CN103707587B - 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 the typical biomaterial of one, owing to having the excellent performance such as good biocompatibility, the property of water-bearing, flexibility, degradability, preparation simplicity, to external world stimuli responsive sensitivity, cell chulture, organizational project, biology sensor and the field such as driver, drug delivery system are widely applied.PEG-DMA(glycol dimethacrylates) be a kind of with PEG(polyethylene glycol) hydrogel of polymeric monomer, because it has good biocompatibility, nontoxic, non-volatile, good stability, and mechanical property parameters (elastic modelling quantity, Poisson's ratio) and human body parts tissue (such as skin, musculature) are close and modifiable advantage, make it standby to be popular, be widely applied to the fields such as organizational project, insoluble drug release and hydrogel surface modification.
At present, the PEG-DMA hydrogel applied in organizational project is all individual layer, isotropic, but biological tissue's (such as skin etc.) is usually all multilayer, anisotropic, and existing individual layer PEG-DMA hydrogel is difficult to the anisotropy requirement meeting biological tissue.And due to PEG-DMA hydrogel be a kind of moisture biological soft material, it is soft, be not easy adhesion and mechanical strength is poor, cause it when building sandwich construction, as easy as rolling off a log appearance destroys, is out of shape, comes off and combines the situations such as unstable between layers, 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 evenly, prepare ground floor PEG-DMA solution;
2) in the ground floor PEG-DMA solution that step 1) is obtained, add initator, lucifuge stirs, and then injects mould, carries out ultraviolet lighting and is cross-linked, obtained ground floor PEG-DMA hydrogel;
3) get PEG-DMA, add deionized water for stirring evenly, prepare second layer PEG-DMA solution;
4) in the second layer PEG-DMA solution that step 3) is obtained, add initator, lucifuge stirs, and then injects the mould that ground floor PEG-DMA hydrogel is housed, carries out ultraviolet lighting and be cross-linked, obtained described double-deck PEG-DMA hydrogel.
Wherein in an embodiment, 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.
Wherein in an embodiment, in step 2) in, the time that ultraviolet lighting is cross-linked is 2 ~ 3 minutes; In step 4), the time that ultraviolet lighting is cross-linked is 10 ~ 15 minutes.
Wherein in an embodiment, described initator is 2-hydroxy-2-methyl propiophenone.
Wherein in an embodiment, the consumption of described initator is 0.5% of described PEG-DMA liquor capacity.
Wherein in an embodiment, the molecular weight of described PEG-DMA is 1000.
Wherein in an embodiment, the U-shaped mould that described mould is made up of glass intermediate plate, silicon rubber bar and geometrical clamp; Described silicon rubber bar is placed between glass intermediate plate, and glass intermediate plate and silicon rubber bar is clamped by geometrical clamp.
A preparation method for multilayer PEG-DMA hydrogel, comprises the following steps:
1) get PEG-DMA, add deionized water for stirring evenly, prepare ground floor PEG-DMA solution;
2) in the ground floor PEG-DMA solution that step 1) is obtained, add initator, lucifuge stirs, and then injects mould, carries out ultraviolet lighting and is cross-linked, obtained ground floor PEG-DMA hydrogel;
3) get PEG-DMA, add deionized water for stirring evenly, prepare second layer PEG-DMA solution;
4) in the second layer PEG-DMA solution that step 3) is obtained, 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, obtained double-deck PEG-DMA hydrogel;
5) repeat step 3), step 4): get PEG-DMA, add deionized water for stirring evenly, preparation n-th layer PEG-DMA solution; In obtained n-th layer PEG-DMA solution, add initator, lucifuge stirs, and then injects the mould that N-1 layer PEG-DMA hydrogel is housed, carries out ultraviolet lighting and be cross-linked, obtained described multilayer PEG-DMA hydrogel; Wherein N be greater than 2 natural number.
Wherein in an embodiment, 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-th layer PEG-DMA solution.
Wherein in an embodiment, ground floor PEG-DMA solution is 2 ~ 3 minutes to the ultraviolet lighting crosslinking time of N-1 layer PEG-DMA solution; The ultraviolet lighting crosslinking time of n-th layer PEG-DMA solution is 10 ~ 15 minutes.
Wherein in an embodiment, described initator is 2-hydroxy-2-methyl propiophenone.
Wherein in an embodiment, the consumption of described initator is 0.5% of described PEG-DMA liquor capacity.
Wherein in an embodiment, the molecular weight of described PEG-DMA is 1000.
Wherein in an embodiment, the U-shaped mould that described mould is made up of glass intermediate plate, silicon rubber bar and geometrical clamp; Described silicon rubber bar is placed between glass intermediate plate, and glass intermediate plate and silicon rubber bar is clamped by geometrical clamp.
Bilayer of the present invention, multilayer PEG-DMA hydrogel preparation method, by controlling the parameters such as PEG-DMA concentration, ultraviolet lighting crosslinking time different in every one deck PEG-DMA solution, control the different crosslinking time of every one deck PEG-DMA solution, crosslinked hardness, make every one deck PEG-DMA hydrogel have the mechanical properties such as different elastic modelling quantity, Poisson's ratio, thus anisotropic bilayer, multilayer PEG-DMA hydrogel can be formed.
In the preparation process in accordance with the present invention, the time that concentration is different and ultraviolet lighting is crosslinked of every one deck PEG-DMA solution is different, and the mechanical property such as elastic modelling quantity, Poisson's ratio of formed every one deck PEG-DMA hydrogel can be made all different.The concentration of PEG-DMA is higher, crosslinking time is longer, and the elastic modelling quantity of the PEG-DMA hydrogel formed is also larger.And mass concentration be the PEG-DMA solution of 10% ~ 20% after ultraviolet lighting is crosslinked, the elastic modelling quantity of the PEG-DMA hydrogel formed and the elastic modelling quantity (10KPa ~ 100KPa) of tissue close, can organizational project be applicable to.
When needs preparation N layer PEG-DMA hydrogel, ground floor all controls at 2 ~ 3 minutes to the ultraviolet lighting crosslinking time of N-1 layer PEG-DMA solution, lower one deck PEG-DMA solution is added under it is in completely not crosslinked state, then carry out ultraviolet lighting to be cross-linked, new being cross-linked can be there is in the PEG-DMA solution newly increased and completely not crosslinked PEG-DMA hydrogel at contact surface place, adjacent two-layer PEG-DMA hydrogel is closely linked, after adding n-th layer PEG-DMA solution, crosslinked 10 ~ 15 minutes of ultraviolet lighting, make each layer PEG-DMA hydrogel abundant, completely crosslinked.And ground floor to the ultraviolet lighting crosslinking time of N-1 layer PEG-DMA solution all controls at 2 ~ 3 minutes, can make between each layer PEG-DMA hydrogel, to reach best adhesion tight ness rating, if this ultraviolet lighting overlong time or too short, the adhesion tight ness rating between adjacent two layers PEG-DMA hydrogel all can be caused to reduce, occur problems such as 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, the initator adopting 2-hydroxy-2-methyl propiophenone to be cross-linked as 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 ensure that the PEG-DMA in PEG-DMA solution system fully can contact initator, produces best cross-linking effect.If initiator amount is too much, initator can be caused to remain and to cause toxic hazard; If initiator amount is very few, then cause hydrogel to be cross-linked 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 adopted in preparation method of the present invention, there is the advantages such as structure is simple, easy and simple to handle, reusable, owing to have employed silicon rubber bar as mould rack, it has good flexibility, PEG-DMA hydrogel can be avoided to be out of shape in preparation process, destroy.
Detailed description of the invention
Embodiment one: the preparation of double-deck PEG-DMA hydrogel
Get two panels glass intermediate plate, U-shaped silicon rubber bar and several geometrical clamps that a thickness is 2mm, be placed in by U-shaped silicon rubber bar between two panels glass intermediate plate, then glass intermediate plate and silicon rubber bar clamped with geometrical clamp, obtained thickness is the U-shaped monolayer mold of 2mm.
In beaker, add 20mL deionized water, 2g PEG-DMA, stir, obtained mass concentration is the PEG-DMA solution of 10%; Then add 0.1mL2-hydroxy-2-methyl propiophenone, wrap up beaker with tinfoil, lucifuge stirs more than 30 minutes, obtained ground floor PEG-DMA solution; With syringe, ground floor PEG-DMA solution is injected U-shaped monolayer mold, under being then placed in UV-crosslinked instrument, illumination is cross-linked 2 minutes, the ground floor PEG-DMA hydrogel that obtained mass concentration is 10%, thickness is 2mm.
In beaker, add 20mL deionized water, 4g PEG-DMA, stir, obtained mass concentration is the PEG-DMA solution of 20%; Then add 0.1mL2-hydroxy-2-methyl propiophenone, wrap up beaker with tinfoil, lucifuge stirs more than 30 minutes, obtained second layer PEG-DMA solution.
Get the U-shaped monolayer mold that ground floor PEG-DMA hydrogel is housed, horizontal positioned, take out geometrical clamp and remove the glass intermediate plate on top, be that the U-shaped silicon rubber bar correspondence of 4mm is placed on the silicon rubber bar of U-shaped monolayer mold by a thickness, then cover glass intermediate plate, and glass intermediate plate and silicon rubber bar are clamped with geometrical clamp, obtained 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 vertically is placed, with syringe, second layer PEG-DMA solution is injected U-shaped double stack mold, then under being placed in UV-crosslinked instrument, illumination is cross-linked 10 minutes, make two-layer PEG-DMA completely crosslinked, take out U-shaped double stack mold, obtained 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 two: the preparation of double-deck PEG-DMA hydrogel
Get two panels glass intermediate plate, U-shaped silicon rubber bar and several geometrical clamps that a thickness is 2mm, be placed in by U-shaped silicon rubber bar between two panels glass intermediate plate, then glass intermediate plate and silicon rubber bar clamped with geometrical clamp, obtained thickness is the U-shaped monolayer mold of 2mm.
In beaker, add 20mL deionized water, 2g PEG-DMA, stir, obtained mass concentration is the PEG-DMA solution of 10%; Then add 0.1mL2-hydroxy-2-methyl propiophenone, wrap up beaker with tinfoil, lucifuge stirs more than 30 minutes, obtained ground floor PEG-DMA solution; With syringe, ground floor PEG-DMA solution is injected U-shaped monolayer mold, under being then placed in UV-crosslinked instrument, illumination is cross-linked 2 minutes, the ground floor PEG-DMA hydrogel that obtained mass concentration is 10%, thickness is 2mm.
In beaker, add 20mL deionized water, 3g PEG-DMA, stir, obtained mass concentration is the PEG-DMA solution of 15%; Then add 0.1mL2-hydroxy-2-methyl propiophenone, wrap up beaker with tinfoil, lucifuge stirs more than 30 minutes, obtained second layer PEG-DMA solution.
Get the U-shaped monolayer mold that ground floor PEG-DMA hydrogel is housed, horizontal positioned, take out geometrical clamp and remove the glass intermediate plate on top, be that the U-shaped silicon rubber bar correspondence of 2mm is placed on the silicon rubber bar of U-shaped monolayer mold by a thickness, then cover glass intermediate plate, and glass intermediate plate and silicon rubber bar are clamped with geometrical clamp, obtained 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 vertically is placed, with syringe, second layer PEG-DMA solution is injected U-shaped double stack mold, then under being placed in UV-crosslinked instrument, illumination is cross-linked 10 minutes, make two-layer PEG-DMA completely crosslinked, take out U-shaped double stack mold, obtained 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 three: the preparation of double-deck PEG-DMA hydrogel
Get two panels glass intermediate plate, U-shaped silicon rubber bar and several geometrical clamps that a thickness is 4mm, be placed in by U-shaped silicon rubber bar between two panels glass intermediate plate, then glass intermediate plate and silicon rubber bar clamped with geometrical clamp, obtained thickness is the U-shaped monolayer mold of 4mm.
In beaker, add 20mL deionized water, 3g PEG-DMA, stir, obtained mass concentration is the PEG-DMA solution of 15%; Then add 0.1mL2-hydroxy-2-methyl propiophenone, wrap up beaker with tinfoil, lucifuge stirs more than 30 minutes, obtained ground floor PEG-DMA solution; With syringe, ground floor PEG-DMA solution is injected U-shaped monolayer mold, under being then placed in UV-crosslinked instrument, illumination is cross-linked 2 minutes, the ground floor PEG-DMA hydrogel that obtained mass concentration is 15%, thickness is 4mm.
In beaker, add 20mL deionized water, 4g PEG-DMA, stir, obtained mass concentration is the PEG-DMA solution of 20%; Then add 0.1mL2-hydroxy-2-methyl propiophenone, wrap up beaker with tinfoil, lucifuge stirs more than 30 minutes, obtained second layer PEG-DMA solution.
Get the U-shaped monolayer mold that ground floor PEG-DMA hydrogel is housed, horizontal positioned, take out geometrical clamp and remove the glass intermediate plate on top, be that the U-shaped silicon rubber bar correspondence of 2mm is placed on the silicon rubber bar of U-shaped monolayer mold by a thickness, then cover glass intermediate plate, and glass intermediate plate and silicon rubber bar are clamped with geometrical clamp, obtained 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 vertically is placed, with syringe, second layer PEG-DMA solution is injected U-shaped double stack mold, then under being placed in UV-crosslinked instrument, illumination is cross-linked 10 minutes, make two-layer PEG-DMA completely crosslinked, take out U-shaped double stack mold, obtained 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 embodiment four: three layers of PEG-DMA hydrogel
Get two panels glass intermediate plate, U-shaped silicon rubber bar and several geometrical clamps that a thickness is 2mm, be placed in by U-shaped silicon rubber bar between two panels glass intermediate plate, then glass intermediate plate and silicon rubber bar clamped with geometrical clamp, obtained thickness is the U-shaped monolayer mold of 2mm.
In beaker, add 20mL deionized water, 2g PEG-DMA, stir, obtained mass concentration is the PEG-DMA solution of 10%; Then add 0.1mL2-hydroxy-2-methyl propiophenone, wrap up beaker with tinfoil, lucifuge stirs more than 30 minutes, obtained ground floor PEG-DMA solution; With syringe, ground floor PEG-DMA solution is injected U-shaped monolayer mold, under being then placed in UV-crosslinked instrument, illumination is cross-linked 2 minutes, the ground floor PEG-DMA hydrogel that obtained mass concentration is 10%, thickness is 2mm.
In beaker, add 20mL deionized water, 3g PEG-DMA, stir, obtained mass concentration is the PEG-DMA solution of 15%; Then add 0.1mL2-hydroxy-2-methyl propiophenone, wrap up beaker with tinfoil, lucifuge stirs more than 30 minutes, obtained second layer PEG-DMA solution.
Get the U-shaped monolayer mold that ground floor PEG-DMA hydrogel is housed, horizontal positioned, take out geometrical clamp and remove the glass intermediate plate on top, be that the U-shaped silicon rubber bar correspondence of 2mm is placed on the silicon rubber bar of U-shaped monolayer mold by a thickness, then glass intermediate plate is covered, and with geometrical clamp, glass intermediate plate and silicon rubber bar are clamped, obtained thickness is the U-shaped double stack mold of 4mm, and 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 vertically is placed, with syringe, second layer PEG-DMA solution is injected U-shaped double stack mold, then under being placed in UV-crosslinked instrument, illumination is cross-linked 2 minutes, and obtained 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, obtained mass concentration is the PEG-DMA solution of 20%; Then add 0.1mL2-hydroxy-2-methyl propiophenone, wrap up beaker with tinfoil, lucifuge stirs more than 30 minutes, obtained third layer 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, be that the U-shaped silicon rubber bar correspondence of 2mm is placed on the silicon rubber bar of U-shaped double stack mold by a thickness, then glass intermediate plate is covered, and with geometrical clamp, glass intermediate plate and silicon rubber bar are clamped, obtained thickness is U-shaped three layers of mould of 6mm, and 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 hydrogel is housed vertically are placed, with syringe, third layer PEG-DMA solution is injected U-shaped three layers of mould, then under being placed in UV-crosslinked instrument, illumination is cross-linked 15 minutes, make three layers of PEG-DMA completely crosslinked, take out U-shaped three layers of mould, obtained 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 the mass concentration of 2mm, third layer PEG-DMA hydrogel is 20%, and thickness is 2mm.
Embodiment five: the performance test of multilayer PEG-DMA hydrogel
Employing micro-indentations is tested, and measure the mechanical property of the every one deck PEG-DMA hydrogel in the multilayer PEG-DMA hydrogel obtained by 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 one to embodiment four, the PEG-DMA concentration of every one deck PEG-DMA hydrogel, ultraviolet lighting crosslinking time, initiator amount and mold thickness, prepare the individual layer PEG-DMA hydrogel reference substance of its correspondence respectively;
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 the contact point found between spherical indenter and PEG-DMA hydrogel, when significant change appears in the force curve of micro-indentations instrument display, represent and arrive contact point;
4, arrange compression distance h and press-in speed v: compression distance h to set according to the thickness of PEG-DMA hydrogel, its size controls in 10% strain; Press-in speed v is set as 300 μm/s;
5, carry out relaxation test, and record power maximum F (0) and the stationary value F (∞) of relaxation curve;
6, by the modulus of shearing of following formulae discovery PEG-DMA hydrogel, Poisson's ratio and elastic modelling quantity:
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 the multilayer PEG-DMA hydrogel obtained by embodiment one to embodiment four, the Poisson's ratio of its every one deck PEG-DMA hydrogel is all not identical with elastic modelling quantity, shows 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 (such as, 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 only have expressed several embodiment of the present invention, and it describes comparatively concrete and detailed, but therefore can not 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 (5)
1. a preparation method for multilayer glycol dimethacrylates PEG-DMA hydrogel, comprises the following steps:
1) get PEG-DMA, add deionized water for stirring evenly, prepare ground floor PEG-DMA solution;
2) in step 1) add initator in obtained ground floor PEG-DMA solution, lucifuge stirs, and then injects mould, carries out ultraviolet lighting and is cross-linked, obtained ground floor PEG-DMA hydrogel;
3) get PEG-DMA, add deionized water for stirring evenly, prepare second layer PEG-DMA solution;
4) in step 3) add initator in obtained second layer PEG-DMA solution, lucifuge stirs, and then injects the mould that ground floor PEG-DMA hydrogel is housed, and carries out ultraviolet lighting and is cross-linked, obtained double-deck PEG-DMA hydrogel;
5) repeat step 3), step 4): get PEG-DMA, it is even to add deionized water for stirring, preparation n-th layer PEG-DMA solution; In obtained n-th layer PEG-DMA solution, add initator, lucifuge stirs, and then injects the mould that N-1 layer PEG-DMA hydrogel is housed, carries out ultraviolet lighting and be cross-linked, obtained described multilayer PEG-DMA hydrogel; Wherein N be greater than 2 natural number.
2. preparation method according to claim 1, is characterized in that: in described ground floor PEG-DMA solution to n-th layer PEG-DMA solution, the PEG-DMA concentration of each layer solution is 10wt% ~ 20wt%; And described ground floor PEG-DMA solution is all not identical to the PEG-DMA concentration of described n-th layer PEG-DMA solution.
3. preparation method according to claim 1, is characterized in that: ground floor PEG-DMA solution is 2 ~ 3 minutes to the ultraviolet lighting crosslinking time of N-1 layer PEG-DMA solution; The ultraviolet lighting crosslinking time of n-th layer PEG-DMA solution is 10 ~ 15 minutes.
4. according to claims 1 to 3 one of them described in preparation method, it is characterized in that: described ground floor PEG-DMA solution is 2-hydroxy-2-methyl propiophenone to the initator in n-th layer PEG-DMA solution.
5. preparation method according to claim 4, is characterized in that: described in join ground floor PEG-DMA solution to the consumption of the initator in n-th layer PEG-DMA solution and be respectively 0.5% of each layer PEG-DMA liquor capacity.
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| US20030052003A1 (en) * | 2002-10-15 | 2003-03-20 | Kelly Patrick | Cast analyte diffusion-limiting membranes using photopolymerizable hydrophylic monomers |
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| 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 |
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