CN101293939B - Isopropyl acrylamide polyalcohol hydrogel and synthesizing method - Google Patents
Isopropyl acrylamide polyalcohol hydrogel and synthesizing method Download PDFInfo
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Abstract
The invention relates to an N-isopropyl acrylamide (NIPA) polymer hydrogel and a synthetic method thereof. The hydrogel comprises the following components (wt%) of: NIPA 8-15%, low critical solution temperature (LCST) regulator 0-4%, initiation reducer 0.02-0.05%, crosslinker 0.1-0.15%, initiation oxidizer 0.03-0.07%, and water 91.85-80.73%. The synthetic method comprises the steps of: (1) determining the composition of the hydrogel; (2) dissolving an NIPA monomer in part of water to obtain an NIPA monomer aqueous solution; (3) adding the crosslinker in the NIPA monomer aqueous solution; (4) respectively dissolving the initiation reducer and the initiation oxidizer in part of water; (5) mixing the NIPA monomer aqueous solution and the aqueous solution of the initiation reducer in a container; (6) replacing the air on the surface and the surroundings of the container with nitrogen gas; (7) adding the aqueous solution of the initiation oxidizer into the container, mixing, and replacing with nitrogen gas for several minutes; (8) sealing the container, and reacting for several hours to obtain a gel product; and (9) washing with water to remove the toxicity of the residual non-reacted monomer on the surface of the gel product.
Description
Technical field
The invention belongs to technical field of chemical synthesis, be specifically related to a kind of N-isopropylacrylamide (NIPA) polyalcohol hydrogel and synthetic method thereof.
Background technology
High-molecular gel is a kind of soft and wet material that has both liquid, both character of solid, be by polymer three-dimensional cross-linked network and the multicomponent system that is fixed in small molecules solvent composition wherein, be that a class can not be dissolved, can not fusion, and having certain elastic cross-linked polymer swelling body. this material can be made soft reaction such as stimulations such as pH value, temperature, light intensity, electric field, magnetic field and chemical substance etc. to the variation of environment.Can be called as thermo-sensitive gel with this high-molecular gel that the temperature variation of environment is made soft reaction, thermo-sensitive gel is a kind of intelligent macromolecule, reversible expansion-contraction can take place with the variation of envrionment temperature, have the lower critical solution temperature that volume changes (lower critical solution temperature, LCST).The research work of intelligent polymer gel is carried out, and it is quite paid close attention in fields such as medical science, pharmacy, life science, biotechnology, electronics and mechanical organs.Poly-N one N-isopropylacrylamide (PNIPA) hydrogel has temperature sensitive property feature, when temperature is lower than LCST, forms good hydrated state in water, is contraction schedule when temperature reaches LCST.Its LCST (lower critical solution temperature, i.e. denaturation temperature) is with a wide range of applications in fields such as temperature sensitive film, feed separation, induction pieces, bionical and medical science about 32 ℃.
The method of existing synthetic isopropyl acrylamide (NIPA) polymer gel also has a lot.As: Xu Zhenqin, Tan Ye nation paper: the application (biomedical engineering research, 2004,01:52-55) of progress in Intelligent Hydrogel in biomedical engineering; Fragrant paper is liked by the Qin: response gathers preparation and performance (fine chemistry industry, 2006,23 (9): 849-852) of (N one N-isopropylacrylamide) hydrogel fast.Its component of the N-isopropylacrylamide of being introduced (NIPA) polymer gel also can contain and cause reductive agent, linking agent or initiated oxidation agent except the N-isopropylacrylamide monomer.But synthetic isopropyl acrylamide (NIPA) polymer gel that obtains in the prior art, the colloidal transparency, elasticity, temperature response performance is all poor, the proportioning that mainly is its component is unreasonable, to react desired temperature, atmosphere surrounding is not done and is offered some clarification on, it or not a more satisfactory reaction environment combination, and lower critical solution temperature (lower critical solution temperature, LCST) can not regulate, therefore the gel product applicable surface of gained is narrow, can not satisfy the needs that actual many-side is used.
Summary of the invention
Technical problem to be solved by this invention is at existing above-mentioned weak point in the prior art, and a kind of N-isopropylacrylamide (NIPA) polyalcohol hydrogel and synthetic method thereof are provided.The applicant has proposed the application for a patent for invention of " a kind of method for preparing monomer of temperature-sensitive polyisopropylacrylamide " on February 7th, 2007, application number is: 200710003153.1, the present invention provides a kind of N-isopropylacrylamide (NIPA) polyalcohol hydrogel and synthetic method thereof on the monomer basis of the produced PNIPAM of this patent application " a kind of monomer synthetic method of temperature-sensitive polyisopropylacrylamide ".
The technical scheme that solution the technology of the present invention problem is adopted is this N-isopropylacrylamide (NIPA) polyalcohol hydrogel, its component comprises N-isopropylacrylamide, water, also comprise and cause reductive agent, linking agent, initiated oxidation agent, also can comprise the lower critical solution temperature conditioning agent, the weight percent of each component can be: N-isopropylacrylamide 8-15%, lower critical solution temperature conditioning agent 0-4%, initiation reductive agent 0.02-0.05%, linking agent 0.1-0.15%, initiated oxidation agent 0.03-0.07%, water 91.85-80.73%.
Chemical reaction by the monomer synthetic polymer is called polyreaction, is called for short polymerization.The type of polyreaction is a lot, its minute chain reaction polymerization, progressively polymerization, ring-opening polymerization and polymer chemistry can be reacted four classes by the mechanism of reaction.Chain reaction polymerization is meant polyreaction Once you begin, and reaction just can be gone down in automatically a series of polymerization, and the prolongation in time of monomeric transformation efficiency improves.In chain reaction polymerization system kind, need the active centre of polyreaction, according to the active centre difference of polyreaction, chain reaction polymerization can be divided into radical polymerization, ionic polymerization.Polymerization methods of the present invention belongs to the radical polymerization in the chain reaction polymerization.
Initiator is meant the material that produces the Raolical polymerizable active centre among the present invention, is the compound that a class contains weak bond, and under the effect of decomposition activation energy, the covalent linkage fracture can produce free radical.In general radical polymerization system, for enough activation energy is provided, polymerization temperature is 40-100 ℃.The used initiator of the present invention can and cause reductive agent by the initiated oxidation agent and constitute, it is to add reductive agent in the peroxide initiator, produce free radical by the oxidation-reduction reaction, this system just is oxidation-reduction initiating system or is claimed the oxidation-reduction initiator.Utilize the oxidation-reduction initiator can reduce decomposition activation energy, thereby polyreaction (15-25 ℃) under lower temperature is carried out, help improving polymer quality and reduce to environment requirement handled easily.
Linking agent is the compound that a class has non-conjugated many pairs of keys among the present invention, and its effect is to convert tridimensional network to caused the linear crosslinking structure of formed N-isopropylacrylamide by free radical, thereby gives gel moulding.
Preferably synthetic used water is two ionized waters that boil off;
Preferably linking agent is N, N '-methylene-bisacrylamide;
Preferably the initiated oxidation agent is an ammonium persulphate;
Preferably causing reductive agent is Sodium Metabisulfite;
Preferably the lower critical solution temperature conditioning agent is an acrylamide.
Acrylamide possess hydrophilic property in the present invention, and the N-isopropylacrylamide monomer is hydrophobic, in N-isopropylacrylamide polymeric gel, add acrylamide, can improve the wetting ability of whole system, more hydrogen bond in the increase system, owing to the be heated reason of phase transformation of gel is due to the fracture of hydrogen bond in the system, increased hydrogen bond, improved with regard to the temperature that makes the system phase transformation.Therefore the lower critical solution temperature conditioning agent can be used to regulate thermo-sensitive gel lower critical solution temperature (lower criticalsolution temperature, LCST).
The synthetic method of N-isopropylacrylamide of the present invention (NIPA) polymer gel may further comprise the steps:
1. determine N-isopropylacrylamide (NIPA) polymer gel component, the weight percent of each component can be: N-isopropylacrylamide 8-15%, lower critical solution temperature (LCST) conditioning agent 0-4%, initiation reductive agent 0.02-0.05%, linking agent 0.1-0.15%, initiated oxidation agent 0.03-0.07%, water 91.85-80.73%;
2. the N-isopropylacrylamide monomer is dissolved in portion water, can be in monomer and quality than (0.1-0.15): 1 ratio dissolving;
3. in step (2) solution, add linking agent, stirring and dissolving;
4. initiated oxidation agent and initiation reductive agent respectively are dissolved in portion water, can be by the concentration of 0.8-1.5%;
5. the aqueous solution mixing of N-isopropylacrylamide monomer solution and linking agent, initiation reductive agent is in vessel;
6. with nitrogen replacement vessel surface and ambient air, the time can be 3-5 minutes;
7. the initiated oxidation agent aqueous solution is joined in the vessel, with nitrogen replacement vessel surface and ambient air, the time can be 1-3 minutes behind the mixing;
8. airtight vessel reaction 3-24 hours, temperature is controlled at 15 ℃-25 ℃, gets gel product;
9. the gained gel product soaks surperficial a few hours with two ionized waters that boil off through repeatedly washing at every turn, outwells water then and dries a few hours, to remove the not toxic of the residual monomer of complete reaction of surface.
The temperature of entire operation process is controlled at 15 ℃-25 ℃, and the too high meeting of temperature causes in operating process with regard to polymerization (implode); Temperature is crossed low then opposite, is difficult to polymerization.
Preferably, in step 1, the lower critical solution temperature conditioning agent in N-isopropylacrylamide (NIPA) the polymer gel component is an acrylamide, and its weight percent content in this polymer gel is 0-4%; In the monomeric aqueous solution of N-isopropylacrylamide that step (2) is made, can add acrylamide, change LCST, to satisfy the requirement of different application targets.The ratio of control N-isopropylacrylamide and acrylamide can reach the purpose that changes LCST.Along with the reduction of N-isopropylacrylamide and acrylamide mol ratio, LCST constantly raises.N-isopropylacrylamide and acrylamide mol ratio are (100-70): regulate when changing between (0-30), can regulate between 32 ℃-70 ℃ the temperature of LCST.Particularly, if do not add acrylamide, then keeping the poly-original LCST of N one N-isopropylacrylamide (PNIPA) hydrogel, is 32 ℃; When N-isopropylacrylamide and acrylamide mol ratio were 95:5, LCST was 40 ℃; When N-isopropylacrylamide and acrylamide mol ratio were 80:20, LCST was 60 ℃; When N-isopropylacrylamide and acrylamide mol ratio were 70:30, LCST was 70 ℃;
Preferably synthetic used water boils off ionized water for two, and deionized water is suitable for chemical reaction, but simple ionized water has generally only passed through the permeation filtration of ion column, can't remove the microorganism in the water fully.Adopt two ionized waters that boil off, both be fit to chemical reaction, do not have microbiological contamination again.Avoided the inner proterties that causes owing to microbial contamination of gelinite to change.
Preferably in step 2, can suitably heat the monomeric dissolving of help N-isopropylacrylamide, but temperature can not surpass 40 ℃, and need be cooled to continue follow-up operation below 25 ℃ after the heating.
Preferably, can the elasticity of gel be changed to some extent, can change the elasticity of gel by changing the content of linking agent by changing the content of linking agent according to service requirements.Linking agent is preferably used N, N '-methylene-bisacrylamide;
Preferably ammonium persulphate is adopted in the initiated oxidation agent, causes reductive agent and adopts Sodium Metabisulfite.
Preferably in the step 8, airtight vessel reaction is to make polyreaction isolate airborne oxygen under the condition of logical nitrogen, has guaranteed that polymeric carries out the quality with gel smoothly.With the reasonable plastics bag of stopping property commonly used in the life, the vessel of the good various raw materials of mixing are put into bag, with the air in the nitrogen replacement bag, tighten sack then, keep its interior pure nitrogen gas environment.
Vessel are glass beaker, and the nitrogen quality is the general industry standard, and the decompression of compression steel cylinder is supplied with.
Preferably in step 9, gel through 5 washings, was soaked the surface 12 hours with two ionized waters that boil off at every turn, outwell water then and dried 12 hours.Number of times is too much, operate too loaded down with trivial details, very few, can not effectively remove the surface residual monomer.Each water logging bubble 12 hours dried 12 hours, the too short effect that do not reach, and long meeting causes the obvious expansion of gel volume.
Preferably further comprising the steps of:
10. after the washing of step 9 gel, the antiseptic solution that adds with the distilled water preparation soaks into gel surface on a small quantity; Described sanitas can be card pine, formaldehyde, nipagin esters series, adding with the antiseptic solution concentration of distilled water preparation is: blocking loose strength of solution is 40-100ug/ml, formaldehyde solution concentration is 0.5-1mg/ml, and the nipagin esters strength of solution is 5-10mg/ml.
The card pine solution that further preferably adds with the distilled water preparation soaks into gel surface on a small quantity, can play the rot-resistant effect.Use formaldehyde can influence the transparency of gel in the impregnating material, and nipagin esters is not soluble in water, influences preservative effect.
N-isopropylacrylamide of the present invention (NIPA) polyalcohol hydrogel is a kind of intelligent polymer gel with temperature sensitive property feature, when temperature is lower than LCST, forms good hydrated state in water, is contraction schedule when temperature reaches LCST.The N-isopropylacrylamide of gained (NIPA) the polyalcohol hydrogel transparency is good, good springiness and its LCST can regulate between 32 ℃-70 ℃ even in the wideer temperature range, can be applied in fields such as temperature sensitive film, feed separation, induction pieces, bionical and medical science widely.
Embodiment
It below is non-limiting specific embodiment of the present invention.
Embodiment 1:LCST is 32 ℃
Proportioning raw materials:
N-isopropylacrylamide 100.0g
Cause reductive agent Sodium Metabisulfite 0.5g
Linking agent N, N '-methylene-bisacrylamide 1g
Initiated oxidation agent ammonium persulphate 0.5g
Water (deionized water) 898g
Operation steps:
1) the N-isopropylacrylamide monomer is dissolved in portion water;
2) in step 1) solution, add linking agent, stirring and dissolving;
3) initiated oxidation agent and initiation reductive agent respectively are dissolved in portion water;
4) N-isopropylacrylamide monomer solution and linking agent, initiation reductive agent aqueous solution mixing are in vessel;
5) vessel are put into the reasonable fresh-keeping plastic bag of stopping property, used nitrogen replacement vessel surface and ambient air 3-5 minutes;
6) the initiated oxidation agent aqueous solution is joined in the vessel, use the interior air of nitrogen replacement bag 1-3 minutes behind the mixing, tighten sack then, keep the pure nitrogen gas environment in it;
7) airtight vessel reaction is 3-24 hours, and temperature is controlled at 15 ℃-25 ℃, gets gel product;
8) gel is through 5 washings, each soaks the surface 12 hours with two ionized waters that boil off, after outwelling water then and drying 12 hours, can surface infiltration a little (concentration is 40-100ug/ml) with the loose solution of the card of distilled water preparation.
Prepared N-isopropylacrylamide (NIPA) polyalcohol hydrogel lower critical solution temperature (LCST) is 32 ℃.
Embodiment 2:LCST is 40 ℃
Proportioning raw materials:
N-isopropylacrylamide 100.0g
Lower critical solution temperature conditioning agent acrylamide 3.31g
Cause reductive agent Sodium Metabisulfite 0.34g
Linking agent N, N '-methylene-bisacrylamide 1g
Initiated oxidation agent ammonium persulphate 0.5g
Water (deionized water) 895g
Operation steps:
1) N-isopropylacrylamide monomer and acrylamide are dissolved in portion water;
2) 1) step adds linking agent, stirring and dissolving in the solution;
3) initiated oxidation agent and initiation reductive agent respectively are dissolved in portion water;
4) N-isopropylacrylamide monomer solution and linking agent, initiation reductive agent aqueous solution mixing are in vessel;
5) vessel are put into the reasonable fresh-keeping plastic bag of stopping property, used nitrogen replacement vessel surface and ambient air 3-5 minutes;
6) the initiated oxidation agent aqueous solution is joined in the vessel, behind the mixing, use the interior air of nitrogen replacement bag 1-3 minutes, tighten sack then, keep the pure nitrogen gas environment in it;
7) airtight vessel reaction is 3-24 hours, and temperature is controlled at 15 ℃-25 ℃, gets gel product;
8) gel is through 5 washings, each soaks the surface 12 hours with two ionized waters that boil off, after outwelling water then and drying 12 hours, can surface infiltration a little (concentration is 40-100ug/ml) with the loose solution of the card of distilled water preparation.
Prepared N-isopropylacrylamide (NIPA) polyalcohol hydrogel lower critical solution temperature (LCST) is 40 ℃.
Embodiment 3:LCST is 60 ℃
Proportioning raw materials:
N-isopropylacrylamide 100.0g
Lower critical solution temperature conditioning agent acrylamide 15.7g
Cause reductive agent Sodium Metabisulfite 0.4g
Linking agent N, N '-methylene-bisacrylamide 1.2g
Initiated oxidation agent ammonium persulphate 0.6g
Water (deionized water) 882g
Operation steps:
1) N-isopropylacrylamide monomer and acrylamide are dissolved in portion water;
2) 1) step adds linking agent, stirring and dissolving in the solution;
3) initiated oxidation agent and initiation reductive agent respectively are dissolved in portion water;
4) N-isopropylacrylamide monomer solution and linking agent, initiation reductive agent aqueous solution mixing are in vessel;
5) vessel are put into the reasonable fresh-keeping plastic bag of stopping property, used nitrogen replacement vessel surface and ambient air 3-5 minutes;
6) the initiated oxidation agent aqueous solution is joined in the vessel, behind the mixing, use the interior air of nitrogen replacement bag 1-3 minutes, tighten sack then, keep the pure nitrogen gas environment in it;
7) airtight vessel (I) reaction is 3-24 hours, and temperature is controlled at 15 ℃-25 ℃, gets gel product;
8) gel is through 5 washings, each soaks the surface 12 hours with two ionized waters that boil off, after outwelling water then and drying 12 hours, can surface infiltration a little (concentration is 40-100ug/ml) with the loose solution of the card of distilled water preparation.
Prepared N-isopropylacrylamide (NIPA) polyalcohol hydrogel lower critical solution temperature (LCST) is 60 ℃.
Embodiment 4:LCST is 70 ℃
Proportioning raw materials:
N-isopropylacrylamide 100.0g
Lower critical solution temperature conditioning agent acrylamide 27g
Cause reductive agent Sodium Metabisulfite 0.4g
Linking agent N, N '-methylene-bisacrylamide 1.2g
Initiated oxidation agent ammonium persulphate 0.5g
Water (deionized water) 871g
Operation steps:
1) N-isopropylacrylamide monomer and acrylamide are dissolved in portion water;
2) 1) step adds linking agent, stirring and dissolving in the solution;
3) initiated oxidation agent and initiation reductive agent respectively are dissolved in portion water;
4) N-isopropylacrylamide monomer solution and linking agent, initiation reductive agent aqueous solution mixing are in vessel;
5) vessel are put into the reasonable fresh-keeping plastic bag of stopping property, used nitrogen replacement vessel surface and ambient air 3-5 minutes;
6) the initiated oxidation agent aqueous solution is joined in the vessel, behind the mixing, use the interior air of nitrogen replacement bag 1-3 minutes, tighten sack then, keep the pure nitrogen gas environment in it;
7) airtight vessel reaction is 3-24 hours, and temperature is controlled at 15 ℃-25 ℃, gets gel product;
8) gel is through 5 washings, each soaks the surface 12 hours with two ionized waters that boil off, after outwelling water then and drying 12 hours, can surface infiltration a little (concentration is 40-100ug/ml) with the loose solution of the card of distilled water preparation.
Prepared N-isopropylacrylamide (NIPA) polyalcohol hydrogel lower critical solution temperature (LCST) is 70 ℃.
Embodiment 5:
Proportioning raw materials:
N-isopropylacrylamide 85.0g
Lower critical solution temperature conditioning agent acrylamide 9.5g
Cause reductive agent Sodium Metabisulfite 0.2g
Linking agent N, N '-methylene-bisacrylamide 1g
Initiated oxidation agent ammonium persulphate 0.3g
Water (deionized water) 898g
Operation steps:
1) N-isopropylacrylamide monomer and acrylamide are dissolved in portion water;
2) 1) step adds linking agent, stirring and dissolving in the solution;
3) initiated oxidation agent and initiation reductive agent respectively are dissolved in portion water;
4) N-isopropylacrylamide monomer solution and linking agent, initiation reductive agent aqueous solution mixing are in vessel;
5) vessel are put into the reasonable fresh-keeping plastic bag of stopping property, used nitrogen replacement vessel surface and ambient air 3-5 minutes;
6) the initiated oxidation agent aqueous solution is joined in the vessel, behind the mixing, use the interior air of nitrogen replacement bag 1-3 minutes, tighten sack then, keep the pure nitrogen gas environment in it;
7) airtight vessel reaction is 3-24 hours, and temperature is controlled at 15 ℃-25 ℃, gets gel product;
8) gel is through 5 washings, each soaks the surface 12 hours with two ionized waters that boil off, after outwelling water then and drying 12 hours, can surface infiltration a little (concentration is 40-100ug/ml) with the loose solution of the card of distilled water preparation.
Prepared N-isopropylacrylamide (NIPA) polyalcohol hydrogel lower critical solution temperature (LCST) is 57 ℃.
Embodiment 6:
Proportioning raw materials:
N-isopropylacrylamide 140.0g
Lower critical solution temperature conditioning agent acrylamide 10g
Cause reductive agent Sodium Metabisulfite 0.5g
Linking agent N, N '-methylene-bisacrylamide 1.5g
Initiated oxidation agent ammonium persulphate 0.7g
Water (deionized water) 848g
Operation steps:
1) N-isopropylacrylamide monomer and acrylamide are dissolved in portion water.
2) 1) step adds linking agent, stirring and dissolving in the solution;
3) initiated oxidation agent and initiation reductive agent respectively are dissolved in portion water;
4) N-isopropylacrylamide monomer solution and linking agent, initiation reductive agent aqueous solution mixing are in vessel;
5) vessel are put into the reasonable fresh-keeping plastic bag of stopping property, used nitrogen replacement vessel surface and ambient air 3-5 minutes;
6) the initiated oxidation agent aqueous solution is joined in the vessel, behind the mixing, use the interior air of nitrogen replacement bag 1-3 minutes, tighten sack then, keep the pure nitrogen gas environment in it;
7) airtight vessel reaction is 3-24 hours, and temperature is controlled at 15 ℃-25 ℃, gets gel product;
8) gel is through 5 washings, each soaks the surface 12 hours with two ionized waters that boil off, after outwelling water then and drying 12 hours, can surface infiltration a little (concentration is 40-100ug/ml) with the loose solution of the card of distilled water preparation.
Prepared N-isopropylacrylamide (NIPA) polyalcohol hydrogel lower critical solution temperature (LCST) is 52 ℃.
Claims (15)
1. isopropyl acrylamide polyalcohol hydrogel, its component comprises N-isopropylacrylamide, water, it is characterized in that also comprising the initiated oxidation agent of oxidation-reduction trigger system, cause reductive agent, also comprise linking agent, the lower critical solution temperature conditioning agent, the weight percent of each component is: N-isopropylacrylamide 8-15%, lower critical solution temperature conditioning agent 0-4%, cause reductive agent 0.02-0.05%, linking agent 0.1-0.15%, initiated oxidation agent 0.03-0.07%, water 91.85-80.73%, the initiated oxidation agent is an ammonium persulphate, cause reductive agent and adopt Sodium Metabisulfite, the lower critical solution temperature conditioning agent is an acrylamide, and N-isopropylacrylamide and acrylamide mol ratio are (100-70): (0-30).
2. isopropyl acrylamide polyalcohol hydrogel according to claim 1 is characterized in that synthetic used water is two ionized waters that boil off.
3. isopropyl acrylamide polyalcohol hydrogel according to claim 1 is characterized in that linking agent is N, N '-methylene-bisacrylamide.
4. isopropyl acrylamide polyalcohol hydrogel synthetic method may further comprise the steps:
(1). determine the isopropyl acrylamide polyalcohol gel component, the weight percentage ranges of each component is: N-isopropylacrylamide 8-15%, lower critical solution temperature (LCST) conditioning agent 0-4%, initiation reductive agent 0.02-0.05%, linking agent 0.1-0.15%, initiated oxidation agent 0.03-0.07%, water 91.85-80.73%, the lower critical solution temperature conditioning agent is an acrylamide, ammonium persulphate is adopted in the initiated oxidation agent, causes reductive agent and adopts Sodium Metabisulfite;
(2). the N-isopropylacrylamide monomer is dissolved in portion water, in monomer and quality than (0.1-0.15): 1 ratio dissolving, in the monomeric aqueous solution of the N-isopropylacrylamide of making, add acrylamide;
(3). in the solution of step (2), add linking agent, stirring and dissolving;
(4). initiated oxidation agent and initiation reductive agent respectively are dissolved in portion water, press the concentration of 0.8-1.5%;
(5). the aqueous solution mixing of N-isopropylacrylamide monomer solution and linking agent, initiation reductive agent is in vessel;
(6). with nitrogen replacement vessel surface and ambient air;
(7). the initiated oxidation agent aqueous solution is joined in the vessel, use nitrogen replacement vessel surface and ambient air behind the mixing;
(8). airtight vessel reaction 3-24 hour, temperature is controlled at 15 ℃-25 ℃, gets gel product.
5. isopropyl acrylamide polyalcohol hydrogel synthetic method according to claim 4, it is characterized in that N-isopropylacrylamide and acrylamide mol ratio are (100-70): regulate when changing (0-30), can between 32 ℃-70 ℃, regulate to the temperature of LCST.
6. isopropyl acrylamide polyalcohol hydrogel synthetic method according to claim 4, it is characterized in that in step (2), can suitably heat and help the monomeric dissolving of N-isopropylacrylamide, but temperature can not surpass 40 ℃, and need be cooled to could continue follow-up operation below 25 ℃ after the heating.
7. isopropyl acrylamide polyalcohol hydrogel synthetic method according to claim 4 is characterized in that water synthetic used in the step (1) is two ionized waters that boil off.
8. isopropyl acrylamide polyalcohol hydrogel synthetic method according to claim 6 is characterized in that changing the elasticity of gel by changing the content of linking agent.
9. isopropyl acrylamide polyalcohol hydrogel synthetic method according to claim 4 is characterized in that linking agent can adopt N, N '-methylene-bisacrylamide.
10. isopropyl acrylamide polyalcohol hydrogel synthetic method according to claim 4, it is characterized in that in the step (8), airtight vessel reaction is the oxygen that makes under the condition of logical nitrogen in the polyreaction air-isolation, and the assurance polymeric carries out the quality with gel smoothly.
11. isopropyl acrylamide polyalcohol hydrogel synthetic method according to claim 10, it is characterized in that with the reasonable plastics bag of stopping property commonly used in the life, the vessel of the good various raw materials of mixing are put into bag, with the air in the nitrogen replacement bag, tighten sack then, keep the pure nitrogen gas environment in it.
12. isopropyl acrylamide polyalcohol hydrogel synthetic method according to claim 4, it is characterized in that (9) also in steps, with the gained gel product through repeatedly the washing, soak surperficial a few hours with two ionized waters that boil off at every turn, outwell water then and dry a few hours, to remove the not toxic of the residual monomer of complete reaction of surface.
13. isopropyl acrylamide polyalcohol hydrogel synthetic method according to claim 12 is characterized in that further comprising the steps of:
(10). after the washing of step (9) gel, the antiseptic solution that adds with the distilled water preparation soaks into gel surface.
14. isopropyl acrylamide polyalcohol hydrogel synthetic method according to claim 13 is characterized in that described sanitas can be card pine, formaldehyde or nipagin esters series.
15. isopropyl acrylamide polyalcohol hydrogel synthetic method according to claim 14 is characterized in that the card pine solution that adds with the distilled water preparation soaks into gel surface on a small quantity, blocking loose strength of solution is 40-100ug/ml.
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| CN109540331A (en) * | 2018-11-08 | 2019-03-29 | 中国科学院理化技术研究所 | Cocktail-type nano assembly-based wide-range fluorescent nano thermometer and preparation method thereof |
| CN109692069B (en) * | 2018-12-25 | 2021-07-06 | 东阳市善水环境工程有限公司 | Intelligent warm keeping patch with overheat protection function |
| CN112898623B (en) * | 2021-02-02 | 2023-01-24 | 中国石油大学(华东) | Liquid phase gel for temperature and pH coupling response type gel foam, preparation method, gel foam, preparation method and application thereof |
| CN113990176B (en) * | 2021-11-19 | 2023-01-17 | 中山大学 | Preparation method and application of anti-counterfeit label based on temperature-induced phase-change hydrogel |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20040248326A1 (en) * | 2001-11-01 | 2004-12-09 | Babak Ziaie | Hydrogel compositions, devices, and microscale components |
| CN1693320A (en) * | 2005-05-20 | 2005-11-09 | 中国科学院长春应用化学研究所 | Process for preparing high water adsorbing resin |
-
2007
- 2007-04-26 CN CN2007100980673A patent/CN101293939B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20040248326A1 (en) * | 2001-11-01 | 2004-12-09 | Babak Ziaie | Hydrogel compositions, devices, and microscale components |
| CN1693320A (en) * | 2005-05-20 | 2005-11-09 | 中国科学院长春应用化学研究所 | Process for preparing high water adsorbing resin |
Non-Patent Citations (8)
| Title |
|---|
| JP特开2004-83619A 2004.03.18 |
| JP特开平6-253831A 1994.09.13 |
| 张先正等.快速温度敏感聚（N-异丙基丙烯酰胺-co-丙烯酰胺）水凝胶的制备及性能研究.高等学校化学学报21 8.2000,21(8),1309-1311. |
| 张先正等.快速温度敏感聚(N-异丙基丙烯酰胺-co-丙烯酰胺)水凝胶的制备及性能研究.高等学校化学学报21 8.2000,21(8),1309-1311. * |
| 王元宵.温度敏感性NIPAAm/HEMA智能材料的制备，性能及药物控释应用.中国优秀博硕士学位论文全文数据库 (硕士)工程科技Ⅰ辑 11.2006,工程科技Ⅰ辑(11),22、30-33. |
| 王元宵.温度敏感性NIPAAm/HEMA智能材料的制备,性能及药物控释应用.中国优秀博硕士学位论文全文数据库 (硕士)工程科技Ⅰ辑 11.2006,工程科技Ⅰ辑(11),22、30-33. * |
| 秦爱香等.快速响应聚(N-异丙基丙烯酰胺)水凝胶的制备及性能.精细化工23 9.2006,23(9),849-852. |
| 秦爱香等.快速响应聚(N-异丙基丙烯酰胺)水凝胶的制备及性能.精细化工23 9.2006,23(9),849-852. * |
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