CN100506865C - Preparation method of interpenetrating network hydrogel - Google Patents
Preparation method of interpenetrating network hydrogel Download PDFInfo
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- CN100506865C CN100506865C CNB200710008807XA CN200710008807A CN100506865C CN 100506865 C CN100506865 C CN 100506865C CN B200710008807X A CNB200710008807X A CN B200710008807XA CN 200710008807 A CN200710008807 A CN 200710008807A CN 100506865 C CN100506865 C CN 100506865C
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- acrylic acid
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- 239000000017 hydrogel Substances 0.000 title claims abstract description 30
- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- 239000000178 monomer Substances 0.000 claims abstract description 39
- NIXOWILDQLNWCW-UHFFFAOYSA-N Acrylic acid Chemical compound OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims abstract description 32
- HRPVXLWXLXDGHG-UHFFFAOYSA-N Acrylamide Chemical compound NC(=O)C=C HRPVXLWXLXDGHG-UHFFFAOYSA-N 0.000 claims abstract description 26
- 229920003169 water-soluble polymer Polymers 0.000 claims abstract description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 31
- 239000000243 solution Substances 0.000 claims description 30
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 claims description 26
- 229920000642 polymer Polymers 0.000 claims description 19
- 239000003795 chemical substances by application Substances 0.000 claims description 17
- 239000003999 initiator Substances 0.000 claims description 17
- 238000013019 agitation Methods 0.000 claims description 12
- 238000003756 stirring Methods 0.000 claims description 12
- 239000004159 Potassium persulphate Substances 0.000 claims description 8
- USHAGKDGDHPEEY-UHFFFAOYSA-L potassium persulfate Chemical compound [K+].[K+].[O-]S(=O)(=O)OOS([O-])(=O)=O USHAGKDGDHPEEY-UHFFFAOYSA-L 0.000 claims description 8
- 235000019394 potassium persulphate Nutrition 0.000 claims description 8
- 238000006243 chemical reaction Methods 0.000 claims description 6
- 238000001035 drying Methods 0.000 claims description 6
- 238000000465 moulding Methods 0.000 claims description 6
- 238000006386 neutralization reaction Methods 0.000 claims description 6
- 238000000746 purification Methods 0.000 claims description 6
- 238000005406 washing Methods 0.000 claims description 6
- 239000003513 alkali Substances 0.000 claims description 4
- 239000012670 alkaline solution Substances 0.000 claims description 4
- 230000015572 biosynthetic process Effects 0.000 claims description 4
- ZIUHHBKFKCYYJD-UHFFFAOYSA-N n,n'-methylenebisacrylamide Chemical compound C=CC(=O)NCNC(=O)C=C ZIUHHBKFKCYYJD-UHFFFAOYSA-N 0.000 claims description 4
- 238000010298 pulverizing process Methods 0.000 claims description 4
- 239000000499 gel Substances 0.000 abstract description 3
- 239000000463 material Substances 0.000 abstract description 3
- 239000003814 drug Substances 0.000 abstract description 2
- 229940079593 drug Drugs 0.000 abstract description 2
- 229910001385 heavy metal Inorganic materials 0.000 abstract description 2
- 210000003205 muscle Anatomy 0.000 abstract description 2
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 8
- 238000000034 method Methods 0.000 description 6
- 238000005516 engineering process Methods 0.000 description 5
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 3
- 229920002125 Sokalan® Polymers 0.000 description 3
- 229920002401 polyacrylamide Polymers 0.000 description 3
- 239000004584 polyacrylic acid Substances 0.000 description 3
- 238000006116 polymerization reaction Methods 0.000 description 3
- 229910052700 potassium Inorganic materials 0.000 description 3
- 239000011591 potassium Substances 0.000 description 3
- 238000010521 absorption reaction Methods 0.000 description 2
- 230000006837 decompression Effects 0.000 description 2
- 238000004821 distillation Methods 0.000 description 2
- 239000004816 latex Substances 0.000 description 2
- 229920000126 latex Polymers 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 230000008961 swelling Effects 0.000 description 2
- 238000012644 addition polymerization Methods 0.000 description 1
- 229920006037 cross link polymer Polymers 0.000 description 1
- 238000004945 emulsification Methods 0.000 description 1
- 238000001879 gelation Methods 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 230000002452 interceptive effect Effects 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000006068 polycondensation reaction Methods 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
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- Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)
Abstract
This invention relates to a preparation method of interpenetrating networks hydrogel. It takes acroleic acid monomer or acrylamide monomer, acroleic acid monomer or acrylamide monomer or water-soluble polymer as materials, through prepolymerization to prepare. The gel strength of this product can reach 1.22 MPa. It has extensive application at aspects such as drug release, artificial muscle, biosensor, disengaging gear, heavy metal ion reclaiming and electric conduction gel.
Description
Technical field
The present invention relates to a kind of preparation method of novel interpenetration network hydrogel, belong to new material technology and new preparation process technical field.
Background technology
Interpenetrating net polymer (IPN) is that cross-linked polymer runs through and the interleaving network polymkeric substance that forms mutually after two kinds or two kinds.Interpenetration network hydrogel is the special hydrogel of a class that is formed by this IPN suction back of containing hydrophilic radical.
Interpenetration network hydrogel is a kind of lightly crosslinked water-swellable polymer that contains the strong hydrophilicity group of the sixties in 20th century exploitation, it can be in solvent swelling but can not be dissolved, be a kind of new function material with good development prospect.
Ipn technology is a kind of new technology that chemically realizes the polymer physics blend.Comprise two kinds of full interpenetrating(polymer)networks (IPN) and semi-intercrossing networks (semi-IPN).Each polymer network has relative independence in the IPN network, has certain dependency again simultaneously, compares with independent polymer network, and the polymer network performance that forms by the IPN technology is more superior, and gel-strength obtains raising by a relatively large margin.
At present, the preparation method of IPN hydrogel is mainly based on same footwork, the method for fractional steps and emulsion method.With footwork is that two kinds of monomers are miscible in together, makes both with each auto-polymerization of non-interfering mode and crosslinked; This method only is applicable to a kind of monomer addition polymerization and another kind of monomer carries out polycondensation.The method of fractional steps is earlier synthesizing cross-linked polymkeric substance I, makes it swelling with the monomer II that contains initiator and linking agent again, makes the monomer II in-situ polymerization then; The macroscopic view of the hydrogel of substep IPN preparation form have certain variable gradient and gel-strength lower.Latex IPN polymerization forms nucleocapsid shape water of constitution gel, and this method only limits within each latex particle scope.
Summary of the invention
The object of the present invention is to provide a kind of cost lower, gel-strength is higher, and is applied widely, prepares the preparation method of simple and easy to do interpenetration network hydrogel.
Technical scheme of the present invention is such: the preparation method of interpenetration network hydrogel, realize as follows:
The first step is removed stopper with acrylamide monomer through purification;
In second step, by acrylamide monomer: the mass ratio of water is 3:2～7, in water acrylamide monomer is dissolved, and forms uniform monomer solution;
In the 3rd step, by acrylamide monomer or water-soluble polymers: the mass ratio of water is 3:2～7, in water with its dissolving, the solution of formation homogeneous;
The 4th step, under certain stirring velocity, 0.02%～0.08% of acrylamide monomer weight linking agent and 0.2～0.5% initiator during adding second goes on foot in the monomer solution of the second step gained, control reaction temperature allows polyreaction carry out under agitation condition at 70 ℃～80 ℃;
The 5th step, treat to add when acrylamide monomer becomes the prepolymerization attitude in the 4th step the solution of the 3rd step gained, and add 0.02%～0.1% linking agent of acrylamide monomer or water-soluble polymers weight in the 3rd step and 0.4～1.2% initiator, and under certain stirring velocity, allow polyreaction proceed, the interpenetrating net polymer that viscosity is bigger forms half higher product of water content in 20 ℃～40 ℃ moulding;
In the 6th step, half product is through washing, and drying obtains the finished product interpenetrating net polymer after the pulverizing, and product suction back forms interpenetration network hydrogel.
Above-mentioned linking agent is N, N '-methylene-bisacrylamide.
Above-mentioned initiator is a Potassium Persulphate.
The preparation method of interpenetration network hydrogel, also can realize as follows:
The first step is removed stopper with Acrylic Acid Monomer through purification;
In second step, by Acrylic Acid Monomer: the mass ratio of water is 3:2～7, in water Acrylic Acid Monomer is dissolved, form uniform monomer solution, and under agitation condition, in this monomer solution, adding alkaline solution, alkali and acrylic acid mol ratio are 60%～85%, and neutralization reaction is carried out fully;
In the 3rd step, by Acrylic Acid Monomer: the mass ratio of water is 3:2～7, and with its dissolving, the solution of formation homogeneous adds alkaline solution in this solution under agitation condition in water, and alkali and acrylic acid mol ratio are 60%～85%, and neutralization reaction is carried out fully;
The 4th step, under certain stirring velocity, 0.02%～0.08% of Acrylic Acid Monomer weight linking agent and 0.2～0.5% initiator during adding second goes on foot in the solution of final gained of second step, control reaction temperature allows polyreaction carry out under agitation condition at 70 ℃～80 ℃;
The 5th step, treat to add when Acrylic Acid Monomer becomes the prepolymerization attitude in the 4th step the solution of final gained of the 3rd step, and add 0.02%～0.1% linking agent of Acrylic Acid Monomer weight in the 3rd step and 0.4～1.2% initiator, and under certain stirring velocity, allow polyreaction proceed, the interpenetrating net polymer that viscosity is bigger forms half higher product of water content in 20 ℃～40 ℃ moulding;
In the 6th step, half product is through washing, and drying obtains the finished product interpenetrating net polymer after the pulverizing, and product suction back forms interpenetration network hydrogel.
Above-mentioned linking agent is N, N '-methylene-bisacrylamide.
Above-mentioned initiator is a Potassium Persulphate.
After adopting such scheme, the present invention reacts by prepolymerization with Acrylic Acid Monomer or acrylamide monomer and Acrylic Acid Monomer or acrylamide monomer or water-soluble polymers and prepares interpenetration network hydrogel, can reach 1.22MPa by the polyacrylic acid potassium of the inventive method preparation or the gel-strength of polyacrylamide interpenetration network hydrogel, and structure homogeneous, manufacture method is simple and easy to do, is widely used at aspects such as drug release, artificial muscle, biosensor, tripping device, heavy metal ion recovery and conducting gelations.
Embodiment
The preparation method of interpenetration network hydrogel, embodiment one realize as follows:
The first step adopts the technical pure Acrylic Acid Monomer of buying on the market, removes stopper through vacuum decompression distillation or absorption purification.
In second step, by vinylformic acid: the mass ratio of water is 1:1, dissolves Acrylic Acid Monomer in water, form uniform monomer solution, and under agitation condition, in monomer solution, adding potassium hydroxide solution, potassium hydroxide and acrylic acid mol ratio are 75%, and neutralization reaction is carried out fully.
In the 3rd step, by vinylformic acid: the mass ratio of water is 1:1, with its dissolving, forms uniform solution in water; And under agitation condition, in this solution, adding potassium hydroxide solution, potassium hydroxide and acrylic acid mol ratio are 75%, and neutralization reaction is carried out fully.
The 4th step, under violent stirring, 0.04% of Acrylic Acid Monomer weight N in second step of adding in the solution of final gained of second step as linking agent, 0.3% of Acrylic Acid Monomer weight Potassium Persulphate during N '-methylene-bisacrylamide and second goes on foot as initiator, control reaction temperature is at 70 ℃～80 ℃, under agitation condition, allow polyreaction slowly carry out, form prepolymerized polyacrylic acid potassium.
The 5th step, the solution that in the 4th step, adds final gained of the 3rd step in the prepolymerized polyacrylic acid potassium, 0.08% the N that adds vinylformic acid weight in the 3rd step again as linking agent, 0.1% of vinylformic acid weight Potassium Persulphate during N '-methylene-bisacrylamide and the 3rd goes on foot as initiator, and under certain stirring velocity, allow polyreaction proceed, the interpenetrating net polymer that viscosity is bigger forms half higher product of water content in 20 ℃～40 ℃ moulding.
In the 6th step, half product is through washing, and drying is pulverized, and obtains the finished product interpenetrating net polymer, and product suction back forms interpenetration network hydrogel, can obtain the interpenetration network hydrogel of gel-strength greater than 1.22MPa.
The preparation method of interpenetration network hydrogel, embodiment two realize as follows:
The first step adopts the pure acrylamide monomer of buying on the market, removes stopper through vacuum decompression distillation or absorption purification.
In second step, by acrylamide: the mass ratio of water is 1:1, dissolves acrylamide monomer in water, forms uniform monomer solution.
In the 3rd step, by acrylamide monomer or water-soluble polymers: the mass ratio of water is 1:1, with its dissolving, forms uniform solution in water.
The 4th step, under violent stirring, 0.04% of acrylamide monomer weight N in second step of adding in the monomer solution of the second step gained as linking agent, 0.3% of acrylamide monomer Potassium Persulphate during N '-methylene-bisacrylamide and second goes on foot as initiator, control reaction temperature is at 70 ℃～80 ℃, under agitation condition, allow polyreaction slowly carry out, form prepolymerized polyacrylamide.
The 5th step, the solution that in the 4th step, adds the 3rd step gained in the prepolymerized polyacrylamide, 0.08% the N that adds acrylamide monomer or water-soluble polymers weight in the 3rd step again as linking agent, 0.1% of acrylamide monomer or water-soluble polymers weight Potassium Persulphate during N '-methylene-bisacrylamide and the 3rd goes on foot as initiator, and under certain stirring velocity, allow polyreaction proceed, the interpenetrating net polymer that viscosity is bigger forms half higher product of water content in 20 ℃～40 ℃ moulding.
In the 6th step, half product is through washing, and drying is pulverized, and obtains the finished product interpenetrating net polymer, and product suction back forms interpenetration network hydrogel, can obtain the interpenetration network hydrogel of gel-strength greater than 1.22MPa.
Claims (6)
1, the preparation method of interpenetration network hydrogel is characterized in that: realize as follows:
The first step is removed stopper with acrylamide monomer through purification;
In second step, by acrylamide monomer: the mass ratio of water is 3:2～7, in water acrylamide monomer is dissolved, and forms uniform monomer solution;
In the 3rd step, by acrylamide monomer or water-soluble polymers: the mass ratio of water is 3:2～7, in water with its dissolving, the solution of formation homogeneous;
The 4th step, under certain stirring velocity, 0.02%～0.08% of acrylamide monomer weight linking agent and 0.2～0.5% initiator during adding second goes on foot in the monomer solution of the second step gained, control reaction temperature allows polyreaction carry out under agitation condition at 70 ℃～80 ℃;
The 5th step, treat to add when acrylamide monomer becomes the prepolymerization attitude in the 4th step the solution of the 3rd step gained, and add 0.02%～0.1% linking agent of acrylamide monomer or water-soluble polymers weight in the 3rd step and 0.4～1.2% initiator, and under certain stirring velocity, allow polyreaction proceed, the interpenetrating net polymer that viscosity is bigger forms half higher product of water content in 20 ℃～40 ℃ moulding;
In the 6th step, half product is through washing, and drying obtains the finished product interpenetrating net polymer after the pulverizing, and product suction back forms interpenetration network hydrogel.
2, the preparation method of interpenetration network hydrogel according to claim 1 is characterized in that: the linking agent in above-mentioned the 4th step and the 5th step is N, N '-methylene-bisacrylamide.
3, the preparation method of interpenetration network hydrogel according to claim 1 is characterized in that: the initiator in above-mentioned the 4th step and the 5th step is a Potassium Persulphate.
4, the preparation method of interpenetration network hydrogel is characterized in that: realize as follows:
The first step is removed stopper with Acrylic Acid Monomer through purification;
In second step, by Acrylic Acid Monomer: the mass ratio of water is 3:2～7, in water Acrylic Acid Monomer is dissolved, form uniform monomer solution, and under agitation condition, in this monomer solution, adding alkaline solution, alkali and acrylic acid mol ratio are 60%～85%, and neutralization reaction is carried out fully;
In the 3rd step, by Acrylic Acid Monomer: the mass ratio of water is 3:2～7, and with its dissolving, the solution of formation homogeneous adds alkaline solution in this solution under agitation condition in water, and alkali and acrylic acid mol ratio are 60%～85%, and neutralization reaction is carried out fully;
The 4th step, under certain stirring velocity, 0.02%～0.08% of Acrylic Acid Monomer weight linking agent and 0.2～0.5% initiator during adding second goes on foot in the solution of final gained of second step, control reaction temperature allows polyreaction carry out under agitation condition at 70 ℃～80 ℃;
The 5th step, treat to add when Acrylic Acid Monomer becomes the prepolymerization attitude in the 4th step the solution of final gained of the 3rd step, and add 0.02%～0.1% linking agent of Acrylic Acid Monomer weight in the 3rd step and 0.4～1.2% initiator, and under certain stirring velocity, allow polyreaction proceed, the interpenetrating net polymer that viscosity is bigger forms half higher product of water content in 20 ℃～40 ℃ moulding;
In the 6th step, half product is through washing, and drying obtains the finished product interpenetrating net polymer after the pulverizing, and product suction back forms interpenetration network hydrogel.
5, the preparation method of interpenetration network hydrogel according to claim 4 is characterized in that: the linking agent in above-mentioned the 4th step and the 5th step is N, N '-methylene-bisacrylamide.
6, the preparation method of interpenetration network hydrogel according to claim 4 is characterized in that: the initiator in above-mentioned the 4th step and the 5th step is a Potassium Persulphate.
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Cited By (1)
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| CN108559108A (en) * | 2018-04-20 | 2018-09-21 | 延安大学 | A kind of preparation method of the three-dimensional interpenetrating polymer network hydrogel with pH responses |
| CN108559108B (en) * | 2018-04-20 | 2021-07-13 | 延安大学 | A kind of preparation method of pH-responsive three-dimensional interpenetrating network hydrogel |
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