CN103739857B - A kind of preparation method of chitosan beads and preparation facilities thereof - Google Patents
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- 229920001661 Chitosan Polymers 0.000 title claims abstract description 164
- 239000011324 bead Substances 0.000 title claims abstract description 117
- 238000002360 preparation method Methods 0.000 title claims abstract description 51
- 238000005406 washing Methods 0.000 claims abstract description 14
- 239000002994 raw material Substances 0.000 claims abstract description 4
- 239000000243 solution Substances 0.000 claims description 54
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 42
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 42
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 24
- 239000007788 liquid Substances 0.000 claims description 15
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 13
- 239000002245 particle Substances 0.000 claims description 11
- 239000008367 deionised water Substances 0.000 claims description 7
- 229910021641 deionized water Inorganic materials 0.000 claims description 7
- 238000003756 stirring Methods 0.000 claims description 6
- 238000003760 magnetic stirring Methods 0.000 claims description 5
- 239000007853 buffer solution Substances 0.000 claims description 3
- 239000006210 lotion Substances 0.000 claims 15
- 238000000465 moulding Methods 0.000 claims 4
- 230000005611 electricity Effects 0.000 claims 1
- 239000012530 fluid Substances 0.000 claims 1
- 235000011389 fruit/vegetable juice Nutrition 0.000 claims 1
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- JKQOBWVOAYFWKG-UHFFFAOYSA-N molybdenum trioxide Chemical compound O=[Mo](=O)=O JKQOBWVOAYFWKG-UHFFFAOYSA-N 0.000 claims 1
- 238000004321 preservation Methods 0.000 claims 1
- 230000015271 coagulation Effects 0.000 abstract description 36
- 238000005345 coagulation Methods 0.000 abstract description 36
- 238000000034 method Methods 0.000 abstract description 10
- 238000004519 manufacturing process Methods 0.000 abstract description 4
- 230000001112 coagulating effect Effects 0.000 abstract description 2
- 238000005265 energy consumption Methods 0.000 abstract description 2
- 231100001234 toxic pollutant Toxicity 0.000 abstract description 2
- 238000004448 titration Methods 0.000 description 5
- 239000000872 buffer Substances 0.000 description 4
- 229910052751 metal Inorganic materials 0.000 description 4
- 239000002184 metal Substances 0.000 description 4
- 238000010586 diagram Methods 0.000 description 3
- 229920002101 Chitin Polymers 0.000 description 2
- 125000003277 amino group Chemical group 0.000 description 2
- 238000001802 infusion Methods 0.000 description 2
- 239000004005 microsphere Substances 0.000 description 2
- 231100000331 toxic Toxicity 0.000 description 2
- 230000002588 toxic effect Effects 0.000 description 2
- 239000002028 Biomass Substances 0.000 description 1
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 description 1
- 108010093096 Immobilized Enzymes Proteins 0.000 description 1
- 229920002678 cellulose Polymers 0.000 description 1
- 239000001913 cellulose Substances 0.000 description 1
- 230000006196 deacetylation Effects 0.000 description 1
- 238000003381 deacetylation reaction Methods 0.000 description 1
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- 229940079593 drug Drugs 0.000 description 1
- 239000003937 drug carrier Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
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- 238000004945 emulsification Methods 0.000 description 1
- 238000007720 emulsion polymerization reaction Methods 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- 239000008103 glucose Substances 0.000 description 1
- 229910001385 heavy metal Inorganic materials 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 239000003999 initiator Substances 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 229920002521 macromolecule Polymers 0.000 description 1
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Abstract
本发明涉及一种壳聚糖珠的制备方法及其制备装置。它是用壳聚糖为原料制备壳聚糖珠，方法包括配制壳聚糖溶液和凝结浴液、壳聚糖凝结成珠、洗涤壳聚糖珠和保存壳聚糖珠。制备装置有一个机架，其底座上包括一个壳聚糖珠成型容器，机架中部安装一个滴管；机架上还有恒流泵、直流电源以及壳聚糖溶液滴珠搅拌器；直流电源的一个电极与滴管连接，另一个电极与凝结浴液中的导电圆环连接，或与金属的壳聚糖珠成型容器连接。本发明优点是：工艺条件稳定、易于操作、连续运行、效率高、产品质量好；制备过程清洁，是一种无毒性污染物产生的壳聚糖珠安全制备方法；壳聚糖珠的制备装置简单、占地小、效率高、能耗低，能实现工业规模化生产。
The invention relates to a preparation method of chitosan beads and a preparation device thereof. It uses chitosan as raw material to prepare chitosan beads, and the method includes preparing chitosan solution and coagulation bath, coagulating chitosan into beads, washing chitosan beads and preserving chitosan beads. The preparation device has a frame, a chitosan bead forming container is included on the base, and a dropper is installed in the middle of the frame; a constant current pump, a DC power supply and a chitosan solution drop bead stirrer are also arranged on the frame; One electrode is connected to the burette and the other electrode is connected to a conductive ring in the coagulation bath or to a metallic chitosan bead forming container. The invention has the advantages of stable process conditions, easy operation, continuous operation, high efficiency and good product quality; the preparation process is clean, and it is a safe preparation method of chitosan beads without toxic pollutants; the preparation device of chitosan beads It is simple, occupies a small area, has high efficiency and low energy consumption, and can realize industrial scale production.
Description
技术领域technical field
本发明涉及一种壳聚糖珠的制备方法及其制备装置，特别涉及到一种连续制备不同粒径壳聚糖珠的方法及装置。The invention relates to a preparation method and a preparation device of chitosan beads, in particular to a method and a device for continuously preparing chitosan beads with different particle sizes.
背景技术Background technique
壳聚糖（Chitosan）是一种甲壳素脱乙酰产物，也是一种天然的大分子化合物，是世界上仅次于纤维素的第二大有机资源。壳聚糖具有良好的亲水性、可再生性和生物相容性，并且无生物学毒性，安全可靠。在自然条件下壳聚糖可以生物降解，是一种储量丰富的可再生生物质资源。Chitosan is a chitin deacetylation product and a natural macromolecular compound. It is the second largest organic resource in the world after cellulose. Chitosan has good hydrophilicity, reproducibility and biocompatibility, and is non-biologically toxic, safe and reliable. Chitosan can be biodegraded under natural conditions and is a renewable biomass resource with abundant reserves.
壳聚糖分子基本单元是带有胺基的葡萄糖，含有丰富的氨基和羟基，这些官能团反应活性强于甲壳素，可以进行酰化、磺化、羧甲基化、烷基化和硝化等多种基团修饰。The basic molecular unit of chitosan is glucose with amine groups, which is rich in amino groups and hydroxyl groups. These functional groups are more reactive than chitin, and can be acylated, sulfonated, carboxymethylated, alkylated and nitrated. A group modification.
壳聚糖可以被制成球珠或微球，可用于药物缓释、药物载体、固定化酶载体、吸附重金属离子和污水处理等。目前壳聚糖珠或微球的常用制备方法有滴定法和反相悬浮法，但目前这些制备方法工艺条件不稳定，难以连续高效生产。Chitosan can be made into beads or microspheres, which can be used for drug sustained release, drug carrier, immobilized enzyme carrier, adsorption of heavy metal ions and sewage treatment. At present, the common preparation methods of chitosan beads or microspheres include titration method and reverse-phase suspension method, but the process conditions of these preparation methods are unstable at present, and it is difficult to produce continuously and efficiently.
发明内容Contents of the invention
本发明的目的在于，提供一种工艺条件稳定、易于操作、连续运行、效率高、产品质量好、制备过程清洁，无毒性污染物产生的壳聚糖珠的制备方法；壳聚糖珠的制备装置简单、占地小、效率高、能耗低，能实现工业规模化生产。The object of the present invention is to provide a method for preparing chitosan beads with stable process conditions, easy operation, continuous operation, high efficiency, good product quality, clean preparation process, and non-toxic pollutants; preparation of chitosan beads The device is simple, occupies a small area, has high efficiency and low energy consumption, and can realize industrial scale production.
本发明壳聚糖珠的制备方法的技术方案是：The technical scheme of the preparation method of chitosan beads of the present invention is:
一种壳聚糖珠的制备方法，其特征在于，它是用壳聚糖为原料制备壳聚糖珠，包括如下步骤：A kind of preparation method of chitosan pearl is characterized in that, it is that raw material prepares chitosan pearl with chitosan, comprises the steps:
A、配制壳聚糖溶液和凝结浴液：将壳聚糖溶解于乙酸溶液中，配制成壳聚糖溶液；将氢氧化钠加入到乙醇溶液中溶解，配制用于促成壳聚糖凝结成珠的凝结浴液；A. Prepare chitosan solution and coagulation bath: dissolve chitosan in acetic acid solution to prepare chitosan solution; add sodium hydroxide to ethanol solution to dissolve, and prepare to promote chitosan to coagulate into beads coagulation bath;
B、壳聚糖凝结成珠：将壳聚糖溶液注入滴管内，通过滴管滴到凝结浴液中并搅拌；滴管为一个能导电的中空管，该滴管与壳聚糖溶液输送管连接，还与一个用于控制滴管与凝结浴液的液面之间电压的直流电源连接，通过调节电压来调节壳聚糖珠的粒径；B. Chitosan condenses into beads: inject the chitosan solution into the dropper, drop it into the coagulation bath through the dropper and stir; the dropper is a conductive hollow tube, and the dropper is transported with the chitosan solution The tube is also connected with a direct current power supply used to control the voltage between the dropper and the liquid level of the coagulation bath, and the particle size of the chitosan beads is adjusted by adjusting the voltage;
C、洗涤壳聚糖珠：洗涤壳聚糖珠上的残留物；C, washing chitosan beads: washing the residue on the chitosan beads;
D、保存壳聚糖珠：将洗涤后的壳聚糖珠保存在缓冲液中。D. Preserving chitosan beads: Preserve the washed chitosan beads in buffer.
进一步的技术方案是：Further technical solutions are:
所述的壳聚糖珠的制备方法，其滴管选自医用针头；洗涤壳聚糖珠上的残留物是用去离子水洗涤壳聚糖珠上的氢氧化钠；洗涤后的壳聚糖珠保存在低温环境下的PBS缓冲液中。The preparation method of described chitosan beads, its dropper is selected from medical needles; washing the residue on the chitosan beads is to wash the sodium hydroxide on the chitosan beads with deionized water; the chitosan after washing Beads are stored in PBS buffer at low temperature.
所述的壳聚糖珠的制备方法，其壳聚糖溶液是通过恒流泵注入到滴管中；壳聚糖溶液通过滴管滴到凝结浴液中后通过磁力搅拌器搅拌。In the preparation method of the chitosan beads, the chitosan solution is injected into the dropper through a constant flow pump; the chitosan solution is dropped into the coagulation bath through the dropper and stirred by a magnetic stirrer.
所述的壳聚糖珠的制备方法，其壳聚糖溶液浓度以壳聚糖质量与乙酸溶液体积W/V百分比计为1.5％～2.5％，其中乙酸溶液浓度以乙酸质量与水体积W/V百分比计为0.5％～2％；凝结浴液浓度以氢氧化钠质量与乙醇溶液体积W/V百分比计为3.5％～4.5％，其中乙醇溶液浓度以乙醇质量与水体积W/V百分比为55％～65％。In the preparation method of the chitosan beads, the concentration of the chitosan solution is 1.5% to 2.5% based on the mass of chitosan and the volume W/V of the acetic acid solution, wherein the concentration of the acetic acid solution is calculated based on the mass of acetic acid and the volume W/V of the water. The percentage of V is 0.5% to 2%; the concentration of the coagulation bath liquid is 3.5% to 4.5% based on the percentage of sodium hydroxide mass and ethanol solution volume W/V, and the concentration of ethanol solution is calculated based on the percentage of ethanol mass and water volume W/V. 55% to 65%.
所述的壳聚糖珠的制备方法，其壳聚糖珠粒径为400～2500μm。In the preparation method of the chitosan beads, the particle size of the chitosan beads is 400-2500 μm.
所述的壳聚糖珠制备方法，其直流电源电压调节范围为10～6000V。In the method for preparing chitosan beads, the adjustment range of the DC power supply voltage is 10-6000V.
所述的壳聚糖珠制备方法，其直流电源电压调节范围为1000～6000V。In the preparation method of chitosan beads, the adjustment range of the DC power supply voltage is 1000-6000V.
用于本发明所述的壳聚糖珠制备方法的壳聚糖珠制备装置技术方案是：The chitosan bead preparation device technical scheme that is used for the chitosan bead preparation method of the present invention is:
一种壳聚糖珠制备装置，它有一个机架，该机架底座上包括一个盛装凝结浴液的壳聚糖珠成型容器；机架中部安装一个支撑并调节滴管高度的滴管支架，滴管出口位于盛装凝结浴液的壳聚糖珠成型容器中凝结浴液的液面上方；机架上还安装一个恒流泵、一个具有控制器的直流电源、以及一个用于对凝结浴液和滴入凝结浴液中的壳聚糖溶液滴珠进行搅拌的搅拌器；滴管通过输液管与恒流泵出液口联通，恒流泵的进液管进口在盛装壳聚糖溶液的容器中；直流电源的一个电极与滴管连接，另一个电极与凝结浴液中的导电圆环连接，或与金属的盛装凝结浴液的壳聚糖珠成型容器连接。A kind of chitosan bead preparation device, it has a frame, and the chitosan bead forming container of a costume coagulation bath liquid is included on this frame base; A dropper support that supports and adjusts the dropper height is installed in the middle of the frame, The outlet of the dropper is located above the liquid level of the coagulation bath in the chitosan bead forming container containing the coagulation bath; a constant flow pump, a DC power supply with a controller, and a device for controlling the coagulation bath are also installed on the frame. A stirrer for stirring with the chitosan solution dripping into the coagulation bath; the dropper communicates with the liquid outlet of the constant-flow pump through the infusion tube, and the inlet of the liquid-inlet pipe of the constant-flow pump is in the container containing the chitosan solution Middle; one electrode of the DC power supply is connected to the dropper, and the other electrode is connected to the conductive ring in the coagulation bath, or connected to the metal chitosan bead forming container containing the coagulation bath.
进一步的技术方案是：Further technical solutions are:
所述的壳聚糖珠制备装置，其搅拌器为磁力搅拌器,转速为180～240rpm；搅拌器位于机架底座上，盛装凝结浴液的壳聚糖珠成型容器放置于搅拌器工作面上。The chitosan beads preparation device, the stirrer is a magnetic stirrer with a rotating speed of 180-240rpm; the stirrer is located on the base of the frame, and the chitosan bead forming container containing the coagulation bath liquid is placed on the working surface of the stirrer .
所述的壳聚糖珠制备装置，其滴管为医用针头，规格为30G；恒流泵速率为0.05mL/min。In the chitosan bead preparation device, the dropper is a medical needle with a specification of 30G; the rate of the constant flow pump is 0.05mL/min.
所述的壳聚糖珠制备装置，其直流电源正极与金属的滴管连接，负极与与凝结浴液中的导电圆环连接。In the chitosan bead preparation device, the positive pole of the DC power supply is connected to the metal dropper, and the negative pole is connected to the conductive ring in the coagulation bath.
本发明的原理和技术效果是：Principle of the present invention and technical effect are:
本发明由恒流泵提供流加力，使滴管滴出壳聚糖溶液滴珠，由直流电源提供电场牵引力，磁力搅拌器增加壳聚糖滴珠在凝结浴中的传质作用，通过调节电压来调节壳聚糖珠的粒径，形成预期大小的壳聚糖珠。本发明为工业规模化生产壳聚糖珠提供了具有显著积极效果的制备方法和装置。能制备不同粒径壳聚糖珠，方法简便、高效稳定，且均一性良好；可实现连续无间断化生产；相比于喷雾干燥制备方法，本发明所需设备简单，占地小且，更加节能；相比于采用油相乳化制备方法，本发明在制备过程中不会引入乳化聚合法制备过程中使用的大量引发剂或有毒有机溶剂，制备过程清洁，无毒性污染物产生。In the present invention, a flow force is provided by a constant-current pump, so that the dropper drips chitosan solution droplets, and the electric field traction force is provided by a DC power supply. Voltage to adjust the particle size of chitosan beads to form chitosan beads of expected size. The invention provides a preparation method and a device with significant positive effects for industrial scale production of chitosan beads. Chitosan beads with different particle sizes can be prepared, the method is simple, efficient and stable, and the uniformity is good; continuous and uninterrupted production can be realized; compared with the spray drying preparation method, the equipment required by the present invention is simple, occupies a small area and is more Energy saving; compared with the oil phase emulsification preparation method, the present invention does not introduce a large amount of initiators or toxic organic solvents used in the emulsion polymerization preparation process during the preparation process, the preparation process is clean, and no toxic pollutants are produced.
附图说明Description of drawings
图1为本发明壳聚糖珠制备装置结构原理图；Fig. 1 is the structural schematic diagram of chitosan beads preparation device of the present invention;
图2为本发明实施例1制得的壳聚糖珠图；Fig. 2 is the chitosan bead figure that the embodiment of the present invention 1 makes;
图3为本发明实施例2制得的壳聚糖珠图；Fig. 3 is the chitosan bead diagram that the embodiment of the present invention 2 makes;
图4为本发明实施例3制得的壳聚糖珠图。Fig. 4 is the chitosan bead figure that the embodiment 3 of the present invention makes.
图中：1－滴管,2－滴管支架,3－盛装壳聚糖溶液的容器,4－恒流泵,5－直流电源,6－盛装凝结浴液的壳聚糖珠成型容器,7－搅拌器。In the figure: 1-dropper, 2-dropper holder, 3-container for chitosan solution, 4-constant flow pump, 5-DC power supply, 6-chitosan bead forming container for coagulation bath, 7 - agitator.
具体实施方式detailed description
结合实施例和附图对本发明进一步说明如下。The present invention is further described as follows in conjunction with embodiments and accompanying drawings.
实施例1：是本发明壳聚糖珠制备方法的一个基本实施例。一种壳聚糖珠的制备方法，它是用壳聚糖为原料制备壳聚糖珠，包括如下步骤：Embodiment 1: is a basic embodiment of the preparation method of chitosan beads of the present invention. A kind of preparation method of chitosan beads, it is to use chitosan as raw material to prepare chitosan beads, comprising the steps:
A、配制壳聚糖溶液和凝结浴液：将壳聚糖溶解于乙酸溶液中，配制成壳聚糖溶液；将氢氧化钠加入到乙醇溶液中溶解，配制用于促成壳聚糖凝结成珠的凝结浴液；A. Prepare chitosan solution and coagulation bath: dissolve chitosan in acetic acid solution to prepare chitosan solution; add sodium hydroxide to ethanol solution to dissolve, and prepare to promote chitosan to coagulate into beads coagulation bath;
B、壳聚糖凝结成珠：将壳聚糖溶液注入滴管内，通过滴管滴到凝结浴液中并搅拌；滴管为一个能导电的中空管，该滴管与壳聚糖溶液输送管连接，还与一个用于控制滴管与凝结浴液的液面之间电压的直流电源连接，通过调节电压来调节壳聚糖珠的粒径；B. Chitosan condenses into beads: inject the chitosan solution into the dropper, drop it into the coagulation bath through the dropper and stir; the dropper is a conductive hollow tube, and the dropper is transported with the chitosan solution The tube is also connected with a direct current power supply used to control the voltage between the dropper and the liquid level of the coagulation bath, and the particle size of the chitosan beads is adjusted by adjusting the voltage;
C、洗涤壳聚糖珠：洗涤壳聚糖珠上的残留物；C, washing chitosan beads: washing the residue on the chitosan beads;
D、保存壳聚糖珠：将洗涤后的壳聚糖珠保存在缓冲液中。D. Preserving chitosan beads: Preserve the washed chitosan beads in buffer.
实施例2：是一个进一步的实施例。与实施例1不同的是：所述的滴管选自医用针头；洗涤壳聚糖珠上的残留物是用去离子水洗涤壳聚糖珠上的氢氧化钠；洗涤后的壳聚糖珠保存在低温环境下的PBS缓冲液中。所述的壳聚糖溶液是通过恒流泵注入到滴管中；壳聚糖溶液通过滴管滴到凝结浴液中后通过磁力搅拌器搅拌。所述的壳聚糖溶液浓度以壳聚糖质量与乙酸溶液体积W/V百分比计为1.5％～2.5％，其中乙酸溶液浓度以乙酸质量与水体积W/V百分比计为0.5％～2％；凝结浴液浓度以氢氧化钠质量与乙醇溶液体积W/V百分比计为3.5％～4.5％，其中乙醇溶液浓度以乙醇质量与水体积W/V百分比为55％～65％。所述的壳聚糖珠粒径为400～2500μm。所述直流电源电压调节范围为10～6000V。Embodiment 2: is a further embodiment. Different from Example 1: the dropper is selected from medical needles; the residue on the washing chitosan beads is to wash the sodium hydroxide on the chitosan beads with deionized water; the chitosan beads after washing Store in PBS buffer at low temperature. The chitosan solution is injected into the dropper through a constant flow pump; the chitosan solution is dropped into the coagulation bath through the dropper and stirred by a magnetic stirrer. The concentration of the chitosan solution is 1.5% to 2.5% based on the mass of chitosan and the W/V percentage of the acetic acid solution volume, wherein the concentration of the acetic acid solution is 0.5% to 2% based on the W/V percentage of the mass of acetic acid and the volume of water The concentration of the coagulation bath liquid is 3.5% to 4.5% in terms of the mass of sodium hydroxide and the percentage of the volume of ethanol solution W/V, wherein the concentration of the ethanol solution is 55% to 65% in terms of the percentage of mass of ethanol and the percentage of W/V of the volume of water. The diameter of the chitosan beads is 400-2500 μm. The adjustment range of the DC power supply voltage is 10-6000V.
实施例3：是一个优选的实施例。与实施例2不同的是：直流电源电压调节范围为1000～6000V。Embodiment 3: is a preferred embodiment. The difference from Embodiment 2 is that the DC power supply voltage can be adjusted in a range of 1000-6000V.
实施例4：是一种用于本发明所述的壳聚糖珠制备方法的壳聚糖珠制备装置的个基本实施例。如图1结构原理图所示，一种壳聚糖珠制备装置，它有一个机架，该机架底座上包括一个盛装凝结浴液的壳聚糖珠成型容器6；机架中部安装一个支撑并调节滴管1高度的滴管支架2，滴管1出口位于盛装凝结浴液的壳聚糖珠成型容器6中凝结浴液的液面上方；机架上还安装一个恒流泵4、一个具有控制器的直流电源5、以及一个用于对凝结浴液和滴入凝结浴液中的壳聚糖溶液滴珠进行搅拌的搅拌器7；滴管1通过输液管与恒流泵4出液口联通，恒流泵4的进液管进口在盛装壳聚糖溶液的容器3中；直流电源5的一个电极与滴管1连接，另一个电极与凝结浴液中的导电圆环连接，当该另一个电极与金属的盛装凝结浴液的壳聚糖珠成型容器6连接，则又是一种实施例。Embodiment 4: be a kind of basic embodiment of the chitosan bead preparation device that is used for the chitosan bead preparation method of the present invention. As shown in Fig. 1 structural schematic diagram, a kind of chitosan bead preparation device has a frame, and the chitosan bead forming container 6 that dresses coagulation bath liquid is included on this frame base; And adjust the dropper support 2 of the dropper 1 height, the dropper 1 outlet is positioned at the top of the liquid level of the coagulation bath in the chitosan bead forming container 6 of the splendid attire coagulation bath; a constant flow pump 4, a A direct current power supply 5 with a controller, and an agitator 7 for stirring the coagulation bath and the chitosan solution drops dripped into the coagulation bath; the dropper 1 is discharged through the infusion tube and the constant flow pump 4 The inlet of the constant flow pump 4 is in the container 3 of the chitosan solution; an electrode of the DC power supply 5 is connected with the dropper 1, and the other electrode is connected with the conductive ring in the coagulation bath. This another electrode is connected with the chitosan bead forming container 6 of the costume coagulation bath liquid of metal, then is another kind of embodiment.
实施例5：是一个进一步的实施例。与实施例4不同的是：所述的搅拌器7为磁力搅拌器,转速为180～240rpm；搅拌器7位于机架底座上，盛装凝结浴液的壳聚糖珠成型容器6放置于搅拌器7工作面上。所述的滴管1为医用针头，规格为30G；恒流泵4速率为0.05mL/min。直流电源正极与金属的滴管连接，负极与凝结浴液中的导电圆环连接。Embodiment 5: is a further embodiment. The difference from Example 4 is that the stirrer 7 is a magnetic stirrer with a rotating speed of 180-240rpm; the stirrer 7 is located on the frame base, and the chitosan bead forming container 6 containing the coagulation bath is placed on the stirrer 7 working surfaces. The dropper 1 is a medical needle with a specification of 30G; the speed of the constant flow pump 4 is 0.05mL/min. The positive pole of the DC power supply is connected to the metal dropper, and the negative pole is connected to the conductive ring in the coagulation bath.
以下是优先的综合实施例。The following is a preferred comprehensive embodiment.
实施例6：是一个优选的实施例。在容器3中，加入2g壳聚糖，再加入100mL的浓度为1％的乙酸溶液，充分搅拌，配制成壳聚糖溶液浓度以壳聚糖质量与乙酸溶液体积W/V百分比计为2％的100mL壳聚糖溶液；在壳聚糖珠成型容器6中，加入400mL浓度为60%的乙醇溶液,再加入16g氢氧化钠，充分溶解，配制成凝结浴液浓度以氢氧化钠质量与乙醇溶液体积W/V百分比计为4％的400mL凝结浴液。针头置于离凝结浴液液面3.5cm处；壳聚糖溶液通过恒流泵以0.05mL/min速率从规格为30G医用针头滴定至凝结浴液中。调节直流电源电压为1000V，磁力搅拌速度为200rpm。滴定完毕后，取出壳聚糖珠，用去离子水反复冲洗，直到壳聚糖珠无氢氧化钠残留。本实施例制备的壳聚糖珠粒径为2430μm，将制备的壳聚糖珠盛放于pH为7.4的PBS缓冲液中，置于4℃下保存。制备后的壳聚糖珠参见图2。Embodiment 6: is a preferred embodiment. In container 3, add 2g chitosan, add the concentration of 100mL again and be the acetic acid solution of 1%, fully stir, the concentration of chitosan solution is prepared as 2% by chitosan quality and acetic acid solution volume W/V percentage 100mL chitosan solution; in the chitosan bead forming container 6, add 400mL concentration of 60% ethanol solution, then add 16g sodium hydroxide, fully dissolve, and prepare the coagulation bath concentration with the quality of sodium hydroxide and ethanol The solution volume W/V percentage is calculated as 4% of 400mL coagulating bath. The needle is placed 3.5cm away from the liquid surface of the coagulation bath; the chitosan solution is titrated from a 30G medical needle into the coagulation bath through a constant flow pump at a rate of 0.05mL/min. Adjust the DC power supply voltage to 1000V, and the magnetic stirring speed to 200rpm. After the titration, the chitosan beads were taken out and washed repeatedly with deionized water until no sodium hydroxide remained in the chitosan beads. The chitosan beads prepared in this example have a particle size of 2430 μm, and the prepared chitosan beads are placed in a PBS buffer solution with a pH of 7.4 and stored at 4° C. See Figure 2 for the prepared chitosan beads.
实施例7、是一个优选的实施例。与实施侧6不同的是：调节直流电源电压为3900V，磁力搅拌速度为200rpm。滴定完毕后，取出壳聚糖珠，用去离子水反复冲洗，直到壳聚糖珠无氢氧化钠残留。本实施例制备的壳聚糖珠粒径为1320μm，参见图3。Embodiment 7 is a preferred embodiment. The difference from the implementation side 6 is that the DC power supply voltage is adjusted to 3900V, and the magnetic stirring speed is 200rpm. After the titration, the chitosan beads were taken out and washed repeatedly with deionized water until no sodium hydroxide remained in the chitosan beads. The chitosan beads prepared in this example have a diameter of 1320 μm, see FIG. 3 .
实施例8：是一个优选的实施例。与实施侧6不同的是：调节直流电源电压为5700V，磁力搅拌速度为200rpm。滴定完毕后，取出壳聚糖珠，用去离子水反复冲洗，直到壳聚糖珠无氢氧化钠残留。本实施例制备的壳聚糖珠粒径为430μm，参见图4。Embodiment 8: is a preferred embodiment. The difference from the implementation side 6 is that the DC power supply voltage is adjusted to 5700V, and the magnetic stirring speed is 200rpm. After the titration, the chitosan beads were taken out and washed repeatedly with deionized water until no sodium hydroxide remained in the chitosan beads. The chitosan beads prepared in this example have a particle size of 430 μm, see FIG. 4 .
实施例9：与实施侧6不同的是：调节直流电源电压为10V，磁力搅拌速度为200rpm。滴定完毕后，取出壳聚糖珠，用去离子水反复冲洗，直到壳聚糖珠无氢氧化钠残留。本实施例制备的壳聚糖珠粒径为2485μm。Embodiment 9: The difference from the implementation side 6 is that the DC power supply voltage is adjusted to 10V, and the magnetic stirring speed is 200rpm. After the titration, the chitosan beads were taken out and washed repeatedly with deionized water until no sodium hydroxide remained in the chitosan beads. The chitosan beads prepared in this example had a particle size of 2485 μm.
本发明权利要求保护范围不限于上述实施例。The protection scope of the claims of the present invention is not limited to the above-mentioned embodiments.
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