CN104147950A - Porous membrane used for emulsification, preparation method and application thereof - Google Patents

Porous membrane used for emulsification, preparation method and application thereof Download PDF

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CN104147950A
CN104147950A CN 201410427440 CN201410427440A CN104147950A CN 104147950 A CN104147950 A CN 104147950A CN 201410427440 CN201410427440 CN 201410427440 CN 201410427440 A CN201410427440 A CN 201410427440A CN 104147950 A CN104147950 A CN 104147950A
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porous membrane
emulsification
membrane
porous
present invention
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CN 201410427440
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胡权
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胡权
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Abstract

The invention provides a porous membrane of which a material is perfluoro plastic. The porous membrane, which is prepared with the perfluoro plastic as a substrate, has a pore size controllable performance and can achieve a large pore size, thereby obtaining large-particle-size microspheres. A result in an embodiment in the invention proves that with a circular porous membrane as an emulsification membrane, polylactic acid microspheres of which an average particle size is 75 [mu]m can be obtained, and with a tubular porous membrane as an emulsification membrane, microshperes of which the average particle size is 115 [mu]m and particle sizes are uniform can be obtained. The porous membrane used for emulsification is obtained by forming penetrating holes in the substrate through a machining method with the perfluoro plastic as the substrate. A preparation method of the porous membrane is easy to carry out and is beneficial to large-scale industrial production.

Description

一种用于乳化的多孔膜、其制备方法及其应用 A porous membrane for emulsification, their preparation and their use

技术领域 FIELD

[0001] 本发明涉及膜乳化技术领域,尤其涉及一种用于乳化的多孔膜、其制备方法及其应用。 [0001] The present invention relates to a membrane emulsification technique, and more particularly relates to a porous membrane for emulsification, their preparation and their use.

背景技术 Background technique

[0002] 乳化是一种液体以微小液滴均匀地分散在互不相溶的另一种液体中的作用,是化学,化工,食品,医药,生化等领域的重要操作单元。 [0002] A liquid emulsion is uniformly dispersed in minute droplets in another role immiscible liquid is an important unit operation in the field of chemistry, chemical engineering, food, medicine, biochemistry and the like. 传统的乳化方式主要是通过机械搅拌,高速剪切等。 Traditional emulsion mainly through mechanical stirring, high speed shearing and the like. 这些传统的方法制备的乳滴粒径分布系数比较大,对于对粒径要求严格的产品,需要引进繁琐的后处理和额外的分离设备,同时也浪费了大量的原料。 Milk prepared using these conventional methods droplet size distribution coefficient of relatively large particle size for products demanding, complicated post-treatment is necessary to introduce additional separation apparatus and also waste a lot of raw material.

[0003] 膜乳化法是近十几年出现的制备均匀乳液的新方法,膜乳化过程用到的多孔膜上大量均匀孔可看作为微量分布器,膜两侧分别是分散相和连续相,膜内外压力差为传质推动力,分散相在压力作用下通过微孔后在另一侧的膜表面形成液滴并生长,长到一定大小时由于受到高速流动的连续相剪切力作用而剥离膜表面,从而形成水包油或油包水型乳液,也可制备复合型乳液。 [0003] The membrane emulsification method is a new method for preparing a homogeneous emulsion of the last ten years there, the porous membrane emulsification process a large number of uniform pore membranes can be used as a minor distributor to see both sides of the membrane are dispersed and continuous phases, pressure difference inside and outside the membrane mass transfer driving force, the dispersed phase droplets are formed by the pressure surface on the other side of the membrane pores and the growth, the length of a certain size due to the shear force of the continuous phase high flow the release film surface, thereby forming an oil in water or water-in-oil emulsions, multiple emulsions can also be prepared. 与传统方法相比,膜乳化方法操作简单、能耗低、表面活性剂用量少、乳液更均匀,因此在各行业都具有潜在的应用前景。 Compared with the conventional method, a membrane emulsification method is simple, low energy consumption, with a small amount of a surfactant, an emulsion is more uniform, so the industry has potential applications.

[0004]目前市场上采用膜乳化法制备均匀微球普遍采用的是SPG膜乳化技术。 [0004] Currently on the market using a film prepared by homogeneous emulsification microspheres are widely used SPG membrane emulsification technique. SPG膜是一种多孔玻璃膜,其典型孔径在0.1 μ m〜20μπι之间。 SPG membrane is a porous glass membrane pore size is typically between 0.1 μ m~20μπι. 其工作原理是采用亲水性的微孔玻璃膜,将油相通过尺寸均匀的膜压入水相,得到尺寸均匀的液滴。 Its working principle is a microporous membrane using the glass hydrophilic phase pressure oil into the water phase by a uniform size of the membrane, to obtain a uniform droplet size. 乳化过程中是利用油相和亲水膜之间的界面张力,使得油相在膜的开口处成长为一个液滴,当界面张力,膜乳化压力,连续相的拽力等达到平衡时,液滴脱落下来。 Emulsification process using the interfacial tension between the oil phase and the hydrophilic membrane such that the membrane at the opening of the oil phase to grow as a droplet, when the interfacial tension, membrane emulsification pressure, the drag force of the continuous phase equilibrium, liquid drops falling down.

[0005] 而目前市场上SPG膜乳化器采用的SPG膜,其典型的孔径一般小于20 μ m,在制备大尺寸的微球上也会存在一些限制。 [0005] The current market film SPG SPG membrane emulsifier employed, the typical pore size is typically less than 20 μ m, also there are some limitations on the preparation of a large-sized microspheres. 比如,目前市场上销售的利培酮微球其平均粒径在90 μ m,采用普通的SPG膜乳化就很难实现。 For example, currently on the market Risperidone microspheres having an average particle size of 90 μ m, the ordinary SPG membrane emulsification is difficult to achieve.

发明内容 SUMMARY

[0006] 本发明的目的在于提供一种用于乳化的多孔膜、其制备方法及其应用,本发明提供的多孔膜孔径具有良好的可调性,从而得到较大粒径的微球。 [0006] The object of the present invention is to provide a porous membrane for emulsification, their preparation and their use, the present invention provides a porous membrane having a pore size of good adjustability, thereby obtaining a larger particle size of the microspheres.

[0007] 本发明提供了一种用于乳化的多孔膜,所述多孔膜的材质为全氟塑料。 [0007] The present invention provides a porous membrane for emulsification, the material of the porous membrane is perfluorinated plastics.

[0008] 优选的,所述多孔膜的材质为聚四氟乙烯、全氟(乙烯丙烯)共聚物、聚全氟烷氧基树脂。 [0008] Preferably, the porous membrane made of polytetrafluoroethylene, perfluoro (ethylene-propylene) copolymer, poly perfluoroalkoxy resin.

[0009] 优选的,所述多孔膜的厚度为0.1mm〜3mm。 [0009] Preferably, the thickness of the porous membrane is 0.1mm~3mm.

[0010] 优选的,所述多孔膜的表面为亲水型。 [0010] Preferably, the surface of the porous membrane is hydrophilic.

[0011] 本发明提供了一种用于乳化的多孔膜的制备方法,包括: [0011] The present invention provides a method of preparing a porous membrane for emulsification, comprising:

[0012] 以全氟塑料为基体,采用机械加工的方法,在所述基体上打多个贯穿孔,得到用于乳化的多孔膜。 [0012] In the porous membrane is a perfluorinated plastic matrix, machining method, a plurality of through-holes in play on the substrate, obtained for emulsification.

[0013] 优选的,所述机械加工的方法为钻孔或激光打孔。 [0013] Preferably, the method of machining or laser drilling of the borehole.

[0014] 优选的,所述在所述基体上打多个贯穿孔后还包括: After [0014] Preferably, the plurality of through-holes in play on the substrate further comprises:

[0015] 对打贯穿孔后的基体进行表面亲水改性处理。 [0015] rally the base through-hole surface after hydrophilic modification treatment.

[0016] 优选的,所述表面亲水改性处理为萘钠化学处理、氨钠法处理、联苯钠法处理,高温熔融法处理、辐射法处理或等离子体处理。 [0016] Preferably, the hydrophilic surface modification treatment is a chemical treatment sodium naphthalene, sodium Treatment ammonia, sodium biphenyl processing method, high temperature melting or plasma treatment processing method, radiation method.

[0017] 本发明提供了上述技术方案所述多孔膜或上述技术方案所述制备方法得到的多孔膜在膜乳化中的应用。 [0017] The present invention provides the use of the above aspect of the porous membrane or porous film above technical solutions obtained in the production method of the membrane emulsification.

[0018] 优选的,所述膜乳化的过程为: [0018] Preferably, the membrane emulsification process is:

[0019] 将分散相和连续相置于所述多孔膜的两侧,所述连续相相对所述多孔膜匀速运动,所述分散相通过所述多孔膜上的孔进入所述连续水相,完成乳化。 [0019] The dispersed and continuous phases disposed on both sides of the porous membrane, said porous membrane relative to the continuous phase of uniform motion, the dispersed phase through the pores of said porous film into the continuous aqueous phase, complete emulsification.

[0020] 本发明提供的多孔膜的材质为全氟塑料,以全氟塑料为基体制备得到的多孔膜,孔径可调性,且能够得到较大的孔径,从而得到较大粒径的微球。 [0020] The material of the porous film of the present invention provides perfluoro plastic, perfluoro plastic substrate is a porous membrane preparation obtained pore size adjustability and larger pore size can be obtained, resulting in a larger particle size of the microspheres . 本发明实施例结果表明,以圆形多孔膜为乳化膜,得到平均粒径为75μπι的聚乳酸微球;以管状多孔膜为乳化膜,得到平均粒径为115 μ m、粒径均匀的微球。 The results show that the embodiments of the invention, the porous membrane is a circular membrane emulsification, an average particle size of polylactic acid microspheres 75μπι; porous membrane is a tubular membrane emulsification, to give an average particle diameter of 115 μ m, a uniform particle size Micro ball. 本发明以全氟塑料为基体,采用机械加工的方法在所述基体上打上贯穿孔,得到用于乳化的多孔膜。 The method of the present invention is a perfluoro plastic substrate, by machining a through-hole marked on the base body to obtain a porous film is used for emulsification. 本发明提供的多孔膜的制备方法简单、易操作,有利于大规模工业生产。 The method of preparing a porous film of the present invention provides a simple, easy to operate, is conducive to large-scale industrial production.

[0021] 而且,本发明采用全氟塑料为基体,形状可调,本领域技术人员可根据需要制备不同形状的多孔膜,如平板状、管状或其他特定形状的多孔膜,利于工业生产的需要。 [0021] Further, the present invention uses perfluorinated plastic as a matrix, a shape control, those skilled in the art according to a porous film is desired to prepare a different shape, such as a porous membrane flat, tubular, or other specific shapes, facilitate the needs of industrial production .

附图说明 BRIEF DESCRIPTION

[0022] 图1为本发明实施例1得到的亲水型圆形平面多孔膜结构示意图; [0022] Fig 1 a schematic view of a circular planar structure of hydrophilic porous membrane obtained in Example 1 of the embodiment of the present invention;

[0023] 图2为本发明实施例3得到的管状多孔膜结构示意图; [0023] FIG. 2 is a schematic structure of the tubular porous membrane obtained in Example 3 of the embodiment of the present invention;

[0024] 图3为本发明实施例2采用的圆形多孔膜乳化装置结构示意图; [0024] FIG. 3 is a schematic structure of a circular porous membrane emulsifying apparatus employed in Example 2 of the present embodiment of the invention;

[0025] 图4为本发明实施例4采用的管状多孔膜乳化装置结构示意图。 [0025] FIG. 4 is a schematic structure of the tubular porous membrane emulsifying apparatus used in Example 4 of the present invention.

具体实施方式 detailed description

[0026] 本发明提供了一种用于乳化的多孔膜,所述多孔膜的材质为全氟塑料。 [0026] The present invention provides for a porous membrane emulsification, the porous membrane made of perfluorinated plastics.

[0027] 本发明提供的多孔膜的材质为全氟塑料,以全氟塑料为基体制备得到的多孔膜,孔径可调性,能够得到较大孔径的全氟塑料,从而得到较大粒径的微球;而且,本发明采用全氟塑料为基体,形状可调,本领域技术人员可根据需要制备不同形状的多孔膜,如平板状、管状或其他特定形状的多孔膜,利于工业生产的需要;再者,与传统的多孔玻璃(SPG)膜相比,本发明提供的用于乳化的多孔膜具有更低的制造成本。 [0027] The material of the porous film of the present invention provides perfluoro plastic, perfluoro plastic substrate is a porous membrane preparation obtained adjustable aperture, perfluoro plastic can be obtained a larger pore size, to give a larger particle size microspheres; Furthermore, the present invention uses perfluorinated plastic as a matrix, a shape control, those skilled in the art according to a porous film is desired to prepare a different shape, such as a porous membrane flat, tubular, or other specific shapes, industrially advantageous production needs ; Furthermore, compared with the conventional porous glass (SPG) membrane, a porous membrane of the present invention provides for emulsification with lower manufacturing costs.

[0028] 本发明提供的多孔膜的材质为全氟塑料,优选为聚四氟乙烯、全氟(乙烯丙烯)共聚物、聚全氟烷氧基树脂,更优选为聚四氟乙烯。 [0028] The material of the porous film of the present invention provides perfluoro plastic, preferably polytetrafluoroethylene, perfluoro (ethylene-propylene) copolymer, poly perfluoroalkoxy resin, and more preferably polytetrafluoroethylene. 本发明对所述全氟塑料的来源没有特殊的限制,采用本领域技术人员熟知的上述全氟塑料的市售商品即可; The present invention is not particularly limited to the source of perfluorinated plastic, use of commercially available well known to those skilled in the perfluoroplastic;

[0029] 本发明对所述多孔膜的厚度没有特殊的限制,本领域技术人员可根据现有技术中膜乳化技术用到的多孔膜的厚度,设定本发明提供的用于乳化的多孔膜的厚度。 [0029] The present invention is not particularly limited to the thickness of the porous film, those skilled in the thickness of the porous film according to the prior art membrane emulsification technique used, the present invention provides a porous film is set for emulsification thickness of. 如在本发明中,所述多孔膜的厚度优选为0.1mm〜3mm,更优选为0.5mm〜2.5mm ;在具体实施例中,所述多孔膜的厚度可具体为0.5mm、1.0mm、1.5mm或2mm ; As in the present invention, the thickness of the porous film is preferably 0.1mm~3mm, more preferably 0.5mm~2.5mm; In a particular embodiment, the thickness of the porous membrane may be embodied as a 0.5mm, 1.0mm, 1.5 mm or 2mm;

[0030] 本发明对所述多孔膜的形状没有特殊的限制,本领域技术人员可根据需要将全氟塑料基体裁剪为不同的形状,从而得到具有不同形状的多孔膜。 [0030] The present invention is not the shape of the porous film particularly limited, those skilled in the art may be a different shape according to need perfluorinated plastic substrate cut to obtain a porous film having a different shape. 如在本发明中,所述多孔膜的形状可以为平面圆形,也可以为管状;具体的,当所述多孔膜为管状多孔膜时,所述孔分布在管状全氟塑料纵剖面的一侧。 As in the present invention, the shape of the porous membrane may be a flat circular shape, it may be tubular; Specifically, when the porous membrane is a tubular porous membrane, the pore distribution in a longitudinal section of the tubular plastic perfluoro a side.

[0031] 本发明对所述多孔膜中孔的孔径没有特殊的限定,本领域技术人员可以根据需要设定合适孔径的多孔膜,如所述多孔膜的孔径可以小于100 μ m,也可以大于等于100 μ m ;在本发明的实施例中,所述多孔膜的孔径可以为ΙΟΟμπι,也可以为150μπι,从而得到较大粒径的微球; [0031] The present invention is not particularly limited, the pore diameter of pores in the porous membrane, those skilled in the art can set an appropriate pore size needs a porous membrane, the porous membrane as pore size may be less than 100 μ m, may be larger than equal to 100 μ m; in an embodiment of the present invention, the pore size of the porous membrane may ΙΟΟμπι, may also 150μπι, to obtain larger particle size of the microspheres;

[0032] 在本发明中,所述多孔膜中的孔可以为无规则分布,也可以为规则分布,如可以为阵列分布,本发明对所述孔的分布方式没有特殊的限定,能够实现膜乳化中即可。 [0032] In the present invention, the porous membrane pores may be distributed as a random, may be a regular distribution, as can be distributed in an array, the present invention is not particularly limited to the manner of distribution holes, the film can be achieved emulsification can be. 在本发明中,所述孔在多孔膜中优选为圆形阵列分布或矩形阵列分布。 In the present invention, the array of apertures is preferably circular or rectangular profile arrayed in the porous membrane. 具体的,当所述多孔膜的形状为平面圆形时,所述多孔膜上的孔可以呈圆形矩阵分布;当所述多孔膜的形状为管状时,所述多孔膜上的孔可以呈矩形阵列分布。 Specifically, when the shape of the porous membrane is a flat circle, pores of the porous membrane may be circular distribution matrix; shape of the porous membrane is tubular, pores of the porous membrane may be in when distribution of a rectangular array.

[0033] 本领域技术人员还可以根据需要,调整孔径和相邻孔间距,从而得到合适尺寸的微球,如孔径为ΙΟΟμπι、相邻孔间距为800 μ m的多孔膜,能够得到平均粒径为75 μ m的微球;再如,孔径为150μπκ相邻孔间距为Imm的多孔膜,可得到平均粒径为115μπι的微球。 [0033] Those skilled in the art may also be required, to adjust the pore diameter and spacing of adjacent apertures, resulting in microspheres of appropriate size, such as pore size ΙΟΟμπι, a porous membrane adjacent hole pitch of 800 μ m, the average particle size can be obtained 75 μ m for the microsphere; another example, the pore size of the porous membrane 150μπκ Imm spacing of adjacent apertures, having an average particle diameter of the microspheres 115μπι.

[0034] 在本发明中,全氟塑料为疏水型,直接打孔得到的多孔膜表面为疏水型,所述疏水型的多孔膜可直接用于油包水体系的制备;本发明对所述疏水型多孔膜制备油包水体系的方法没有特殊的限制,采用本领域技术人员熟知的膜乳化领域油包水体系制备的技术方案即可。 [0034] In the present invention, perfluorinated plastics hydrophobic porous membrane surface is obtained directly perforated hydrophobic, the hydrophobic porous membrane may be used directly for the preparation of water-in-oil systems; the present invention the method of preparation of a hydrophobic porous membrane water in oil system is not particularly limited, and use is well known to those skilled in the art emulsified oil film prepared technical solution to the aqueous system. 为了得到水包油体系,本发明优选提供一种表面亲水型的多孔膜。 In order to obtain oil in water systems, preferably the present invention provides a surface of the hydrophilic porous membrane. 在本发明中,所述表面亲水型的多孔膜优选由全氟塑料多孔膜进行表面亲水改性处理制得。 In the present invention, the surface of the hydrophilic porous membrane is preferably subjected to a surface modification treatment to obtain the hydrophilic perfluorinated plastic porous membrane. 本发明对所述表面亲水改性处理的方法没有特殊的限制,采用本领域技术人员熟知的表面亲水改性的技术方案即可。 The present invention is not particularly limited to the method of the hydrophilic surface modification treatment, the technical solution to the hydrophilic surface-modified to those skilled in the art. 在本发明中,所述表面亲水改性处理优选为萘钠化学处理、氨钠法处理、联苯钠法处理,高温熔融法处理、辐射法处理或等离子体处理,更优选为萘钠化学处理。 In the present invention, the hydrophilic surface modification treatment is preferably a chemical treatment, sodium naphthalene, sodium Treatment ammonia, sodium biphenyl processing method, a high temperature melt processing method, radiation treatment or a plasma treatment, more preferably sodium naphthalene Chemicals deal with.

[0035] 本发明优选将所述打孔后的全氟塑料多孔膜浸入萘钠溶液中,静置,得到表面亲水型的多孔膜。 [0035] The present invention is preferably a porous perfluorinated plastic film after immersing the punctured sodium naphthalene solution was allowed to stand to obtain a surface of the hydrophilic porous membrane. 在本发明中,所述萘钠溶液的摩尔浓度优选为0.lmol/L〜2mol/L,更优选为0.4mol/L〜0.7mol/L,最优选为0.5mol/L〜0.6mol/L ;在本发明中,本领域技术人员可根据表面亲水改性处理的需要,设定合适的静置时间,可以静置过夜,也可以静置几分钟;在本发明的具体实施方式中,所述静置的时间优选为2min〜15min,更优选为3min〜5min,最优选为3min〜4min ;本发明对所述静置的温度没有特殊的限制,无需对静置的体系进行加热或冷却,在室温中进行即可。 In the present invention, the molar naphthalene solution of sodium concentration is preferably 0.lmol / L~2mol / L, and more preferably 0.4mol / L~0.7mol / L, and most preferably 0.5mol / L~0.6mol / L ; in the present invention, one skilled in the art according to the needs hydrophilic surface modification treatment, to set an appropriate resting time, allowed to stand overnight, may stand a few minutes; in a specific embodiment of the present invention, the standing time is preferably 2min~15min, more preferably 3min~5min, and most preferably 3min~4min; the present invention is not particularly limited in the temperature of the was allowed to stand, without standing on the heating or cooling system, , can be performed at room temperature.

[0036] 完成所述静置后,本发明优选将所述静置后的全氟塑料多孔膜进行清洗,得到表面亲水型多孔膜。 [0036] After the completion of the standing, the present invention is preferably whole fluoroplastic porous film was allowed to stand after the washing, to obtain a porous hydrophilic membrane surface. 本发明对所述清洗的方法没有特殊的限制,采用本领域技术人员熟知的、上述亲水处理后的清洗的技术方案即可。 The present invention is not particularly limited to the method of cleaning using well known to the skilled person, the above-described hydrophilic treatment aspect can be cleaned. 本发明优选将所述静置后的全氟塑料多孔膜依次进行丙酮清洗和无水乙醇清洗,得到亲水型多孔膜。 The present invention preferably perfluorinated plastic porous membrane after the washing with acetone and allowed to stand sequentially washed ethanol to obtain a hydrophilic porous membrane.

[0037] 本发明提供了一种用于乳化的多孔膜的制备方法,包括: [0037] The present invention provides a method of preparing a porous membrane for emulsification, comprising:

[0038] 以全氟塑料为基体,采用机械加工的方法,在所述基体上打多个贯穿孔,得到用于乳化的多孔膜。 [0038] In the porous membrane is a perfluorinated plastic matrix, machining method, a plurality of through-holes in play on the substrate, obtained for emulsification.

[0039] 本发明提供的方法以全氟塑料为基体,采用机械加工的方法,在所述基体上打多个贯穿孔,得到用于乳化的多孔膜。 [0039] The method of the present invention provides a porous film of perfluorinated plastic matrix, machining method, a plurality of through-holes in play on the substrate, obtained for emulsification. 本发明提供的方法简单,易于操作,利于大规模工业化生产。 The present invention provides a simple, easy to operate, conducive to large-scale industrial production. 在本发明中,所述机械加工的方法优选为钻孔或激光打孔,本领域机械人员可按照需要的孔径,采用钻孔或机械打孔的方法,在全氟塑料基体上打多个贯穿孔。 In the present invention, the method is preferably machined drilling or laser drilling, mechanical skilled in the art in accordance with desired pore size, a method of drilling or mechanical drilling, through playing on a plurality of perfluorinated plastic base hole. 本发明对所述钻孔或激光打孔的方法没有特殊的限制,采用本领域技术人员熟知的钻孔或激光打孔的技术方案即可。 The present invention is not particularly limited to the method of drilling or laser drilling, laser drilling or using well known to those skilled in the art technical solutions can be punctured.

[0040] 在本发明中,所述全氟塑料的来源、厚度、形状等参数与上述技术方案所述用于乳化的多孔膜方案中全氟塑料的来源、种类和形状等参数一致;所述多孔膜上贯穿孔的分布、孔径、相邻孔间距等参数与上述技术方案所述用于乳化的多孔膜方案中多孔膜上的孔分布、孔径和相邻孔间距等参数一致,在此不再赘述。 [0040] In the present invention, the same source of perfluorinated plastic, the type and shape of the source program parameters porous film of perfluorinated plastic, thickness, shape and other parameters of the above technical solutions for emulsification; and the the porous membrane through hole distribution, pore size, pore spacing porous membrane program parameters for the above technical solutions emulsifiable adjacent pore distribution of the porous film, pore size and spacing adjacent apertures same parameters, which is not then repeat.

[0041] 完成所述打孔后,得到的用于乳化的多孔膜表面为疏水型,可采用膜乳化技术,直接用来制备油包水体系。 [0041] After completion of the punching, the obtained porous membrane surface is used for emulsification of the hydrophobic, membrane emulsification techniques may be used directly for the preparation of water in oil system. 为了能够制备水包油体系,需要将打孔后得到的多孔膜进行表面亲水处理改性,得到表面亲水型多孔膜。 For systems capable of producing oil in water, the porous membrane needs to be punctured obtained after hydrophilic treatment of the surface modified, hydrophilic surface to obtain a porous film. 在本发明中,所述表面亲水型多孔膜的制备方法优选与上述技术方案所述表面亲水型多孔膜的制备方法一致,在此不再赘述。 In the present invention, the preferred method of preparing the surface of the hydrophilic porous membrane preparation uniform surface of the hydrophilic porous membrane and the above technical solutions, not described herein again.

[0042] 本发明上述技术方案所述的多孔膜或上述技术方案所述的制备方法得到的多孔膜,能够用于膜乳化技术领域,制备得到乳化体系,如乳液、微球或微囊等。 [0042] The porous film of the present invention, the above-described aspect of the production method of the porous film, or obtained according to the above aspect, the field can be used for membrane emulsification techniques, prepared by emulsifying system, such as an emulsion, microspheres, microcapsules, or the like. 本发明还提供了一种上述技术方案所述多孔膜或上述技术方案所述的制备方法得到的多孔膜在膜乳化中的应用。 The present invention also provides the use of porous film production method of the above aspect of the porous film or the above technical solutions obtained in the membrane emulsification. 在本发明中,所述膜乳化的过程优选具体为: In the present invention, the membrane emulsification process is preferred:

[0043] 将分散相和连续相置于所述多孔膜的两侧,所述连续相相对所述多孔膜匀速运动,所述分散相通过所述多孔膜上的孔进入所述连续水相,完成乳化。 [0043] The dispersed and continuous phases disposed on both sides of the porous membrane, said porous membrane relative to the continuous phase of uniform motion, the dispersed phase through the pores of said porous film into the continuous aqueous phase, complete emulsification.

[0044] 本发明对所述膜乳化的过程采用的膜乳化装置没有特殊的限制,采用本领域技术人员熟知的膜乳化装置即可,本领域技术人员可根据多孔膜的形状,选择合适的膜乳化装置。 [0044] The film of the present invention the emulsifying device emulsification process using a membrane is not particularly limited, and use of membrane emulsification device can be well known to those skilled in this art in the art according to the shape of the porous membrane may be choose suitable membrane emulsifying device. 如当所述多孔膜为平面圆形时,本发明可采用如图3所示的圆形多孔膜乳化装置,图3中,I为多孔膜,2为注射泵、3为磁力搅拌子、4为液体容器。 The circular porous membrane emulsification device when the porous membrane is a circular plane, the present invention is shown in Figure 3 may be employed, in FIG. 3, I is a porous membrane, 2 denotes a syringe pump, 3 is a magnetic stirrer, 4 a liquid container. 在所述液体容器4中盛放有连续相,在磁力搅拌子3的搅拌下,所述连续相在所述烧杯中做匀速运动;将分散相置于注射泵2中,将注射泵2中的分散相通过多孔膜推入到匀速运动的连续相中,分散相在孔的开口处形成液滴并不断长大,当液滴长到一定的程度,在连续相的拖拽下,脱离所述多孔膜进入连续水相,完成所述乳化过程。 In the liquid accommodating container 4 has a continuous phase, under stirring in a magnetic stirrer 3, the continuous phase made uniform motion in the beaker; dispersed phase 2 was placed in the syringe pump, the syringe pump 2 dispersed phase through the porous membrane is pushed into the continuous phase of uniform motion, the dispersed phase droplets are formed at the opening of the hole and continue to grow, when droplets grow to a certain extent, in the continuous phase of the drag, departing from said porous film into the continuous aqueous phase, to complete the emulsification.

[0045] 再如,当所述多孔膜为管状时,本发明可采用如图4所示的管状多孔膜乳化装置进行乳化,图4中,I为管状多孔膜,2为循环泵,3为注射泵,4为液体容器,所述液体容器侧壁开口,所述液体容器下端开有漏斗状开口,所述侧壁的开口、漏斗状开口和循环泵通过管道相连通;所述漏斗状开口与所述管状多孔膜的出口相连,所述注射泵与所述管状多孔膜上的孔相连。 [0045] As another example, when the porous membrane is tubular, the present invention may employ a tubular porous membrane emulsification apparatus shown in FIG emulsified in FIG. 4, I tubular porous membrane, the circulation pump 2, 3 injection pump, 4 is the liquid container, the liquid container side wall opening, the lower end opening of the liquid container is a funnel-shaped opening, said side wall opening, a funnel-shaped opening and a circulation pump through a conduit in communication; the funnel-shaped opening and an outlet connected to said tubular porous membrane, the injection pump is connected with the bore of the tubular porous membrane. 注射泵中盛有分散相,液体容器中盛有连续水相,开启循环泵和注射泵,将分散相通过多孔膜挤入连续水相中,挤压完成后停止循环泵和注射泵,得到乳液;为了得到微球,本发明还可以将所述乳液转移到另一容器中,搅拌直至溶剂挥发完全,得到粒径均匀的微球。 Syringe pump filled with a dispersed phase liquid container filled with a continuous aqueous phase, the circulating pump and the injection pump, the disperse phase extruded into the continuous aqueous phase through the porous membrane, the circulation pump is stopped and the injection pump after completion of the extrusion, to give an emulsion ; in order to obtain microspheres of the present invention may also be the emulsion was transferred to another vessel and stirred until complete evaporation of the solvent, to obtain a uniform microsphere size.

[0046] 在本发明中,所述微球的粒径受到多孔膜的孔径、相邻孔间距和连续相相对多孔膜的速度的影响,一般而言,大尺寸的微孔适合制备尺寸比较大的微球,而小尺寸的微孔适合制备尺寸较小的微球;而对于微孔的间距,过大的间距会导致微球制备效率变慢,而孔过于密集可能会导致在膜表面形成的液滴相互接触或碰撞而聚集,液滴变得不均匀。 [0046] In the present invention, the particle size of the microspheres by the pore size of the porous membrane, the hole spacing and the continuous phase relative impact velocity adjacent porous membrane, in general, large pore size suitable for producing large microspheres, and small pore size for smaller size microspheres prepared; and the spacing of micropores, too large distance will lead to slower microsphere preparation efficiency, but may result in too dense holes formed in the film surface the droplets collide with each other or in contact with gathered, liquid droplets becomes uneven. 本领域技术人员可根据现有技术中膜乳化技术中,膜孔径、相邻孔间距和连续相相对多孔膜的速度之间的关系,对本发明中多孔膜的孔径和相连孔间距,以及连续相相对多孔膜的速度进行调整,从而获得所需最优的效果。 Those skilled in the art according to the prior art, membrane emulsification technique, membrane pore size, the relationship between the hole pitch and a continuous phase of the relative speed of the adjacent porous membrane, pore size of the porous membrane of the present invention and connected to the hole spacing, and a continuous phase speed is relatively porous film were adjusted to achieve the desired optimal effect.

[0047] 本发明提供的多孔膜的材质为全氟塑料,以全氟塑料为基体制备得到的多孔膜,孔径可调性,能够得到较大孔径的全氟塑料,从而得到较大粒径的微球。 [0047] The material of the porous film of the present invention provides perfluoro plastic, perfluoro plastic substrate is a porous membrane preparation obtained adjustable aperture, perfluoro plastic can be obtained a larger pore size, to give a larger particle size Microspheres. 本发明实施例结果表明,以圆形多孔膜为乳化膜,得到平均粒径为75 μ m的聚乳酸微球;以管状多孔膜为乳化膜,得到平均粒径为115 μ m、粒径均匀的微球。 The results show that the embodiments of the invention, the porous membrane is a circular membrane emulsification, to give an average particle diameter of 75 μ m polylactic acid microspheres; porous membrane is a tubular membrane emulsification, to give an average particle diameter of 115 μ m, a uniform particle size the microspheres. 本发明以全氟塑料为基体,采用机械加工的方法在所述基体上打上贯穿孔,得到用于乳化的多孔膜。 The method of the present invention is a perfluoro plastic substrate, by machining a through-hole marked on the base body to obtain a porous film is used for emulsification. 本发明提供的多孔膜的制备方法简单、易操作,有利于大规模工业生产。 The method of preparing a porous film of the present invention provides a simple, easy to operate, is conducive to large-scale industrial production.

[0048] 而且,本发明采用全氟塑料为基体,形状可调,本领域技术人员可根据需要制备不同形状的多孔膜,如平板状、管状或其他特定形状的多孔膜,利于工业生产的需要。 [0048] Further, the present invention uses perfluorinated plastic as a matrix, a shape control, those skilled in the art according to a porous film is desired to prepare a different shape, such as a porous membrane flat, tubular, or other specific shapes, facilitate the needs of industrial production .

[0049] 为了进一步说明本发明,下面结合实施例对本发明提供的用于乳化的多孔膜、其制备方法及其应用进行详细地描述,但不能将它们理解为对本发明保护范围的限定。 [0049] In order to further illustrate the present invention, the following embodiments in conjunction with the porous membrane of the embodiment of the present invention provides for emulsification, their preparation and their use are described in detail, but they should not be construed as limiting the scope of the present invention.

[0050] 实施例1 [0050] Example 1

[0051] 采用直径为25mm圆形聚四氟乙烯平板膜为基体,该平板膜的厚度为0.5mm,在所述基体上钻上贯穿孔采用直径0.1mm的钻孔,相邻钻孔间距0.8mm。 [0051] with a diameter of 25mm circular polytetrafluoroethylene film is a flat substrate, the thickness of the plate film is 0.5mm, the through hole using the drill hole diameter of 0.1mm on the substrate, adjacent to the distance between holes 0.8 mm. 孔围绕中心环形排列,将钻孔加工后获得的多孔圆片使用浸入0.5M的萘钠溶液中室温下处理4分钟,依次使用丙酮,无水乙醇清洗干净,获得表面亲水型圆形平面多孔膜。 A circular arrangement around a central hole, a porous disc after drilling obtained using an immersion for 4 minutes at room temperature a 0.5M solution of sodium naphthalene, successively using acetone, ethanol clean, hydrophilic surface to obtain a circular planar porous membrane.

[0052] 本实施例得到的亲水型圆形平面多孔膜的结构如图1所示,图1为本发明实施例1制备得到的亲水型圆形平面多孔膜的结构示意图,本实施例得到的亲水型圆形平面多孔膜上的孔孔径一致,相邻孔间距一致,呈圆形阵列分布。 [0052] The planar circular configuration hydrophilic porous membrane obtained in Example 1 of the present embodiment, FIG. 1 is a schematic structure of the porous hydrophilic membrane of Example 1 was prepared in the circular plane of the embodiment of the present invention, the present embodiment circular holes obtained hydrophilic porous membrane of the same aperture plane adjacent the hole spacing consistent, circular array of distribution.

[0053] 实施例2 [0053] Example 2

[0054] 将Ig聚乳酸溶解在1mL的三氯甲烷中,得到分散油相,将4g聚乙烯醇溶解在200mL去离子水,得到连续水相。 [0054] The Ig is dissolved in 1mL of polylactic acid in chloroform, to give the dispersed oil phase, 4g of polyvinyl alcohol was dissolved in 200mL of deionized water to obtain a continuous aqueous phase. 采用实施例1制备表面亲水型圆形平面多孔膜,采用图3的装置进行膜乳化过程,将连续水相置于液体容器4中,液体容器底部放有磁力搅拌子3,搅拌速度设定为400rpm ;将分散油相置于注射泵2中,通过注射泵按照lmL/min的速度推动注射器中的油相通过多孔膜,推进完成后,降低搅拌速度到10rpm,继续搅拌干燥后获得平均粒径75微米的聚乳酸微球。 Example 1 was prepared using a circular planar surface of a porous hydrophilic membrane embodiment, using the apparatus of FIG. 3 is membrane emulsification, the continuous aqueous phase was placed in the liquid container 4, the bottom of the liquid container 3 placed a magnetic stirrer, the stirring speed set is of 400 rpm; the dispersed oil phase is placed in a syringe pump 2, a syringe pushing the oil phase through the porous membrane, to promote the complete, to reduce the speed of 10 rpm stirring, to obtain an average particle after drying continued stirring at the speed lmL / min by syringe pump 75 micron diameter microspheres of polylactic acid.

[0055] 实施例3 [0055] Example 3

[0056] 采用外径为8mm、内径为6mm的聚四氟乙烯管为基体,在聚四氟乙烯管纵剖面一侧的管壁上打孔径为0.15mm微孔,相邻微孔间距为1mm,数量504个,呈矩形矩阵分布。 [0056] The outer diameter of 8mm, an inner diameter of 6mm polytetrafluoroethylene tube matrix, play an aperture in the wall of the tube on one side of a longitudinal section of a microporous polytetrafluoroethylene 0.15mm, 1mm spacing adjacent micropores , number 504, a rectangular matrix distribution. 将获得多孔管浸入摩尔浓度为0.5mol/L的萘钠溶液中室温下处理3分钟,依次使用丙酮、无水乙醇清洗干净,获得表面亲水型管状多孔膜。 The obtained porous tube was immersed in treatment at a molar concentration of 0.5mol / L sodium naphthalene solution at room temperature for 3 minutes successively using acetone, ethanol clean, hydrophilic surface of the tubular to obtain a porous film.

[0057] 本实施例得到的亲水型圆形平面多孔膜的结构如图2所示,图2为本发明实施例3制备得到的表面亲水型管状多孔膜的结构示意图,本实施例得到的表面亲水型管状多孔膜上的孔孔径一致,相邻孔间距一致,呈矩形阵列分布。 [0057] The present circular plane configuration hydrophilic porous membrane obtained in Example 2 of the embodiment, FIG. 2 is a schematic structure of the surface of the tubular hydrophilic porous membrane obtained in Preparation Example 3 of the embodiment of the present invention obtained in this embodiment hydrophilic porous surface of the tubular porous membrane pore size consistent, uniform hole spacing of adjacent, rectangular array of distribution.

[0058] 实施例4 [0058] Example 4

[0059] 将Ig聚乳酸、5mg罗丹明溶解在1mL的三氯甲烷中,得到分散油相,将4g聚乙烯醇溶解在200mL去离子水中,得到连续水相。 [0059] The Ig polylactic acid, Rhodamine 5mg dissolved in 1mL chloroform to give the dispersed oil phase, 4g of polyvinyl alcohol was dissolved in 200mL of deionized water to give a continuous aqueous phase. 采用实施例3制备的表面亲水型管状多孔膜,采用图4所示的膜乳化装置进行膜乳化过程,将连续水相置于液体容器中,将分散油相置于注射泵中,开启循环泵,将油相以1.6mL/min的速度通过管状多孔膜挤入连续水相中,挤压完成,停止循环泵,将获得乳液转移到另外一个烧杯中,调节搅拌速度到lOOrpm,直到溶剂挥发完全。 Using hydrophilic surface of the tubular porous membrane prepared in Example 3, using membrane emulsification apparatus shown in FIG. 4 membrane emulsification, the continuous liquid aqueous phase was placed in a container, the dispersed oil phase is placed in a syringe pump, the circulating pump, the oil phase at a rate of 1.6mL / min is extruded through the tubular porous membrane continuous aqueous phase, completion of pressing, the circulation pump is stopped, the obtained emulsion was transferred to another beaker, the stirring speed was adjusted to lOOrpm, until the solvent is volatilized complete. 获得平均粒径在115微米的均匀微球。 To obtain a uniform microspheres of average particle size of 115 microns.

[0060] 由以上实施例可知,本发明提供的多孔膜的材质为全氟塑料,以全氟塑料为基体制备得到的多孔膜,孔径可调性,能够得到较大孔径的全氟塑料,从而得到较大粒径的微球。 [0060] From the above embodiment, the porous film material of the present invention provides perfluoro plastic, perfluoro plastic substrate is a porous membrane preparation obtained adjustable aperture, perfluoro plastic can be obtained a larger pore size, so that to give a larger particle size of the microspheres. 本发明实施例结果表明,以圆形多孔膜为乳化膜,得到平均粒径为75μπι的聚乳酸微球;以管状多孔膜为乳化膜,得到平均粒径为115 μ m、粒径均匀的微球。 The results show that the embodiments of the invention, the porous membrane is a circular membrane emulsification, an average particle size of polylactic acid microspheres 75μπι; porous membrane is a tubular membrane emulsification, to give an average particle diameter of 115 μ m, a uniform particle size Micro ball. 本发明以全氟塑料为基体,采用机械加工的方法在所述基体上打上贯穿孔,得到用于乳化的多孔膜。 The method of the present invention is a perfluoro plastic substrate, by machining a through-hole marked on the base body to obtain a porous film is used for emulsification. 本发明提供的多孔膜的制备方法简单、易操作,有利于大规模工业生产。 The method of preparing a porous film of the present invention provides a simple, easy to operate, is conducive to large-scale industrial production.

[0061] 以上所述仅是本发明的优选实施方式,应当指出,对于本技术领域的普通技术人员来说,在不脱离本发明原理的前提下,还可以做出若干改进和润饰,这些改进和润饰也应视为本发明的保护范围。 [0061] The above are only preferred embodiments of the present invention, it should be noted that those of ordinary skill in the art, in the present invention without departing from the principles of the premise, can make various improvements and modifications, such modifications and modifications should also be regarded as the protection scope of the present invention.

Claims (10)

  1. 1.一种用于乳化的多孔膜,所述多孔膜的材质为全氟塑料。 A porous membrane for emulsification, the material of the porous membrane is perfluorinated plastics.
  2. 2.根据权利要求1所述的多孔膜,其特征在于,所述多孔膜的材质为聚四氟乙烯、全氟(乙烯丙烯)共聚物、聚全氟烷氧基树脂。 2. The porous film according to claim 1, characterized in that, the porous membrane made of polytetrafluoroethylene, perfluoro (ethylene-propylene) copolymer, poly perfluoroalkoxy resin.
  3. 3.根据权利要求1所述的多孔膜,其特征在于,所述多孔膜的厚度为0.1mm〜3mm。 3. The porous film according to claim 1, wherein the thickness of the porous membrane is 0.1mm~3mm.
  4. 4.根据权利要求1所述的多孔膜,其特征在于,所述多孔膜的表面为亲水型。 4. The porous membrane as claimed in claim 1, characterized in that the surface of the porous membrane is hydrophilic.
  5. 5.一种用于乳化的多孔膜的制备方法,包括: 以全氟塑料为基体,采用机械加工的方法,在所述基体上打多个贯穿孔,得到用于乳化的多孔膜。 5. A production method for a porous membrane emulsification, comprising: perfluorinated plastics as matrix, machining method, a plurality of through-holes in the playing of the base body to obtain a porous film is used for emulsification.
  6. 6.根据权利要求5所述的制备方法,其特征在于,所述机械加工的方法为钻孔或激光打孔。 6. The production method according to claim 5, characterized in that the method of machining or laser drilling of the borehole.
  7. 7.根据权利要求5所述的制备方法,其特征在于,所述在所述基体上打多个贯穿孔后还包括: 对打贯穿孔后的基体进行表面亲水改性处理。 7. The production method according to claim 5, characterized in that, the hit on the substrate after a plurality of through holes further comprises: a base after sparring through hole hydrophilic surface modification treatment.
  8. 8.根据权利要求7所述的制备方法,其特征在于,所述表面亲水改性处理为萘钠化学处理、氨钠法处理、联苯钠法处理,高温熔融法处理、辐射法处理或等离子体处理。 8. The production method according to claim 7, characterized in that the hydrophilic surface modification treatment is a chemical treatment, sodium naphthalene, sodium Treatment of ammonia, sodium biphenyl processing method, a high temperature melt processing method, radiation treatment or plasma treatment.
  9. 9.权利要求1〜4任意一项所述多孔膜或权利要求5〜8任意一项所述制备方法得到的多孔膜在膜乳化中的应用。 9. any one of claims 1 ~ 4 The porous membrane as claimed in claim 5 ~ 8, or any one application of a porous membrane obtained in the production method of the membrane emulsification.
  10. 10.根据权利要求9所述的应用,其特征在于,所述膜乳化的过程为: 将分散相和连续相置于所述多孔膜的两侧,所述连续相相对所述多孔膜匀速运动,所述分散相通过所述多孔膜上的孔进入所述连续水相,完成乳化。 10. The use according to claim 9, wherein said process is a membrane emulsification: the dispersed and continuous phases disposed on both sides of the porous membrane, said porous membrane relative to the continuous phase of uniform motion , the dispersed phase into the continuous aqueous pores through the porous membrane phase, emulsification is completed.
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