CN114702693A - Synthesis method and application of trehalose-modified PNIPAm temperature-sensitive intelligent hydrogel - Google Patents
Synthesis method and application of trehalose-modified PNIPAm temperature-sensitive intelligent hydrogel Download PDFInfo
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- 238000001308 synthesis method Methods 0.000 title claims abstract description 8
- HDTRYLNUVZCQOY-UHFFFAOYSA-N α-D-glucopyranosyl-α-D-glucopyranoside Natural products OC1C(O)C(O)C(CO)OC1OC1C(O)C(O)C(O)C(CO)O1 HDTRYLNUVZCQOY-UHFFFAOYSA-N 0.000 claims abstract description 59
- HDTRYLNUVZCQOY-WSWWMNSNSA-N Trehalose Natural products O[C@@H]1[C@@H](O)[C@@H](O)[C@@H](CO)O[C@@H]1O[C@@H]1[C@H](O)[C@@H](O)[C@@H](O)[C@@H](CO)O1 HDTRYLNUVZCQOY-WSWWMNSNSA-N 0.000 claims abstract description 59
- HDTRYLNUVZCQOY-LIZSDCNHSA-N alpha,alpha-trehalose Chemical compound O[C@@H]1[C@@H](O)[C@H](O)[C@@H](CO)O[C@@H]1O[C@@H]1[C@H](O)[C@@H](O)[C@H](O)[C@@H](CO)O1 HDTRYLNUVZCQOY-LIZSDCNHSA-N 0.000 claims abstract description 59
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- 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
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- 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
- C08J3/24—Crosslinking, e.g. vulcanising, of macromolecules
- C08J3/246—Intercrosslinking of at least two polymers
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- E—FIXED CONSTRUCTIONS
- E06—DOORS, WINDOWS, SHUTTERS, OR ROLLER BLINDS IN GENERAL; LADDERS
- E06B—FIXED OR MOVABLE CLOSURES FOR OPENINGS IN BUILDINGS, VEHICLES, FENCES OR LIKE ENCLOSURES IN GENERAL, e.g. DOORS, WINDOWS, BLINDS, GATES
- E06B9/00—Screening or protective devices for wall or similar openings, with or without operating or securing mechanisms; Closures of similar construction
- E06B9/24—Screens or other constructions affording protection against light, especially against sunshine; Similar screens for privacy or appearance; Slat blinds
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- 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
- C08J2305/00—Characterised by the use of polysaccharides or of their derivatives not provided for in groups C08J2301/00 or C08J2303/00
- C08J2305/04—Alginic acid; Derivatives thereof
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- 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
- C08J2333/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Derivatives of such polymers
- C08J2333/24—Homopolymers or copolymers of amides or imides
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- 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
- C08J2433/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Derivatives of such polymers
- C08J2433/24—Homopolymers or copolymers of amides or imides
Abstract
The invention relates to a synthesis method and application of trehalose modified PNIPAm temperature-sensitive intelligent hydrogel, wherein the synthesis method comprises the following steps: 1. respectively adding N-isopropylacrylamide and N, N' -methylenebisacrylamide to the trehalose solution and mixing to obtain a mixed solution; 2. adding ammonium persulfate into the mixed solution in the previous step and stirring; 3. adding N, N, N ', N' -tetramethyl ethylenediamine into the mixed solution in the previous step, and stirring to obtain a gel solution; 4. standing at 20-30 ℃ for 2-3 hours to obtain trehalose modified PNIPAm temperature-sensitive hydrogel. The invention provides a simple preparation process of Trehalose modified PNIPAm-Trehalose temperature-sensitive hydrogel and a method for the Trehalose modified PNIPAm-Trehalose intelligent window, and opens up a new way for building energy conservation.
Description
Technical Field
The invention relates to the field of hydrogel synthesis methods, in particular to a synthesis method and application of trehalose modified PNIPAm temperature-sensitive intelligent hydrogel.
Background
Synthesizing PNIPAm temperature-sensitive hydrogel in deionized water by an in-situ polymerization method. Because PNIPAm is single-network temperature-sensitive hydrogel, the mechanical strength is poor, and the durability and the reutilization property are low; in addition, the thermal response rate of the PNIPAm temperature-sensitive hydrogel is relatively slow, and delta TsolAnd Δ TlumIt is not ideal and not beneficial to practical application.
Disclosure of Invention
A synthesis method of trehalose modified PNIPAm temperature-sensitive intelligent hydrogel comprises the following steps:
step 1, dissolving Trehalose (Trehalose) (0, 2, 4 and 6g) in 20ml of deionized water to form Trehalose solutions with the mass fractions of 0%, 10%, 20% and 30%, respectively;
step 2, respectively adding N-isopropylacrylamide and N, N' -methylenebisacrylamide to the trehalose solution obtained in the step 1, and uniformly mixing to obtain a mixed solution; the mass ratio of the trehalose solution to the N-isopropylacrylamide to the N, N' -methylenebisacrylamide is 20: (1-2): (0.01-0.03);
and 3, adding ammonium persulfate into the mixed solution obtained in the step 2 and stirring, wherein the mass ratio of the trehalose solution to the ammonium persulfate is 20: (0.01-0.03);
step 4, adding 4-7 mu m of N, N, N ', N' -tetramethyl ethylenediamine into the mixed solution obtained in the step 3, and stirring to obtain a gel solution;
and 5, standing at the temperature of 20-30 ℃ for 2-3 hours to obtain the trehalose modified PNIPAm temperature-sensitive hydrogel.
Further, the mass ratio of the trehalose solution to the N-isopropylacrylamide to the N, N' -methylenebisacrylamide is 20: 1.34: 0.02.
further, the mass ratio of ammonium persulfate to deionized water in the step 3 is 20: 0.02.
further, the mass fraction of trehalose in the trehalose solution in the step 1 is 30%.
The application of the trehalose modified PNIPAm temperature-sensitive intelligent hydrogel in the temperature-sensitive intelligent window comprises the following specific application methods: coating a layer of trehalose modified PNIPAm hydrogel on the upper surface of one glass slide, covering a layer of glass slide on the upper surface of the trehalose modified PNIPAm hydrogel to form a sandwich structure, and finally sealing the periphery of the trehalose modified PNIPAm hydrogel by using sealant to obtain the trehalose modified PNIPAm temperature-sensitive hydrogel intelligent window.
The invention has the beneficial effects that: according to the invention, through a physical crosslinking method, the PNIPAm single-network temperature-sensitive hydrogel is prepared into trehalose modified PNIPAm double-network temperature-sensitive hydrogel, and the prepared trehalose modified PNIPAm double-network temperature-sensitive hydrogel is well applied to an intelligent window, and the loss of building energy is well reduced. Compared with the prior art, the trehalose modified PNIPAm temperature-sensitive intelligent material has the following advantages: (1) the PNIPAm single-network hydrogel is prepared into trehalose modified PNIPAm double-network hydrogel through a physical crosslinking method, so that the mechanical strength of the PNIPAm temperature-sensitive hydrogel can be improved, and the thermal response rate of the PNIPAm temperature-sensitive hydrogel is also improved; the addition of the trehalose not only solves the problem of volume change of the common PNIPAm temperature-sensitive hydrogel after phase change, but also slightly reduces the LCST of the PNIPAm. The prepared trehalose-modified PNIPAm double-network temperature-sensitive hydrogel is well applied to an intelligent window, and the strong mechanical strength can enhance the reusability of the trehalose-modified PNIPAm temperature-sensitive intelligent window, so that the trehalose-modified PNIPAm double-network temperature-sensitive hydrogel is more beneficial to practical application. In addition, the trehalose modified PNIPAm intelligent window can realize excellent optical performance, high light transmittance and high solar modulation, and has excellent energy-saving performance. (2) Different from the previous method, the physical crosslinking method has the advantages of simple operation, no toxicity, low cost and environmental protection. More importantly, the trehalose modified PNIPAm temperature-sensitive material is an energy-saving and climate-adaptive intelligent window material with great prospect at present. (3) The invention uses N, N, N ', N' -tetramethyl ethylenediamine as catalyst to accelerate reaction speed and promote cross-linking between monomers, so that the formed hydrogel is more transparent and uniform and is more beneficial to practical application.
Drawings
FIG. 1 is a schematic diagram of synthesis of trehalose-modified PNIPAm temperature-sensitive intelligent hydrogel.
Detailed Description
The following is a description of the principles and features of the present invention, the examples being included merely for purposes of illustration and are not intended to limit the scope of the invention.
(1) Synthesis of trehalose modified PNIPAm temperature-sensitive hydrogel
As shown in figure 1, PNIPAm and Trehalose (Trehalose) are taken as raw materials to successfully prepare the PNIPAm-Trehalose hydrogel with temperature-sensitive property by a simple physical crosslinking method. The method mainly comprises the following steps:
trehalose (trehalase) (0, 2, 4 and 6g) was dissolved in 20ml of deionized water to form Trehalose solutions with mass fractions of 0%, 10%, 20% and 30%, respectively.
② adding 1.34g (0.07mol) of (N-isopropyl acrylamide) (NIPAm) and 0.02g (0.0014mol) of N, N' -methylene-bis-acrylamide (MBA) into the trehalose solutions with different concentrations respectively;
secondly, mixing evenly;
stirring for 30-60 min to obtain homogeneous transparent solution;
adding 0.02g of Ammonium Persulfate (APS);
continuously stirring for 30-60 minutes;
sixthly, 6 mu m N of N, N ', N' -tetramethyl ethylenediamine (TEMED) is added;
seventhly, continuing stirring for 3 minutes;
placing at room temperature (20 ℃) for 2-3 hours to obtain trehalose modified PNIPAm temperature-sensitive hydrogel;
and (3) experimental comparison: PNIPAm and trehalose are dissolved in 20ml of deionized water according to the mass ratio of 1:0-1: 30.
Example 1:1:0, the LCST of the temperature-sensitive material is 32 ℃, and the volume of the temperature-sensitive material shrinks by 20 percent after phase change.
Example 2:1:10, LCST of the temperature-sensitive material is 31 ℃, and volume shrinkage after phase change is 15%.
Example 3: 1:20, the LCST of the temperature-sensitive material is 29 ℃, and the volume of the temperature-sensitive material shrinks by 10 percent after phase change.
Example 4:1:30, LCST of the temperature-sensitive material is 28.5 ℃, and the volume of the temperature-sensitive material shrinks by 3 percent after phase change.
From examples 1 to 4, it is understood that the temperature-sensitive material LCST to which trehalose was added was significantly reduced and the volume was significantly reduced, and among them, the embodiment of example 4 was the least in volume and the most reduced in LCST, and the effect was the best.
The PNIPAm-based smart window has the defects of fragility, water loss, volume shrinkage, temperature response delay, LCST higher than the comfortable temperature of a human body and the like. The invention develops a simple and convenient method for preparing the novel PNIPAm-Trehalose temperature-sensitive hydrogel. The addition of trehalose obviously reduces the LCST of the PNIPAm hydrogel and greatly improves the thermal response rate of the PNIPAm hydrogel; more importantly, the trehalose modified PNIPAm hydrogel solves the problem of volume shrinkage before and after phase change of the common PNIPAm hydrogel. The high-performance temperature-responsive PNIPAm-Trehalose hydrogel can promote the development of a thermochromic intelligent window area and provides a new design scheme for an energy-saving material.
(2) Preparation of trehalose modified PNIPAm temperature-sensitive intelligent window
The experiment used a glass slide as the substrate. Firstly, a certain amount of trehalose modified PNIPAm hydrogel is added to the front surface of a glass slide, then a layer of glass slide is covered to form a sandwich structure, and finally the periphery of the sandwich structure is sealed by sealant. A7101 sailboat plate with 47.0mm by 20.5mm size was used as a high light transmittance slide. Samples with the thickness of 0.5mm, 0.75 mm and 0.10mm are successfully manufactured, and the trehalose modified PNIPAm temperature-sensitive hydrogel intelligent window is obtained. In addition, the sealing is tight, the water evaporation is prevented, and the safety and the durability in practical use are ensured. The trehalose-modified PNIPAm hydrogel film may remain completely transparent at room temperature below the LCST, but may be effectively protected from solar radiation by being translucent at temperatures above the LCST.
(3) Characterization of
The invention utilizes the synergistic effect of hydrophilic and hydrophobic groups and selects polymer monomers containing two end groups to synthesize the functional polymer with low-temperature thermochromic performance.
Determining the chemical structure of the new material by characterization means such as IR, MS, element analysis and the like; characterization of the absorption spectrum of the new polymer by UV; the thermophysical properties of the polymer material are characterized through TGA and DSC, and the glass transition temperature and LCST of the polymer material are determined; the rheological parameters of the polymer at different temperatures were determined by rheometer.
Measuring the internal microstructure of the polymer through SEM, TEM and AFM, exploring the construction condition of a hydrophilic-hydrophobic network interpenetrating structure, changing the film-forming morphology of the intelligent polymer through methods of mixed solvents, additives and the like, and determining the influence of the morphology on light transmittance.
Characterization of the light transmittance and Δ T at different temperatures of the polymers by UV-VIS-NIRsol,ΔTlum,ΔTIRTo determine the thermal insulation and other functional effects of the smart polymer film.
Compared with the polymerization of PNIPAm monomers, the physically crosslinked trehalose modified PNIPAm intelligent hydrogel has the characteristics of small volume swelling degree, easiness in molding, high stretching property, high toughness and the like. Based on the previous research, the method has abundant experience in synthesizing the intelligent polymer hydrogel with the physical cross-linked network, and the mechanical property of the hydrogel is obviously improved.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and should not be taken as limiting the scope of the present invention, which is intended to cover any modifications, equivalents, improvements, etc. within the spirit and scope of the present invention.
Claims (5)
1. A synthesis method of trehalose modified PNIPAm temperature-sensitive intelligent hydrogel is characterized by comprising the following steps:
step 1, dissolving trehalose in deionized water to form a trehalose solution with the mass fraction of 10-30%;
step 2, respectively adding N-isopropylacrylamide and N, N' -methylenebisacrylamide to the trehalose solution obtained in the step 1, and uniformly mixing to obtain a mixed solution; the mass ratio of the trehalose solution to the N-isopropylacrylamide to the N, N' -methylenebisacrylamide is 20: (1-2): (0.01-0.03);
and 3, adding ammonium persulfate into the mixed solution obtained in the step 2 and stirring, wherein the mass ratio of the trehalose solution to the ammonium persulfate is 20: (0.01-0.03);
step 4, adding 4-7 mu m of N, N, N ', N' -tetramethyl ethylenediamine into the mixed solution obtained in the step 3, and stirring to obtain a gel solution;
and 5, standing at the temperature of 20-30 ℃ for 2-3 hours to obtain the trehalose modified PNIPAm temperature-sensitive hydrogel.
2. The method for synthesizing the trehalose-modified PNIPAm temperature-sensitive intelligent hydrogel according to claim 1, wherein the mass ratio of the trehalose solution to N-isopropylacrylamide to N, N' -methylenebisacrylamide is 20: 1.34: 0.02.
3. the method for synthesizing the trehalose-modified PNIPAm temperature-sensitive intelligent hydrogel according to claim 1, wherein the mass ratio of trehalose solution to ammonium persulfate in the step 3 is 20: 0.02.
4. the method for synthesizing the trehalose-modified PNIPAm temperature-sensitive intelligent hydrogel as claimed in claim 1, wherein the trehalose solution in the step 1 contains trehalose in an amount of 30% by mass.
5. The application of the trehalose modified PNIPAm temperature-sensitive intelligent hydrogel in the temperature-sensitive intelligent window is characterized in that the specific application method is as follows: coating a layer of trehalose modified PNIPAm temperature-sensitive intelligent hydrogel on the upper surface of one glass slide, covering a layer of glass slide on the upper surface of the trehalose modified PNIPAm temperature-sensitive intelligent hydrogel to form a sandwich structure, and finally sealing the periphery of the hydrogel by using sealant to obtain the trehalose modified PNIPAm temperature-sensitive hydrogel intelligent window.
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