, the inlet air temperature of the vibrating fluidized bed granulation section can be 60-70°C. It should be emphasized that although the inlet air temperature of this section is 60-70°C, this section is wetted under the condition of spray solution Adhesion, the core material suffers less thermal damage than conventional dry agglomeration. In a specific embodiment of the present invention, it also includes drying and/or cooling the product obtained by wet granulation to obtain a finished product. In the specific embodiment of the present invention, the vibrating fluidized bed can have both vibration and blowing functions, and drying and cooling can be achieved by controlling the temperature of the wind. The drying section time can be 5-15 minutes. Among them, the inlet air temperature of the drying section can be 45-55°C, and the inlet air temperature of the cooling section can be 15-25°C. In the specific embodiment of the present invention, the vibrating fluidized bed may include a granulation section, a drying section and a cooling section in sequence, and the three sections are continuous and performed simultaneously in the fluidized bed. In the vibrating fluidized bed section, dry hot air and cooling air are discharged from the upper end of the vibrating fluidized bed.
在本发明一个优选实施方式中,还可以将步骤1)、步骤2)和步骤3)中排出的空气分离除尘,得到细粉,将所述细粉与步骤2)得到的二次干燥的产品同时加入振动流化床中,进行步骤3)。该步骤和步骤3)连续且同时进行。对细粉进行再利用,使其参与后续造粒粘合。In a preferred embodiment of the present invention, the air discharged in step 1), step 2) and step 3) can also be separated and dusted to obtain fine powder, and the fine powder is combined with the secondary dried product obtained in step 2) At the same time, add it to the vibrating fluidized bed and proceed to step 3). This step and step 3) are performed continuously and simultaneously. The fine powder is reused to participate in subsequent granulation and bonding.
使用上述制备方法得到的微胶囊是结构松散微胶囊,具有很好的速溶效果,同时油脂依然得到了良好包埋保护。即本发明的另一目的在于提供了上述制备方法得到的微胶囊。The microcapsules obtained using the above preparation method are microcapsules with a loose structure and have good instant dissolving effect, while the oil is still well embedded and protected. That is, another object of the present invention is to provide microcapsules obtained by the above preparation method.
本发明的再一目的在于提供了上述制备方法使用的微胶囊的制备系统,该制备系统包括:压力喷雾干燥塔、振动流化床、气流喷雾装置和旋风分离器;Another object of the present invention is to provide a preparation system for microcapsules used in the above preparation method. The preparation system includes: a pressure spray drying tower, a vibrating fluidized bed, an airflow spray device and a cyclone separator;
所述压力喷雾干燥塔中还设有内置流化床,对乳液使用压力喷雾干燥得到的潮粉落入所述内置流化床中经过干燥热空气处理5-10min后得到二次干燥的产品;The pressure spray drying tower is also equipped with a built-in fluidized bed. The moist powder obtained by pressure spray drying of the emulsion falls into the built-in fluidized bed and is treated with dry hot air for 5-10 minutes to obtain a secondary dried product;
所述气流喷雾装置,用于通过气流喷雾粘合剂在所述振动流化床上对所述二次干燥的产品进行湿造粒;The airflow spray device is used for wet granulating the secondary dried product on the vibrating fluidized bed by airflow spraying the binder;
所述旋风分离器用于分离所述压力喷雾干燥塔和振动流化床中排出的空气中的细粉;所述旋风分离器与所述振动流化床通过管道连接,以使所述细粉输送至所述振动流化床。The cyclone separator is used to separate fine powder in the air discharged from the pressure spray drying tower and the vibrating fluidized bed; the cyclone separator is connected to the vibrating fluidized bed through a pipeline to transport the fine powder to the vibrating fluidized bed.
在本发明一个优选实施方式中,还包括空气过滤系统,用于为所述压力喷雾干燥塔和振动流化床分别提供干燥的空气。空气过滤系统包括泵和过滤装置,用于提供干燥的热空气或冷空气。In a preferred embodiment of the present invention, an air filtration system is further included for providing dry air to the pressure spray drying tower and the vibrating fluidized bed respectively. Air filtration systems include pumps and filtration devices that provide dry hot or cold air.
在本发明的具体实施方式中,振动流化床可以设置在压力喷雾干燥塔的下方,以使二次干燥的产品落入振动流化床中。振动流化床可以包括造粒段、干燥段和冷却段。压力喷雾干燥塔的产品出口处可以正对振动流化床的造粒段。气流喷雾装置优选设置在振动流化床的造粒段,可以将气流喷雾装置与振动流化床活动连接,例如可以将气流喷雾装置插在振动流化床上。In a specific embodiment of the present invention, the vibrating fluidized bed may be disposed below the pressure spray drying tower, so that the secondary dried product falls into the vibrating fluidized bed. The vibrating fluidized bed may include a granulation section, a drying section and a cooling section. The product outlet of the pressure spray drying tower can be directly facing the granulation section of the vibrating fluidized bed. The airflow spray device is preferably arranged in the granulation section of the vibrating fluidized bed. The airflow spraying device can be movably connected to the vibrating fluidized bed. For example, the airflow spraying device can be inserted into the vibrating fluidized bed.
在本发明的具体实施方式中,旋风分离器可以根据实际需要设置多级旋风分离器。旋风分离器用于分离所述压力喷雾干燥塔和振动流化床中排出的空气中的细粉,尾气经水膜除尘后排出。In the specific embodiment of the present invention, the cyclone separator can be provided with multi-stage cyclone separators according to actual needs. The cyclone separator is used to separate the fine powder in the air discharged from the pressure spray drying tower and the vibrating fluidized bed, and the tail gas is discharged after being dedusted by a water film.
在本发明的具体实施方式中,还可以包括集料装置,集料装置用于收集振动流化床得到的最终产品,可以设在振动流化床的产品出口处,例如可以设在振动流化床的冷却段的产品出口处。In the specific embodiment of the present invention, a collecting device may also be included. The collecting device is used to collect the final product obtained from the vibrating fluidized bed. The collecting device may be located at the product outlet of the vibrating fluidized bed. For example, it may be located at the vibrating fluidized bed. Product outlet of the cooling section of the bed.
在本发明一个优选实施方式中,如图1所示,该微胶囊的制备系统包括压力喷雾干燥塔1、振动流化床3、气流喷雾装置7、旋风分离器4、空气过滤系统6和集料装置5。在压力喷雾干燥塔1中设有内置流化床2,内置流化床2设在压力喷雾干燥塔1的下方,该内置流化床2用于通过干燥热空气处理潮粉,从而得到二次干燥的产品。干燥热空气从压力喷雾干燥塔1的上端通入,处理结束后干燥热空气也从压力喷雾干燥塔1的上端排出(包括经过内置流化床2的干燥热空气也是从压力喷雾干燥1的上端排出)。振动流化床3设在压力干燥塔1的下方,以使二次干燥的产品落入振动流化床3中。同时,干燥热空气和冷却空气也是从振动流化床3的上端排出。气流喷雾装置7插在振动流化床3的造粒段,用于通过气流喷雾粘合剂在振动流化床3上对二次干燥的产品进行湿造粒。旋风分离器4用于分离压力喷雾干燥塔1和振动流化床3中排出的空气中的细粉,旋风分离器4与振动流化床3通过管道连接,以使细粉输送至振动流化床3上。旋风分离器4包括两级旋风分离器。空气过滤系统6用于为压力喷雾干燥塔1和振动流化床3分别提供干燥的空气。集料装置5设在振动流化床(冷却段)的下方,用于收集从振动流化床3得到的微胶囊成品。In a preferred embodiment of the present invention, as shown in Figure 1, the microcapsule preparation system includes a pressure spray drying tower 1, a vibrating fluidized bed 3, an air spray device 7, a cyclone separator 4, an air filtration system 6 and a collector. Material device 5. There is a built-in fluidized bed 2 in the pressure spray drying tower 1. The built-in fluidized bed 2 is located below the pressure spray drying tower 1. The built-in fluidized bed 2 is used to process the wet powder by drying hot air to obtain secondary Dry product. The hot dry air is introduced from the upper end of the pressure spray drying tower 1. After the treatment, the hot dry air is also discharged from the upper end of the pressure spray drying tower 1 (including the dry hot air that passes through the built-in fluidized bed 2 is also discharged from the upper end of the pressure spray drying tower 1 discharge). The vibrating fluidized bed 3 is arranged below the pressure drying tower 1 so that the secondary dried product falls into the vibrating fluidized bed 3 . At the same time, the dry hot air and cooling air are also discharged from the upper end of the vibrating fluidized bed 3. The airflow spray device 7 is inserted into the granulation section of the vibrating fluidized bed 3 and is used to wet-granulate the secondary dried product on the vibrating fluidized bed 3 by spraying the binder with airflow. The cyclone separator 4 is used to separate the fine powder in the air discharged from the pressure spray drying tower 1 and the vibrating fluidized bed 3. The cyclone separator 4 is connected to the vibrating fluidized bed 3 through a pipeline to transport the fine powder to the vibrating fluidized bed. On bed 3. Cyclone 4 includes a two-stage cyclone. The air filtration system 6 is used to provide dry air to the pressure spray drying tower 1 and the vibrating fluidized bed 3 respectively. The collecting device 5 is provided below the vibrating fluidized bed (cooling section) and is used to collect the finished microcapsules obtained from the vibrating fluidized bed 3 .
在本发明一个优选实施方式中,如图1所示,使用该微胶囊的制备系统制备微胶囊的制备方法包括如下步骤:In a preferred embodiment of the present invention, as shown in Figure 1, the preparation method of microcapsules using the microcapsule preparation system includes the following steps:
步骤1:将乳液高压泵至压力喷雾干燥塔1中,从压力喷雾塔上端通入干燥热空气,进行喷雾干燥,得到干燥的潮粉,并从压力喷雾干燥塔上端排出干燥热空气;Step 1: Pump the emulsion into the pressure spray drying tower 1 at high pressure, introduce dry hot air from the upper end of the pressure spray drying tower, perform spray drying to obtain dry moist powder, and discharge the dry hot air from the upper end of the pressure spray drying tower;
步骤2:步骤1获得的干燥的潮粉落入内置流化床2中,往内置流化床中通入干燥热空气进一步干燥、附聚,得到二段干燥产品,该过程时间为5-10min,并从压力喷雾干燥塔1上端排出干燥热空气;Step 2: The dry tidal powder obtained in step 1 falls into the built-in fluidized bed 2, and dry hot air is passed into the built-in fluidized bed to further dry and agglomerate to obtain a second-stage dry product. This process takes 5-10 minutes. , and discharge hot dry air from the upper end of the pressure spray drying tower 1;
步骤3:步骤2获得的二段干燥产品落入振动流化床3中,在造粒段通过气流喷雾装置7气流喷雾粘合剂再湿造粒,经干燥段干燥和冷却段冷却后得到成品,并从振动流化床3上端排出干燥热空气和冷却空气,其中干燥段时间为5-15min;Step 3: The second-stage dry product obtained in step 2 falls into the vibrating fluidized bed 3. In the granulation section, the adhesive is air-sprayed through the air-flow spray device 7 and then wet-granulated. After drying in the drying section and cooling in the cooling section, the finished product is obtained. , and discharge hot dry air and cooling air from the upper end of the vibrating fluidized bed 3, where the drying period is 5-15 minutes;
步骤4:将步骤1、步骤2和步骤3中排出的空气通入旋风分离器4中(在图1中设有两级分离器,一级旋风分离器和二级旋风分离器)分离除尘,获得细粉,尾气经水膜除尘后排出;Step 4: Pass the air discharged in steps 1, 2 and 3 into the cyclone separator 4 (there is a two-stage separator in Figure 1, a primary cyclone separator and a secondary cyclone separator) for separation and dust removal. Fine powder is obtained, and the tail gas is discharged after dust removal by water film;
步骤5:将步骤4中收集的细粉由管道输送到振动流化床3,与二段干燥产品混合均匀,进行步骤3(即再湿造粒,进一步干燥冷却后得到成品)。Step 5: Transport the fine powder collected in Step 4 to the vibrating fluidized bed 3 through a pipeline, mix it evenly with the second-stage drying product, and proceed to Step 3 (i.e., rewetting and granulating, and further drying and cooling to obtain the finished product).
其中步骤3/4/5是连续、同时的过程。Steps 3/4/5 are continuous and simultaneous processes.
本发明提供的微胶囊制备方法制备得到的产品可以避免脂溶性芯材遭受二次高温的干燥,影响产品质量,特别是感官、稳定性等。本发明提供的微胶囊制备方法可以得到松散的附聚葡萄型产品,具有更好的速溶效果,产品具备良好的感官性能。The products prepared by the microcapsule preparation method provided by the present invention can avoid the fat-soluble core material from being dried at a secondary high temperature, which affects product quality, especially sensory, stability, etc. The microcapsule preparation method provided by the invention can obtain a loose agglomerated grape-type product, which has better instant dissolving effect and the product has good sensory properties.
附图说明Description of the drawings
图1为实施例和具体实施方式中提供的微胶囊的制备系统;其中,1-压力喷雾干燥塔,2-内置流化床,3-振动流化床,4-旋风分离器,5-集料装置,6-空气过滤系统(包括泵、过滤装置),7-气流喷雾装置。Figure 1 shows the microcapsule preparation system provided in the examples and specific implementations; wherein, 1-pressure spray drying tower, 2-built-in fluidized bed, 3-vibrating fluidized bed, 4-cyclone separator, 5-collector Material device, 6-air filtration system (including pump, filter device), 7-air spray device.
具体实施方式Detailed ways
下面结合实施例,对本发明的具体实施方式作进一步详细描述。以下实施例,用于说明本发明,但不止用来限制本发明的范围。Specific implementations of the present invention will be described in further detail below with reference to examples. The following examples are used to illustrate the present invention, but are not used to limit the scope of the present invention.
除了特别说明,本发明中“%”为质量百分比。Unless otherwise specified, "%" in the present invention refers to mass percentage.
其中溶解性实验为:将样品按照6.5%的比例加入到45℃的温水中并开始计时,测量粉体从接触液面到全部沉入液面以下所需要的时间,这就是扩散速度。然后用玻棒以3转/秒的速度搅拌15秒后静置,观察溶液的表面和内部的情况并进行评分。“0”分代表没有明显的不溶物质被观察到;“1”分代表有少量不溶物质可以被观察到;“2”分代表有中等不溶物质可以被观察到;“3”分代表有较多不溶物质可以被观察到;“4”分代表有大量不溶物质可以被观察到。The solubility test is as follows: add the sample into warm water at 45°C at a ratio of 6.5% and start timing. Measure the time it takes for the powder to completely sink below the liquid surface from contact with the liquid surface. This is the diffusion rate. Then use a glass rod to stir at a speed of 3 rpm for 15 seconds and then let it stand. Observe the surface and internal conditions of the solution and make a score. A score of "0" means that no obvious insoluble matter is observed; a score of "1" means that a small amount of insoluble matter can be observed; a score of "2" means that a moderate amount of insoluble matter can be observed; a score of "3" means that a lot of insoluble matter can be observed Insoluble material can be observed; a score of "4" indicates that a large amount of insoluble material can be observed.
口中速溶实验为:取1g样品记录从样品放入口中到口腔中完全无颗粒感的时间。The oral instant dissolution test is as follows: take 1g sample and record the time from when the sample is placed in the mouth to when there is no grainy feeling in the mouth.
实施例1Example 1
本实施例提供一种松散型多不饱和脂肪酸微胶囊,制备系统如图1所示的制备系统,制备方法包括如下步骤:This embodiment provides a loose polyunsaturated fatty acid microcapsule. The preparation system is as shown in Figure 1. The preparation method includes the following steps:
微胶囊原料的组分为:酪蛋白酸钠6%,DHA油脂26%,抗坏血酸钠4%,单双甘酯1%,固体玉米糖浆63%。The components of the microcapsule raw materials are: 6% sodium caseinate, 26% DHA oil, 4% sodium ascorbate, 1% monoglycerides and 63% solid corn syrup.
(1)将酪蛋白酸钠、单双甘酯、固体玉米糖浆、抗坏血酸钠依次投入70℃热纯水中,充分剪切溶解,获得水相;(1) Put sodium caseinate, monoglycerides, solid corn syrup, and sodium ascorbate into 70°C hot pure water in sequence, and fully shear and dissolve to obtain the water phase;
(2)将DHA油脂添加到上述水相中,在10000r/min的条件下剪切10min;(2) Add DHA oil to the above water phase and shear it for 10 minutes at 10000r/min;
(3)以上乳液经高压均质机800bar均质2遍,得到固形物含量为50%的乳液。(3) The above emulsion is homogenized twice by a high-pressure homogenizer at 800 bar to obtain an emulsion with a solid content of 50%.
(4)将乳液高压泵至压力喷雾干燥塔1中,从压力喷雾塔1上端通入干燥热空气,进行喷雾干燥,喷雾压力为200bar,得到干燥的潮粉,并从压力喷雾干燥塔上端排出干燥热空气;其中塔内上进风温度180±2℃,上出风温度80±2℃。(4) High-pressure pump the emulsion into the pressure spray drying tower 1, introduce dry hot air from the upper end of the pressure spray drying tower 1, and perform spray drying. The spray pressure is 200bar to obtain dry moist powder, which is discharged from the upper end of the pressure spray drying tower. Dry hot air; the upper air inlet temperature in the tower is 180±2℃, and the upper air outlet temperature is 80±2℃.
(5)步骤(4)获得的一段干燥的潮粉落入内置流化床2中,往内置流化床2中通入干燥热空气进一步干燥、附聚,得到二段干燥产品,该过程时间为5min,内置流化床进风温度65±2℃。(5) The first-stage dry moisture powder obtained in step (4) falls into the built-in fluidized bed 2, and dry hot air is passed into the built-in fluidized bed 2 for further drying and agglomeration to obtain the second-stage dried product. The process time It is 5 minutes, and the air inlet temperature of the built-in fluidized bed is 65±2℃.
(6)步骤(5)获得的二段干燥的产品落入振动流化床3中,在造粒段通过气流喷雾装置7气流喷雾粘合剂(本实施例中粘合剂为水),再湿造粒,喷出水量为微胶囊总原料的3%,再经干燥段干燥和冷却段冷却后得到成品,并从振动流化床上端排出干燥热空气和冷却空气,其中干燥(边干燥边造粒)段时间为5min;振动流化床造粒段进风温度65±2℃,干燥段进风温度50±2℃,冷却段进风温度20℃。(6) The second-stage dried product obtained in step (5) falls into the vibrating fluidized bed 3, and in the granulation section, the adhesive (the adhesive is water in this embodiment) is air-sprayed through the air-spray device 7, and then Wet granulation, the amount of sprayed water is 3% of the total raw materials of microcapsules, and then the finished product is obtained after drying in the drying section and cooling in the cooling section, and the dry hot air and cooling air are discharged from the upper end of the vibrating fluidized bed, in which drying (drying while Granulation) for 5 minutes; the air inlet temperature of the vibrating fluidized bed granulation section is 65±2℃, the air inlet temperature of the drying section is 50±2℃, and the air inlet temperature of the cooling section is 20℃.
(7)将步骤(4)、步骤(5)和步骤(6)中排出的空气通入旋风分离器4中,在一级旋风分离器和二级旋风分离器中分离除尘,获得细粉,尾气经水膜除尘后排出;(7) Pass the air discharged in steps (4), (5) and (6) into the cyclone separator 4, and separate and remove dust in the first-level cyclone separator and the second-level cyclone separator to obtain fine powder, The exhaust gas is discharged after dust removal by water film;
(8)将步骤(7)中收集的细粉由管道输送到振动流化床,与二段干燥产品混合均匀,再湿造粒,进一步干燥冷却后得到成品,成品进入集料装置5;步骤(8)和步骤(6)是同时连续进行的。(8) Transport the fine powder collected in step (7) to the vibrating fluidized bed through the pipeline, mix it evenly with the second-stage drying product, and then wet and granulate it. After further drying and cooling, the finished product is obtained, and the finished product enters the aggregate device 5; Step (8) and step (6) are performed simultaneously and continuously.
本实施例得到的产品指标,DHA含量为10%,溶解考察指标为0,口中的速溶时间为1s,表面油为0.3%,气味及入口感官无明显腥味。The product indicators obtained in this example include DHA content of 10%, dissolution index of 0, instant dissolution time in the mouth of 1 s, surface oil of 0.3%, and no obvious fishy smell in the mouth.
实施例2Example 2
本实施例的制备方法和系统与实施例1的相同,不同之处为:The preparation method and system of this example are the same as those of Example 1, with the following differences:
本实施例的微胶囊原料的组分为:酪蛋白酸钠6%,DHA油脂26%,抗坏血酸钠4%,乳清蛋白5%,固体玉米糖浆剩余。The components of the microcapsule raw materials in this embodiment are: 6% sodium caseinate, 26% DHA oil, 4% sodium ascorbate, 5% whey protein, and the remainder of solid corn syrup.
步骤(3)乳液的固形物含量为40%。The solid content of the emulsion in step (3) is 40%.
步骤(6)中粘合剂为10%的酪蛋白酸钠溶液,喷出量为微胶囊总原料的3%。In step (6), the adhesive is 10% sodium caseinate solution, and the spray amount is 3% of the total raw materials of the microcapsules.
本实施例得到的产品指标,DHA含量为10%,溶解考察指标为0,口中的速溶时间为2s,表面油为0.28%,气味及入口感官无明显腥味。The product indicators obtained in this example include DHA content of 10%, dissolution index of 0, instant dissolution time in the mouth of 2 seconds, surface oil of 0.28%, and no obvious fishy smell in the mouth.
对比例1Comparative example 1
本对比例的制备方法和系统与实施例1的相同,不同之处为:The preparation method and system of this comparative example are the same as those of Example 1, with the following differences:
步骤(6)中粘合剂的喷出量为微胶囊总原料的8%。The amount of adhesive sprayed in step (6) is 8% of the total raw materials of the microcapsules.
本对比例会有塌床现象,无法得到松散的微胶囊产品。In this comparative example, there will be a bed collapse phenomenon, and a loose microcapsule product cannot be obtained.
对比例2Comparative example 2
本对比例的制备方法和系统与实施例1的相同,不同之处为:The preparation method and system of this comparative example are the same as those of Example 1, with the following differences:
步骤(6)中粘合剂的喷出量为微胶囊总原料的1%。The amount of adhesive sprayed in step (6) is 1% of the total raw materials of the microcapsules.
本对比例中产品粘合度不够,未充分黏合的粉剂过细,溶解考察中无法良好分散,指标为3。The product in this comparative example has insufficient adhesion, and the insufficiently adhered powder is too fine and cannot be dispersed well during the dissolution test. The index is 3.
该对比例同时还说明,未附聚或未充分黏合造粒的粉剂由于过细、密度等问题都会影响其溶解性。This comparative example also shows that powders that are not agglomerated or insufficiently bonded and granulated will affect their solubility due to problems such as excessive fineness and density.
对比例3Comparative example 3
本对比例采用常规的气流喷雾-塔内附聚工艺中描述的工艺流程,工艺设备与本发明的区别在于无外置流化床,喷雾设备为气流喷雾塔,旋风分离器通过管道与塔内部相连,附聚发生在内置流化床中,且细粉通过旋风分离重返塔内参与附聚,附聚条件为内置流化床60-70℃的环境下进行黏附2小时,得到的微胶囊产品表面油0.42%,溶解考察指标为0,口中的速溶时间为5s,气味感官虽然无明显腥味,但产品直接入口后有微腥味。This comparative example adopts the process flow described in the conventional air flow spray-tower agglomeration process. The difference between the process equipment and the present invention is that there is no external fluidized bed, the spray equipment is an air flow spray tower, and the cyclone separator is connected to the inside of the tower through a pipeline. Connected, agglomeration occurs in the built-in fluidized bed, and the fine powder returns to the tower through cyclone separation to participate in agglomeration. The agglomeration condition is that the built-in fluidized bed is adhered for 2 hours at 60-70°C to obtain microcapsules. The surface oil of the product is 0.42%, the dissolution index is 0, and the instant dissolution time in the mouth is 5 seconds. Although there is no obvious fishy smell in the odor sense, the product has a slight fishy smell after being directly ingested.
对比例4Comparative example 4
本对比例与对比例3的区别在于尝试改变附聚时间,减少为0.5小时,从而改善入口滋味,但由于喷雾、黏附是连续过程,黏附时间的降低会导致乳液喷雾量的降低,从而使得终产品中DHA含量无法达到10%。如果为了减少时间又试图保证含量达标,就必须提高乳液中ARA/DHA等多不饱和脂肪酸油脂的比例,同样要提高乳化剂的比例,又不能降低浓度,所以乳液粘度会提高,从而影响乳液输送、均质和雾化,最终影响产品质量,而改善优化过程又过于复杂。The difference between this comparative example and Comparative Example 3 is that the attempt was made to change the agglomeration time and reduce it to 0.5 hours, thereby improving the taste in the mouth. However, since spraying and adhesion are continuous processes, the reduction of adhesion time will lead to a reduction in the amount of emulsion spray, thus making the final The DHA content in the product cannot reach 10%. If you are trying to reduce time and ensure that the content reaches the standard, you must increase the proportion of polyunsaturated fatty acid oils such as ARA/DHA in the emulsion. You must also increase the proportion of emulsifier without reducing the concentration. Therefore, the viscosity of the emulsion will increase, thus affecting the delivery of the emulsion. , homogenization and atomization, which ultimately affects product quality, and the improvement and optimization process is too complicated.
对比例5Comparative example 5
采用CN201310217380.X中的中描述的工艺设备和工艺流程,虽然塔内附聚时间为0.5h,得到的微胶囊产品溶解考察指标为1,口中的速溶时间为9s,速溶性较本发明较差,不适用应用于一些对速溶性要求较高的终端产品。而进一步降低附聚时间会出现对比例4的问题。Using the process equipment and process flow described in CN201310217380. , not suitable for use in some end products that require higher instant solubility. However, further reducing the agglomeration time will cause the problem of Comparative Example 4.
对比例6Comparative example 6
本对比例与实施例1的区别在于,尝试替换压力喷雾为离心喷雾,但由于离心喷雾与压力喷雾排风方式不同,离心喷雾为底部排风,工艺过程需将粉剂物料全部引入旋风分离器内再落入振动流化床,不仅设备改装难度较高,该工艺得到的再造粒产品由于进入振动流化床之前的粉剂较细,无法实现较好的粘合附聚,影响产品最后的速溶性。The difference between this comparative example and Example 1 is that an attempt was made to replace the pressure spray with centrifugal spray. However, due to the different exhaust modes of centrifugal spray and pressure spray, centrifugal spray is bottom exhaust, and the process requires all powder materials to be introduced into the cyclone separator. Then it falls into the vibrating fluidized bed. Not only is it difficult to modify the equipment, but the re-granulated product obtained by this process cannot achieve good adhesion and agglomeration due to the fine powder before entering the vibrating fluidized bed, which affects the final instant dissolution of the product. sex.
最后,本发明的方法仅为较佳的实施方案,并非用于限定本发明的保护范围。凡在本发明的精神和原则之内,所作的任何修改、等同替换、改进等,均应包含在本发明的保护范围之内。Finally, the method of the present invention is only a preferred embodiment and is not used to limit the protection scope of the present invention. Any modifications, equivalent substitutions, improvements, etc. made within the spirit and principles of the present invention shall be included in the protection scope of the present invention.
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