CN101401962B - Glutin spherical honeycombed grain material, producing method and apparatus thereof - Google Patents
Glutin spherical honeycombed grain material, producing method and apparatus thereof Download PDFInfo
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- CN101401962B CN101401962B CN2008102350752A CN200810235075A CN101401962B CN 101401962 B CN101401962 B CN 101401962B CN 2008102350752 A CN2008102350752 A CN 2008102350752A CN 200810235075 A CN200810235075 A CN 200810235075A CN 101401962 B CN101401962 B CN 101401962B
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Abstract
The invention relates to a gelatin spherical porous particle material, and a method and a device for preparing the same. The method comprises the following steps: step one, preparing a gelatin solution with distilled water; step two, adding the gelatin solution into a material storage tank from a feed opening, and controlling the pressure in the storage tank between 0.08 and 0.5 MPa to ensure that the gelatin solution evenly flows out of a liquid guiding tube with the diameter between phi 0.5 and 3 millimeters at a speed of between 10 to 60 drops per minute, the gelatin solution flowing out of the liquid guiding tube grows big and similar to a spherical particle with the diameter between phi 0.8 and 4 millimeters and then drops off, and the gelatin solution is dripped into a condensate with a temperature between 10 and 20 DEG C below zero in a thermal insulation container to be condensed so that a gelatin spherical porous particle material with good sphericity and uniform particle diameter is formed; and step three, separating, freezing, drying, crosslinking and cleaning the spherical particle after the condensation in the step two to obtain the gelatin spherical porous particle material. The spherical particle material has homogeneous particle diameter distribution, contains a large number of micropores communicated with one another therein, has higher specific surface area, and can be applied to tissue repair and medicament slow release.
Description
One, technical field
The invention belongs to a kind of spherical particle material preparation technology that is applied to biomedical sector, be specifically related to a kind of preparation method of natural polymer glutin spherical honeycombed grain material.
Two, background technology
Prior art:
Gelatin is a kind of protein that the collagen triple-helix structure is converted into random chain and obtains, and is the soluble mixtures of polypeptides of a kind of hot water, thereby has biodegradability and good biocompatibility.Owing to have good film property, gelatin is used widely in the capsule of oral drug; Simultaneously, gelatin also has activated macrophage and anastalsis, can be used for making wound dressing, hemostatic material and artificial skin, and the hard tissue repair packing material.Except being used for preparing the block body stephanoporate support, gelatin also can be used for preparing the granulated packing material.。
Micro-sphere material has the unexistent excellent properties of a lot of irregular particles, as being difficult for causing stress concentration etc. after high flowability, high bulk density, difficult reunion, the filling.At present, reparation, the alveolar ridge of frontal resorption increase due to the filling, periodontal disease of root canal and exodontia nest, the filling of jaw bones blister cavities, atrophic rhinitis's filling, mastoid cavity filling, shaping (such as the nasus incurvus beauty treatment) reach in the damaged filling of bone with other position of skeleton, and the microsphere particle packing material is used widely.The polymer-matrix microsphere particle has multiple preparation method, and commonly used have emulsifying-chemical crosslink technique, emulsion solvent evaporation technique and a spray drying method.The microsphere diameter distribution of using these method preparations is larger, and packed density is large, and when being applied to tissue filling, intergranular hole is very few, is unfavorable for growing into of cambium.
Three, summary of the invention
The present invention is directed to above-mentioned technological deficiency, a kind of preparation method for preparing the glutin spherical honeycombed grain material with homogeneous distributed granule diameter is provided.
Technical scheme of the present invention is a kind of glutin spherical honeycombed grain material, the spheroidal particle of described glutin spherical honeycombed grain material, particle diameter is φ 0.8～4mm, the granule body interior is that the aperture is less than the micropore of 150 μ m, intercommunication between the micropore, the porosity of glutin spherical honeycombed grain material are 80～95%.
A kind of preparation method for preparing described glutin spherical honeycombed grain material, preparation process is:
The first step take the gelatin solution of distilled water preparation mass concentration as 5～20%, stirs gelatin is dissolved fully;
Second step, the gelatin solution that the first step is prepared adds storage tank from charge door, the pressure of controlling in the storage tank by Pressure gauge and pressure-control valve is 0.08～0.5MPa, evenly flows out with the speed of 10～60/min to guarantee the catheter of gelatin solution from caliber as φ 0.5～3mm.The gelatin solution that flows out from catheter drips behind the subsphaeroidal granule of about φ 0.8～4mm greatly mouth of pipe director, in dropping process, because capillary effect forms spherical, the temperature that then splashes in the cool-bag is condensation in the-condensed fluid of (10～20) ℃, forms the glutin spherical honeycombed grain material of good sphericity, uniform particle diameter.
According to the surface tension formula:
mg＝2πrσ
In the formula: m is drop mass; R is the extracapillary radius; σ is surface tension; G is acceleration of gravity.When density and viscosity one timing of gelatin solution, under the condition without external interference, this method can be prepared the spheroidal particle of good sphericity, uniform particle diameter.
The 3rd step is with the condensed spheroidal particle separation of second step, lyophilization; It is 0.25～2.5% cross-linking agent crosslinking Treatment that spheroidal particle after the lyophilization is put into mass concentration, then cleans with dehydrated alcohol, obtains glutin spherical honeycombed grain material.Described condensed fluid is dimethicone or vegetable oil.Described cross-linking agent is any one in formaldehyde, glutaraldehyde, the Biformyl.
The device for preparing described glutin spherical honeycombed grain material, formed by storage tank and cool-bag, be provided with charge door at the storage tank top, on storage tank, also be provided with Pressure gauge, Pressure gauge is connected with pressure-control valve, bottom at storage tank is provided with catheter, is provided with flow control valve at catheter, is provided with cool-bag below catheter.
Beneficial effect: the glutin spherical honeycombed grain material of the present invention's preparation::
(1) contain a large amount of intercommunication micropores in the granule body interior, form three-dimensional netted stereochemical structure, this granule has higher specific surface area, is conducive to the Flow of tissue fluid of the adhesion of cell;
(2) gelatin particle has the particle size distribution of homogeneous, does not need to sieve the granular materials that processing can obtain having same particle size; Because according to the surface tension formula:
mg＝2πrσ
In the formula: m is drop mass; R is the extracapillary radius; σ is surface tension; G is acceleration of gravity.When density and viscosity one timing of collagen solution, under the condition without external interference, this method can be prepared the spheroidal particle of good sphericity, uniform particle diameter.
(3) uniform particle diameter because of the glutin spherical granular materials for preparing according to this method is good, and the spherical granular material of same particle size, the intergranular space rate is maximum after the filling, so be conducive to the migration growth of Flow of tissue fluid and cell after the glutin spherical granular materials of the present invention filling.
Four, Figure of description:
Fig. 1 spheroidal particle forming device sketch map.
Device mainly is comprised of charge door 1, Pressure gauge 2, pressure-control valve 3, storage tank 4, flow control valve 5, catheter 6, condensed fluid 7 and cool-bag 8.
Fig. 2 is the photo of glutin spherical honeycombed grain.
Fig. 3 is the internal void photo of glutin spherical honeycombed grain.
Five, the specific embodiment:
Embodiment 1:
(1) adds hot distilled water to 60 ℃ with water bath with thermostatic control, gelatin is added to stir in the distilled water it is fully dissolved, be formulated as mass concentration and be 5% gelatin solution;
(2) as shown in Figure 1, the gelatin solution for preparing is added storage tank 4 from charge door 1, the pressure of controlling in the storage tanks 4 by Pressure gauge 2 and pressure-control valve 3 is 0.08MPa, to guarantee that gelatin solution evenly flows out from φ 0.5mm catheter 6, be 10/min by flow control valve 5 coutroi velocities.The gelatin solution that flows out from catheter 6 drips behind the subsphaeroidal granule of φ 0.8mm greatly mouth of pipe director, in dropping process, because that capillary effect forms is spherical, then splash into condensation in the condensed fluid 7 in the cool-bag 8, the temperature of condensed fluid is-10 ℃, forms spheroidal particle.Condensed fluid is dimethicone.
(3) condensed microsphere separates, and processes 8h-5 ℃ temperature lyophilization; It is 0.25% glutaraldehyde solution crosslinking Treatment 3h that spheroidal particle after the lyophilization is put into first mass concentration, clean with dehydrated alcohol again, obtain glutin spherical honeycombed grain material, as shown in Figure 2, the good sphericity of granule, uniform particle diameter, particle diameter is 0.8mm, as shown in Figure 3, and the porosity of granule is high, and porosity is 80%, the hole intercommunication forms three-dimensional netted stereochemical structure.
Embodiment 2:
(1) adds hot distilled water to 60 ℃ with water bath with thermostatic control, gelatin is added to stir in the distilled water it is fully dissolved, be formulated as mass concentration and be 20% gelatin solution;
(2) gelatin solution for preparing being added storage tank 4 from charge door 1, is 0.5MPa by the pressure in the control storage tank 4, to guarantee that gelatin solution evenly flows out from φ 3mm catheter 6.The gelatin solution that flows out from catheter 6 drips behind the subsphaeroidal granule of φ 4mm greatly mouth of pipe director, in dropping process, because that capillary effect forms is spherical, then splash into condensation in the condensed fluid 7 in the cool-bag 8, the temperature of condensed fluid is-20 ℃, forms spheroidal particle.Condensed fluid is vegetable oil.
(3) condensed microsphere separates, and processes 24h-10 ℃ temperature lyophilization; It is 2.5% formalin crosslinking Treatment 24h that spheroidal particle after the lyophilization is put into first mass concentration, cleans with dehydrated alcohol again, obtains glutin spherical honeycombed grain material.
Embodiment 3:
(1) adds hot distilled water to 60 ℃ with water bath with thermostatic control, gelatin is added to stir in the distilled water it is fully dissolved, be formulated as mass concentration and be 12% gelatin solution;
(2) gelatin solution for preparing being added storage tank 4 from charge door 1, is 0.28MPa by the pressure in the control storage tank 4, to guarantee that gelatin solution evenly flows out from φ 1.25mm catheter 6.The gelatin solution that flows out from catheter 6 drips behind the subsphaeroidal granule of φ 2.3mm greatly mouth of pipe director, in dropping process, because that capillary effect forms is spherical, then splash into condensation in the condensed fluid 7 in the cool-bag 8, the temperature of condensed fluid is-15 ℃, forms spheroidal particle.Condensed fluid is dimethicone.
(3) condensed microsphere separates, and processes 18h-7 ℃ temperature lyophilization; It is 1.25% glyoxal solution crosslinking Treatment 12h that spheroidal particle after the lyophilization is put into first mass concentration, cleans with dehydrated alcohol again, obtains glutin spherical honeycombed grain material.
Claims (5)
1. glutin spherical honeycombed grain material, it is characterized in that described glutin spherical honeycombed grain material, particle diameter is φ 0.8～4mm, and the granule body interior is that the aperture is less than the micropore of 150 μ m, intercommunication between the micropore, the porosity of glutin spherical honeycombed grain material are 80～95%.
2. a preparation method for preparing glutin spherical honeycombed grain material as claimed in claim 1 is characterized in that, preparation process is:
The first step take the gelatin solution of distilled water preparation mass concentration as 5～20%, stirs gelatin is dissolved fully;
Second step, the gelatin solution that the first step is prepared is the pipe of φ 0.5～3mm from caliber, evenly flows out with the speed of 10～60/min, splashes into temperature for condensation in the-condensed fluid of (10～20) ℃, forms spheroidal particle;
The 3rd step is with the condensed spheroidal particle separation of second step, lyophilization; It is 0.25～2.5% cross-linking agent crosslinking Treatment that spheroidal particle after the lyophilization is put into mass concentration, then cleans with dehydrated alcohol, obtains glutin spherical honeycombed grain material.
3. the preparation method of glutin spherical honeycombed grain material as claimed in claim 2 is characterized in that, described condensed fluid is dimethicone or vegetable oil.
4. the preparation method of glutin spherical honeycombed grain material as claimed in claim 2 is characterized in that, described cross-linking agent is any one in formaldehyde, glutaraldehyde, the Biformyl.
5. the device for preparing glutin spherical honeycombed grain material as claimed in claim 1, it is characterized in that, described device is comprised of storage tank (4) and cool-bag (8), be provided with charge door (1) at storage tank (4) top, on storage tank (4), also be provided with Pressure gauge (2), Pressure gauge (2) is connected with pressure-control valve (3), be provided with catheter (6) in the bottom of storage tank (4), be provided with flow control valve (5) at catheter (6), below catheter, be provided with cool-bag (8).
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5810988A (en) * | 1994-09-19 | 1998-09-22 | Board Of Regents, University Of Texas System | Apparatus and method for generation of microspheres of metals and other materials |
| CN1272383A (en) * | 2000-05-19 | 2000-11-08 | 清华大学 | Preparation method of nanometer phase calcium-phosphorus salt/collagen/polylactic acid bone composite material |
| CN1546181A (en) * | 2003-12-12 | 2004-11-17 | 清华大学 | Degradable material capable of guiding the regeneration and renovation process of hard tissue and its preparation |
| CN1607033A (en) * | 2003-10-15 | 2005-04-20 | 中国科学院过程工程研究所 | Chitose microsphere and microcapsule with uniform size and its preparation method |
| CN1931378A (en) * | 2006-09-29 | 2007-03-21 | 清华大学 | Micro rack for bone tissue engineering and its prepn process and application |
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5810988A (en) * | 1994-09-19 | 1998-09-22 | Board Of Regents, University Of Texas System | Apparatus and method for generation of microspheres of metals and other materials |
| CN1272383A (en) * | 2000-05-19 | 2000-11-08 | 清华大学 | Preparation method of nanometer phase calcium-phosphorus salt/collagen/polylactic acid bone composite material |
| CN1607033A (en) * | 2003-10-15 | 2005-04-20 | 中国科学院过程工程研究所 | Chitose microsphere and microcapsule with uniform size and its preparation method |
| CN1546181A (en) * | 2003-12-12 | 2004-11-17 | 清华大学 | Degradable material capable of guiding the regeneration and renovation process of hard tissue and its preparation |
| CN1931378A (en) * | 2006-09-29 | 2007-03-21 | 清华大学 | Micro rack for bone tissue engineering and its prepn process and application |
Non-Patent Citations (1)
| Title |
|---|
| 卢勰炜等.新型壳聚糖-海藻酸钠胃漂浮小丸的制备.《中国现代应用医学杂志》.2004,第21卷(第6期), * |
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Owner name: SOWTHEAST UNIV. Effective date: 20131016 Owner name: HAIAN BROTHERS SYNTHETIC FIBER CO., LTD. Free format text: FORMER OWNER: SOWTHEAST UNIV. Effective date: 20131016 |
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Effective date of registration: 20131016 Address after: 226600, Jiangsu province Nantong city Haian county head Town Industrial Park Patentee after: Haian County Brothers Synthetic Fiber Co.,Ltd. Patentee after: Southeast University Address before: 210096 Jiangsu city Nanjing Province four pailou No. 2 Patentee before: Southeast University |
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