CN107141493A - A kind of preparation method of the viscous tough hydrogel of double-decker - Google Patents
A kind of preparation method of the viscous tough hydrogel of double-decker Download PDFInfo
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- 239000000017 hydrogel Substances 0.000 title claims abstract description 138
- 238000002360 preparation method Methods 0.000 title claims abstract description 46
- 239000000178 monomer Substances 0.000 claims abstract description 124
- 230000002209 hydrophobic effect Effects 0.000 claims abstract description 19
- 239000003292 glue Substances 0.000 claims abstract description 18
- 239000002243 precursor Substances 0.000 claims abstract description 9
- 238000006116 polymerization reaction Methods 0.000 claims abstract description 6
- 239000002585 base Substances 0.000 claims description 111
- RWQNBRDOKXIBIV-UHFFFAOYSA-N thymine Chemical compound CC1=CNC(=O)NC1=O RWQNBRDOKXIBIV-UHFFFAOYSA-N 0.000 claims description 96
- GFFGJBXGBJISGV-UHFFFAOYSA-N Adenine Chemical compound NC1=NC=NC2=C1N=CN2 GFFGJBXGBJISGV-UHFFFAOYSA-N 0.000 claims description 71
- 229930024421 Adenine Natural products 0.000 claims description 64
- 229960000643 adenine Drugs 0.000 claims description 64
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 54
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 claims description 48
- 229940113082 thymine Drugs 0.000 claims description 48
- 239000003513 alkali Substances 0.000 claims description 46
- 238000006243 chemical reaction Methods 0.000 claims description 44
- 238000003756 stirring Methods 0.000 claims description 38
- IQFYYKKMVGJFEH-XLPZGREQSA-N Thymidine Chemical compound O=C1NC(=O)C(C)=CN1[C@@H]1O[C@H](CO)[C@@H](O)C1 IQFYYKKMVGJFEH-XLPZGREQSA-N 0.000 claims description 32
- HRPVXLWXLXDGHG-UHFFFAOYSA-N Acrylamide Chemical compound NC(=O)C=C HRPVXLWXLXDGHG-UHFFFAOYSA-N 0.000 claims description 27
- 201000004283 Shwachman-Diamond syndrome Diseases 0.000 claims description 27
- 239000011780 sodium chloride Substances 0.000 claims description 27
- 235000019333 sodium laurylsulphate Nutrition 0.000 claims description 27
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 26
- 238000012986 modification Methods 0.000 claims description 20
- 230000004048 modification Effects 0.000 claims description 20
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 18
- HFBMWMNUJJDEQZ-UHFFFAOYSA-N acryloyl chloride Chemical compound ClC(=O)C=C HFBMWMNUJJDEQZ-UHFFFAOYSA-N 0.000 claims description 18
- 230000000977 initiatory effect Effects 0.000 claims description 18
- 239000000463 material Substances 0.000 claims description 18
- 125000000913 palmityl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 claims description 18
- 239000002798 polar solvent Substances 0.000 claims description 18
- 239000004094 surface-active agent Substances 0.000 claims description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 18
- DWRXFEITVBNRMK-UHFFFAOYSA-N Beta-D-1-Arabinofuranosylthymine Natural products O=C1NC(=O)C(C)=CN1C1C(O)C(O)C(CO)O1 DWRXFEITVBNRMK-UHFFFAOYSA-N 0.000 claims description 16
- IQFYYKKMVGJFEH-UHFFFAOYSA-N beta-L-thymidine Natural products O=C1NC(=O)C(C)=CN1C1OC(CO)C(O)C1 IQFYYKKMVGJFEH-UHFFFAOYSA-N 0.000 claims description 16
- 229940104230 thymidine Drugs 0.000 claims description 16
- 239000003643 water by type Substances 0.000 claims description 14
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 9
- 239000003999 initiator Substances 0.000 claims description 9
- 229910052757 nitrogen Inorganic materials 0.000 claims description 9
- 238000000967 suction filtration Methods 0.000 claims description 9
- 230000003068 static effect Effects 0.000 claims description 8
- CZPWVGJYEJSRLH-UHFFFAOYSA-N Pyrimidine Chemical compound C1=CN=CN=C1 CZPWVGJYEJSRLH-UHFFFAOYSA-N 0.000 claims description 7
- 150000003926 acrylamides Chemical class 0.000 claims description 7
- 238000005352 clarification Methods 0.000 claims description 7
- 229910052700 potassium Inorganic materials 0.000 claims description 7
- 239000011591 potassium Substances 0.000 claims description 7
- 210000005056 cell body Anatomy 0.000 claims description 5
- 239000000499 gel Substances 0.000 claims description 5
- 239000007788 liquid Substances 0.000 claims description 5
- 210000001541 thymus gland Anatomy 0.000 claims description 5
- 239000008367 deionised water Substances 0.000 claims description 4
- 229910021641 deionized water Inorganic materials 0.000 claims description 4
- 238000001035 drying Methods 0.000 claims description 4
- 210000004907 gland Anatomy 0.000 claims description 4
- 230000010148 water-pollination Effects 0.000 claims description 4
- QUSNBJAOOMFDIB-UHFFFAOYSA-N Ethylamine Chemical compound CCN QUSNBJAOOMFDIB-UHFFFAOYSA-N 0.000 claims description 2
- -1 acryloyl Amine Chemical class 0.000 claims description 2
- USHAGKDGDHPEEY-UHFFFAOYSA-L potassium persulfate Chemical compound [K+].[K+].[O-]S(=O)(=O)OOS([O-])(=O)=O USHAGKDGDHPEEY-UHFFFAOYSA-L 0.000 claims description 2
- 238000004062 sedimentation Methods 0.000 claims description 2
- 230000015572 biosynthetic process Effects 0.000 abstract description 4
- 238000004026 adhesive bonding Methods 0.000 abstract description 3
- 230000006978 adaptation Effects 0.000 abstract description 2
- 229920000642 polymer Polymers 0.000 abstract description 2
- 238000004804 winding Methods 0.000 abstract description 2
- 238000011065 in-situ storage Methods 0.000 abstract 1
- 238000003556 assay Methods 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 4
- 238000011161 development Methods 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- 230000006399 behavior Effects 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 238000010998 test method Methods 0.000 description 2
- 239000004964 aerogel Substances 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical group [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 210000004027 cell Anatomy 0.000 description 1
- 230000008094 contradictory effect Effects 0.000 description 1
- 238000013270 controlled release Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- BXKDSDJJOVIHMX-UHFFFAOYSA-N edrophonium chloride Chemical compound [Cl-].CC[N+](C)(C)C1=CC=CC(O)=C1 BXKDSDJJOVIHMX-UHFFFAOYSA-N 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 229920002521 macromolecule Polymers 0.000 description 1
- 238000000034 method Methods 0.000 description 1
- 210000003205 muscle Anatomy 0.000 description 1
- 210000003739 neck Anatomy 0.000 description 1
- 210000000056 organ Anatomy 0.000 description 1
- 230000009329 sexual behaviour Effects 0.000 description 1
- 239000007779 soft material Substances 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 230000008961 swelling Effects 0.000 description 1
- 210000002435 tendon Anatomy 0.000 description 1
- 239000003106 tissue adhesive Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- 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
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F2/00—Processes of polymerisation
- C08F2/46—Polymerisation initiated by wave energy or particle radiation
- C08F2/48—Polymerisation initiated by wave energy or particle radiation by ultraviolet or visible light
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F220/00—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 a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/52—Amides or imides
- C08F220/54—Amides, e.g. N,N-dimethylacrylamide or N-isopropylacrylamide
- C08F220/56—Acrylamide; Methacrylamide
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- 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
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2351/00—Characterised by the use of graft polymers in which the grafted component is obtained by reactions only involving carbon-to-carbon unsaturated bonds; Derivatives of such polymers
Abstract
A kind of preparation method for gluing tough hydrogel of the present invention, including：（1）The preparation of toughening type hydrophobic association hydrogel；（2）By cohesive hydrogel precursor solution as the toughening type hydrogel surface prepared, ultraviolet irradiation is directly carried out on its surface triggers monomer to carry out carrying out in-situ polymerization formation second layer cohesive hydrogel in toughening type hydrogel surface, and finally obtained double-decker glues tough hydrogel.Toughening type hydrogel and cohesive hydrogel acted on by the IPN and winding of polymer chain to be formed it is good link, realize that hydrogel is provided simultaneously with excellent viscosity and toughness.The present invention expands the application of toughening type hydrogel and cohesive hydrogel simultaneously, and the problem of excellent viscosity and toughness can not be provided simultaneously with by breaching hydrogel.Preparation method of the present invention is simple, it is easy to operate, and with certain universality, is applicable to the perfect adaptation of most of toughening type hydrogels and cohesive hydrogel.
Description
Technical field
The invention belongs to macromolecule hydrogel technical field, it is related to the preparation method that a kind of double-decker glues tough hydrogel.
Background technology
Hydrogel has been assigned its " soft material " due to containing substantial amounts of water, and with perfect three-dimensional net structure
Characteristic, this structure is similar to bio-tissue, and hydrogel has in fields such as organizational project, medical dressing and drug controlled releases
There are greatly Research Significance and DEVELOPMENT PROSPECT.The toughness and viscosity of hydrogel are always the critical nature that people are pursued, and this two
Plant property significant to practical application.Toughening type hydrogel is wide due to its excellent tensility and fatigue resistance
General is applied to the fields such as tendon, artificial muscle, man-made organ and hydrogel scaffold.However, toughening type hydrogel is because have
Higher cohesive force, causes molecular chain movement difficult, toughening type hydrogel is lost the ability for bonding other objects, makes water-setting
Glue can not combine closely with effect object in certain circumstances, and this just limits toughening type hydrogel in necks such as viscosity applications
The development in domain.Hydrogel contains substantial amounts of water due to its own, and hydrone can reduce viscosity with bound groups formation interaction,
So the development of cohesive hydrogel is always challenging.But pass through being continually striving to for scientist, have been developed for being permitted
There is excellent sticky hydrogel more.Cohesive hydrogel is widely used in aerogel dressing, tissue adhesive, cell carrier
With the biological field such as wearable device.The power of water-setting adhesivity is determined that this is resulted in by the balance of cohesive force and cohesive force
Much have excellent sticky hydrogel mechanical property relatively low, it is impossible to bear larger external force, while also greatly limiting viscosity
Application of the hydrogel in top load environment.
In hydrogel field, the toughness and viscosity of hydrogel are a pair of mutually contradictory properties, it is impossible to while coexisting in one
Individual hydrogel, so the realization of viscous toughness hydrogel is a huge challenge.This is also perplex numerous scientists always one
Individual problem.Based on current present Research, we be directed to developing it is a kind of it is brand-new, with pervasive meaning, simple to operate
Method realizes the successful preparation of viscous toughness hydrogel, makes hydrogel while having excellent viscosity and mechanical property, to widen
The application of hydrogel, the problem of excellent viscous behavior and tough sexual behaviour can not be had simultaneously by breaking through hydrogel.
The content of the invention
Can not be while the problem of having excellent viscosity and toughness, the present invention seeks to tough in order to solve hydrogel
In the case that type hydrogel is bottom plate, second layer cohesive hydrogel, toughening type hydrogel are formed in toughening type hydrogel surface
Act on by the IPN and winding of polymer chain with cohesive hydrogel and to form good link.Make hydrogel while having excellent
Obdurability and adhering performance, the great difficult problem of toughness and viscosity can not be provided simultaneously with by breaking through previous hydrogel.
A kind of preparation method for gluing tough hydrogel of the present invention, including：（1）The preparation of toughening type hydrogel；（2）Making
The toughening type hydrogel surface formation second layer cohesive hydrogel got ready, realizes that hydrogel possesses excellent viscosity and toughness.
（1）The step of described preparation method and condition are as follows：
A. the preparation of toughening type hydrogel
By sodium chloride（NaCl）, Surfactant SDS（SDS）It is added in deionized water, is stirred at room temperature to complete
Fully dissolved；Then hydrophobic grouping hexadecyl metrhacrylate is added, and continues stirring to solution clear；Then add hydrophilic
Property monomeric acrylamide and initiator potassium persulfate, and stir to solution clear, the quality of above-mentioned each material is dense in solution
Degree is respectively 20~40g/L, 50~100g/L, 10~50g/L, 200g/L, 2g/L.Finally, the solution prepared is poured into
In the reaction mould of 100mm × 20mm × 3mm specifications, reaction mould is placed on 5~7h of reaction in 65~75oC baking oven, system
Obtain toughening type hydrogel；Sodium chloride：Surfactant SDS：Hydrophobic grouping hexadecyl metrhacrylate：It is hydrophilic
Property monomeric acrylamide：The mass ratio of light trigger 2959 is 0.20~0.40:0.5~1.0：0.1~0.5:2:0.02.
B. the modification of base
Adenine and thymine is dissolved in dimethylformamide respectively（DMF）In be configured to molar concentration be 0.5mol/L gland
Adenine solution and thymidine solution；Triethylamine is separately added into above-mentioned solution again, is placed in ice bath and stirs 30min；Respectively
Acryloyl chloride is added, under nitrogen protection, 5~7h of stirring reaction, obtains each base monomer solution of modification at room temperature；By gained
To solution in modified base monomer settled out respectively with polar solvent ether, then carries out suction filtration with Buchner funnel, general
The base monomer drying of the modification filtered out, obtains being connected to the base monomer of double bond；Base monomer used, acryloyl chloride and three
The mol ratio of ethamine is 1:1.1~1.3:1.4~1.6；The volumetric usage of polar solvent used with by sedimentation liquor capacity
Than for 7~10：1；
C. the preparation of tough hydrogel is glued
Adenine base monomer and thymine alkali bases monomer, the hydrophilic monomer acrylamide and light trigger of double bond will be connected to
2959 are added in deionized water, and stir to being completely dissolved, in solution the mass concentration of above-mentioned each material be respectively 10~
30g/L, 10~30g/L, 200g/L, 2g/L, will（a）The toughening type hydrogel of preparation is placed on 100mm × 20mm × 6mm reactions
Mould bottom, the solution configured is placed directly within and reacted equipped with toughening type hydrogel in mould, the sticky water-setting for getting well configuration
Glue precursor solution is stored in toughening type hydrogel upper surface, then will be anti-by mould in the static 10~30min of horizontal positioned of room temperature
Mould is answered to be placed in and then reaction mould is placed in ultraviolet initiation instrument, in 85% time 10~30min of initiation polymerization of light intensity, final system
Tough hydrogel must be glued；It is connected to the adenine base monomer of double bond：It is connected to the thymine alkali bases monomer of double bond：Hydrophilic monomer third
Acrylamide：The mass ratio of light trigger 2959 is 5~15:5~15:100:1.
Beneficial effect：The present invention is successfully realized while hydrogel has an excellent adhering performance with good tough
Property, the application of hydrogel is expanded, the problem of viscosity and toughness can not be provided simultaneously with by breaching hydrogel.It is of the present invention
Preparation method it is simple, it is easy to operate, with certain universality, be applicable to all toughening type water-settings with swelling behavior
The perfect adaptation of glue and cohesive hydrogel, makes hydrogel have excellent viscous tough performance.
A kind of preparation method for gluing tough aquogel system of the present invention, including（1）The preparation of toughening type hydrogel；（2）
The tough hydrogel surface formation second layer cohesive hydrogel prepared, realizes that hydrogel is provided simultaneously with excellent sticky and tough
Property.Viscous tough water-setting adhesivity produced by the present invention can reach 8N, and toughness can reach 900KPa.
Embodiment
Embodiment 1
A. the preparation of toughening type hydrogel
By 0.2g sodium chloride（NaCl）, 0.5g Surfactant SDSs（SDS）It is added in 10mL deionized waters,
It is stirred at room temperature to being completely dissolved；Then 0.1mL hydrophobic grouping hexadecyl metrhacrylates are added, and continue stirring to solution clarification
It is transparent；Then 2g hydrophilic monomers acrylamide and 0.02g initiator potassium persulfates are added, and is stirred to solution clear,
The mass concentration of above-mentioned each material is respectively 20g/L, 50g/L, 10g/L, 200g/L, 2g/L in solution.Finally, it will prepare
Solution is poured into the reaction mould of 100mm × 20mm × 3mm specifications, and reaction mould is placed in 65oC baking oven and reacts 7h,
Toughening type hydrogel is made;Sodium chloride：Surfactant SDS：Hydrophobic grouping hexadecyl metrhacrylate：Parent
Aqueous monomers acrylamide：The mass ratio of light trigger 2959 is 0.2:0.5：0.1:2:0.02.
B. the modification of base
By 1.35g（0.01mol）Adenine and 1.26g（0.01mol）Thymidine is dissolved in 20mL dimethylformamides respectively
（DMF）In, it is configured to adenine solution and thymidine solution that molar concentration is 0.5mol/L；Again into above-mentioned solution respectively
Add 1.94mL（0.014mol）Triethylamine, is placed in ice bath and stirs after 30min, adds 0.9mL（0.011mol）Acryloyl chloride,
Under nitrogen protection, stirring reaction 5h at room temperature, obtains modified adenine base monomer solution and thymine alkali bases monomer
Solution；Adenine base monomer and thymine alkali bases monomer modified in resulting solution are used into polar solvent ether respectively
Settle out, then carry out suction filtration with Buchner funnel, the adenine base monomer and thymine alkali bases of the modification that will filter out
Monomer drying, respectively obtains the adenine base monomer and thymine alkali bases monomer for being connected to double bond；Adenine and chest used
Mol ratio between gland pyrimidine and acryloyl chloride and triethylamine is 1:1.1:1.4；The volumetric usage of polar solvent used is with being sunk
The ratio for dropping liquor capacity is 7:1.
C. the preparation of tough hydrogel is glued
0.1g is connected to the adenine base monomer, 0.1g thymine alkali bases monomer, 2g hydrophilic monomer acrylamides of double bond
It is added in 10mL ionized waters, and stirs to being completely dissolved, the matter of above-mentioned each material in solution with 0.02g light triggers 2959
Amount concentration is respectively 10g/L, 10g/L, 200g/L, 2g/L, is incited somebody to action（a）The toughening type hydrogel of preparation is placed on 100mm × 20mm
The reaction mould bottom of × 6mm specifications, the solution configured is placed directly within and reacted equipped with toughening type hydrogel in mould, makes to match somebody with somebody
The cohesive hydrogel precursor solution put is stored in toughening type hydrogel upper surface, by mould in the static horizontal positioned of room temperature
Reaction mould, is then placed in ultraviolet initiation instrument by 10min, and in 85% time initiation polymerization 10min of light intensity, final be made glues tough water
Gel；It is connected to the adenine base monomer of double bond：It is connected to the thymine alkali bases monomer of double bond：Hydrophilic monomer acrylamide：
The mass ratio of light trigger 2959 is 5:5:100:1.
The method of testing of the viscous tough hydrogel tensile property prepared：Preparation length is 40mm, and width is 30mm, and thickness is
6mm hydrogel style, uses Shimadzu tensilon（Model：SHIMADZU AGS-X 10KN）Tensile property test is carried out, is surveyed
Examination speed is 40mm/min.
The method of testing of the viscous tough hydrogel peeling force prepared：Preparation length is 100mm, and width is 20mm, and thickness is 6mm
Hydrogel style, 90 ° of peel test forces are carried out with CT3 Texture instruments, peel distance is 8cm, triggering point load be 0.067N, stripping
It is 5mm/s from speed, test substrate is aluminum.
It is respectively 300KPa and 2.56N that viscous tough hydrogel tensile strength and peeling force are made in embodiment 1.
Embodiment 2
A. the preparation of toughening type hydrogel
By 0.3g sodium chloride（NaCl）, 0.7g Surfactant SDSs（SDS）It is added in 10mL deionized waters,
It is stirred at room temperature to being completely dissolved；Then 0.3mL hydrophobic grouping hexadecyl metrhacrylates are added, and continue stirring to solution clarification
It is transparent；Then add 2g monomeric acrylamides and 0.02g initiator potassium persulfates, and stir to solution clear, in solution
The mass concentration of above-mentioned each material is respectively 30g/L, 70g/L, 30 g/L, 200g/L, 2g/L.Finally, by the solution prepared
In the reaction mould for pouring into 100mm × 20mm × 3mm specifications, reaction mould is placed in 70oC baking oven and reacts 6h, is made
Toughening type hydrogel；Sodium chloride：Surfactant SDS：Hydrophobic grouping hexadecyl metrhacrylate：Hydrophily
Monomeric acrylamide：The mass ratio of light trigger 2959 is 0.3:0.7：0.3:2:0.02.
B. the modification of base
By 1.35g（0.01mol）Adenine and 1.26g（0.01mol）Thymidine is dissolved in 20mL dimethylformamides（DMF）
In, it is configured to adenine solution and thymidine solution that molar concentration is 0.5mol/L；It is separately added into again into above-mentioned solution
2.10mL（0.015mol）Triethylamine, is placed in ice bath and stirs after 30min, adds 0.95mL（0.012mol）Acryloyl chloride,
Under nitrogen protection, stirring reaction 6h at room temperature, obtains modified adenine base monomer solution and thymine alkali bases monomer is molten
Liquid；Adenine base monomer and thymine alkali bases monomer modified in resulting solution are sunk with polar solvent ether respectively
Drop is separated out, and then carries out suction filtration with Buchner funnel, the adenine base monomer and thymine alkali bases list of the modification that will filter out
Soma is dry, respectively obtains the adenine base monomer and thymine alkali bases monomer for being connected to double bond；Adenine and thymus gland used
Mol ratio between pyrimidine and acryloyl chloride and triethylamine is 1:1.2:1.5；The volumetric usage of polar solvent used is with being settled
The ratio of liquor capacity is 8:1.
C. the preparation of tough hydrogel is glued
0.2g adenine base monomer, the 0.2g for being connected to double bond is connected to the thymine alkali bases monomer of double bond, 2g hydrophily lists
Body acrylamide and 0.02g light triggers 2959 are added in 10mL ionized waters, and are stirred to being completely dissolved, above-mentioned in solution
The mass concentration of each material is respectively 20g/L, 20g/L, 200g/L, 2g/L, is incited somebody to action（a）The toughening type hydrogel of preparation is placed on
100mm × 20mm × 6mm reaction mould bottoms, the solution configured is placed directly within and reacts mould equipped with toughening type hydrogel
In, the cohesive hydrogel precursor solution for getting well configuration is stored in toughening type hydrogel upper surface, by mould in the static level of room temperature
20min is placed, then reaction mould is placed in ultraviolet initiation instrument, polymerize 20min in 85% time initiation of light intensity, it is final to be made viscous
Tough hydrogel；It is connected to the adenine base monomer of double bond：It is connected to the thymine alkali bases monomer of double bond：Hydrophilic monomer acryloyl
Amine：The mass ratio of light trigger 2959 is 10:10:100:1.
It is made with the assay method of embodiment 1, in embodiment 2 and glues tough hydrogel tensile strength and peeling force and be respectively
500KPa and 5.2N.
Embodiment 3
A. the preparation of toughening type hydrogel
By 0.4g sodium chloride（NaCl）, 1.0g Surfactant SDSs（SDS）It is added in 10mL deionized waters,
It is stirred at room temperature to being completely dissolved；Then 0.5mL hydrophobic grouping hexadecyl metrhacrylates are added, and continue stirring to solution clarification
It is transparent；Then 2g hydrophilic monomers acrylamide and 0.02g initiator potassium persulfates are added, and is stirred to solution clear,
The mass concentration of above-mentioned each material is respectively 40g/L, 100g/L, 50g/L, 200g/L, 2g/L in solution.Finally, it will prepare
Solution pour into the reaction mould of 100mm × 20mm × 3mm specifications, will reaction mould be placed in 75oC baking oven react
5h, is made toughening type hydrogel；Sodium chloride：Surfactant SDS：Hydrophobic grouping hexadecyl metrhacrylate：
Hydrophilic monomer acrylamide：The mass ratio of light trigger 2959 is 0.4:1：0.5:2:0.02.
B. the modification of base
By 1.35g（0.01mol）Adenine and 1.26g（0.01mol）Thymidine is dissolved in 20mL dimethylformamides（DMF）
In, it is configured to adenine solution and thymidine solution that molar concentration is 0.5mol/L；It is separately added into again into above-mentioned solution
2.20mL（0.016mol）Triethylamine, is placed in ice bath and stirs after 30min, adds 1.05mL（0.013mol）Acryloyl chloride,
Under nitrogen protection, stirring reaction 7h at room temperature, obtains modified adenine base monomer solution and thymine alkali bases monomer is molten
Liquid；Adenine base monomer and thymine alkali bases monomer modified in resulting solution are sunk with polar solvent ether respectively
Drop is separated out, and then carries out suction filtration with Buchner funnel, the adenine base monomer and thymine alkali bases list of the modification that will filter out
Soma is dry, respectively obtains the adenine base monomer and thymine alkali bases monomer for being connected to double bond；Adenine and thymus gland used
Mol ratio between pyrimidine and acryloyl chloride and triethylamine is 1:1.3:1.6；The volumetric usage of polar solvent used is with being settled
The ratio of liquor capacity is 10:1.
C. the preparation of tough hydrogel is glued
0.3g is connected to the adenine base monomer, 0.3g thymine alkali bases monomer, 2g hydrophilic monomer acrylamides of double bond
It is added in 10mL ionized waters, and stirs to being completely dissolved, the matter of above-mentioned each material in solution with 0.02g light triggers 2959
Amount concentration is respectively 30g/L, 30g/L, 200g/L, 2g/L, is incited somebody to action（a）The toughening type hydrogel of preparation is placed on 100mm × 20mm
× 6mm reacts mould bottom, and the solution configured is placed directly within and reacted equipped with toughening type hydrogel in mould, makes what configuration was got well
Cohesive hydrogel precursor solution is stored in toughening type hydrogel upper surface, by mould in the static horizontal positioned 30min of room temperature, then
Reaction mould is placed in ultraviolet initiation instrument, in 85% time initiation polyase 13 0min of light intensity, final be made glues tough hydrogel；It is connected to double
The adenine base monomer of key：It is connected to the thymine alkali bases monomer of double bond：Hydrophilic monomer acrylamide：Light trigger 2959
Mass ratio is 15:15:100:1.
It is made with the assay method of embodiment 1, in embodiment 3 and glues tough hydrogel tensile strength and peeling force and be respectively
900KPa and 8N.
Comparative example 1
A. the preparation of toughening type hydrogel
By 0.4g sodium chloride（NaCl）, 1.0g Surfactant SDSs（SDS）It is added in 10mL deionized waters,
It is stirred at room temperature to being completely dissolved；Then 0.5mL hydrophobic grouping hexadecyl metrhacrylates are added, and continue stirring to solution clarification
It is transparent；Then 2g hydrophilic monomers acrylamide and 0.02g initiator potassium persulfates are added, and is stirred to solution clear,
The mass concentration of above-mentioned each material is respectively 40g/L, 100g/L, 50g/L, 200g/L, 2g/L in solution.Finally, it will prepare
Solution pour into the reaction mould of 100mm × 20mm × 3mm specifications, will reaction mould be placed in 75oC baking oven react
5h, is made toughening type hydrogel；Sodium chloride：Surfactant SDS：Hydrophobic grouping hexadecyl metrhacrylate：
Hydrophilic monomer acrylamide：The mass ratio of light trigger 2959 is 0.4:1：0.5:2:0.02.
Toughening type water-setting glue gel tensile strength and peeling force difference are made with the assay method of embodiment 1, in comparative example 1
For 900KPa and 0.01N.
Comparative example 2
A. the modification of base
By 1.35g（0.01mol）Adenine and 1.26g（0.01mol）Thymidine is dissolved in 20mL dimethylformamides（DMF）
In, it is configured to adenine solution and thymidine solution that molar concentration is 0.5mol/L；It is separately added into again into above-mentioned solution
2.20mL（0.016mol）Triethylamine, is placed in ice bath and stirs after 30min, adds 1.05mL（0.013mol）Acryloyl chloride,
Under nitrogen protection, stirring reaction 7h at room temperature, obtains modified adenine base monomer solution and thymine alkali bases monomer is molten
Liquid；Adenine base monomer and thymine alkali bases monomer modified in resulting solution are sunk with polar solvent ether respectively
Drop is separated out, and then carries out suction filtration with Buchner funnel, the adenine base monomer and thymine alkali bases list of the modification that will filter out
Soma is dry, respectively obtains the adenine base monomer and thymine alkali bases monomer for being connected to double bond；Adenine and thymus gland used
Mol ratio between pyrimidine and acryloyl chloride and triethylamine is 1:1.3:1.6；The volumetric usage of polar solvent used is with being settled
The ratio of liquor capacity is 10:1.
B. the preparation of cohesive hydrogel
0.3g is connected to the adenine base monomer, 0.3g thymine alkali bases monomer, 2g hydrophilic monomer acrylamides of double bond
It is added in 10mL ionized waters, and stirs to being completely dissolved, the matter of above-mentioned each material in solution with 0.02g light triggers 2959
It is respectively 30g/L, 30g/L, 200g/L, 2g/L to measure concentration, and it is anti-that the solution configured is placed directly within into 100mm × 20mm × 3mm
Mould is answered, then reaction mould is placed in ultraviolet initiation instrument, in 85% time initiation polymerization 10min of light intensity, final be made glues tough water
Gel；It is connected to the adenine base monomer of double bond：It is connected to the thymine alkali bases monomer of double bond：Hydrophilic monomer acrylamide：
The mass ratio of light trigger 2959 is 15:15:100:1.
With the assay method of embodiment 1, cohesive hydrogel gel tensile strength is made in comparative example 2 and peeling force is respectively
30KPa and 7.89N.
Claims (4)
1. a kind of double-decker glues the preparation method of the preparation method of tough hydrogel, it is characterised in that step and condition are as follows：
A. the preparation of toughening type hydrogel
By sodium chloride（NaCl）, Surfactant SDS（SDS）It is added in deionized water, is stirred at room temperature to complete
Fully dissolved；Then hydrophobic grouping hexadecyl metrhacrylate is added, and continues stirring to solution clear；Then add hydrophilic
Property monomeric acrylamide and initiator potassium persulfate, and stir to solution clear, the quality of above-mentioned each material is dense in solution
Degree is respectively 20~40g/L, 50~100g/L, 10~50 g/L, 200g/L, 2g/L；Finally, the solution prepared is poured into
In the reaction mould of 100mm × 20mm × 3mm specifications, reaction mould is placed on 5~7h of reaction in 65~75oC baking oven, system
Obtain toughening type hydrogel；Sodium chloride：Surfactant SDS：Hydrophobic grouping hexadecyl metrhacrylate：It is hydrophilic
Property monomeric acrylamide：The mass ratio of light trigger 2959 is 0.20~0.40:0.5~1.0：0.1~0.5:2:0.02；
B. the modification of base
Adenine and thymine is dissolved in dimethylformamide respectively（DMF）In be configured to molar concentration be 0.5mol/L gland
Adenine solution and thymidine solution；Triethylamine is separately added into above-mentioned solution again, is placed in ice bath and stirs 30min；Respectively
Acryloyl chloride is added, under nitrogen protection, 5~7h of stirring reaction, obtains each base monomer solution of modification at room temperature；By gained
To solution in modified base monomer settled out respectively with polar solvent ether, then carries out suction filtration with Buchner funnel, general
The base monomer drying of the modification filtered out, obtains being connected to the base monomer of double bond；Base monomer used, acryloyl chloride and three
The mol ratio of ethamine is 1:1.1~1.3:1.4~1.6；The volumetric usage of polar solvent used with by sedimentation liquor capacity
Than for 7~10：1；
C. the preparation of tough hydrogel is glued
Adenine base monomer and thymine alkali bases monomer, the hydrophilic monomer acrylamide and light trigger of double bond will be connected to
2959 are added in deionized water, and stir to being completely dissolved, in solution the mass concentration of above-mentioned each material be respectively 10~
30g/L, 10~30g/L, 200g/L, 2g/L, will（a）The toughening type hydrogel of preparation is placed on 100mm × 20mm × 6mm reactions
Mould bottom, the solution configured is placed directly within and reacted equipped with toughening type hydrogel in mould, the sticky water-setting for getting well configuration
Glue precursor solution is stored in toughening type hydrogel upper surface, then will be anti-by mould in the static 10~30min of horizontal positioned of room temperature
Mould is answered to be placed in and then reaction mould is placed in ultraviolet initiation instrument, in 85% time 10~30min of initiation polymerization of light intensity, final system
Tough hydrogel must be glued；It is connected to the adenine base monomer of double bond：It is connected to the thymine alkali bases monomer of double bond：Hydrophilic monomer third
Acrylamide：The mass ratio of light trigger 2959 is 5~15:5~15:100:1.
2. a kind of double-decker as claimed in claim 1 glues the preparation method of tough hydrogel, it is characterised in that step and condition
It is as follows：
A. the preparation of toughening type hydrogel
By 0.2g sodium chloride（NaCl）, 0.5g Surfactant SDSs（SDS）It is added in 10mL deionized waters,
It is stirred at room temperature to being completely dissolved；Then 0.1mL hydrophobic grouping hexadecyl metrhacrylates are added, and continue stirring to solution clarification
It is transparent；Then 2g hydrophilic monomers acrylamide and 0.02g initiator potassium persulfates are added, and is stirred to solution clear,
The mass concentration of above-mentioned each material is respectively 20g/L, 50g/L, 10g/L, 200g/L, 2g/L in solution；Finally, it will prepare
Solution is poured into the reaction mould of 100mm × 20mm × 3mm specifications, and reaction mould is placed in 65oC baking oven and reacts 7h,
Toughening type hydrogel is made;Sodium chloride：Surfactant SDS：Hydrophobic grouping hexadecyl metrhacrylate：Parent
Aqueous monomers acrylamide：The mass ratio of light trigger 2959 is 0.2:0.5：0.1:2:0.02；
B. the modification of base
By 1.35g（0.01mol）Adenine and 1.26g（0.01mol）Thymidine is dissolved in 20mL dimethylformamides respectively
（DMF）In, it is configured to adenine solution and thymidine solution that molar concentration is 0.5mol/L；Again into above-mentioned solution respectively
Add 1.94mL（0.014mol）Triethylamine, is placed in ice bath and stirs after 30min, adds 0.9mL（0.011mol）Acryloyl chloride,
Under nitrogen protection, stirring reaction 5h at room temperature, obtains modified adenine base monomer solution and thymine alkali bases monomer
Solution；Adenine base monomer and thymine alkali bases monomer modified in resulting solution are used into polar solvent ether respectively
Settle out, then carry out suction filtration with Buchner funnel, the adenine base monomer and thymine alkali bases of the modification that will filter out
Monomer drying, respectively obtains the adenine base monomer and thymine alkali bases monomer for being connected to double bond；Adenine and chest used
Mol ratio between gland pyrimidine and acryloyl chloride and triethylamine is 1:1.1:1.4；The volumetric usage of polar solvent used is with being sunk
The ratio for dropping liquor capacity is 7:1；
C. the preparation of tough hydrogel is glued
0.1g is connected to the adenine base monomer, 0.1g thymine alkali bases monomer, 2g hydrophilic monomer acrylamides of double bond
It is added in 10mL ionized waters, and stirs to being completely dissolved, the matter of above-mentioned each material in solution with 0.02g light triggers 2959
Amount concentration is respectively 10g/L, 10g/L, 200g/L, 2g/L, is incited somebody to action（a）The toughening type hydrogel of preparation is placed on 100mm × 20mm
The reaction mould bottom of × 6mm specifications, the solution configured is placed directly within and reacted equipped with toughening type hydrogel in mould, makes to match somebody with somebody
The cohesive hydrogel precursor solution put is stored in toughening type hydrogel upper surface, by mould in the static horizontal positioned of room temperature
Reaction mould, is then placed in ultraviolet initiation instrument by 10min, and in 85% time initiation polymerization 10min of light intensity, final be made glues tough water
Gel；It is connected to the adenine base monomer of double bond：It is connected to the thymine alkali bases monomer of double bond：Hydrophilic monomer acrylamide：
The mass ratio of light trigger 2959 is 5:5:100:1.
3. a kind of double-decker as claimed in claim 1 glues the preparation method of tough hydrogel, it is characterised in that step and condition
It is as follows：
A. the preparation of toughening type hydrogel
By 0.3g sodium chloride（NaCl）, 0.7g Surfactant SDSs（SDS）It is added in 10mL deionized waters,
It is stirred at room temperature to being completely dissolved；Then 0.3mL hydrophobic grouping hexadecyl metrhacrylates are added, and continue stirring to solution clarification
It is transparent；Then add 2g monomeric acrylamides and 0.02g initiator potassium persulfates, and stir to solution clear, in solution
The mass concentration of above-mentioned each material is respectively 30g/L, 70g/L, 30 g/L, 200g/L, 2g/L；Finally, by the solution prepared
In the reaction mould for pouring into 100mm × 20mm × 3mm specifications, reaction mould is placed in 70oC baking oven and reacts 6h, is made
Toughening type hydrogel；Sodium chloride：Surfactant SDS：Hydrophobic grouping hexadecyl metrhacrylate：Hydrophily
Monomeric acrylamide：The mass ratio of light trigger 2959 is 0.3:0.7：0.3:2:0.02；
B. the modification of base
By 1.35g（0.01mol）Adenine and 1.26g（0.01mol）Thymidine is dissolved in 20mL dimethylformamides（DMF）
In, it is configured to adenine solution and thymidine solution that molar concentration is 0.5mol/L；It is separately added into again into above-mentioned solution
2.10mL（0.015mol）Triethylamine, is placed in ice bath and stirs after 30min, adds 0.95mL（0.012mol）Acryloyl chloride,
Under nitrogen protection, stirring reaction 6h at room temperature, obtains modified adenine base monomer solution and thymine alkali bases monomer is molten
Liquid；Adenine base monomer and thymine alkali bases monomer modified in resulting solution are sunk with polar solvent ether respectively
Drop is separated out, and then carries out suction filtration with Buchner funnel, the adenine base monomer and thymine alkali bases list of the modification that will filter out
Soma is dry, respectively obtains the adenine base monomer and thymine alkali bases monomer for being connected to double bond；Adenine and thymus gland used
Mol ratio between pyrimidine and acryloyl chloride and triethylamine is 1:1.2:1.5；The volumetric usage of polar solvent used is with being settled
The ratio of liquor capacity is 8:1；
C. the preparation of tough hydrogel is glued
0.2g adenine base monomer, the 0.2g for being connected to double bond is connected to the thymine alkali bases monomer of double bond, 2g hydrophily lists
Body acrylamide and 0.02g light triggers 2959 are added in 10mL ionized waters, and are stirred to being completely dissolved, above-mentioned in solution
The mass concentration of each material is respectively 20g/L, 20g/L, 200g/L, 2g/L, is incited somebody to action（a）The toughening type hydrogel of preparation is placed on
100mm × 20mm × 6mm reaction mould bottoms, the solution configured is placed directly within and reacts mould equipped with toughening type hydrogel
In, the cohesive hydrogel precursor solution for getting well configuration is stored in toughening type hydrogel upper surface, by mould in the static level of room temperature
20min is placed, then reaction mould is placed in ultraviolet initiation instrument, polymerize 20min in 85% time initiation of light intensity, it is final to be made viscous
Tough hydrogel；It is connected to the adenine base monomer of double bond：It is connected to the thymine alkali bases monomer of double bond：Hydrophilic monomer acryloyl
Amine：The mass ratio of light trigger 2959 is 10:10:100:1.
4. a kind of double-decker as claimed in claim 1 glues the preparation method of tough hydrogel, it is characterised in that step and condition
It is as follows：
A. the preparation of toughening type hydrogel
By 0.4g sodium chloride（NaCl）, 1.0g Surfactant SDSs（SDS）It is added in 10mL deionized waters,
It is stirred at room temperature to being completely dissolved；Then 0.5mL hydrophobic grouping hexadecyl metrhacrylates are added, and continue stirring to solution clarification
It is transparent；Then 2g hydrophilic monomers acrylamide and 0.02g initiator potassium persulfates are added, and is stirred to solution clear,
The mass concentration of above-mentioned each material is respectively 40g/L, 100g/L, 50g/L, 200g/L, 2g/L in solution；Finally, it will prepare
Solution pour into the reaction mould of 100mm × 20mm × 3mm specifications, will reaction mould be placed in 75oC baking oven react
5h, is made toughening type hydrogel；Sodium chloride：Surfactant SDS：Hydrophobic grouping hexadecyl metrhacrylate：
Hydrophilic monomer acrylamide：The mass ratio of light trigger 2959 is 0.4:1：0.5:2:0.02；
B. the modification of base
By 1.35g（0.01mol）Adenine and 1.26g（0.01mol）Thymidine is dissolved in 20mL dimethylformamides（DMF）
In, it is configured to adenine solution and thymidine solution that molar concentration is 0.5mol/L；It is separately added into again into above-mentioned solution
2.20mL（0.016mol）Triethylamine, is placed in ice bath and stirs after 30min, adds 1.05mL（0.013mol）Acryloyl chloride,
Under nitrogen protection, stirring reaction 7h at room temperature, obtains modified adenine base monomer solution and thymine alkali bases monomer is molten
Liquid；Adenine base monomer and thymine alkali bases monomer modified in resulting solution are sunk with polar solvent ether respectively
Drop is separated out, and then carries out suction filtration with Buchner funnel, the adenine base monomer and thymine alkali bases list of the modification that will filter out
Soma is dry, respectively obtains the adenine base monomer and thymine alkali bases monomer for being connected to double bond；Adenine and thymus gland used
Mol ratio between pyrimidine and acryloyl chloride and triethylamine is 1:1.3:1.6；The volumetric usage of polar solvent used is with being settled
The ratio of liquor capacity is 10:1；
C. the preparation of tough hydrogel is glued
0.3g is connected to the adenine base monomer, 0.3g thymine alkali bases monomer, 2g hydrophilic monomer acrylamides of double bond
It is added in 10mL ionized waters, and stirs to being completely dissolved, the matter of above-mentioned each material in solution with 0.02g light triggers 2959
Amount concentration is respectively 30g/L, 30g/L, 200g/L, 2g/L, is incited somebody to action（a）The toughening type hydrogel of preparation is placed on 100mm × 20mm
× 6mm reacts mould bottom, and the solution configured is placed directly within and reacted equipped with toughening type hydrogel in mould, makes what configuration was got well
Cohesive hydrogel precursor solution is stored in toughening type hydrogel upper surface, by mould in the static horizontal positioned 30min of room temperature, then
Reaction mould is placed in ultraviolet initiation instrument, in 85% time initiation polyase 13 0min of light intensity, final be made glues tough hydrogel；It is connected to double
The adenine base monomer of key：It is connected to the thymine alkali bases monomer of double bond：Hydrophilic monomer acrylamide：Light trigger 2959
Mass ratio is 15:15:100: 1.
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| CN107597735A (en) * | 2017-09-19 | 2018-01-19 | 长春工业大学 | A kind of hydrogel cleaning cleaner and preparation method |
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| CN112898483A (en) * | 2021-01-24 | 2021-06-04 | 南开大学 | Preparation method of bionic hydrophobic association conductive hydrogel with high resilience and high sensitivity |
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| CN112898483A (en) * | 2021-01-24 | 2021-06-04 | 南开大学 | Preparation method of bionic hydrophobic association conductive hydrogel with high resilience and high sensitivity |
| CN112898483B (en) * | 2021-01-24 | 2022-04-15 | 南开大学 | Preparation method of bionic hydrophobic association conductive hydrogel with high resilience and high sensitivity |
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