CN114103281A - Moisturizing three-layer material and preparation method thereof - Google Patents
Moisturizing three-layer material and preparation method thereof Download PDFInfo
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- CN114103281A CN114103281A CN202111404818.6A CN202111404818A CN114103281A CN 114103281 A CN114103281 A CN 114103281A CN 202111404818 A CN202111404818 A CN 202111404818A CN 114103281 A CN114103281 A CN 114103281A
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- 239000000463 material Substances 0.000 title claims abstract description 83
- 230000003020 moisturizing effect Effects 0.000 title claims abstract description 47
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- 229920001971 elastomer Polymers 0.000 claims abstract description 86
- 239000000806 elastomer Substances 0.000 claims abstract description 85
- 239000007822 coupling agent Substances 0.000 claims abstract description 80
- 239000000017 hydrogel Substances 0.000 claims abstract description 74
- 229920005557 bromobutyl Polymers 0.000 claims abstract description 58
- -1 polysiloxane Polymers 0.000 claims abstract description 30
- 229920001296 polysiloxane Polymers 0.000 claims abstract description 6
- 229920002401 polyacrylamide Polymers 0.000 claims abstract description 5
- 239000011159 matrix material Substances 0.000 claims abstract description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 33
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- 239000004205 dimethyl polysiloxane Substances 0.000 claims description 22
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 claims description 22
- 239000003431 cross linking reagent Substances 0.000 claims description 19
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims description 18
- 239000003054 catalyst Substances 0.000 claims description 17
- 125000004435 hydrogen atom Chemical group [H]* 0.000 claims description 17
- 229920001577 copolymer Polymers 0.000 claims description 16
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 16
- 239000003999 initiator Substances 0.000 claims description 14
- 230000009471 action Effects 0.000 claims description 12
- 239000011259 mixed solution Substances 0.000 claims description 11
- UUIMDJFBHNDZOW-UHFFFAOYSA-N 2-tert-butylpyridine Chemical compound CC(C)(C)C1=CC=CC=N1 UUIMDJFBHNDZOW-UHFFFAOYSA-N 0.000 claims description 10
- KWYHDKDOAIKMQN-UHFFFAOYSA-N N,N,N',N'-tetramethylethylenediamine Chemical group CN(C)CCN(C)C KWYHDKDOAIKMQN-UHFFFAOYSA-N 0.000 claims description 10
- 229910052697 platinum Inorganic materials 0.000 claims description 8
- MTCFGRXMJLQNBG-REOHCLBHSA-N (2S)-2-Amino-3-hydroxypropansäure Chemical compound OC[C@H](N)C(O)=O MTCFGRXMJLQNBG-REOHCLBHSA-N 0.000 claims description 6
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- 239000000178 monomer Substances 0.000 claims description 5
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- 238000000034 method Methods 0.000 claims description 4
- IXPNQXFRVYWDDI-UHFFFAOYSA-N 1-methyl-2,4-dioxo-1,3-diazinane-5-carboximidamide Chemical compound CN1CC(C(N)=N)C(=O)NC1=O IXPNQXFRVYWDDI-UHFFFAOYSA-N 0.000 claims description 3
- 239000011837 N,N-methylenebisacrylamide Substances 0.000 claims description 3
- HFTNNOZFRQLFQB-UHFFFAOYSA-N ethenoxy(trimethyl)silane Chemical group C[Si](C)(C)OC=C HFTNNOZFRQLFQB-UHFFFAOYSA-N 0.000 claims description 3
- ZIUHHBKFKCYYJD-UHFFFAOYSA-N n,n'-methylenebisacrylamide Chemical group C=CC(=O)NCNC(=O)C=C ZIUHHBKFKCYYJD-UHFFFAOYSA-N 0.000 claims description 3
- USHAGKDGDHPEEY-UHFFFAOYSA-L potassium persulfate Chemical group [K+].[K+].[O-]S(=O)(=O)OOS([O-])(=O)=O USHAGKDGDHPEEY-UHFFFAOYSA-L 0.000 claims description 3
- 229960001153 serine Drugs 0.000 claims description 3
- 235000010413 sodium alginate Nutrition 0.000 claims description 3
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- 229940005550 sodium alginate Drugs 0.000 claims description 3
- 229940045920 sodium pyrrolidone carboxylate Drugs 0.000 claims description 3
- HYRLWUFWDYFEES-UHFFFAOYSA-M sodium;2-oxopyrrolidine-1-carboxylate Chemical compound [Na+].[O-]C(=O)N1CCCC1=O HYRLWUFWDYFEES-UHFFFAOYSA-M 0.000 claims description 3
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 claims description 3
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- 230000000052 comparative effect Effects 0.000 description 16
- NKSJNEHGWDZZQF-UHFFFAOYSA-N ethenyl(trimethoxy)silane Chemical compound CO[Si](OC)(OC)C=C NKSJNEHGWDZZQF-UHFFFAOYSA-N 0.000 description 15
- 238000003756 stirring Methods 0.000 description 14
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- FWDBOZPQNFPOLF-UHFFFAOYSA-N ethenyl(triethoxy)silane Chemical compound CCO[Si](OCC)(OCC)C=C FWDBOZPQNFPOLF-UHFFFAOYSA-N 0.000 description 8
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- 238000009792 diffusion process Methods 0.000 description 4
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 3
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- 235000002597 Solanum melongena Nutrition 0.000 description 1
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- 230000006399 behavior Effects 0.000 description 1
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- GDTBXPJZTBHREO-UHFFFAOYSA-N bromine Substances BrBr GDTBXPJZTBHREO-UHFFFAOYSA-N 0.000 description 1
- 229910052794 bromium Inorganic materials 0.000 description 1
- 125000000484 butyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- 229920005549 butyl rubber Polymers 0.000 description 1
- CREMABGTGYGIQB-UHFFFAOYSA-N carbon carbon Chemical compound C.C CREMABGTGYGIQB-UHFFFAOYSA-N 0.000 description 1
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Images
Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B7/00—Layered products characterised by the relation between layers; Layered products characterised by the relative orientation of features between layers, or by the relative values of a measurable parameter between layers, i.e. products comprising layers having different physical, chemical or physicochemical properties; Layered products characterised by the interconnection of layers
- B32B7/04—Interconnection of layers
- B32B7/10—Interconnection of layers at least one layer having inter-reactive properties
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29D—PRODUCING PARTICULAR ARTICLES FROM PLASTICS OR FROM SUBSTANCES IN A PLASTIC STATE
- B29D7/00—Producing flat articles, e.g. films or sheets
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B25/00—Layered products comprising a layer of natural or synthetic rubber
- B32B25/04—Layered products comprising a layer of natural or synthetic rubber comprising rubber as the main or only constituent of a layer, which is next to another layer of the same or of a different material
- B32B25/08—Layered products comprising a layer of natural or synthetic rubber comprising rubber as the main or only constituent of a layer, which is next to another layer of the same or of a different material of synthetic resin
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B25/00—Layered products comprising a layer of natural or synthetic rubber
- B32B25/18—Layered products comprising a layer of natural or synthetic rubber comprising butyl or halobutyl rubber
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B27/00—Layered products comprising a layer of synthetic resin
- B32B27/28—Layered products comprising a layer of synthetic resin comprising synthetic resins not wholly covered by any one of the sub-groups B32B27/30 - B32B27/42
- B32B27/283—Layered products comprising a layer of synthetic resin comprising synthetic resins not wholly covered by any one of the sub-groups B32B27/30 - B32B27/42 comprising polysiloxanes
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B7/00—Layered products characterised by the relation between layers; Layered products characterised by the relative orientation of features between layers, or by the relative values of a measurable parameter between layers, i.e. products comprising layers having different physical, chemical or physicochemical properties; Layered products characterised by the interconnection of layers
- B32B7/04—Interconnection of layers
- B32B7/12—Interconnection of layers using interposed adhesives or interposed materials with bonding properties
-
- 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
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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
- C08J2333/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Derivatives of such polymers
- C08J2333/24—Homopolymers or copolymers of amides or imides
- C08J2333/26—Homopolymers or copolymers of acrylamide or methacrylamide
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- Chemical & Material Sciences (AREA)
- Dispersion Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Compositions Of Macromolecular Compounds (AREA)
- Laminated Bodies (AREA)
Abstract
The invention provides a moisturizing three-layer material and a preparation method thereof, wherein the moisturizing three-layer material is formed by chemically connecting an upper-layer elastomer, a middle-layer hydrogel and a lower-layer brush-shaped elastomer through a coupling agent; the hydrogel is polyacrylamide hydrogel containing a moisturizing factor and a coupling agent, and the elastomer is brominated butyl rubber containing the coupling agent; the brush-shaped elastomer is an elastomer with brush-shaped polysiloxane as a matrix; the material disclosed by the invention is good in bonding effect and water retention effect, can intelligently regulate and control the release and absorption of the material to moisture according to the humidity change of the external environment, has excellent mechanical properties and a buffering liner effect, and is very suitable for moisture retention protection of cigars and the like.
Description
Technical Field
The invention belongs to the field of composite materials, and particularly relates to a moisturizing three-layer material and a preparation method thereof.
Background
The cigar is produced, stored and sold, and finally, the cigar can be in the hand of the consumer for 1-2 years, and the temperature of 18-20 ℃ and the relative humidity of 65-70% are the most suitable conditions for preserving and maintaining the cigar. However, the environment outside the cigar undergoes different humidity and temperature variations, and the moisture content of the cigar will change dramatically if there is no effective moisture retention measure. Cigars with high water content are difficult to ignite and keep burning, and the smoking quality is also influenced; when the water content is low, even the eggplant clothes crack and other adverse phenomena can occur. Therefore, regulating the humidity of the cigar preservation microenvironment is of great significance in the transportation, storage and sale processes of cigars. Therefore, how to regulate and control the humidity of the cigar packaging microenvironment, maintain the sensory quality of cigar products and improve the market competitiveness of cigar storage is an important problem to be solved urgently.
The polymer hydrogel is a water-swellable functional polymer material formed by a three-dimensional cross-linked network, and has excellent water absorption and water retention characteristics. The hydrogel has wide application prospect in the fields of biomedicine, wet cultural relic protection, wearable, implantation equipment and the like. Brominated butyl rubber (BIIR) is an isobutylene-isoprene elastomer copolymer containing active bromine, and the carbon-carbon main chain structure endows the copolymer with good flexibility, chemical inertness, acid and alkali corrosion resistance, barrier property and excellent weather resistance, and plays roles in buffering, damping and isolating oxygen. Brush polymers, also known as polymer molecular brushes, refer to a class of macromolecular systems with a particular structure formed by grafting a macromolecular polymer chain onto a polymer backbone. Due to the existence of steric hindrance, the polymer side chains repel each other and extend outwards, so that a structure similar to a laboratory flask brush is realized on a molecular level; the brush-shaped polymer has adjustable free volume, plays a role in regulating and controlling the diffusion and absorption of water, can prevent the loss of water of the cigar in a low-humidity environment when applied to the protection of the cigar, and inhibits the water absorption of the cigar in a high-humidity environment, thereby keeping the constant moisture content of the cigar for a long time.
Disclosure of Invention
The brominated butyl rubber elastomer material, the moisturizing hydrogel material and the brush-shaped polymer material for preventing reverse osmosis of water in the hydrogel are organically combined together to form a three-layer material with an inner layer of a brush-shaped elastomer, a middle layer of the moisturizing hydrogel and an outer layer of an elastomer layer. However, the application of the material with a special three-layer structure in the field of the regulation and control of the micro-humidity environment of the cigar is rarely reported.
The invention aims to provide a composite material with excellent humidity regulation performance, and specifically adopts the following technical scheme:
a moisture-retaining three-layer material is formed by chemically connecting an upper layer elastomer, a middle layer hydrogel and a lower layer brush-shaped elastomer through a coupling agent;
the hydrogel is polyacrylamide hydrogel at least containing a moisturizing factor and a coupling agent, and the elastomer is brominated butyl rubber containing the coupling agent; the brush-shaped elastomer is an elastomer with brush-shaped polysiloxane as a matrix.
The polyacrylamide hydrogel is formed by polymerizing monomers under the action of an initiator, a catalyst and a cross-linking agent, and the monomers comprise acrylamide.
The thickness ratio of the elastomer, the hydrogel and the brush-shaped elastomer is (0.2-10): (0.5-30): 0.2-10). Preferably, the thickness ratio of the elastomer, the hydrogel to the brush-like elastomer is (0.1-0.6):1 (0.1-0.7).
One scheme of the invention is that in the moisture-retaining three-layer material, the thickness of the brush-shaped elastic body accounts for 10-30% of the total thickness of the moisture-retaining three-layer material, for example, the thickness of the brush-shaped elastic body accounts for 11%, 15%, 17%, 20%, 22%, 25%, 26.5%, 27%, 29% and the like; the thickness of the elastomer (brominated butyl rubber) accounts for 15-20% of the total thickness of the moisturizing three-layer material, for example, the thickness of the elastomer accounts for 16%, 17%, 17.5%, 18%, 19%, 20% and the like; the thickness of the hydrogel accounts for 50-75% of the total thickness of the moisturizing three-layer material, such as 55%, 60%, 65%, 68%, 70%, 72%, 75% of the thickness of the hydrogel. The total thickness of the moisturizing three-layer material is selected according to actual needs.
The brush polysiloxane is: any one of copolymers such as trimethylsiloxane-terminated vinylmethylsiloxane-dimethylsiloxane copolymer, trimethylsiloxane-terminated tetramethyldivinyldisiloxane-dimethylsiloxane copolymer, trimethylsiloxane-terminated tris (trimethylsilyl) oxyethylene silane-dimethylsiloxane copolymer, etc. is used as a main chain, and the number average molecular weight thereof is about 50000-; the end group is a hydrogen atom-terminated polydimethylsiloxane as a side chain, and the number average molecular weight is about 3000-6000 g/mol; the end group is polydimethylsiloxane terminated by two hydrogen atoms and is used as a cross-linking agent, and the number average molecular weight of the cross-linking agent is about 6000-10000 g/mol. The mass ratio of the main chain, the side chain and the cross-linking agent is 1 (1.4-1.6) to 0.04-0.06; preferably, the mass ratio of the main chain, the side chain and the cross-linking agent is 1:1.5: 0.05.
The coupling agent is a silane coupling agent, preferably a silane coupling agent containing vinyl such as vinyltrimethoxysilane or vinyltriethoxysilane.
The mass fraction of the coupling agent contained in the hydrogel relative to the acrylamide monomer is 0.1-0.5%, preferably 0.33%.
The mass fraction of the coupling agent contained in the elastomer relative to the brominated butyl rubber is 0.1-0.8%, preferably 0.5%.
The hydrogel contains 20-60% of moisturizing factors, preferably 40% of moisturizing factors relative to the mass of acrylamide monomers; the moisturizing factor is at least one of glycerol, L-serine, sodium alginate and sodium pyrrolidone carboxylate.
The initiator is potassium persulfate, and the dosage of the initiator is 0.01-0.04 g per 15g of acrylamide monomer; the catalyst is tetramethylethylenediamine, and the dosage of the catalyst is 20-40 mu L per 15g of acrylamide monomer; the cross-linking agent is N, N-methylene bisacrylamide, and the dosage of the cross-linking agent is 3-5 mg per 15g of acrylamide monomer.
The preparation method of the three-layer material comprises the following steps:
(1) dissolving acrylamide, a cross-linking agent, a moisturizing factor and a coupling agent in water, adding an initiator and a catalyst under an anaerobic condition, uniformly mixing to obtain a mixed solution, and curing the mixed solution at 30-60 ℃ for 1-3 h to obtain hydrogel;
(2) and (2) uniformly mixing a coupling agent and brominated butyl rubber, curing to obtain an elastomer, uniformly mixing the coupling agent and siloxane, wherein the siloxane comprises the main chain, the side chain and polydimethylsiloxane with two hydrogen atom end caps as end groups, curing to obtain a brush-shaped elastomer, placing the hydrogel obtained in the step (1) between the elastomer and the brush-shaped elastomer, and standing at room temperature for 20-30 hours to obtain the three-layer material.
The step (2) of uniformly mixing and curing the coupling agent and the brominated butyl rubber is as follows: uniformly mixing a coupling agent and brominated butyl rubber, and curing for 2-10 min at 100-150 ℃ under the action of a cross-linking agent tert-butylpyridine;
the coupling agent and the siloxane are uniformly mixed and cured as follows: one of main chains of trimethylsiloxane end-capped vinyl methylsiloxane-dimethylsiloxane and the like, monohydrogen end-capped polydimethylsiloxane (side chain), dihydride end-capped polydimethylsiloxane (cross-linking agent) and a coupling agent are uniformly mixed, and the mixture is cured for 25 to 40 hours at 70 to 90 ℃ under the action of a platinum catalyst.
When preparing the brominated butyl rubber elastomer, a cross-linking agent of tert-butyl pyridine is also used, and the mass ratio of the brominated butyl rubber to the tert-butyl pyridine is (95-155): 1. the coupling agent used in the brush elastomer is a silane coupling agent containing a vinyl group such as vinyltrimethoxysilane or vinyltriethoxysilane.
The invention has the beneficial effects that: according to the invention, the functional hydrogel and the two high-molecular elastomers are compounded to obtain the sandwich-type bionic skin transparent moisturizing material, the brominated butyl rubber is used for buffering and damping and isolating oxygen, the hydrogel is used for humidifying, and the brush-shaped elastomer is used for regulating and controlling the diffusion and absorption of water, so that the cigar can be prevented from losing water in a low-humidity environment, and the cigar can be inhibited from absorbing water in a high-humidity environment, and thus the cigar can keep constant moisture content for a long time. The hydrogel and the elastomer form covalent bonding through reaction between bonding molecules, so that the hydrogel is prevented from being separated in the using process. The material has the characteristics of high transparency, good water retention effect, excellent mechanical property and the like, and is suitable for regulating and controlling the humidity of the cigars.
Obviously, many modifications, substitutions, and variations are possible in light of the above teachings of the invention, without departing from the basic technical spirit of the invention, as defined by the following claims.
Drawings
Fig. 1 is a structural diagram of the bionic skin transparent moisturizing material. In the figure, numeral 1 denotes an upper layer elastomer, numeral 2 denotes an intermediate layer hydrogel, and numeral 3 denotes a lower layer brush elastomer.
FIG. 2 is a graph showing the adhesion properties of the material of the present invention.
FIG. 3 is a graph showing the mechanical properties of the materials of comparative examples 1 and 2 and example 1 of the present invention.
FIG. 4 is a graph of the moisturizing performance of the materials of comparative examples 1 and 2 and example 1 of the present invention.
FIG. 5 is a graph of the humidity control performance of the material on the cigar microenvironment in example 1.
Detailed Description
The present invention will be described in further detail with reference to the following examples. This should not be understood as limiting the scope of the above-described subject matter of the present invention to the following examples. All the technologies realized based on the above contents of the present invention belong to the scope of the present invention.
The raw materials and equipment used in the invention are known products and are obtained by purchasing commercial products.
Example 1 preparation of a three-layer Material according to the invention
Adding 15g of Acrylamide (AM) into 50g of water to form a mixed solution, adding 0.005g of cross-linking agent N, N-Methylene Bisacrylamide (MBA) after the AM is uniformly dissolved, stirring for 2min on a magnetic stirrer, adding 6g of glycerol, removing oxygen for 15min, adding 0.05g of coupling agent vinyl trimethoxy silane, adding 0.04g of initiator potassium persulfate (KPS) and 25 mu L of catalyst tetramethyl ethylenediamine (TMEDA), stirring for 3min, pouring into a mold, and carrying out water bath at 60 ℃ for 3h to obtain the moisture-retaining hydrogel material.
According to the mass ratio of 1: 4 brominated butyl rubber (10g) and toluene were mixed, 0.1g of t-butylpyridine was added thereto, and mixed at room temperature to obtain a BIIR precursor solution. To the precursor solution was added 0.05g of the coupling agent vinyltrimethoxysilane. Standing for 20h at room temperature, after the solvent is volatilized, crosslinking and curing at 130 ℃ for 5 minutes to obtain the brominated butyl rubber (BIIR) containing the coupling agent.
According to the mass ratio of 1:1.5:0.05 mixture of trimethylsiloxane-terminated vinylmethylsiloxane-dimethylsiloxane copolymer (number average molecular weight 65000g/mol), polydimethylsiloxane terminated with one hydrogen atom as the terminal group (number average molecular weight 4500g/mol) and polydimethylsiloxane terminated with two hydrogen atoms as the terminal group (number average molecular weight 8000g/mol), a precursor solution was obtained, and 2. mu.L of vinyltrimethoxysilane as a coupling agent was added to the precursor solution. Reacting for 40h at 80 ℃ under the action of a platinum catalyst to obtain the brush-shaped elastomer containing the bonding molecules.
Curing the brominated butyl rubber elastomer containing the coupling agent in a surface dish to form a film, wherein the thickness of the film is about 3mm, forming a film by a brush-shaped elastomer containing the coupling agent in the surface dish, the thickness of the film is 2mm, the thickness of the film formed by hydrogel containing the coupling agent is 15mm, respectively attaching the brominated butyl rubber elastomer containing the coupling agent and the brush-shaped elastomer to two surfaces of the hydrogel film containing the coupling agent, and forming an adhesive joint at the interface after 30 hours at room temperature to obtain the bionic skin transparent moisturizing material C, wherein the thickness of the bionic skin transparent moisturizing material C is 20 mm. The structure schematic diagram is shown in figure 1.
Example 2 preparation of a three-layer Material according to the invention
Adding 15g of AM into 50g of water to form a mixed solution, adding 0.005g of MBA after the AM is uniformly dissolved, stirring for 2min on a magnetic stirrer, adding 6g L-serine, deoxidizing for 15min, adding 0.015g of coupling agent vinyl trimethoxy silane, adding 0.04g of initiator KPS and 25 mu L of tetramethyl ethylene diamine, stirring for 3min, pouring into a mold, and carrying out water bath at 60 ℃ for 3h to obtain the moisturizing gel material.
Brominated butyl rubber (10g) and toluene are mixed according to the mass ratio of 1:3, then 0.1g of tert-butylpyridine is added, and the mixture is mixed at normal temperature to obtain BIIR precursor solution. To the precursor solution was added 0.01g of the coupling agent vinyltrimethoxysilane. Standing for 20h at room temperature, after the solvent is volatilized, crosslinking and curing at 130 ℃ for 5min to obtain the brominated butyl rubber (BIIR) containing the coupling agent.
According to the mass ratio of 1:1.5:0.05 Trimethylsiloxane-terminated vinylmethylsiloxane-dimethylsiloxane copolymer (number average molecular weight of 50000g/mol), polydimethylsiloxane having one hydrogen atom as a terminal group (number average molecular weight of 3000g/mol) and polydimethylsiloxane having two hydrogen atoms as a terminal group (number average molecular weight of 6000g/mol) were mixed, a precursor solution was obtained by mixing at normal temperature, and 2. mu.L of vinyltriethoxysilane was added to the precursor solution. Reacting for 40h at 80 ℃ under the action of a platinum catalyst to obtain the brush-shaped elastomer containing the bonding molecules.
Curing the brominated butyl rubber elastomer containing the coupling agent in a surface dish to form a film, wherein the thickness of the film is about 3mm, forming a film in the surface dish by using a brush-shaped elastomer containing the coupling agent, the thickness of the film is 2mm, the thickness of the film formed by hydrogel containing the coupling agent is 15mm, respectively attaching the brominated butyl rubber elastomer containing the coupling agent and the brush-shaped elastomer to two surfaces of the hydrogel film containing the coupling agent, and forming an adhesive joint at room temperature for 20h to obtain the bionic skin transparent moisturizing material D, wherein the thickness of the bionic skin transparent moisturizing material D is 20 mm.
Example 3 preparation of a three-layer Material according to the invention
Adding 15g of AM into 50g of water to form a mixed solution, adding 0.005g of MBA after the AM is uniformly dissolved, stirring for 2min on a magnetic stirrer, adding 6g of sodium alginate, deoxidizing for 15min, adding 0.075g of coupling agent vinyl trimethoxy silane, adding 0.04g of initiator KPS and 25 mu L of tetramethyl ethylene diamine, stirring for 3min, pouring into a mold, and carrying out water bath at 60 ℃ for 3h to obtain the moisturizing hydrogel material.
According to the mass ratio of 1: 4 brominated butyl rubber (10g) and toluene were mixed, 0.1g of t-butylpyridine was added thereto, and mixed at room temperature to obtain a BIIR precursor solution. To the precursor solution was added 0.08g of the coupling agent vinyltrimethoxysilane. Standing for 20h at room temperature, after the solvent is volatilized, crosslinking and curing at 130 ℃ for 5min to obtain the brominated butyl rubber (BIIR) containing the coupling agent.
According to the mass ratio of 1:1.5:0.05 Trimethylsiloxane-terminated tetramethyldivinyldisiloxane-dimethylsiloxane copolymer (number average molecular weight 80000g/mol), polydimethylsiloxane terminated with one hydrogen atom (number average molecular weight 6000g/mol) and polydimethylsiloxane terminated with two hydrogen atoms (number average molecular weight 10000g/mol) were mixed at normal temperature to obtain a precursor solution, and 2. mu.L of vinyltriethoxysilane was added to the precursor solution. Reacting for 40h at 70 ℃ under the action of a platinum catalyst to obtain the brush-shaped elastomer containing the bonding molecules.
Curing the brominated butyl rubber elastomer containing the coupling agent in a surface dish to form a film, wherein the thickness of the film is about 0.3mm, forming a film of a brush-shaped elastomer containing the coupling agent in the surface dish, the thickness of the film is 0.2mm, forming a film of hydrogel containing the coupling agent in the thickness of 0.5mm, respectively attaching the brominated butyl rubber elastomer containing the coupling agent and the brush-shaped elastomer to two sides of the hydrogel film containing the coupling agent, and forming an adhesive joint on an interface after 30 hours at room temperature to obtain the bionic skin transparent moisturizing material E, wherein the thickness of the bionic skin transparent moisturizing material E is 1 mm.
Example 4 preparation of a three-layer Material according to the invention
Adding 15g of AM into 50g of water to form a mixed solution, adding 0.005g of MBA after the AM is uniformly dissolved, stirring for 1min on a magnetic stirrer, adding 3g of glycerol, deoxidizing for 10min, adding 0.05g of coupling agent vinyl trimethoxy silane, adding 0.04g of initiator KPS and 25 mu L of tetramethyl ethylene diamine, stirring for 2min, pouring into a mold, and carrying out water bath at 60 ℃ for 1h to obtain the moisturizing hydrogel material.
According to the mass ratio of 1: 4 brominated butyl rubber (10g) and toluene were mixed, 0.1g of t-butylpyridine was added thereto, and mixed at room temperature to obtain a BIIR precursor solution. To the precursor solution was added 0.05g of the coupling agent vinyltrimethoxysilane. Standing for 20h at room temperature, after the solvent is volatilized, crosslinking and curing for 2min at 130 ℃ to obtain the brominated butyl rubber (BIIR) containing the coupling agent.
According to the mass ratio of 1: 1.4: 0.04 Trimethylsiloxane-terminated tris (trimethylsilyl) oxyethylene silane-dimethylsiloxane copolymer (number average molecular weight of 65000g/mol), polydimethylsiloxane terminated with one hydrogen atom as the terminal group (number average molecular weight of 4500g/mol) and polydimethylsiloxane terminated with two hydrogen atoms as the terminal group (number average molecular weight of 8000g/mol) were mixed at room temperature to obtain a precursor solution, and 2. mu.L of vinyltriethoxysilane was added to the precursor solution. Reacting for 25h at 90 ℃ under the action of a platinum catalyst to obtain the brush-shaped elastomer containing the bonding molecules.
Curing a brominated butyl rubber elastomer containing a coupling agent in a surface dish to form a film, wherein the thickness of the film is about 10mm, forming a brush-shaped elastomer containing the coupling agent in the surface dish to form a film, the thickness of the film is 10mm, the thickness of the film formed by hydrogel containing the coupling agent is 30mm, respectively attaching the brominated butyl rubber elastomer containing the coupling agent and the brush-shaped elastomer to two surfaces of the hydrogel film containing the coupling agent, and forming an adhesive joint on an interface after 30 hours at room temperature to obtain the bionic skin transparent moisturizing material F, wherein the thickness of the bionic skin transparent moisturizing material F is 50 mm.
Example 5 preparation of a three-layer Material according to the invention
Adding 15g of AM into 50g of water to form a mixed solution, adding 0.005g of MBA after the AM is uniformly dissolved, stirring for 3min on a magnetic stirrer, adding 6g of sodium pyrrolidone carboxylate, deoxidizing for 30min, adding 0.05g of coupling agent vinyl triethoxysilane, adding 0.04g of initiator KPS and 25 mu L of tetramethyl ethylenediamine, stirring for 5min, pouring into a mold, and carrying out water bath at 50 ℃ for 3h to obtain the moisturizing hydrogel material.
According to the mass ratio of 1: 4 brominated butyl rubber (10g) and toluene were mixed, 0.1g of t-butylpyridine was added thereto, and mixed at room temperature to obtain a BIIR precursor solution. To the precursor solution was added 0.05g of the coupling agent vinyltriethoxysilane. Standing for 20h at room temperature, after the solvent is volatilized, crosslinking and curing at 100 ℃ for 10min to obtain the brominated butyl rubber (BIIR) containing the coupling agent.
According to the mass ratio of 1: 1.6: 0.06 part of a trimethylsiloxane-terminated vinylmethylsiloxane-dimethylsiloxane copolymer (number average molecular weight: 65000g/mol), a polydimethylsiloxane having a terminal group of one hydrogen atom (number average molecular weight: 4500g/mol), and a polydimethylsiloxane having a terminal group of two hydrogen atoms (number average molecular weight: 8000g/mol) were mixed to obtain a precursor solution, and 2. mu.L of vinyltriethoxysilane was added to the precursor solution. Reacting for 40h at 80 ℃ under the action of a platinum catalyst to obtain the brush-shaped elastomer containing the bonding molecules.
Curing the brominated butyl rubber elastomer containing the coupling agent in a surface dish to form a film, wherein the thickness of the film is about 3mm, forming a film by a brush-shaped elastomer containing the coupling agent in the surface dish, the thickness of the film is 2mm, the thickness of the film formed by hydrogel containing the coupling agent is 15mm, respectively attaching the brominated butyl rubber elastomer containing the coupling agent and the brush-shaped elastomer to two surfaces of the hydrogel film containing the coupling agent, and forming an adhesive joint at the interface after 30 hours at room temperature to obtain the bionic skin transparent moisturizing material G with the thickness of 20 mm.
Comparative example 1 preparation of hydrogel and elastomeric bilayer Material
Adding 15g of AM into 50g of water to form a mixed solution, adding 0.005g of MBA after the AM is uniformly dissolved, stirring for 2min on a magnetic stirrer, adding 6g of glycerol, deoxidizing for 15min, adding 0.05g of coupling agent vinyl trimethoxy silane, adding 0.04g of initiator KPS and 25 mu L of tetramethyl ethylene diamine, stirring for 3min, pouring into a mold, and carrying out water bath at 60 ℃ for 3h to obtain the moisturizing hydrogel material.
According to the mass ratio of 1: 4 brominated butyl rubber (10g) and toluene were mixed, 0.1g of t-butylpyridine was added thereto, and mixed at room temperature to obtain a BIIR precursor solution. To the precursor solution was added 0.05g of the coupling agent vinyltrimethoxysilane. Standing for 20h at room temperature, after the solvent is volatilized, crosslinking and curing at 130 ℃ for 5 minutes to obtain the brominated butyl rubber (BIIR) containing the coupling agent.
And (3) forming a film of the brominated butyl rubber elastomer containing the coupling agent and the hydrogel in a watch glass, wherein the thickness of the film of the brominated butyl rubber elastomer is 3mm, and the thickness of the hydrogel film is 17 mm. The brominated butyl rubber elastomer containing the coupling agent was bonded to the hydrogel film containing the coupling agent, and after 30 hours at room temperature, an interface was formed and adhered to obtain comparative example A, which had a thickness of 20 mm.
Comparative example 2 preparation of hydrogel and Brush-like elastomeric bilayer Material
Adding 15g of AM into 50g of water to form a mixed solution, adding 0.005g of MBA after the AM is uniformly dissolved, stirring for 2min on a magnetic stirrer, adding 6g of glycerol and 0.05g of vinyl trimethoxy silane, deoxidizing for 15min, adding 0.04g of initiator KPS and 25 mu L of tetramethyl ethylene diamine, stirring for 3min, pouring into a mold, and carrying out water bath at 60 ℃ for 3h to obtain the moisturizing hydrogel material containing bonding molecules.
According to the mass ratio of 1:1.5:0.05 part of a trimethylsiloxane-terminated vinylmethylsiloxane-dimethylsiloxane copolymer (number average molecular weight: 65000g/mol), a polydimethylsiloxane having a terminal group of one hydrogen atom (number average molecular weight: 4500g/mol), and a polydimethylsiloxane having a terminal group of two hydrogen atoms (number average molecular weight: 8000g/mol) were mixed at room temperature to obtain a precursor solution, and 0.05 part of vinyltrimethoxysilane was added to the precursor solution. Reacting for 40h at 80 ℃ under the action of a platinum catalyst to obtain the brush-shaped elastomer containing the bonding molecules.
The hydrogel containing the coupling agent and the brush-shaped elastomer are subjected to film formation in a watch glass, wherein the thickness of the hydrogel film is 18mm, and the thickness of the brush-shaped elastomer film is 2 mm. The brush-shaped elastomer containing the coupling agent was bonded to the hydrogel film containing the coupling agent, and after 30 hours at room temperature, an interface was formed and adhered to obtain comparative example B having a thickness of 20 mm.
The beneficial effects of the present invention are demonstrated by the following experimental examples.
Experimental example 1 characterization of the Properties of the three-layer Material according to the invention
1. Experimental methods
(1) Mechanical Property test
The tensile stress-strain behavior of examples 1 and comparative examples 1 to 2 (comparative example a, comparative example B) was tested with a universal tensile tester Instron 5567 at a tensile rate of 100mm/min, the samples were stretched until breaking and the stress-strain curves were recorded.
(2) Characterization of adhesive Properties
And (3) peeling the upper layer elastomer from the other two layers of materials, and observing the condition of the hydrogel remained on the surface of the peeled upper layer elastomer. In addition, to distinguish whether the three-layer material was crushed during the peeling process due to poor mechanical properties of the hydrogel, a uniaxial tensile test was performed on a bulk hydrogel having the same thickness as the hydrogel in the three-layer material, and the mechanical properties were evaluated.
(3) Test for moisture retention
The materials of example 1, comparative example 1 and comparative example 2 were weighed at 25 ℃ at different time points within 12 hours after saturation in water absorption, and the moisture retention rate was calculated according to the following formula to evaluate the moisture retention capacity of the materials:
W＝m2/m1×100％
in the formula: w is the moisture retention rate, m1Mass of sample saturated with water, m2Is the mass of the sample when weighed.
(4) Performance test for regulating and controlling humidity of cigar microenvironment by material
The moisturizing material obtained in example 1 was placed in a cigar pack, and a blank cigar pack without the moisturizing material was used as a control. The two groups of cigar boxes are respectively placed in the environment of 40% RH and 90% RH, and the change of the internal humidity of the cigar boxes along with time is monitored, so that the regulation and control effect of the material on the microenvironment humidity of the cigar is examined.
2. Results of the experiment
As can be seen from fig. 1, the humidity control material C of example 1 of the present invention has a three-layer structure, in which the upper and lower layers are the silicone elastomer layer and the brush-like elastomer layer, respectively, and function as a buffer barrier and control of water diffusion; the middle part is a hydrogel layer which has the functions of releasing and absorbing water.
As can be seen from FIG. 2a, after the upper layer elastomer of the three-layer material obtained in example 1 of the present invention was peeled from the other two layers, a large number of hydrogel fragments of the middle layer remained on the surface of the upper layer elastomer, indicating that good adhesion was formed between the elastomer and the hydrogel. In addition, the middle layer hydrogel was found to have good mechanical properties by tensile testing alone (fig. 2b), which demonstrates that the formation of hydrogel debris during peeling is not due to poor mechanical properties of the hydrogel itself, but rather due to good adhesion between the elastomer and the hydrogel.
From fig. 3, it can be found that the breaking strength and breaking strain of comparative example a of the two-layer structure formed of the brominated butyl rubber and the hydrogel are 0.84MPa and 430% respectively, and the breaking strength and breaking strain of comparative example B of the two-layer structure formed of the hydrogel and the brush elastomer are 0.43MPa and 240% respectively. The rupture strength and the rupture strain of the moisturizing three-layer material C in the embodiment 1 are respectively 1.53MPa and 825%, and are higher than the mechanical properties of the comparative examples A and B, even obviously higher than the sum of the mechanical properties of the comparative examples A and B, which shows that the mechanical properties of the bionic skin moisturizing material are improved by the composite cooperation of the brominated butyl rubber, the hydrogel and the brush-shaped elastomer three-layer material.
As can be seen from fig. 4, the moisturizing rate of the moisturizing three-layer material C of example 1 of the present invention was higher than the corresponding moisturizing rates of comparative examples 1(a) and 2(B) within 12 hours, indicating that the biomimetic skin moisturizing material of the three-layer structure had more excellent moisturizing performance than the brominated butyl rubber and hydrogel or hydrogel and brush-like elastomer of the two-layer structure.
As can be seen from fig. 5, after the cigar box is placed at 40 ℃ and 40% RH for 48 hours, the humidity inside the blank cigar box without the moisture retention material is reduced to below 60% RH, while the humidity control material C of the present invention can increase the humidity inside the cigar box to about 70% RH; after the cigar box is placed for 48 hours at the temperature of 40 ℃ and the RH of 90 percent, the internal humidity of the blank cigar box is increased to about 90 percent RH, and the humidity conditioning material C can control the internal humidity of the cigar box to about 80 percent RH. The above results show that the humidity control material of the present invention can control the release and absorption of moisture in the material according to the change of external humidity, so as to prevent the loss of moisture of the cigars in the low humidity environment and inhibit the absorption of moisture of the cigars in the high humidity environment, thereby reducing the influence of the external environment and maintaining the constant moisture content of the cigars.
In conclusion, the invention provides a three-layer material with an intelligent humidity-regulating effect, which plays a role in regulating and controlling the diffusion and absorption of water, can prevent the loss of water of cigars in a low-humidity environment and inhibit the water absorption of the cigars in a high-humidity environment when applied to the protection of the cigars, so that the cigars can keep constant moisture content for a long time, and has excellent mechanical properties and a buffer liner effect, thereby being very suitable for regulating and controlling the micro-humidity environment of the cigars.
Claims (10)
1. A moisture-retaining three-layer material is characterized in that the material is formed by chemically connecting an upper-layer elastomer, a middle-layer hydrogel and a lower-layer brush-shaped elastomer through a coupling agent;
the hydrogel is polyacrylamide hydrogel at least containing a moisturizing factor and a coupling agent, and the elastomer is brominated butyl rubber containing the coupling agent; the brush-shaped elastomer is an elastomer with brush-shaped polysiloxane as a matrix;
the polyacrylamide hydrogel is formed by polymerizing monomers under the action of an initiator, a catalyst and a cross-linking agent, and the monomers comprise acrylamide.
2. The three-layer material of claim 1, wherein the ratio of the thickness of the elastomer, hydrogel and brush elastomer is (0.2-10): (0.5-30): (0.2-10).
3. Three-layer material according to claim 1 or 2, characterized in that the brush polysiloxane is: any one copolymer of trimethylsiloxane end-capped vinyl methyl siloxane-dimethyl siloxane copolymer, trimethylsiloxane end-capped tetramethyl divinyl disiloxane-dimethyl siloxane copolymer and trimethylsiloxane end-capped tri (trimethylsilyl) oxyethylene silane-dimethyl siloxane copolymer is taken as a main chain, and the number average molecular weight of the copolymer is 50000-80000 g/mol; the end group is a hydrogen atom-terminated polydimethylsiloxane as a side chain, and the number average molecular weight of the polydimethylsiloxane is 3000-6000 g/mol; the end group is polydimethylsiloxane terminated by two hydrogen atoms and is used as a cross-linking agent to prepare the brush-shaped polysiloxane, and the number average molecular weight of the cross-linking agent is 6000-10000 g/mol.
4. The three-layer material of claim 1 or 2, wherein the coupling agent is a silane coupling agent containing vinyl groups.
5. The three-layer material according to claim 4, wherein the hydrogel contains a coupling agent in a mass fraction of 0.1% to 0.5% with respect to the acrylamide monomer.
6. The three-layer material according to claim 4, wherein the elastomer contains a coupling agent in a mass fraction of 0.1% to 0.8% with respect to the bromobutyl rubber.
7. Three-layer material according to claim 1 or 2, characterized in that the hydrogel contains a moisturizing factor in a mass fraction of 20% to 60% with respect to the acrylamide monomer; the moisturizing factor is at least one of glycerol, L-serine, sodium alginate and sodium pyrrolidone carboxylate.
8. The three-layer material according to claim 1 or 2, wherein the initiator is potassium persulfate in an amount of 0.01 to 0.04g per 15g of acrylamide monomer; the catalyst is tetramethylethylenediamine, and the dosage of the catalyst is 20-40 mu L per 15g of acrylamide monomer; the cross-linking agent is N, N-methylene bisacrylamide, and the dosage of the cross-linking agent is 3-5 mg per 15g of acrylamide monomer.
9. A method of producing a three-layer material according to any one of claims 1 to 8, characterised in that it comprises the following steps:
(1) dissolving acrylamide, a cross-linking agent, a moisturizing factor and a coupling agent in water, adding an initiator and a catalyst under an anaerobic condition, uniformly mixing to obtain a mixed solution, and curing the mixed solution at 30-60 ℃ for 1-3 h to obtain hydrogel;
(2) and (2) uniformly mixing a coupling agent and brominated butyl rubber, curing to obtain an elastomer, uniformly mixing the coupling agent and siloxane, wherein the siloxane comprises a main chain, a side chain and polydimethylsiloxane with two hydrogen atom end caps as end groups, curing to obtain a brush-shaped elastomer, placing the hydrogel obtained in the step (1) between the elastomer and the brush-shaped elastomer, and standing at room temperature for 20-30 hours to obtain the three-layer material.
10. The preparation method of claim 9, wherein the step (2) of uniformly mixing and curing the coupling agent and the brominated butyl rubber is as follows: uniformly mixing a coupling agent and brominated butyl rubber, and curing for 2-10 min at 100-150 ℃ under the action of a cross-linking agent tert-butylpyridine;
the coupling agent and the siloxane are uniformly mixed and cured as follows: and uniformly mixing the polydimethylsiloxane terminated by two hydrogen atoms in the main chain, the side chain and the end group with a coupling agent, and curing for 25-40 h at 70-90 ℃ under the action of a platinum catalyst.
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