CN103707587A - Preparation method of multilayer PEG-DMA hydrogel - Google Patents
Preparation method of multilayer PEG-DMA hydrogel Download PDFInfo
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Abstract
The invention discloses a preparation method of a multilayer PEG-DMA hydrogel. The preparation method comprises the following steps: 1) taking PEG-DMA, and adding into deionized water to uniformly stir to prepare a first-layer PEG-DMA solution; (2) adding an evocating agent into the first-layer PEG-DMA solution prepared in the step (1), uniformly stirring while keeping out of the sun, feeding into a mold, and performing ultraviolet illumination cross-linking to prepare a first-layer PEG-DMA hydrogel; (3) taking the PEG-DMA, adding into the deionized water to uniformly stir to prepare a second-layer PEG-DMA solution; (4) adding the evocating agent into the second-layer PEG-DMA solution prepared in the step (3), uniformly stirring while keeping out of the sun, feeding into the mold filled with the first-layer PEG-DMA hydrogel, and performing ultraviolet illumination cross-linking to prepare a double-layer PEG-DMA hydrogel; (5) repeating the steps (3) and (4) to prepare the multilayer PEG-DMA hydrogel. By adopting the preparation method provided by the invention, a stable multilayer PEG-DMA hydrogel structure with anisotropism can be constructed.
Description
Technical field
The present invention relates to a kind of preparation method of PEG-DMA hydrogel, particularly relate to a kind of preparation method of multilayer PEG-DMA hydrogel.
Background technology
In recent years, biomaterial is widely used in every field, and hydrogel is as a kind of typical biomaterial, owing to thering is good biocompatibility, the property of water-bearing, flexibility, degradability, preparation simplicity, the excellent performance such as stimuli responsive sensitivity to external world, the fields such as cell cultivation, organizational project, biology sensor and driver, drug delivery system have been widely applied.PEG-DMA(polyethylene glycol dimethacrylate) be a kind of with PEG(polyethylene glycol) hydrogel of large monomer, because it has good biocompatibility, nontoxic, non-volatile, good stability, and mechanical property parameters (elastic modelling quantity, Poisson's ratio) for example, approaches and modifiable advantage with human body parts tissue (skin, musculature), make it standby and be popular, be widely applied to the fields such as organizational project, medicine release and hydrogel surface modification.
At present, in organizational project, applied PEG-DMA hydrogel is all individual layer, isotropic, yet biological tissue's (such as skin etc.) is all multilayer, anisotropic conventionally, existing individual layer PEG-DMA hydrogel is difficult to meet the anisotropy requirement of biological tissue.And because PEG-DMA hydrogel is a kind of moisture biological soft material, its softness, be not easy adhesion and mechanical strength is poor, cause it when building sandwich construction, as easy as rolling off a log appearance destroys between layers, is out of shape, comes off and in conjunction with the situation such as unstable, is difficult to construct stable multilayer PEG-DMA hydrogel structure.
Summary of the invention
Based on this, be necessary for the problems referred to above, a kind of preparation method of multilayer PEG-DMA hydrogel is provided, adopt the method can construct stable multilayer PEG-DMA hydrogel structure.
A preparation method for double-deck PEG-DMA hydrogel, comprises the following steps:
1) get PEG-DMA, add deionized water for stirring even, prepare ground floor PEG-DMA solution;
2) in the ground floor PEG-DMA solution making in step 1), add initator, lucifuge stirs, and then injects mould, carries out ultraviolet lighting and is cross-linked, and makes ground floor PEG-DMA hydrogel;
3) get PEG-DMA, add deionized water for stirring even, prepare second layer PEG-DMA solution;
4) in the second layer PEG-DMA solution making in step 3), add initator, lucifuge stirs, and then injects the mould that ground floor PEG-DMA hydrogel is housed, and carries out ultraviolet lighting and is cross-linked, and makes described double-deck PEG-DMA hydrogel.
In an embodiment, the PEG-DMA concentration of described PEG-DMA solution is 10wt%～20wt% therein; And described ground floor PEG-DMA solution is not identical with the PEG-DMA concentration of described second layer PEG-DMA solution.
Therein in an embodiment, in step 2) in, the crosslinked time of ultraviolet lighting is 2～3 minutes; In step 4), the crosslinked time of ultraviolet lighting is 10～15 minutes.
In an embodiment, described initator is 2-hydroxy-2-methyl propiophenone therein.
In an embodiment, the consumption of described initator is 0.5% of described PEG-DMA liquor capacity therein.
In an embodiment, the molecular weight of described PEG-DMA is 1000 therein.
Therein in an embodiment, the U-shaped mould that described mould is comprised of glass intermediate plate, silicon rubber bar and geometrical clamp; Described silicon rubber bar is placed between glass intermediate plate, and by geometrical clamp, glass intermediate plate and silicon rubber bar is clamped.
A preparation method for multilayer PEG-DMA hydrogel, comprises the following steps:
1) get PEG-DMA, add deionized water for stirring even, prepare ground floor PEG-DMA solution;
2) in the ground floor PEG-DMA solution making in step 1), add initator, lucifuge stirs, and then injects mould, carries out ultraviolet lighting and is cross-linked, and makes ground floor PEG-DMA hydrogel;
3) get PEG-DMA, add deionized water for stirring even, prepare second layer PEG-DMA solution;
4) in the second layer PEG-DMA solution making in step 3), add initator, lucifuge stirs, and then injects the mould that ground floor PEG-DMA hydrogel is housed, and carries out ultraviolet lighting and is cross-linked, and makes double-deck PEG-DMA hydrogel;
5) repeating step 3), step 4): get PEG-DMA, add deionized water for stirring even, preparation N layer PEG-DMA solution; In prepared N layer PEG-DMA solution, add initator, lucifuge stirs, and then injects the mould that N-1 layer PEG-DMA hydrogel is housed, and carries out ultraviolet lighting and is cross-linked, and makes described multilayer PEG-DMA hydrogel; Wherein N is greater than 2 natural number.
In an embodiment, the PEG-DMA concentration of described PEG-DMA solution is 10wt%～20wt% therein; And described ground floor PEG-DMA solution is all not identical to the PEG-DMA concentration of described N layer PEG-DMA solution.
In an embodiment, the ultraviolet lighting crosslinking time of ground floor PEG-DMA solution to the N-1 layer PEG-DMA solution is 2～3 minutes therein; The ultraviolet lighting crosslinking time of N layer PEG-DMA solution is 10～15 minutes.
In an embodiment, described initator is 2-hydroxy-2-methyl propiophenone therein.
In an embodiment, the consumption of described initator is 0.5% of described PEG-DMA liquor capacity therein.
In an embodiment, the molecular weight of described PEG-DMA is 1000 therein.
Therein in an embodiment, the U-shaped mould that described mould is comprised of glass intermediate plate, silicon rubber bar and geometrical clamp; Described silicon rubber bar is placed between glass intermediate plate, and by geometrical clamp, glass intermediate plate and silicon rubber bar is clamped.
Bilayer of the present invention, multilayer PEG-DMA hydrogel preparation method, by controlling the parameters such as PEG-DMA concentration different in every one deck PEG-DMA solution, ultraviolet lighting crosslinking time, control the different crosslinking time of every one deck PEG-DMA solution, crosslinked hardness, make every one deck PEG-DMA hydrogel there is the mechanical properties such as different elastic modelling quantity, Poisson's ratio, thereby can form anisotropic bilayer, multilayer PEG-DMA hydrogel.
In preparation method of the present invention, the concentration difference of every one deck PEG-DMA solution and the crosslinked asynchronism(-nization) of ultraviolet lighting thereof, can make the mechanical properties such as elastic modelling quantity, Poisson's ratio of formed every one deck PEG-DMA hydrogel all different.The concentration of PEG-DMA is higher, crosslinking time is longer, and the elastic modelling quantity of formed PEG-DMA hydrogel is also larger.And the PEG-DMA solution that mass concentration is 10%～20% is after ultraviolet lighting is crosslinked, the elastic modelling quantity of formed PEG-DMA hydrogel and the elastic modelling quantity of tissue (10KPa～100KPa) are approaching, can be applicable to organizational project.
When needs are prepared N layer PEG-DMA hydrogel, the ultraviolet lighting crosslinking time of ground floor to the N-1 layer PEG-DMA solution is all controlled at 2～3 minutes, at it, under completely not crosslinked state, add lower one deck PEG-DMA solution, then carry out ultraviolet lighting crosslinked, at contact-making surface place, can there is new being cross-linked with completely not crosslinked PEG-DMA hydrogel in the PEG-DMA solution newly increasing, adjacent two-layer PEG-DMA hydrogel is closely linked, after adding N layer PEG-DMA solution, crosslinked 10～15 minutes of ultraviolet lighting, make each layer of PEG-DMA hydrogel abundant, completely crosslinked.And the ultraviolet lighting crosslinking time of ground floor to the N-1 layer PEG-DMA solution is all controlled at 2～3 minutes, can make to reach between each layer of PEG-DMA hydrogel best adhesion tight ness rating, if this ultraviolet lighting overlong time or too short, all can cause adhesion tight ness rating between adjacent two layers PEG-DMA hydrogel to reduce, the problem such as occur coming off between layers.And ultraviolet lighting crosslinking time is longer, the crosslinked hardness of PEG-DMA hydrogel is larger, and its elastic modelling quantity is also larger.
In addition, adopt 2-hydroxy-2-methyl propiophenone as the crosslinked initator of ultraviolet lighting, can accelerate the crosslinking rate of PEG-DMA hydrogel.The consumption of initator is preferably 0.5% of PEG-DMA liquor capacity, to guarantee that the PEG-DMA in PEG-DMA solution system can fully contact initator, produces best cross-linking effect.If initiator amount is too much, can cause the residual toxic hazard that causes of initator; If initiator amount is very few, cause hydrogel crosslinked insufficient, the performance of hydrogel is inconsistent.The molecular weight of PEG-DMA is preferably 1000, and it has best biocompatibility and swelling behavior.
The mould adopting in preparation method of the present invention, there is the advantages such as simple in structure, easy and simple to handle, reusable, owing to having adopted silicon rubber bar as mould rack, it has good flexibility, can avoid PEG-DMA hydrogel in preparation process, to be out of shape, to destroy.
The specific embodiment
Embodiment mono-: the preparation of double-deck PEG-DMA hydrogel
Get two sheet glass intermediate plates, U-shaped silicon rubber bar and several geometrical clamp that thickness is 2mm, U-shaped silicon rubber bar is placed between two sheet glass intermediate plates, then with geometrical clamp, glass intermediate plate and silicon rubber bar are clamped, making thickness is the U-shaped individual layer mould of 2mm.
In beaker, add 20mL deionized water, 2g PEG-DMA, stir, make mass concentration and be 10% PEG-DMA solution; Then add 0.1mL2-hydroxy-2-methyl propiophenone, with tinfoil, wrap up beaker, lucifuge stirs more than 30 minutes, makes ground floor PEG-DMA solution; With syringe, ground floor PEG-DMA solution is injected to U-shaped individual layer mould, be then placed under UV-crosslinked instrument illumination crosslinked 2 minutes, the ground floor PEG-DMA hydrogel that make mass concentration and be 10%, thickness is 2mm.
In beaker, add 20mL deionized water, 4g PEG-DMA, stir, make mass concentration and be 20% PEG-DMA solution; Then add 0.1mL2-hydroxy-2-methyl propiophenone, with tinfoil, wrap up beaker, lucifuge stirs more than 30 minutes, makes second layer PEG-DMA solution.
Get the U-shaped individual layer mould that ground floor PEG-DMA hydrogel is housed, horizontal positioned, take out geometrical clamp and remove the glass intermediate plate on top, the U-shaped silicon rubber bar correspondence that is 4mm by a thickness is placed on the silicon rubber bar of U-shaped individual layer mould, then cover glass intermediate plate, and with geometrical clamp, glass intermediate plate and silicon rubber bar are clamped, making thickness is the U-shaped double stack mold of 6mm, wherein the thickness of the U-shaped silicon rubber bar of ground floor is 2mm, and the thickness of the U-shaped silicon rubber bar of the second layer is 4mm.
The U-shaped double stack mold that ground floor PEG-DMA hydrogel is housed is vertically placed, with syringe, second layer PEG-DMA solution is injected to U-shaped double stack mold, then be placed in illumination under UV-crosslinked instrument and be cross-linked 10 minutes, make two-layer PEG-DMA completely crosslinked, take out U-shaped double stack mold, making thickness is the double-deck PEG-DMA hydrogel of 6mm.Wherein, the mass concentration of ground floor PEG-DMA hydrogel is 10%, and thickness is 2mm; The mass concentration of second layer PEG-DMA hydrogel is 20%, and thickness is 4mm.
Embodiment bis-: the preparation of double-deck PEG-DMA hydrogel
Get two sheet glass intermediate plates, U-shaped silicon rubber bar and several geometrical clamp that thickness is 2mm, U-shaped silicon rubber bar is placed between two sheet glass intermediate plates, then with geometrical clamp, glass intermediate plate and silicon rubber bar are clamped, making thickness is the U-shaped individual layer mould of 2mm.
In beaker, add 20mL deionized water, 2g PEG-DMA, stir, make mass concentration and be 10% PEG-DMA solution; Then add 0.1mL2-hydroxy-2-methyl propiophenone, with tinfoil, wrap up beaker, lucifuge stirs more than 30 minutes, makes ground floor PEG-DMA solution; With syringe, ground floor PEG-DMA solution is injected to U-shaped individual layer mould, be then placed under UV-crosslinked instrument illumination crosslinked 2 minutes, the ground floor PEG-DMA hydrogel that make mass concentration and be 10%, thickness is 2mm.
In beaker, add 20mL deionized water, 3g PEG-DMA, stir, make mass concentration and be 15% PEG-DMA solution; Then add 0.1mL2-hydroxy-2-methyl propiophenone, with tinfoil, wrap up beaker, lucifuge stirs more than 30 minutes, makes second layer PEG-DMA solution.
Get the U-shaped individual layer mould that ground floor PEG-DMA hydrogel is housed, horizontal positioned, take out geometrical clamp and remove the glass intermediate plate on top, the U-shaped silicon rubber bar correspondence that is 2mm by a thickness is placed on the silicon rubber bar of U-shaped individual layer mould, then cover glass intermediate plate, and with geometrical clamp, glass intermediate plate and silicon rubber bar are clamped, making thickness is the U-shaped double stack mold of 4mm, wherein the thickness of the U-shaped silicon rubber bar of ground floor is 2mm, and the thickness of the U-shaped silicon rubber bar of the second layer is 2mm.
The U-shaped double stack mold that ground floor PEG-DMA hydrogel is housed is vertically placed, with syringe, second layer PEG-DMA solution is injected to U-shaped double stack mold, then be placed in illumination under UV-crosslinked instrument and be cross-linked 10 minutes, make two-layer PEG-DMA completely crosslinked, take out U-shaped double stack mold, making thickness is the double-deck PEG-DMA hydrogel of 4mm.Wherein, the mass concentration of ground floor PEG-DMA hydrogel is 10%, and thickness is 2mm; The mass concentration of second layer PEG-DMA hydrogel is 15%, and thickness is 2mm.
Embodiment tri-: the preparation of double-deck PEG-DMA hydrogel
Get two sheet glass intermediate plates, U-shaped silicon rubber bar and several geometrical clamp that thickness is 4mm, U-shaped silicon rubber bar is placed between two sheet glass intermediate plates, then with geometrical clamp, glass intermediate plate and silicon rubber bar are clamped, making thickness is the U-shaped individual layer mould of 4mm.
In beaker, add 20mL deionized water, 3g PEG-DMA, stir, make mass concentration and be 15% PEG-DMA solution; Then add 0.1mL2-hydroxy-2-methyl propiophenone, with tinfoil, wrap up beaker, lucifuge stirs more than 30 minutes, makes ground floor PEG-DMA solution; With syringe, ground floor PEG-DMA solution is injected to U-shaped individual layer mould, be then placed under UV-crosslinked instrument illumination crosslinked 2 minutes, the ground floor PEG-DMA hydrogel that make mass concentration and be 15%, thickness is 4mm.
In beaker, add 20mL deionized water, 4g PEG-DMA, stir, make mass concentration and be 20% PEG-DMA solution; Then add 0.1mL2-hydroxy-2-methyl propiophenone, with tinfoil, wrap up beaker, lucifuge stirs more than 30 minutes, makes second layer PEG-DMA solution.
Get the U-shaped individual layer mould that ground floor PEG-DMA hydrogel is housed, horizontal positioned, take out geometrical clamp and remove the glass intermediate plate on top, the U-shaped silicon rubber bar correspondence that is 2mm by a thickness is placed on the silicon rubber bar of U-shaped individual layer mould, then cover glass intermediate plate, and with geometrical clamp, glass intermediate plate and silicon rubber bar are clamped, making thickness is the U-shaped double stack mold of 6mm, wherein the thickness of the U-shaped silicon rubber bar of ground floor is 4mm, and the thickness of the U-shaped silicon rubber bar of the second layer is 2mm.
The U-shaped double stack mold that ground floor PEG-DMA hydrogel is housed is vertically placed, with syringe, second layer PEG-DMA solution is injected to U-shaped double stack mold, then be placed in illumination under UV-crosslinked instrument and be cross-linked 10 minutes, make two-layer PEG-DMA completely crosslinked, take out U-shaped double stack mold, making thickness is the double-deck PEG-DMA hydrogel of 6mm.Wherein, the mass concentration of ground floor PEG-DMA hydrogel is 15%, and thickness is 4mm; The mass concentration of second layer PEG-DMA hydrogel is 20%, and thickness is 2mm.
The preparation of tetra-: three layers of PEG-DMA hydrogel of embodiment
Get two sheet glass intermediate plates, U-shaped silicon rubber bar and several geometrical clamp that thickness is 2mm, U-shaped silicon rubber bar is placed between two sheet glass intermediate plates, then with geometrical clamp, glass intermediate plate and silicon rubber bar are clamped, making thickness is the U-shaped individual layer mould of 2mm.
In beaker, add 20mL deionized water, 2g PEG-DMA, stir, make mass concentration and be 10% PEG-DMA solution; Then add 0.1mL2-hydroxy-2-methyl propiophenone, with tinfoil, wrap up beaker, lucifuge stirs more than 30 minutes, makes ground floor PEG-DMA solution; With syringe, ground floor PEG-DMA solution is injected to U-shaped individual layer mould, be then placed under UV-crosslinked instrument illumination crosslinked 2 minutes, the ground floor PEG-DMA hydrogel that make mass concentration and be 10%, thickness is 2mm.
In beaker, add 20mL deionized water, 3g PEG-DMA, stir, make mass concentration and be 15% PEG-DMA solution; Then add 0.1mL2-hydroxy-2-methyl propiophenone, with tinfoil, wrap up beaker, lucifuge stirs more than 30 minutes, makes second layer PEG-DMA solution.
Get the U-shaped individual layer mould that ground floor PEG-DMA hydrogel is housed, horizontal positioned, take out geometrical clamp and remove the glass intermediate plate on top, the U-shaped silicon rubber bar correspondence that is 2mm by a thickness is placed on the silicon rubber bar of U-shaped individual layer mould, then cover glass intermediate plate, and with geometrical clamp, glass intermediate plate and silicon rubber bar are clamped, making thickness is the U-shaped double stack mold of 4mm, the thickness of the U-shaped silicon rubber bar of every one deck is 2mm.
The U-shaped double stack mold that ground floor PEG-DMA hydrogel is housed is vertically placed, with syringe, second layer PEG-DMA solution is injected to U-shaped double stack mold, then be placed in illumination under UV-crosslinked instrument and be cross-linked 2 minutes, making thickness is the double-deck PEG-DMA hydrogel of 4mm.Wherein, the mass concentration of ground floor PEG-DMA hydrogel is 10%, and thickness is 2mm; The mass concentration of second layer PEG-DMA hydrogel is 15%, and thickness is 2mm.
In beaker, add 20mL deionized water, 4g PEG-DMA, stir, make mass concentration and be 20% PEG-DMA solution; Then add 0.1mL2-hydroxy-2-methyl propiophenone, with tinfoil, wrap up beaker, lucifuge stirs more than 30 minutes, makes the 3rd layer of PEG-DMA solution.
Get the U-shaped double stack mold that double-deck PEG-DMA hydrogel is housed, horizontal positioned, take out geometrical clamp and remove the glass intermediate plate on top, the U-shaped silicon rubber bar correspondence that is 2mm by a thickness is placed on the silicon rubber bar of U-shaped double stack mold, then cover glass intermediate plate, and with geometrical clamp, glass intermediate plate and silicon rubber bar are clamped, making thickness is U-shaped three layers of mould of 6mm, the thickness of the U-shaped silicon rubber bar of every one deck is 2mm.
U-shaped three layers of mould that two PEG-DMA hydrogels are housed are vertically placed, with syringe, the 3rd layer of PEG-DMA solution is injected to U-shaped three layers of mould, then be placed in illumination under UV-crosslinked instrument and be cross-linked 15 minutes, make three layers of PEG-DMA completely crosslinked, take out U-shaped three layers of mould, making thickness is three layers of PEG-DMA hydrogel of 6mm.Wherein, the mass concentration of ground floor PEG-DMA hydrogel is 10%, and thickness is 2mm; The mass concentration of second layer PEG-DMA hydrogel is 15%, and thickness is 2mm, and the mass concentration of the 3rd layer of PEG-DMA hydrogel is 20%, and thickness is 2mm.
Embodiment five: the performance test of multilayer PEG-DMA hydrogel
The test of employing micro-indentations, the mechanical property of the every one deck PEG-DMA hydrogel in the prepared multilayer PEG-DMA hydrogel of mensuration the present invention, its test result is as shown in table 1 below.
The operating procedure of micro-indentations test is as follows:
1, the preparation of sample: according in embodiment mono-to embodiment tetra-, the PEG-DMA concentration of every one deck PEG-DMA hydrogel, ultraviolet lighting crosslinking time, initiator amount and mold thickness, prepare respectively its corresponding individual layer PEG-DMA hydrogel reference substance;
2, open micro-indentations instrument, select spherical indenter;
3, respectively PEG-DMA hydrogel reference substance is immersed in pure water, the spherical indenter of micro-indentations instrument is moved to the top of PEG-DMA hydrogel, and find the contact point between spherical indenter and PEG-DMA hydrogel, when significant change appears in the force curve of micro-indentations instrument demonstration, represent to have arrived contact point;
4, compression distance h and press-in speed v are set: compression distance h sets according to the thickness of PEG-DMA hydrogel, and its size is controlled in 10% strain; Press-in speed v is set as 300 μ m/s;
5, carry out relaxation test, and record power maximum F (0) and the stationary value F (∞) of relaxation curve;
6, by following formula, calculate modulus of shearing, Poisson's ratio and the elastic modelling quantity of PEG-DMA hydrogel:
F(0)/F(∞)=2(1-μ)
F(0)=16Gah/3
E=2G(1+μ)
Wherein, μ is Poisson's ratio, and G is modulus of shearing, and E is elastic modelling quantity; A is contact radius, and R is spherical indenter radius, and h is compression distance.
The performance test results of table 1 PEG-DMA hydrogel
The performance test results is as shown in Table 1 known, and in embodiment mono-to embodiment tetra-prepared multilayer PEG-DMA hydrogel, the Poisson's ratio of its every one deck PEG-DMA hydrogel and elastic modelling quantity are all not identical, show that it all has anisotropic character.In addition, the elastic modelling quantity of above-mentioned multilayer PEG-DMA hydrogel and the elastic modelling quantity of tissue are (for example, the elastic modelling quantity of skin histology is 10KPa～50Kpa, the elastic modelling quantity of musculature is 10KPa～100KPa,) close, show that it can simulate anisotropic tissue, can apply and the fields such as organizational project.
The above embodiment has only expressed several embodiment of the present invention, and it describes comparatively concrete and detailed, but can not therefore be interpreted as the restriction to the scope of the claims of the present invention.It should be pointed out that for the person of ordinary skill of the art, without departing from the inventive concept of the premise, can also make some distortion and improvement, these all belong to protection scope of the present invention.Therefore, the protection domain of patent of the present invention should be as the criterion with claims.
Claims (10)
1. a preparation method for double-deck PEG-DMA hydrogel, comprises the following steps:
1) get PEG-DMA, add deionized water for stirring even, prepare ground floor PEG-DMA solution;
2) in the ground floor PEG-DMA solution making in step 1), add initator, lucifuge stirs, and then injects mould, carries out ultraviolet lighting and is cross-linked, and makes ground floor PEG-DMA hydrogel;
3) get PEG-DMA, add deionized water for stirring even, prepare second layer PEG-DMA solution;
4) in the second layer PEG-DMA solution making in step 3), add initator, lucifuge stirs, and then injects the mould that ground floor PEG-DMA hydrogel is housed, and carries out ultraviolet lighting and is cross-linked, and makes described double-deck PEG-DMA hydrogel.
2. preparation method according to claim 1, is characterized in that: the PEG-DMA concentration of described PEG-DMA solution is 10wt%～20wt%; And described ground floor PEG-DMA solution is not identical with the PEG-DMA concentration of described second layer PEG-DMA solution.
3. preparation method according to claim 1, is characterized in that: step 2) in, the crosslinked time of ultraviolet lighting is 2～3 minutes; In step 4), the crosslinked time of ultraviolet lighting is 10～15 minutes.
4. according to the preparation method described in one of them of claims 1 to 3, it is characterized in that: described initator is 2-hydroxy-2-methyl propiophenone.
5. preparation method according to claim 4, is characterized in that: the consumption of described initator is 0.5% of described PEG-DMA liquor capacity.
6. a preparation method for multilayer PEG-DMA hydrogel, comprises the following steps:
1) get PEG-DMA, add deionized water for stirring even, prepare ground floor PEG-DMA solution;
2) in the ground floor PEG-DMA solution making in step 1), add initator, lucifuge stirs, and then injects mould, carries out ultraviolet lighting and is cross-linked, and makes ground floor PEG-DMA hydrogel;
3) get PEG-DMA, add deionized water for stirring even, prepare second layer PEG-DMA solution;
4) in the second layer PEG-DMA solution making in step 3), add initator, lucifuge stirs, and then injects the mould that ground floor PEG-DMA hydrogel is housed, and carries out ultraviolet lighting and is cross-linked, and makes double-deck PEG-DMA hydrogel;
5) repeating step 3), step 4): get PEG-DMA, add deionized water for stirring even, preparation N layer PEG-DMA solution; In prepared N layer PEG-DMA solution, add initator, lucifuge stirs, and then injects the mould that N-1 layer PEG-DMA hydrogel is housed, and carries out ultraviolet lighting and is cross-linked, and makes described multilayer PEG-DMA hydrogel; Wherein N is greater than 2 natural number.
7. preparation method according to claim 6, is characterized in that: the PEG-DMA concentration of described PEG-DMA solution is 10wt%～20wt%; And described ground floor PEG-DMA solution is all not identical to the PEG-DMA concentration of described N layer PEG-DMA solution.
8. preparation method according to claim 6, is characterized in that: the ultraviolet lighting crosslinking time of ground floor PEG-DMA solution to the N-1 layer PEG-DMA solution is 2～3 minutes; The ultraviolet lighting crosslinking time of N layer PEG-DMA solution is 10～15 minutes.
9. according to the preparation method described in one of them of claim 6 to 8, it is characterized in that: described initator is 2-hydroxy-2-methyl propiophenone.
10. preparation method according to claim 9, is characterized in that: the consumption of described initator is 0.5% of described PEG-DMA liquor capacity.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106243410A (en) * | 2016-08-02 | 2016-12-21 | 西安交通大学 | A kind of hydroxyethyl chitosan/hyaluronic acid double-network hydrogel and preparation method thereof |
| CN109876193A (en) * | 2019-04-01 | 2019-06-14 | 西安交通大学 | A kind of two-layer compound paradental defect repair materials and preparation method thereof based on photocrosslinkable hydrogel |
| CN112999425A (en) * | 2021-03-01 | 2021-06-22 | 浙江大学 | Double-layer hydrogel tubular tissue engineering scaffold and preparation method thereof |
| CN113663117A (en) * | 2021-08-17 | 2021-11-19 | 南方科技大学 | Anti-swelling biological adhesive and preparation method and application thereof |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20030052003A1 (en) * | 2002-10-15 | 2003-03-20 | Kelly Patrick | Cast analyte diffusion-limiting membranes using photopolymerizable hydrophylic monomers |
| EP1803442A1 (en) * | 2005-10-28 | 2007-07-04 | Zimmer Inc. | Mineralized hydrogels and methods of making and using mineralized hydrogels |
| US20110262493A1 (en) * | 2010-04-23 | 2011-10-27 | Krishnendu Roy | Multi-layered hydrogel constructs and associated methods |
| CN102266589A (en) * | 2011-07-28 | 2011-12-07 | 西安交通大学 | Preparation method of mechanically-enhanced cell-loaded microchannel hydrogel |
-
2013
- 2013-12-24 CN CN201310722478.0A patent/CN103707587B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20030052003A1 (en) * | 2002-10-15 | 2003-03-20 | Kelly Patrick | Cast analyte diffusion-limiting membranes using photopolymerizable hydrophylic monomers |
| EP1803442A1 (en) * | 2005-10-28 | 2007-07-04 | Zimmer Inc. | Mineralized hydrogels and methods of making and using mineralized hydrogels |
| US20110262493A1 (en) * | 2010-04-23 | 2011-10-27 | Krishnendu Roy | Multi-layered hydrogel constructs and associated methods |
| CN102266589A (en) * | 2011-07-28 | 2011-12-07 | 西安交通大学 | Preparation method of mechanically-enhanced cell-loaded microchannel hydrogel |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106243410A (en) * | 2016-08-02 | 2016-12-21 | 西安交通大学 | A kind of hydroxyethyl chitosan/hyaluronic acid double-network hydrogel and preparation method thereof |
| CN106243410B (en) * | 2016-08-02 | 2018-10-30 | 西安交通大学 | A kind of hydroxyethyl chitosan/hyaluronic acid double-network hydrogel and preparation method thereof |
| CN109876193A (en) * | 2019-04-01 | 2019-06-14 | 西安交通大学 | A kind of two-layer compound paradental defect repair materials and preparation method thereof based on photocrosslinkable hydrogel |
| CN112999425A (en) * | 2021-03-01 | 2021-06-22 | 浙江大学 | Double-layer hydrogel tubular tissue engineering scaffold and preparation method thereof |
| CN113663117A (en) * | 2021-08-17 | 2021-11-19 | 南方科技大学 | Anti-swelling biological adhesive and preparation method and application thereof |
| CN113663117B (en) * | 2021-08-17 | 2022-06-21 | 南方科技大学 | Anti-swelling biological adhesive and preparation method and application thereof |
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