CN106832137A - A kind of high-strength composite hydrogel and preparation method thereof - Google Patents
A kind of high-strength composite hydrogel and preparation method thereof Download PDFInfo
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- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F265/00—Macromolecular compounds obtained by polymerising monomers on to polymers of unsaturated monocarboxylic acids or derivatives thereof as defined in group C08F20/00
- C08F265/10—Macromolecular compounds obtained by polymerising monomers on to polymers of unsaturated monocarboxylic acids or derivatives thereof as defined in group C08F20/00 on to polymers of amides or imides
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- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F120/00—Homopolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride, ester, amide, imide or nitrile thereof
- C08F120/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F120/52—Amides or imides
- C08F120/54—Amides, e.g. N,N-dimethylacrylamide or N-isopropylacrylamide
- C08F120/56—Acrylamide; Methacrylamide
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- C08F2/00—Processes of polymerisation
- C08F2/44—Polymerisation in the presence of compounding ingredients, e.g. plasticisers, dyestuffs, fillers
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- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/02—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques
- C08J3/03—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques in aqueous media
- C08J3/075—Macromolecular gels
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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- C08K3/36—Silica
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- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2333/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Derivatives of such polymers
- C08J2333/24—Homopolymers or copolymers of amides or imides
- C08J2333/26—Homopolymers or copolymers of acrylamide or methacrylamide
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Abstract
The invention belongs to biomedicine field, a kind of high-strength composite hydrogel and preparation method thereof is specifically disclosed.Polyacrylamide is bonded simultaneously by the SiO 2 molecular sieve of Nano grade inside its surface and duct to form.Take SiO 2 molecular sieve, acrylamide and the ammonium persulfate aqueous solution of Nano grade, stirring to dirty solution；After ultrasonic disperse is uniform, vacuumize, be centrifuged, take out precipitation, be dried to obtain composite molecular screen；The composite molecular screen that will be prepared is well mixed with acrylamide aqueous solution, vacuumizes, and is warming up to 75 ~ 85 DEG C, and 30 ~ 40min of isothermal reaction obtains viscous liquid；It is put into mould, adds N, the N bismethacrylamide aqueous solution heats 7 ~ 8h, obtains final product composite aquogel in 50 ~ 60 DEG C.Gained high-strength composite hydrogel of the invention has good mechanical property, and preparation method is easy to operate.
Description
Technical field
The invention belongs to biomedicine field, and in particular to a kind of high-strength composite hydrogel and preparation method thereof.
Background technology
In today's society, hydrogel increasingly changes the life of people, and it can be as protection cell or other materials
Medium, and with conductibility and biocompatibility very high.Additionally, it can also inject and be easy to be modified, in medical treatment side
Face has very big proper value, can solve the problem that many social concerns.Specifically there are following several applications, one can be used as biological doctor
Use material（Pharmaceutical carrier, contact lenses, artificial-muscle）；Two is in terms of petrochemical industry（Oil displacement agent, dehydrating agent）；Three is in agriculture
Industry aspect（Water-loss reducer, condensation preventing agent）；Four can serve as daily, cosmetics（Sanitary napkin, paper diaper, facial mask etc.）.Wherein most
Important field is exactly biological medicine engineering.However, because hydrogel mechanical strength is relatively low, greatly limit it in many fields
Application, such as nondegradable pharmaceutical carrier, tissue engineering bracket, enzyme engineering, cell engineering.It is well known that substantial amounts of life
Modulus rank needed for thing material is kPa level, because the modulus of many natural tissues is exactly this rank.Such as the nasal cartilages of people
（234kPa±27kPa）, ox articular cartilage（990kPa±50kPa）, pig thoracic aorta（43.2kPa±15kPa）Deng.
In tissue engineering bracket field, the mechanical strength of polymer substrate must match with the environment of surrounding tissue.Therefore, hydrogel
Mechanical strength be it as bio-medical material one of important performance indexes.Recent domestic researcher be devoted to as
What improves the mechanical strength of hydrogel.
The content of the invention
To solve the deficiencies in the prior art, it is an object of the invention to provide a kind of preparation side of high-strength composite hydrogel
Method, gained high-strength composite hydrogel has good mechanical property, and preparation method is easy to operate.
To achieve the above object, the technical scheme that the present invention takes is as follows：
A kind of high-strength composite hydrogel, is bonded simultaneously by the SiO 2 molecular sieve of Nano grade inside its surface and duct
Polyacrylamide is formed.
Preparation method, comprises the following steps：
S0, the prior acrylamide aqueous solution of preparation respectively, ammonium persulfate aqueous solution and N, N- the bismethacrylamide aqueous solution：
The mass percent concentration of acrylamide aqueous solution is 15 ~ 40%, the mass percent concentration of ammonium persulfate aqueous solution for 0.5 ~
The mass percent concentration of 3%, N, N- the bismethacrylamide aqueous solution is 0.4 ~ 1%；
The preparation of S1, composite molecular screen：
S1.1, according to mass volume ratio meter, SiO 2 molecular sieve: acrylamide: ammonium persulfate aqueous solution=0.3 ~ 0.7g: 2 ~
4g: 20 ~ 30mL, takes SiO 2 molecular sieve, acrylamide and the ammonium persulfate aqueous solution of Nano grade, and stirring is to as uniform
Dirty solution；
S1.2, by dirty solution ultrasonic disperse it is uniform after, the bubble being evacuated in SiO 2 molecular sieve is wholly absent；
S1.3, will vacuumize gained mixed liquor be centrifuged, take out precipitation, be dried to obtain composite molecular screen；
The initiation polymerization of S2, high-strength composite hydrogel：
S2.1, the composite molecular screen that S1 is prepared is well mixed with acrylamide aqueous solution, vacuumized；
S2.2, S2.1 gained systems are warming up to 75 ~ 85 DEG C, 30 ~ 40min of isothermal reaction obtains viscous liquid；
S2.3, viscous liquid is put into mould, adds N, the N- bismethacrylamide aqueous solution, in 50 ~ 60 DEG C plus
7 ~ 8h of heat, obtains final product composite aquogel；
Wherein, in S2.1 and S2.3, according to mass volume ratio meter, composite molecular screen: acrylamide aqueous solution: N, N- dimethyl are double
Acrylamide aqueous solution=0.5 ~ 2.5g: 45 ~ 55mL: 0.2 ~ 0.4mL.
The SiO 2 molecular sieve addressed in the present invention, macroshape is powdered, and micro-shape is in elliposoidal, with short
And regular duct, be conducive to making full use of the activity of its inner surface；Particle diameter size is about in 10nm-15nm, particle size
It is of substantially equal, it is dispersed, with many powder structure cells exposed to outside.The structure makes the side of SiO 2 molecular sieve powder one
Face has a larger specific surface area, and is easy in surface and duct that ammonium persulfate etc. draws in attachment with short and regular duct
Hair agent, preferably triggers acrylamide polymerization；On the other hand there is more preferable adsorption capacity, initiator is in its surface and duct
Can effectively be loaded, so as to make acrylamide monomer trigger growth with effectively attachment in duct in its surface.
The present invention triggers acrylamide homopolymerization method to prepare high intensity water rubber using nanometer grade silica molecular sieve low pressure：
First, the nanometer grade silica molecular sieve with pore passage structure is scattered in acrylamide monomer and initiator（Ammonium persulfate）
The aqueous solution in, then by well-mixed liquid draw vacuum so that the bubble in molecular sieve replaces with mixed liquor completely, then is centrifuged
It is composite molecular screen to obtain molecular sieve solid；Then, added composite molecular screen as initiator in the aqueous solution of acrylamide
Vacuumize, low-pressure heating triggers acrylamide polymerization, obtain viscous liquid；Finally, crosslinking agent is further added（N, N- bis-
Bisacrylamide）Reaction is allowed to continue to, hydrogel is obtained.
Beneficial effect：
1st, after molecular sieve is vacuumized by the ultrasonic disperse in the initiator, initiator, dioxy are contained among microporous molecular sieve
SiClx molecular sieve is both the center for triggering acrylamide polymerization, is also the center for reinforcing polymer strength, and the addition of molecular sieve makes
Acrylamide carries out network polymerization centered on molecular sieve, portion's structure of the hydrogel that standardized so that hydrogel is in stress
When be able to be uniformly distributed stress, prevent stress concentrate cause fracture etc. plastic strain, and Nano grade molecular sieve powder
Surface area can be greatly increased, so as to improve the active forces such as the hydrogen bond on surface, increases intensity, improve mechanical property.
2nd, nanometer grade silica molecular sieve of the present invention triggers acrylamide polymerization under low pressure, in eliminating traditional handicraft
Logical nitrogen link, and reduce heating-up temperature and heat time, reduce cost.
Brief description of the drawings
Fig. 1 is embodiment 1（A, multiplication factor 300）With reference examples 1（B, multiplication factor 500）Method gained hydrogel
SEM schemes.
Fig. 2 is embodiment 1（A）Stretching with reference examples 1 (B) method gained hydrogel is contrasted.
Fig. 3 is the stretching that the different initiator concentrations of embodiment 1 and 2 and the ultraviolet microwave of embodiment 3 trigger lower gained hydrogel
Contrast.
Fig. 4 is the stretching contrast of gained hydrogel under the different acrylamide aqueous solution concentration of embodiment 1 and 4.
Specific embodiment
Embodiment 1
A kind of high-strength composite hydrogel, is bonded simultaneously by the SiO 2 molecular sieve of Nano grade inside its surface and duct
Polyacrylamide is formed.
Nanometer grade silica molecular sieve low pressure is taken to trigger acrylamide homopolymerization method to prepare high intensity water rubber, including with
Lower step：
S0, the prior acrylamide aqueous solution of preparation respectively, ammonium persulfate aqueous solution and N, N- the bismethacrylamide aqueous solution：
The mass percent concentration of acrylamide aqueous solution is 30%, and the mass percent concentration of ammonium persulfate aqueous solution is 2%, N, N- bis-
The mass percent concentration of the bisacrylamide aqueous solution is 1%；
The preparation of S1, composite molecular screen：
S1.1, to take 0.5g particle diameter distributions water-soluble in the SiO 2 molecular sieve of 10-15nm, 2g acrylamides and 30mL ammonium persulfates
In 250mL beakers, stirring is to as uniform dirty solution for liquid；
S1.2, dirty solution is put into ultrasonic instrument, regulating frequency is 8000 hertz, and temperature is 45 DEG C, after ultrasonic 10min, is taken out
Bubble in vacuum to SiO 2 molecular sieve is wholly absent；
S1.3, gained mixed liquor will be vacuumized averagely pour into four centrifuge tubes, be put into centrifuge, turn speed to 8000r/
Min, is centrifuged 5min；
S1.4, the precipitation taken out in centrifuge tube, are dried to obtain composite molecular screen；
The initiation polymerization of S2, high-strength composite hydrogel：
S2.1, the composite molecular screen that 0.5g S1 are prepared and 50mL acrylamide aqueous solutions are mixed into round-bottomed flask, take out true
It is empty；
S2.2, S2.1 gained system oil baths are warming up to 80 DEG C, isothermal reaction 35min obtains viscous liquid；
S2.3, viscous liquid is put into mould, adds 0.2mL N, the N- bismethacrylamide aqueous solution, in 55 DEG C
Heating 7h, obtains final product composite aquogel.
Reference examples 1
Acrylamide homopolymerization method is triggered to prepare high intensity water rubber with the nanometer grade silica molecular sieve low pressure of embodiment 1（It is real
Matter process is：Ammonium persulfate is first loaded over a molecular sieve, triggers polymerization again afterwards）Difference, this example is to be directly added into ammonium persulfate
Initiator prepares hydrogel, and step is as follows：
S0, the prior acrylamide aqueous solution of preparation respectively, ammonium persulfate aqueous solution and N, N- the bismethacrylamide aqueous solution：
The mass percent concentration of acrylamide aqueous solution is 30%, and the mass percent concentration of ammonium persulfate aqueous solution is 2%, N, N- bis-
The mass percent concentration of the bisacrylamide aqueous solution is 1%；
The initiation polymerization of S1, hydrogel：
S1.1,50mL acrylamide aqueous solutions are added in round-bottomed flask, 0.2mL ammonium persulfate aqueous solutions are added dropwise, vacuumized；
S1.2, S1.1 gained system oil baths are warming up to 80 DEG C, isothermal reaction 35min obtains viscous liquid；
S1.3, viscous liquid is put into mould, adds 0.2mL N, the N- bismethacrylamide aqueous solution, in 55 DEG C
Heating 7h, obtains final product hydrogel.
Fig. 1 is embodiment 1（A, multiplication factor 300）With reference examples 1（B, multiplication factor 500）Method gained hydrogel
SEM schemes.The hydrogel that two methods are obtained all is cellular, but as can be seen from the figure：The honeycomb of A more tight and
Tiny, when being stressed, stress distribution is more uniform；The honeycomb of B is more loose and irregular, honeycomb distribution dispersion,
Cavity is larger, and consistency is significantly less than the honeycomb of A, is also more prone to be broken in stress raiser when being stressed；
Show that the addition of nanometer grade silica molecular sieve improves the inner homogeneous degree and crosslinked polymer degree of hydrogel, it is regular
The structure of hydrogel, at the same molecular sieve for nanoscale contains many micropores, increased surface area so as to increase hydrogen bond number and work
Firmly, so as to increase the mechanical strength of hydrogel.
Fig. 2 is embodiment 1（A）Stretching with reference examples 1 (B) method gained hydrogel is contrasted.It can be seen that：Identical should
Under the conditions of power, the hydrogel that the molecular sieve after load is prepared has more excellent tensile property；Under identical tension, molecular sieve
The hydrogel of initiation possesses more preferable intensity, should change it is small, deformation more not substantially, fracture tension also reach
36.5Mpa, and then deformation substantially and under the stress less than 15MPa is just sent out under unitstress to be directly added into initiator ammonium persulfate
Fracture is given birth to.Illustrate the improvement of hydrogel tensile strength and molecular sieve use so that acrylamide polymerization it is more regular it is uniform,
The increase of polyacrylamide strand crosslink density is relevant.
Embodiment 2
Difference with embodiment 1 is：In S0, the mass percent concentration difference of the initiator ammonium persulfate aqueous solution is adjusted
It is 0.5%, 1%, 3%.
Embodiment 3
Difference with embodiment 1 is that S2 takes ultraviolet microwave to trigger polymerization, and its step is：
S2.1, the composite molecular screen that 0.5g S1 are prepared and 50mL acrylamide aqueous solutions are placed in pipe, are passed through nitrogen
Sealing orifice after 15min；
S2.2, pipe is placed in the microwave ultraviolet ultrasonic wave Trinity synthesis extractive reaction instrument in, at lower 80 DEG C of ultraviolet microwave
Reason 3h, is obtained composite aquogel.
Fig. 3 is the stretching that the different initiator concentrations of embodiment 1 and 2 and the ultraviolet microwave of embodiment 3 trigger lower gained hydrogel
Contrast.It can be seen that：Under identical tension, with the increase of initiator concentration, just start tensile strength as increase is notable, but
Tensile property has micro decline on the contrary after initiator concentration reaches 2 percent, it may be possible to because kinetic chain length is with triggering
Two/first power of agent concentration is inversely proportional { according to v=Kp/2（fKd*Kt）2* [M]/[I] }, initiator concentration draws after improving
Hair speed is too fast, and rate of chain growth increases unhappy, kinetic chain length（That is molecular chain length）Decline, therefore be in initiator concentration
Tensile strength reaches maximum when 2%, and mechanical property is the most excellent；And during ultraviolet microwave initiation, microwave can increase molecular sieve table
Face activity, increases the energy needed for providing initiation reaction, and because ultraviolet microwave triggers, trigger rate is too fast to cause what is prepared
Hydrogel intensity is too low, and tensile property is poor.
Embodiment 4
Difference with embodiment 1 is：In S0, the mass percent concentration for adjusting acrylamide aqueous solution is respectively 15%,
20%、25%、35%、40%。
Fig. 4 is the stretching contrast of gained hydrogel under the different acrylamide aqueous solution concentration of embodiment 1 and 4.It can be seen that：
With the increase of acrylamide aqueous solution concentration, the mechanical property of the hydrogel prepared is gradually more excellent, tensile strength by
It is cumulative plus, unit tensile elongation needs bigger tensile force, especially reached when acrylamide aqueous solution concentration is 30% it is best,
Then when acrylamide aqueous solution concentration is improved to 35% and 40%, although but unit length tensile force increases its fracture strength
Decline, it may be possible to cause that the hydrogel prepared there are substantial amounts of monomer remnants because acrylamide aqueous solution concentration is excessive,
So that the mechanical property of hydrogel has declined on the contrary.
Claims (2)
1. a kind of high-strength composite hydrogel, it is characterised in that：By the SiO 2 molecular sieve of Nano grade in its surface and hole
Road inside is bonded polyacrylamide and forms simultaneously.
2. a kind of method for preparing high-strength composite hydrogel as claimed in claim 1, it is characterised in that comprise the following steps：
S0, the prior acrylamide aqueous solution of preparation respectively, ammonium persulfate aqueous solution and N, N- the bismethacrylamide aqueous solution：
The mass percent concentration of acrylamide aqueous solution is 15 ~ 40%, the mass percent concentration of ammonium persulfate aqueous solution for 0.5 ~
The mass percent concentration of 3%, N, N- the bismethacrylamide aqueous solution is 0.4 ~ 1%；
The preparation of S1, composite molecular screen：
S1.1, according to mass volume ratio meter, SiO 2 molecular sieve: acrylamide: ammonium persulfate aqueous solution=0.3 ~ 0.7g: 2 ~
4g: 20 ~ 30mL, takes SiO 2 molecular sieve, acrylamide and the ammonium persulfate aqueous solution of Nano grade, and stirring is to as uniform
Dirty solution；
S1.2, by dirty solution ultrasonic disperse it is uniform after, the bubble being evacuated in SiO 2 molecular sieve is wholly absent；
S1.3, will vacuumize gained mixed liquor be centrifuged, take out precipitation, be dried to obtain composite molecular screen；
The initiation polymerization of S2, high-strength composite hydrogel：
S2.1, the composite molecular screen that S1 is prepared is well mixed with acrylamide aqueous solution, vacuumized；
S2.2, S2.1 gained systems are warming up to 75 ~ 85 DEG C, 30 ~ 40min of isothermal reaction obtains viscous liquid；
S2.3, viscous liquid is put into mould, adds N, the N- bismethacrylamide aqueous solution, in 50 ~ 60 DEG C plus
7 ~ 8h of heat, obtains final product composite aquogel；
Wherein, in S2.1 and S2.3, according to mass volume ratio meter, composite molecular screen: acrylamide aqueous solution: N, N- dimethyl are double
Acrylamide aqueous solution=0.5 ~ 2.5g: 45 ~ 55mL: 0.2 ~ 0.4mL.
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| CN111333864A (en) * | 2020-03-16 | 2020-06-26 | 东北大学秦皇岛分校 | Preparation method of environment-friendly self-healing conductive hydrogel |
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