WO2017088459A1 - 一种片状微胶囊及其制备方法 - Google Patents

一种片状微胶囊及其制备方法 Download PDF

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Publication number
WO2017088459A1
WO2017088459A1 PCT/CN2016/086360 CN2016086360W WO2017088459A1 WO 2017088459 A1 WO2017088459 A1 WO 2017088459A1 CN 2016086360 W CN2016086360 W CN 2016086360W WO 2017088459 A1 WO2017088459 A1 WO 2017088459A1
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solution
microcapsule
sheet
alginate
gel
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PCT/CN2016/086360
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English (en)
French (fr)
Inventor
袁彦洁
卢颖
杜森垚
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重庆小丸科贸有限公司
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Publication of WO2017088459A1 publication Critical patent/WO2017088459A1/zh

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    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00—Cosmetics or similar toiletry preparations
    • A61K8/02—Cosmetics or similar toiletry preparations characterised by special physical form
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00—Cosmetics or similar toiletry preparations
    • A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/72—Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds
    • A61K8/73—Polysaccharides
    • A61K8/733—Alginic acid; Salts thereof
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00—Cosmetics or similar toiletry preparations
    • A61K8/02—Cosmetics or similar toiletry preparations characterised by special physical form
    • A61K8/0241—Containing particulates characterized by their shape and/or structure
    • A61K8/0254—Platelets; Flakes
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00—Cosmetics or similar toiletry preparations
    • A61K8/02—Cosmetics or similar toiletry preparations characterised by special physical form
    • A61K8/11—Encapsulated compositions
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00—Cosmetics or similar toiletry preparations
    • A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/72—Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds
    • A61K8/73—Polysaccharides
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00—Cosmetics or similar toiletry preparations
    • A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/72—Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds
    • A61K8/73—Polysaccharides
    • A61K8/731—Cellulose; Quaternized cellulose derivatives
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00—Cosmetics or similar toiletry preparations
    • A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/72—Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds
    • A61K8/73—Polysaccharides
    • A61K8/735—Mucopolysaccharides, e.g. hyaluronic acid; Derivatives thereof
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q19/00—Preparations for care of the skin
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q19/00—Preparations for care of the skin
    • A61Q19/02—Preparations for care of the skin for chemically bleaching or whitening the skin
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2800/00—Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
    • A61K2800/10—General cosmetic use
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2800/00—Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
    • A61K2800/40—Chemical, physico-chemical or functional or structural properties of particular ingredients
    • A61K2800/56—Compounds, absorbed onto or entrapped into a solid carrier, e.g. encapsulated perfumes, inclusion compounds, sustained release forms
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2800/00—Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
    • A61K2800/40—Chemical, physico-chemical or functional or structural properties of particular ingredients
    • A61K2800/59—Mixtures
    • A61K2800/594—Mixtures of polymers

Definitions

  • the invention belongs to the technical field of microcapsules, and in particular relates to a chip microcapsule and a preparation method thereof.
  • microcapsules to cosmetics or toiletries
  • the current microcapsule products are mostly spherical, the shape is relatively simple, there is no flaky microcapsules, and the flaky microcapsules have the same wrapping function compared with the spherical microcapsules, and can also bring unique visual effects to consumers.
  • the prior art does not have a related study on the preparation of sheet-like microcapsules, because the gel solution usually shrinks into a spherical or irregular gel block due to surface tension, and the microcapsule material cannot be expanded to the periphery. Further, it is impossible to form a microcapsule in the form of a sheet or a strip, and thus there are certain defects.
  • the technical problem to be solved by the present invention is how to provide a chip-shaped microcapsule and a preparation method thereof, which breaks the deficiency of the microcapsule products in the prior art, and has stability. Good, good quality features.
  • the present invention adopts the following technical solution: a sheet-like microcapsule characterized in that the outer shape is a sheet shape or a strip shape, and the thickness of the sheet or the strip shape is smaller than the width, and the thickness is 0.01. ⁇ 1 mm; the mass percentage of the flaky microcapsule shell, comprising the following components: alginate 0.1-3%, hot melt gel 0.1-3%, water soluble film forming material 0.1-5%, and preservative 0.1 ⁇ 1%; the rest is water;
  • microcapsule core of the tablet is the other active ingredient and auxiliary material.
  • a microcapsule which comprises, in parts by weight, 30 parts by weight of alginic acid or alginate gel, and 20 to 40 parts of hot melt gel. 5 to 10 parts of a water-soluble film-forming material and 0.1 to 1 part of a preservative.
  • the invention also provides a preparation method of the above-mentioned sheet microcapsule, comprising the following steps:
  • Step 1) weigh the other raw materials in the raw material at 60 ⁇ 70 ° C, to obtain a mixture B;
  • a calcium or magnesium salt solution having a mass concentration of 0.5 to 3% onto a trough having one end high and one end low to form a slope of a downwardly inclined calcium or magnesium salt solution, and the homogenate obtained in the step 3) C is added from the high end of the trough to the slope of the calcium salt or magnesium salt solution to obtain the sheet microcapsule; wherein the thickness of the slope of the calcium salt or magnesium salt solution is 1 to 3 mm, The volume acceleration rate of the homogenate C is 5 to 100 mL/min, and the flow rate of the calcium salt or magnesium salt solution is 300 to 2000 mL/min; the wire groove may be linear, zigzag or spiral.
  • the invention also provides a preparation method of another above-mentioned sheet microcapsule, comprising the following steps:
  • Step 1) weigh the other raw materials in the raw material at 60 ⁇ 70 ° C, to obtain a mixture B;
  • the homogenization C is controlled to have a dropping acceleration rate of 5 to 100 mL/min, and a stirring rate of 100 to 1000 rpm/min.
  • the present invention has the following beneficial effects:
  • the present invention utilizes the principle that alginate encounters a divalent metal salt solution to form a gel to prepare a sheet-shaped capsule, but in the prior art, the alginic acid solution shrinks due to surface tension when it encounters a divalent metal salt solution. a spherical or irregular gel block, and therefore cannot be prepared into a sheet-like microcapsule; for the above reasons, the present invention has found through research that the preservative or surfactant selected in the present invention is added to the alginic acid solution.
  • the surface tension of the compound after the compounding is lower than that of the salt solution, and the surface tension reducing material allows the alginic acid solution to spread on the surface of the divalent metal salt solution and react with the salt solution to form a circle.
  • a sheet or ribbon gel film, the shape of these gel films is mutated by the flow of saline to the sheet-like microcapsules.
  • the present invention forms a mosaic structure in which a sheet-like capsule is network cross-linked, and can be described as a wall of reinforced concrete.
  • the hot-melt gel forms a three-dimensional network cage structure, like the steel bars inside the building wall.
  • the core material is embedded in these cages.
  • the alginate gel is like the material filling the cage gap.
  • the chimerism of the heart is more tight; the film-forming material is coated on the structure to reduce the risk of the core being leaked by the wrapped material.
  • the raw material of the present invention is further compounded with other colloidal or polymeric materials, and the raw materials are passed through each raw material.
  • the synergistic compatibility makes the tablet microcapsules of the invention more stable and good in the base materials such as enamel, cream, shower gel and shampoo.
  • the synergistic compatibility between the raw materials in the present invention makes the sheet-like microcapsules of the present invention easy to soften in the base-containing material, and is easy to apply, and has a better skin feel.
  • the raw materials used in the invention are all internationally certified raw materials for skin external use, and have good safety performance.
  • the method of the invention can realize a large number of industrial productions which are completely automated, no manual operation, less process pollution, high product quality, good controllability and reproducibility.
  • the method of the present invention drops the raw material solution onto the inclined surface of the calcium chloride solution, and the salt solution reacts with the raw material solution to rapidly cure the contact surface, and the lower temperature salt solution cools the effect and strengthens the effect.
  • the microcapsules are initially formed, and the flowing salt solution continues to solidify and cool in the process of transporting the initially formed sheet-like microcapsules, and finally forms a sheet-like microcapsule, and the flowing salt solution has a thickness of 1 to 3 mm, so that the raw material
  • the droplets of the solution can float on the salt solution without sinking to the bottom, thereby ensuring that the microcapsules can be obtained, and the salt solution of the invention is flowing, avoiding the droplets caused by the dropping of the colloidal solution or the overlapping of the streamlines.
  • the accumulation ensures that the sheet-like microcapsules are formed into a crosslinked structure.
  • the special nature of the production process and capsule formulation of the present invention ensures that the microcapsule shell and the core form a network of cross
  • the homogenate C slowly falls from the dripper, and when it is in contact with the salt solution, it is spread into a sheet shape under the impact force, and the salt solution and the homogenization
  • the reaction of the substance C causes the contact surface to solidify rapidly, and the cooling of the salt solution with a lower temperature also strengthens the effect, so that the microcapsules of the microcapsules are initially formed; the slowly stirred salt solution causes the initially formed microcapsules to continue to occur. Curing, cooling The role, and eventually form a sheet of microcapsules; the shell material, are the colloids will be entangled. Calcium salt triggers the coagulation of this colloidal solution. This method is easier to operate and the equipment used is simpler.
  • Figure 1 is a schematic view of the apparatus used in the preparation method of the bevel dropping method of the present invention.
  • Figure 2 is a schematic view of the apparatus used in the agitating production method of the present invention.
  • the device shown in FIG. 1 includes a gel delivery drip system, a salt solution circulation system, a microcapsule shaper, and a microcapsule collector; a raw material tank having a raw material solution, the gel transfer drip system comprising a raw material transfer pump 2 and a dripper 3 for delivering a raw material solution to the dripper 3 at a set flow rate
  • the dripper 3 has a tubular shape, one end is in communication with the liquid outlet of the raw material transfer pump 2, and the other end is located above the microcapsule former for allowing the gel solution to be droplets or liquid columns.
  • the shape of the microcapsule is dropped from the dripper 3;
  • the microcapsule shaper is a wire trough 4 having a high end and a low end, and the high end of the trough 4 is an inlet end, located below the dripper 3, and the lower end is An outlet end for discharging the salt solution and the condensed sheet-shaped microcapsules;
  • the microcapsule collector being located below the outlet end of the wire trough 4 for collecting the sheet-like microcapsules, the collector being a salt solution recovery tank 6 and a collection net 5 disposed at an opening thereof, said The collector is located below the outlet end of the wire trough 4, and the collector functions to facilitate separation of the flake microcapsules from the salt solution;
  • the salt solution circulation system is composed of a salt solution tank 9 and a circulation pump 8, the salt
  • the solution tank 9 is provided with a salt solution output pipe 7 with a valve for conveying the salt solution to the inlet end of the wire trough 4, and the salt solution recovery tank 6, the circulation pump
  • the raw material solution slowly falls from the dripper 3, when it comes into contact with the salt solution in the wire tank 4, Under the impact force, the sheet is formed into a sheet shape; at the same time, the salt solution reacts with the gel solution to rapidly cure the contact surface, and the lower temperature salt solution cools the effect, thereby strengthening the effect and forming the microcapsules. .
  • the flowing salt solution continues to solidify, cool and eventually form flaky microcapsules during the downward transport of the initially formed flaky microcapsules. The flowing salt solution also prevents the drop of falling gel solution from affecting the forming effect.
  • the size of the droplet formed by the gel solution can be controlled to affect the size of the microcapsules; when the droplets form a continuous liquid column, the shape of the microcapsules become a ribbon.
  • a device as shown in FIG. 2 including a gel delivery drip system and a microcapsule molding system; the delivery drip system includes a transfer pump 11 and a dripper 12, and the transfer pump 11 is used.
  • the homogenate C is delivered to the dripper 12; the dripper 12 has a tubular shape, one end is connected to the liquid outlet of the transfer pump 11, and the other end is located above the microcapsule molding system.
  • the microcapsule molding system comprising a forming tank 2 and a stirrer, the stirrer being driven by the motor 203 and as a stirring rotor
  • the fan blade 201 is disposed in the forming pool 2, and the center of the blade 201 is connected to the motor 203 located above the forming pool 2 through a connecting rod 202, the forming pool 2 is located below the dripper 12 for containing a salt solution; the agitator rotor of the agitator is located in the forming tank for driving the salt solution to rotate.
  • the homogeneous substance C slowly falls from the dripper 12, and when it comes into contact with the salt solution in the forming tank 2, it is spread into a sheet shape under the impact force; meanwhile, the salt solution reacts with the homogeneous substance C to make the contact surface Rapid curing, and the lower temperature of the salt solution to cool it also strengthens this effect, so that the microcapsules are initially formed.
  • the slowly rotating salt solution continues to cure, cool and initially form the sheet-like microcapsules. The slow rotation of the salt solution also prevents the drop of the falling gel solution from affecting the forming effect.
  • the size of the droplets formed by the homogenate C can be controlled, thereby affecting the size of the microcapsules; when the droplets form a continuous liquid column, the microcapsules The shape is banded.
  • both the microcapsule shell and the core of the capsule form a network-like crosslinked structure.
  • Example 1 Moisturizing anti-aging sleep mask containing seaweed essence:
  • step 2) After heating the solution prepared in step 1) to 60 ° C, the three solutions are mixed in proportion and kept warm for use;
  • step 5 After heating the mixed raw materials in step 4) to 60-80 ° C and adding the mixed solution in step 2), homogenizing, and maintaining the temperature of the mixture at 60-70 ° C, to obtain a homogeneous substance for use;
  • the obtained blue seaweed morphological tablet capsule is transparent and ultra-thin, and the blue color is derived from natural blue seaweed extract, which is natural and makes the product performance more stable.
  • Table 2 contains blue seaweed sleep mask formula
  • B1 and B2 water bath heating and melting, adding D1 and D2 to mix evenly;
  • step 4 Add E to the mixed raw materials in step 3 to stir evenly, that is, the capsule shell and the core of the capsule form a network of cross-linked microcapsules.
  • step 2) After heating the solution prepared in step 1) to 60-70 ° C, mix the four solutions in proportion and keep warm for use;
  • step 6) heating the mixed raw material of step 5) to 75 ° C, and adding the mixed solution in step 2), homogenizing, and maintaining the temperature of the mixture at 60-70 ° C, to obtain a homogeneous substance for use;
  • step 6) The homogenate after step 6) homogenization is pumped and dropped into a slope of about 10-30 degrees on the inclined surface, and the calcium chloride solution having a mass concentration of 2% is flowed on the inclined surface to obtain silver white. a shiny micro-capsule; wherein the calcium chloride solution has a slope of 1 to 3 mm, the homogenate C has a droplet acceleration rate of 50 mL/min, and the calcium chloride solution has a flow rate of 1000 mL/min. .
  • the obtained snowflake-shaped tablet capsule has the characteristics of transparency, ultra-thinness and beauty, and is particularly suitable for use in facial cosmetics.
  • honeysuckle flake microcapsules for shower gel can obviously improve the aesthetics of the product, and the honeysuckle and the leaves of the leaves are also effective for cooling blood, relieving itching and deworming.
  • a sodium alginate solution having a mass concentration of 2% Preparing a sodium alginate solution having a mass concentration of 2%, a gellan gum solution having a mass concentration of 1%, a polyvinyl alcohol solution having a mass concentration of 0.5%, and a sodium carboxymethylcellulose solution having a mass concentration of 1%;
  • step 1) The solution prepared in step 1) is heated to 60 ° C and mixed, and kept warm for use;
  • the C raw material is milled and mixed, and mixed into the B raw material after the step 3) mixing, and stirred at 60 ° C;
  • the D raw material is mixed and added to the mixed material in the step 4), and stirred at 60 ° C to obtain a mixed raw material;
  • step 5 the step 5) mixed raw materials are heated to 60 ° C, added to the mixed solution of step 2), homogenized, and the temperature of the mixture is maintained at 60 ⁇ 70 ° C, to obtain a homogeneous material for use;
  • step 6 The homogenate after step 6) homogenization and heat preservation is added to the calcium chloride solution having a mass concentration of 2%, and the calcium chloride solution is stirred by using a stirring device to obtain a microcapsule containing the honeysuckle extract.
  • the dropping acceleration rate of the controlled homogeneous substance C was 60 mL/min, and the stirring rate was 300 rpm/min.
  • Sodium alginate is prepared into a solution having a mass concentration of 2% by using pure water, and the agar is prepared into a solution having a mass concentration of 1% by using pure water, and hydroxyethyl cellulose is formulated into a mass concentration of 1% with pure water.
  • a solution of sodium hyaluronate in purified water to a solution having a mass concentration of 1%;
  • step 1) After heating the solution prepared in step 1) to 60 ° C, mix the four solutions and keep warm for use;
  • step 5 mixed raw materials are heated to 75 ° C, and added to the mixed solution in step 2, homogenized, and the temperature of the mixture is maintained at 60-70 ° C to obtain a homogeneous substance for use;
  • step 6 The homogenate after homogenization and heat preservation in step 6 is outputted by a pump and added dropwise to the inclined surface, and the calcium chloride solution having a mass concentration of 2% is flowed on the inclined surface to obtain a micro-capsule of pink rose whitening effect. .
  • a microcapsule containing a cooling mint formulation the composition of which is shown in the following table:
  • step 2 The solution prepared in step 1 is heated to 60 ° C and mixed, and kept warm for use;
  • the B material in the above table is uniformly mixed and heated to 60 ° C;
  • step 5 mixed raw materials are heated to 60 ° C, added to the mixed solution in step 2, homogenized, and the temperature of the mixture is maintained at 60-70 ° C to obtain a homogeneous substance for use;
  • step 6 The homogeneous substance after homogenization and heat preservation in step 6 is outputted by a pump and added to the inclined surface, and a calcium chloride solution having a mass concentration of 2% is flowed on the inclined surface to obtain a microcapsule containing a cool mint formula. .

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Abstract

一种片状微胶囊及其制备方法，所述片状微胶囊为薄片状或条状带，所述薄片或条状带的厚度均小于宽度，厚度均为0.01～1mm；所述片状微胶囊囊壳的质量百分比，包括如下成分：海藻酸盐0.1-3%、热熔性凝胶0.1-3%、水溶性成膜材料0.1-5%和防腐剂0.1-1%；其余部分是水；片状微胶囊囊芯为其他活性成分和辅料。本发明通过各原料成分之间的协同配伍作用，使复配后的原料表面张力低于氯化钙等盐溶液，凝胶在盐水表面延展，摊开成薄膜，形成片状微胶囊。

Description

一种片状微胶囊及其制备方法 技术领域
本发明属于微胶囊技术领域，具体涉及一种片状微胶囊及其制备方法。
背景技术
消费者日益追求化妆品个人护理品的天然和功效，作为一个日用品不仅仅外观要优美富于吸引力和天然想象力，而且要稳定和有功效。
在化妆品或洗浴品中添加微胶囊，一方面是增加功能性元素，更为重要的是为了改善化妆品或洗浴品的美观度。而目前的微胶囊产品多为圆球状，形状比较单一，没有片状微胶囊，而片状相比于球形的微胶囊除了具备相同的包裹功能，还可以给消费者带来独特的视觉效果。现有技术并没有制备片状微胶囊的相关研究，究其原因是因为通常凝胶溶液会由于表面张力而收缩成球或不规则的凝胶块，没法使微胶囊原料向四周扩展开，进而没法做成片状或带状的微胶囊，因而存在着一定的缺陷。
发明内容
针对现有技术存在的上述不足，本发明所要解决的技术问题是：如何提供一种片状微胶囊及其制备方法，打破现有技术中微胶囊产品均为圆球状的不足，且具有稳定性好、品质优良的特点。
为了解决上述技术问题，本发明采用如下技术方案：一种片状微胶囊，其特征在于，外形为薄片状或条带状，所述薄片或条带状的厚度均小于宽度，厚度均为0.01～1mm；所述片状微胶囊囊壳的质量百分比，包括如下成分：海藻酸盐0.1-3％、热熔性凝胶0.1-3％、水溶性成膜材料0.1-5％和防腐剂0.1～1％；其余部分是水；
片状微胶囊囊芯为其他活性成分和辅料。
进一步，还提供一种片状微胶囊，所述片状微胶囊囊壳以重量份计，包括如下成分：30～50份海藻酸或海藻酸盐凝胶、20～40份热熔性凝胶、5～10份水溶性成膜材料和0.1～1份防腐剂。
本发明还提供了上述片状微胶囊的制备方法，包括如下步骤：
1)按照上述配方换算称取原料，分别配制质量浓度为0.1～3％的海藻酸或海藻酸盐水溶液、质量浓度为0.1～3％的热熔性凝胶水溶液和质量浓度为0.1～5％的水溶性成膜材料水溶液，将三种水溶液分别加热至60～70℃后混合均匀，得到溶液A，将溶液A在60～70℃进行保温；
2)将步骤1)称取原料中的其它原料在60～70℃混合均匀，得到混合物B；
3)将步骤2)所述混合物B加热至60～80℃后，加入到步骤1)得到的溶液A中并进行均质，均质过程中保持温度为60～70℃，得到均质物C；
4)使质量浓度0.5～3％的钙盐或镁盐溶液流淌到一端高一端低的线槽上，形成一个倾斜向下的钙盐或镁盐溶液斜面，将步骤3)得到的均质物C从所述线槽高的一端滴加到所述钙盐或镁盐溶液斜面上，制得所述片状微胶囊；其中，所述钙盐或镁盐溶液斜面的厚度为1～3mm，所述均质物C的滴加速率为5～100mL/min，所述钙盐或镁盐溶液的流速为300～2000mL/min；所述线槽可以为直线形、Z字形或螺旋形。
本发明还提供了另一种上述片状微胶囊的制备方法，包括如下步骤：
1)按照上述配方换算称取原料，分别配制质量浓度为0.1～3％的海藻酸或海藻酸盐水溶液、质量浓度为0.1～3％的热熔性凝胶水溶液和质量浓度为0.1～5％的水溶性成膜材料水溶液，将三种水溶液分别加热至60～70℃后混合均匀，得到溶液A，将溶液A在60～70℃进行保温；
2)将步骤1)称取原料中的其它原料在60～70℃混合均匀，得到混合物B；
3)将步骤2)所述混合物B加热至60～80℃后，加入到步骤1)得到的溶液A中并进行均质，均质过程中保持温度为60～70℃，得到均质物C；
4)将步骤3)得到的均质物C滴加入质量浓度0.5～3％的钙盐或镁盐溶液中，同时使用搅拌装置对钙盐或镁盐溶液进行搅拌，制得所述片状微胶囊；其中，控制均质物C的滴加速率为5～100mL/min，搅拌速率为100～1000rpm/min。
相比现有技术，本发明具有如下有益效果：
1、本发明利用海藻酸盐遇到二价金属盐溶液可以生成凝胶的原理来制备薄片形胶囊，但是现有技术中海藻酸溶液遇到二价金属盐溶液的时候会由于表面张力而收缩成球或不规则的凝胶块，因此不能制备成片状微胶囊；基于上述原因，本发明通过研究发现在海藻酸溶液中加入本发明选择的防腐剂或表面活性剂，可 以使胶体的表面张力降低，使复配后的原料表面张力低于盐溶液，这些降低表面张力的物质让海藻酸溶液在二价金属盐溶液的表面铺展开，同时和盐溶液反应成类圆片或带状凝胶薄膜，通过盐水的流动让这些凝胶薄膜形状得到变异而到片状微胶囊。
2、本发明形成片状胶囊呈网络交联的嵌合式结构，可以形容成钢筋水泥的墙体。热溶性凝胶形成一个立体的网状的笼结构，犹如房屋建筑墙体里面的钢筋，囊芯物质嵌合在这些网笼里面，海藻酸盐凝胶犹如填充这个网笼间隙的物质，使囊心物的嵌合更加紧密；成膜材料是在这个结构上面覆膜，降低囊芯被包裹物质泄露的风险。
3、由于单一的海藻酸盐凝胶对很多物质不稳定，容易被碱，螯合剂，表面活性剂等溶胀和溶解，所以本发明原料中还复配了其他胶体或高分子材料，通过各原料的协同配伍作用，使本发明片状微胶囊在基料例如着哩，霜乳，沐浴露，香波中更加稳定，性质良好。
4、本发明中各原料之间的协同配伍作用，使本发明片状微胶囊在含有基料中容易软化而变得容易涂抹，肤感更好。
5、本发明采用的原料均为国际认证可用于皮肤外用的原料，安全性能好。
6、本发明方法可以实现完全自动化的大量工业生产，无需人工操作，流程污染少，产品质量高，可控性和重现性好。
7、本发明方法将原料溶液滴加到氯化钙溶液斜面上，盐溶液与原料溶液反应，使接触面迅速固化，而温度较低的盐溶液使其冷却也强化了这一效果，使片状微胶囊初步成形，流动的盐溶液在向下输送初步成形的片状微胶囊的过程中继续发生固化、冷却作用并最终形成片状微胶囊，流动的盐溶液厚度为1～3mm，使得原料溶液的液滴可以漂浮在盐溶液上，而不会沉底，进而保证了可以制得片状微胶囊，且本发明盐溶液为流动的，避免胶体溶液滴点或流线重叠造成的液滴累加，保证了片状微胶囊的成型为交联结构。本发明生产工艺和囊壳配方的特殊性质确保微胶囊囊壳和囊芯形成网状的交联结构。
8、本发明另一种片状微胶囊制备方法中，均质物C缓慢地从滴头中下落，在其与盐溶液接触时，在冲击力作用下展开成片状，盐溶液与均质物C反应，使接触面迅速固化，而温度较低的盐溶液使其冷却也强化了这一效果，使片状微胶囊初步成形；缓慢搅动的盐溶液使初步成形的片状微胶囊继续发生固化、冷却 作用，并最终形成片状微胶囊；囊壳材料，都是胶体会缠绕起来。钙盐触发这个胶体溶液凝固这种方法更加易于操作，使用的设备更加简单。
附图说明
图1为本发明斜面滴加制备方法中使用的装置示意图。
附图中：1-原料罐，2-原料输送泵，3-滴头，4-线槽，5-收集网，6-盐溶液回收池，7-盐溶液输出管，8-循环泵，9-盐溶液箱。
图2为本发明搅拌生产方法中使用的装置示意图。
附图中：11—送泵；12—滴头；13—调节套管；2—成形池；201—扇叶；202—连杆；203—电机；21—收集网；3—储存器。
具体实施方式
下面结合实施例和说明书附图对本发明作进一步详细说明。
本发明片状微胶囊斜面滴加制备过程中，采用如图1所示装置，图1装置包括凝胶输送滴液系统、盐溶液循环系统、微胶囊成型器、微胶囊收集器；1为盛装有原料溶液的原料罐，所述的凝胶输送滴液系统包括原料输送泵2和滴头3，所述原料输送泵2用于将原料溶液以设定的流速输送到所述的滴头3；所述的滴头3呈管形，一端与所述原料输送泵2的出液口连通，另一端位于所述的微胶囊成型器的上方，用于让凝胶溶液以液滴或液柱的形态从滴头3中下落；所述的微胶囊成型器是一端高一端低的线槽4，该线槽4高的一端为入口端，位于所述滴头3的下方，低的一端为出口端，用于将盐溶液和凝结成的片状微胶囊排出；所述的微胶囊收集器位于所述线槽4的出口端的下方，用于收集片状微胶囊，所述的收集器由盐溶液回收池6和设置在其敞口处的收集网5组成，所述的收集器位于所述线槽4的出口端的下方，收集器的作用是方便将片状微胶囊与盐溶液分离；所述盐溶液循环系统由盐溶液箱9和循环泵8组成，所述的盐溶液箱9上设置有带阀门的盐溶液输出管7，用于将盐溶液输送到所述线槽4的入口端，所述的盐溶液回收池6、循环泵8和盐溶液箱9依次连通，用于将盐溶液回收池6中的盐溶液循环到盐溶液箱9中，盐溶液循环系统实现了资源的回收利用，也有利于连续化生产。
制备时，原料溶液缓慢地从滴头3中下落，在其与线槽4中的盐溶液接触时， 在冲击力作用下展开成片状；同时，盐溶液与凝胶溶液反应，使接触面迅速固化，而温度较低的盐溶液使其冷却也强化了这一效果，使片状微胶囊初步成形。流动的盐溶液在向下输送初步成形的片状微胶囊的过程中继续发生固化、冷却作用并最终形成片状微胶囊。流动的盐溶液还可以避免下落的凝胶溶液液滴累加而影响成型效果。通过调节原料输送泵2来控制凝胶溶液的流速，可以控制凝胶溶液形成的液滴的大小，从而影响片状微胶囊的大小；当液滴形成连续的液柱时，微胶囊的形状则成为带状。
本发明搅拌生产过程中，采用如图2所示装置，包括凝胶输送滴液系统和微胶囊成型系统；所述的输送滴液系统包括输送泵11和滴头12，所述输送泵11用于将均质物C输送到所述滴头12；所述的滴头12呈管形，一端与所述输送泵11的出液口连通，另一端位于所述的微胶囊成型系统的上方，用于让均质物C以液滴或液柱的形态从滴头12中下落；所述的微胶囊成型系统包括成形池2和搅拌器，所述的搅拌器由电机203和作为搅拌转子的扇叶201组成，该扇叶201设置在所述的成形池2内，所述扇叶201的中心通过连杆202与位于所述成形池2上方的所述电机203连接，所述的成形池2位于滴头12的下方，用于盛装盐溶液；所述的搅拌器的搅拌转子位于所述的成型池中，用于带动盐溶液转动。
均质物C缓慢地从滴头12中下落，在其与成形池2中的盐溶液接触时，在冲击力作用下展开成片状；同时，盐溶液与均质物C反应，使接触面迅速固化，而温度较低的盐溶液使其冷却也强化了这一效果，使片状微胶囊初步成形。缓慢转动的盐溶液使初步成形的片状微胶囊继续发生固化、冷却作用并最终形成片状微胶囊。盐溶液的缓慢转动还可以避免下落的凝胶溶液液滴累加而影响成型效果。通过调节输送泵11来控制均质物C的滴加速率，可以控制均质物C形成的液滴的大小，从而影响片状微胶囊的大小；当液滴形成连续的液柱时，微胶囊的形状则成为带状。以下实施例中微胶囊囊壳和囊芯均形成网状的交联结构。
实施例1：含海藻精华的保湿抗衰老睡眠面膜：
一、蓝色海藻形态片状胶囊成份：
表1蓝色海藻形态片状微胶囊原料
  成分 百分比
A1 2％海藻酸钠溶液 40％
A2 1％琼脂溶液 30％
A3 1％透明质酸钠溶液 10％
B1 藻酸丙二醇脂 5％
B2 甘油 10％
B3 兰藻提取物 1.5％
B4 神经酰胺 0.5％
B5 维生素E 1％
C1 丙二醇 1％
C2 乙基己基甘油 0.5％
C3 1,2辛二醇 0.5％
  合计 100％
二、制备方法：
1)将海藻酸钠用纯净水配制成质量浓度为2％的溶液，将琼脂用纯净水加热配制成质量浓度为1％的溶液保温，将透明质酸钠用纯净水配制成质量浓度为1％的溶液；
2)将步骤1)配制的溶液加热到60℃后，按照比例混合3种溶液并保温，备用；
3)将上表1中B原料在60～70℃混合均匀；
4)将上表1中C原料按比例在60～70℃混合，并混合入步骤3)混合后的B原料中，在60℃搅拌均匀；
5)将步骤4)混合原料加热至60～80℃后并加入步骤2)混合后的溶液中，进行均质，并保持混合物的温度为60～70℃，得均质物备用；
6)将步骤5)均质保温后的均质物用泵输出并滴加到斜面上，所述斜面上流淌有质量浓度为2％的氯化钙溶液，得到蓝色状微胶囊；其中，所述氯化钙溶液斜面的厚度为1～3mm，所述均质物C的滴加速率为100mL/min，所述氯化钙溶液的流速为800mL/min。
得到的蓝色海藻形态片状胶囊透明超薄，蓝色来自天然兰色海藻提取物，天然美而且使产品性能更为稳定。
三、含蓝色海藻睡眠面膜配方
表2含蓝色海藻睡眠面膜配方
Figure PCTCN2016086360-appb-000001
制备方法：
1、将A2溶解到A1纯水中搅拌均匀加热到70度
2、B1和B2水浴加热融化，加入D1和D2混合均匀；
3、将步骤2混合后的原料混合搅拌入步骤1混合原料中，冷却。
4、加入E到步骤3混合后的原料中搅拌均匀，即得囊壳和囊芯形成网状的交联结构微胶囊。
实施例2：
一、一种雪花形态片状胶囊
表3雪花形态片状微胶囊原料配方
  成分 百分比
A1 2％海藻酸钠溶液 35％
A2 1％卡拉胶溶液 35％
A3 1％羟乙基纤维素溶液 10％
A4 1％透明质酸钠溶液 5％
B1 丁二醇 5％
B2 维他命E醋酸酯 1％
B3 维生素B1 1％
B4 尿囊素 1％
B5 吐温20 1％
C1 银白色珠光粉 0.5％
D1 苯氧乙醇 0.5％
D2 乙基己基甘油 0.1％
D3 1,2辛二醇 0.3％
  纯净水 加到100％
  合计 100％
二、制备方法：
1)将海藻酸钠用纯净水配制成质量浓度为2％的溶液，将卡拉胶用纯净水配制成质量浓度为1％的溶液，将羟乙基纤维素用纯净水配制成质量浓度为1％的溶液，将透明质酸钠用纯净水配制成质量浓度为1％的溶液；
2)将步骤1)配制的溶液加热到60～70℃后，按照比例混合四种溶液并保温，备用；
3)将上表1中B原料在60～70℃混合均匀；
4)将上表1中C原料混合入步骤3)混合后的B原料中，在60～70℃下搅拌均匀；
5)将D原料混合加入到步骤4)混合后的料中，在60～70℃下搅拌均匀，得到混合原料；
6)将步骤5)混合原料加热到75℃，并加入步骤2)混合后的溶液中，进行均质，并保持混合物的温度为60～70℃，得均质物备用；
7)将步骤6)均质保温后的均质物用泵输出并滴加到角度大约10-30度斜面上，所述斜面上流淌有质量浓度为2％的氯化钙溶液，得到银白色闪亮片状微胶囊；其中，所述氯化钙溶液斜面的厚度为1～3mm，所述均质物C的滴加速率为50mL/min，所述氯化钙溶液的流速为1000mL/min。
得到的雪花形态片状胶囊具有透明、超薄和美观的特点，特别适合用于面部用化妆品。
三、雪花嫩白柔肤水配方
表4雪花嫩白柔肤水配方
Figure PCTCN2016086360-appb-000002
实施例3：金银花清凉沐浴露
一、金银花片状胶囊
表5金银花片状胶囊原料配方
  成分 百分比(％)
A1 2％海藻酸钠溶液 30
A2 1％结冷胶溶液 40
A3 0.5％聚乙烯醇溶液 5
A4 1％羧甲基纤维素钠溶液 5
B1 薄荷醇 5
B2 乳酸薄荷酯 5
B3 薄荷油 0.5
B4 艾叶提取物 1
B5 金银花提取物 1
B6 蔗糖硬脂酸酯 2
B7 十二烷基苯磺酸钠 0.3
C1 CI77492 0.3
C2 CI77891 0.3
D1 乙基己基甘油 0.1
D2 1,2辛二醇 0.6
D3 纯净水 加到100
  合计 100
得到的金银花片状微胶囊用于沐浴露可明显提高了产品的美观度，且金银花、艾叶提取物还具有凉血、止痒、驱虫的效果。
二、金银花片状微胶囊制备方法如下：
配制质量浓度为2％的海藻酸钠溶液，质量浓度为1％的结冷胶溶液，质量浓度为0.5％的聚乙烯醇溶液和质量浓度为1％的羟甲基纤维素钠溶液；
1、将步骤1)配制的溶液加热到60℃后混合，保温备用；
2、将上表2中B原料均匀混合并加热到60℃；
3、将C原料碾磨混合，并混合入步骤3)混合后的B原料中，在60℃下搅拌均匀；
4、将D原料混合加入到步骤4)混合后的料中，在60℃下搅拌均匀，得到混合原料；
5、将步骤5)混合原料加热到60℃，加入步骤2)混合后的溶液中，进行均质，并保持混合物的温度为60～70℃，得均质物备用；
6、将步骤6)均质保温后的均质物滴加入质量浓度为2％的氯化钙溶液中，同时使用搅拌装置对氯化钙溶液进行搅拌，得到含有金银花提取物的片状微胶囊；其中，控制均质物C的滴加速率为60mL/min，搅拌速率为300rpm/min。
实施例4：
一种片状微胶囊(粉色玫瑰美白功效)，成分如下表所示：
表6粉色玫瑰美白片状微胶囊原料配方
  成分 重量份
A1 海藻酸钠 50
A2 琼脂 20
A3 羟乙基纤维素 10
A4 透明质酸钠 5
B1 甘油 10
B2 维他命E醋酸酯 1
B3 玫瑰精露 1
B4 熊果苷 1
B5 吐温20 1
C1 红30色淀CI73360 0.1
C2 钛白粉 0.1
D1 苯氧乙醇 0.5
D2 乙基己基甘油 0.1
D3 1,2辛二醇 0.3
上述粉色玫瑰美白功效的片状微胶囊采用如下方法制备：
1、将海藻酸钠用纯净水配制成质量浓度为2％的溶液，将琼脂用纯净水配制成质量浓度为1％的溶液，将羟乙基纤维素用纯净水配制成质量浓度为1％的溶液，将透明质酸钠用纯净水配制成质量浓度为1％的溶液；
2、将步骤1)配制的溶液加热到60℃后，混合四种溶液并保温，备用；
3、将上表中B原料混合均匀；
4、将上表中C原料碾磨混合，并混合入步骤3混合后的B原料中，搅拌均匀；
5、将D原料混合加入到步骤4混合后的料中，得到混合原料；
6、将步骤5混合原料加热到75℃，并加入步骤2混合后的溶液中，进行均质，并保持混合物的温度为60～70℃，得均质物备用；
7、将步骤6均质保温后的均质物用泵输出并滴加到斜面上，所述斜面上流淌有质量浓度为2％的氯化钙溶液，得到粉色玫瑰美白功效的片状微胶囊。
实施例5：
一种含有清凉薄荷配方的片状微胶囊，所述成分如下表所示：
  成分 重量份
A1 海藻酸钠 30
A2 结冷胶 40
A3 聚乙烯醇 5
A4 羧甲基纤维素钠 5
B1 薄荷醇 5
B2 乳酸薄荷酯 5
B3 薄荷油 0.5
B4 荷荷巴油 5
B5 维生素E 1
B6 蔗糖硬脂酸酯 2
B7 十二烷基苯磺酸钠 0.3
C1 铬绿CI77289 0.3
D1 乙基己基甘油 0.1
D2 1,2辛二醇 0.6
本实施例片状微胶囊采用如下方法制备：
1、配制质量浓度为2％的海藻酸钠溶液，质量浓度为1％的结冷胶溶液，质量浓度为0.5％的聚乙烯醇溶液和质量浓度为1％的羟甲基纤维素钠溶液；
2、将步骤1配制的溶液加热到60℃后混合，保温备用；
3、将上表中B原料均匀混合并加热到60℃；
4、将C原料碾磨混合，并混合入步骤3混合后的B原料中，搅拌均匀；
5、将D原料混合加入到步骤4混合后的料中，得到混合原料；
6、将步骤5混合原料加热到60℃，加入步骤2混合后的溶液中，进行均质，并保持混合物的温度为60～70℃，得均质物备用；
7、将步骤6均质保温后的均质物用泵输出并滴加到斜面上，所述斜面上流淌有质量浓度为2％的氯化钙溶液，得到含有清凉薄荷配方的片状微胶囊。
最后说明的是，以上实施例仅用以说明本发明的技术方案而非限制，尽管申请人参照较佳实施例对本发明进行了详细说明，本领域的普通技术人员应当理解，对本发明的技术方案进行修改或者等同替换，而不脱离本发明技术方案的宗旨和范围的，均应涵盖在本发明的权利要求范围当中。

Claims (14)

  1. 一种片状微胶囊，其特征在于，外形为薄片状或条带状，所述薄片或条带状的厚度均小于宽度，厚度均为0.01～1mm；所述片状微胶囊囊壳的质量百分比，包括如下成分：海藻酸盐0.1-3％、热熔性凝胶0.1-3％、水溶性成膜材料0.1-5％和防腐剂0.1～1％；其余部分是水；
    片状微胶囊囊芯为其他活性成分和辅料。
  2. 一种片状微胶囊，其特征在于，所述片状微胶囊囊壳以重量份计，包括如下成分：30～50份海藻酸或海藻酸盐凝胶、20～40份热熔性凝胶、5～10份水溶性成膜材料和0.1～1份防腐剂。
  3. 根据权利要求1或2所述片状微胶囊，其特征在于，所述海藻酸盐包括海藻酸钠、海藻酸钾或海藻酸铵。
  4. 根据权利要求1或2所述片状微胶囊，其特征在于，所述热熔性凝胶是指其水溶液在高温是流动液态，在室温是固态和半固态的凝胶，包括可得燃胶、结冷胶、果胶、琼脂、卡拉胶、明胶、芦荟凝胶和魔芋胶中的一种或多种。
  5. 根据权利要求1或2所述片状微胶囊，其特征在于，所述水溶性成膜材料包括聚乙烯醇、羟丙基甲基纤维素、羟乙基纤维素、羧甲基纤维素、甲基纤维素、壳聚糖、卡波姆、聚丙烯酸钠、普鲁兰和透明质酸钠中的一种或多种。
  6. 根据权利要求1或2所述片状微胶囊，其特征在于，所述防腐剂包括乙基己基甘油、1,2辛二醇、1,2己二醇、苯氧乙醇、苯甲酸钠、苯钾酸钾、尼铂金甲酯、尼铂金丙酯、尼铂金丁酯和甲基异噻啉酮中的一种或多种。
  7. 根据权利要求1或2所述片状微胶囊，其特征在于，囊芯还包括颜料。
  8. 根据权利要求1或2所述片状微胶囊，其特征在于，还包括油溶性、水溶性或固体粉末态的活性成分，所述活性成分的质量份数为1-40％。
  9. 根据权利要求1或2所述片状微胶囊，其特征在于，囊芯还包括质量份数为1-20份的润肤剂。
  10. 根据权利要求2所述片状微胶囊，其特征在于，囊壳还包括0.01～1份有降低表面张力表面活性剂；所述表面活性剂为聚季铵盐-11、十二烷基苯磺酸钠、烷基硫酸钠、月桂酸基磺酸钠和聚山梨醇酯中的一种或多种。
  11. 一种片状微胶囊的制备方法，其特征在于，包括如下步骤：
    1)按照权利要求1～10任一所述片状微胶囊的成分配方换算称取原料，分别配制质量浓度为0.1～3％的海藻酸或海藻酸盐水溶液、质量浓度为0.1～3％的热熔性凝胶水溶液和质量浓度为0.1～5％的水溶性成膜材料水溶液，将三种水溶液分别加热至60～70℃后混合均匀，得到溶液A，将溶液A在60～70℃进行保温；
    2)将步骤1)称取原料中的其它原料在60～70℃混合均匀，得到混合物B；
    3)将步骤2)所述混合物B加热至60～80℃后，加入到步骤1)得到的溶液A中并进行均质，均质过程中保持温度为60～70℃，得到均质物C；
    4)使质量浓度0.5～3％的钙盐或镁盐溶液流淌到一端高一端低的线槽上，形成一个倾斜向下的钙盐或镁盐溶液斜面，将步骤3)得到的均质物C从所述线槽高的一端滴加到所述钙盐或镁盐溶液斜面上，制得所述片状微胶囊；其中，所述钙盐或镁盐溶液斜面的厚度为1-3mm，所述均质物C的滴加速率为5～100mL/min，所述钙盐或镁盐溶液的流速为300～2000mL/min。
  12. 根据权利要求11所述片状微胶囊的制备方法，其特征在于，所述线槽为直线形、Z形或螺旋形线槽。
  13. 根据权利要求11所述片状微胶囊的制备方法，其特征在于，所述线槽的倾斜角度为1～30°。
  14. 一种片状微胶囊的制备方法，其特征在于，包括如下步骤：
    1)按照权利要求1～10任一所述片状微胶囊的成分配方换算称取原料，分别配制质量浓度为0.1～3％的海藻酸或海藻酸盐水溶液、质量浓度为0.1～3％的热熔性凝胶水溶液和质量浓度为0.1～5％的水溶性成膜材料水溶液，将三种水溶液分别加热至60～70℃后混合均匀，得到溶液A，将溶液A在60～70℃进行保温；
    2)将步骤1)称取原料中的其它原料在60～70℃混合均匀，得到混合物B；
    3)将步骤2)所述混合物B加热至60～80℃后，加入到步骤1)得到的溶液A中并进行均质，均质过程中保持温度为60～70℃，得到均质物C；
    4)将步骤3)得到的均质物C滴加入质量浓度0.5～3％的钙盐或镁盐溶液中，同时使用搅拌装置对钙盐或镁盐溶液进行搅拌，制得所述片状微胶囊；其中，控制均质物C的滴加速率为5～100mL/min，搅拌速率为100～1000rpm/min。
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