CN112341822A - Polymer film material with hydrogen absorption function and preparation method thereof - Google Patents

Polymer film material with hydrogen absorption function and preparation method thereof Download PDF

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CN112341822A
CN112341822A CN202011242689.0A CN202011242689A CN112341822A CN 112341822 A CN112341822 A CN 112341822A CN 202011242689 A CN202011242689 A CN 202011242689A CN 112341822 A CN112341822 A CN 112341822A
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hydrogen
water
film material
absorbing
polymer film
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邢涛
李保强
徐勇
吴菊英
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General Engineering Research Institute China Academy of Engineering Physics
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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
    • C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
    • C08J5/18—Manufacture of films or sheets
    • 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
    • C08J2309/00—Characterised by the use of homopolymers or copolymers of conjugated diene hydrocarbons
    • 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
    • C08J2353/00—Characterised by the use of block copolymers containing at least one sequence of a polymer obtained by reactions only involving carbon-to-carbon unsaturated bonds; Derivatives of such polymers
    • C08J2353/02—Characterised by the use of block copolymers containing at least one sequence of a polymer obtained by reactions only involving carbon-to-carbon unsaturated bonds; Derivatives of such polymers of vinyl aromatic monomers and conjugated dienes
    • 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
    • C08J2383/00—Characterised by the use of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen, or carbon only; Derivatives of such polymers
    • C08J2383/04—Polysiloxanes
    • C08J2383/07—Polysiloxanes containing silicon bound to unsaturated aliphatic groups
    • 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
    • C08J2483/00—Characterised by the use of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen, or carbon only; Derivatives of such polymers
    • C08J2483/04—Polysiloxanes
    • C08J2483/05—Polysiloxanes containing silicon bound to hydrogen
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/16—Halogen-containing compounds
    • C08K2003/162—Calcium, strontium or barium halides, e.g. calcium, strontium or barium chloride
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/38—Boron-containing compounds
    • C08K2003/387—Borates
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K2201/00—Specific properties of additives
    • C08K2201/002—Physical properties
    • C08K2201/005—Additives being defined by their particle size in general
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/38—Boron-containing compounds
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K7/00—Use of ingredients characterised by shape
    • C08K7/22—Expanded, porous or hollow particles
    • C08K7/24—Expanded, porous or hollow particles inorganic

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Manufacturing & Machinery (AREA)
  • Materials Engineering (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • Solid-Sorbent Or Filter-Aiding Compositions (AREA)
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Abstract

The invention discloses a polymer film material with a hydrogen absorption function, which comprises the following raw materials: a water absorbent, a noble metal catalyst, and a polymer matrix; the preparation method comprises the steps of uniformly mixing the water absorbent, the polymer matrix and the noble metal catalyst, and preparing the thermoplastic and thermosetting hydrogen-absorbing materials with different structures and application forms by a physical and chemical molding method. The invention avoids complex chemical preparation, has simple preparation process and high hydrogen absorption performance, and can be directly processed and cut due to the film.

Description

Polymer film material with hydrogen absorption function and preparation method thereof
Technical Field
The invention relates to the field of preparation of functional polymers, in particular to a preparation method of a polymer film material with a hydrogen absorption function.
Background
The polymer hydrogen absorption material has the characteristics of polymer processing and cutting and the characteristics of hydrogen absorption of the hydrogen absorption material, so that the hydrogen elimination in the nuclear industry and the nuclear material field aiming at complex application scenes has important application value. The traditional organic hydrogen absorbing material based on p-Diphenylethynylbenzene (DEB) is widely applied in the field of nuclear industry, but due to the characteristics of p-diphenylethynylbenzene powder, packaging is needed when in use, and the extra mass and volume problems of the packaging material cause great limitation when aiming at complex and narrow application environments. Various hydrogen-absorbing materials based on DEB mixed systems and unsaturated polymers with different chemical structures are reported in documents and patents, but the materials have the defects of complex preparation process, high cost, poor hydrogen-absorbing performance and the like.
Disclosure of Invention
In order to solve the problems, the invention provides a novel polymer film material with a hydrogen absorption function and a preparation method thereof.
In order to achieve the purpose, the invention adopts the following technical scheme:
the polymer material with the hydrogen absorption function comprises the following raw materials: a water absorbent, a noble metal catalyst, and a polymer matrix; the weight ratio of the water absorbent particles to the polymer matrix is in the range of 2.3-0.5%, the amount of the noble metal catalyst is 0.05 wt% -1wt%, and the film thickness is less than 1.5 mm;
wherein the water absorbent absorbs water molecules by physical adsorption and chemical reaction, and specifically can be CaCl2、MgSO4、K2CO3、Na2SO4Water-absorbing agents that can absorb water by generating bound water; or porous materials such as molecular sieves, attapulgite, porous organic framework materials, porous inorganic framework materials and the like which are subjected to moisture removal by a porous adsorption method; or organic or inorganic materials which undergo moisture absorption by means of chemical reactions, e.g. B2O3Organic boric anhydride, organic boric acid ester and P2O5And other types of solid organic anhydrides;
the polymer matrix is thermoplastic and thermosetting elastomer material, the thermoplastic elastomer material can be SBS, polyurethane and other thermoplastic elastomer materials with block structures, and the thermosetting rubber material can be silicone rubber, ethylene propylene diene monomer, nitrile rubber, natural rubber and other rubber materials which can be formed by hot vulcanization;
the noble metal catalyst is Pt, Pd or Au and a load thereof.
Most of application objects of the hydrogen absorption material are hydrogen in an oxygen environment, the polymer material is applied to a hydrogen and oxygen coexistence environment, the noble metal catalyst catalyzes hydrogen and oxygen composite reaction to generate water in the oxygen and hydrogen coexistence environment, and the water is further absorbed by the water absorbent in the polymer material in a physical adsorption or chemical reaction mode, so that the hydrogen absorption effect is achieved.
The invention also provides a preparation method of the polymer film material with the hydrogen absorption function, which is to mix the water absorbent, the polymer matrix and the noble metal catalyst uniformly and prepare thermoplastic and thermosetting hydrogen absorption materials with different structures and application forms by a physical or chemical forming method;
during mixing, the adopted method is open mixing, banburying, solution or melt compounding;
the molding method can be hot pressing, coating, extrusion, blow molding and other molding methods.
Compared with the prior art, the invention has the beneficial effects that:
the polymer film material with the hydrogen absorption function avoids complex chemical preparation, has simple preparation process and high hydrogen absorption performance, can be directly processed and cut due to the film, overcomes the defects of single application form of DEB powder hydrogen absorption agent and complex preparation process of unsaturated polymer hydrogen absorption material, and makes up the defects of the traditional material.
The invention is suitable for the environment with coexisting oxygen and hydrogen, and the materials have wide application prospect in the related fields of daily life, national defense and military industry and the like due to the combustion and explosion hidden troubles when the hydrogen and the oxygen coexist.
Detailed Description
The present invention will be further described with reference to the following examples, which are intended to illustrate only some, but not all, of the embodiments of the present invention. All other embodiments that can be obtained by a person skilled in the art based on the embodiments of the present invention without any creative effort belong to the protection scope of the present invention.
Example 1
Weighing 20g of polydimethylsiloxane (3500cst) containing 5% of vinyl, putting the polydimethylsiloxane into a 250mL plastic beaker, then adding 0.2g of hydrogen-containing silicone oil, 8g of anhydrous calcium chloride powder (200 meshes) and 2.0g of Pd @ C catalyst, stirring uniformly, adding 0.05g of 2.0 wt% of card type catalyst, quickly stirring uniformly, pouring the mixture into a stainless steel disc, and curing at 60 ℃ for 15h to obtain the white flexible film material.
The hydrogen concentration of the resulting flexible film (0.2g,220 μm) was changed by placing it in a mixed gas (250mL of a 4.8% hydrogen, 10% oxygen, 85.2% nitrogen mixture) over time as shown in Table 1:
TABLE 1
Time of day 15min 30min 100min 240min
Hydrogen gas concentration (%) 3.7 2.5 0.1 0
The hydrogen concentration of the resulting film (0.2g,220 μm) after exposure to a mixed gas (250mL of a 1% hydrogen, 5% oxygen, 94% nitrogen mixture) over time was varied as shown in Table 2:
TABLE 2
Time per hour 2 6 10 16 24
Hydrogen gas concentration (%) 0.83 0.65 0.23 0.12 0.02
Example 2
20g of polybutadiene (Mn 25000) is weighed into a 250mL plastic beaker, then 2.5g of hydrogen-containing silicone oil, 8g of anhydrous molecular sieve powder (200 meshes) and 2.0g of Pd @ C catalyst are added, after uniform stirring, 0.05g of 2 wt% of blocked catalyst is added, after rapid uniform stirring, the mixture is poured into a stainless steel plate, and after curing is carried out for 15h at 80 ℃, a white flexible film material is obtained.
The hydrogen concentration of the resulting white flexible film (0.2g,402 μm) was varied after exposure to a mixed gas (250mL of a 4.8% hydrogen, 10% oxygen, 85.2% nitrogen mixture) over time as shown in Table 3:
TABLE 3
Time of day 15min 30min 100min 240min
Hydrogen gas concentration (%) 4.2 3.0 0.8 0
The hydrogen concentration of the resulting flexible film (0.2g,402 μm) after exposure to a mixed gas (250mL of a 1% hydrogen, 5% oxygen, 94% nitrogen mixture) over time was varied as shown in Table 4:
TABLE 4
Time per hour 2 6 10 16 24
Hydrogen gas concentration (%) 0.91 0.74 0.33 0.14 0.03
Example 3
Weighing 20g of polybutadiene-polystyrene-polybutadiene triblock copolymer (the styrene content is 25 wt%), adding 30mL of tetrahydrofuran for dissolving, adding 8g of anhydrous molecular sieve powder (200 meshes) and 3.0g of Pd @ C catalyst after the polymer is completely dissolved, uniformly stirring, pouring the mixture into a stainless steel disc, and curing at 80 ℃ for 15 hours to obtain a white flexible material. And (3) continuously drying at 80 ℃ after the solvent is volatilized at room temperature to obtain the flexible white film material.
The resulting white flexible film (0.2g,580 μm) was placed in a mixed gas (250mL of a 4.8% hydrogen, 10% oxygen, 85.2% nitrogen mixture) for various times, and the hydrogen concentration of the system was changed as shown in Table 5:
TABLE 5
Time of day 15min 30min 100min 240min
Hydrogen gas concentration (%) 6.9 4.8 2.1 0.7
The hydrogen concentration of the resulting flexible film (0.2g,580 μm) after exposure to a mixed gas (250mL of a 1% hydrogen, 5% oxygen, 94% nitrogen mixture) over time was varied as shown in Table 6:
TABLE 6
Time per hour 2 6 10 16 24
Hydrogen gas concentration (%) 0.88 0.79 0.45 0.23 0.08
Example 4
20g of polybutadiene-polystyrene-polybutadiene triblock copolymer (styrene content 25 wt%) is weighed, mixed with 8.0g of molecular sieve powder and 1.0g of porous palladium black on an open mill at 120 ℃, the mixture is uniformly mixed, and then a sample is transferred to a stainless steel grinding tool and is subjected to die pressing (5MPa) at 100 ℃ for 10min to obtain a composite film with the thickness of 1 mm.
The resulting film (0.2g,260 μm) was placed in a mixed gas (250mL of a 4.8% hydrogen, 10% oxygen, 85.2% nitrogen mixture) for various times, and the change in hydrogen concentration of the system was as shown in Table 7:
TABLE 7
Time of day 15min 30min 100min 240min
Hydrogen gas concentration (%) 4.1 2.9 0.12 0
The hydrogen concentration of the resulting flexible film (0.2g,260 μm) after exposure to a mixed gas (250mL of a 1% hydrogen, 5% oxygen, 94% nitrogen mixture) over time was varied as shown in Table 8:
TABLE 8
Time per hour 2 6 10 16 24
Hydrogen gas concentration (%) 0.84 0.69 0.36 0.11 0
Example 5
20g of 5% vinyl containing polydimethylsiloxane (3500cst) was weighed into a 250mL plastic beaker, after which 0.2g of hydrogen silicone oil, 8g B, was added2O3Powder (200 meshes), 2.0g of Pd @ C catalyst, 0.05g of 2 wt% of catalyst card is added after uniform stirring, the mixture is poured into a stainless steel plate after rapid uniform stirring, and the mixture is cured for 15 hours at 60 ℃ to obtain the flexible film material.
The hydrogen concentration of the resulting flexible film (0.2g,350 μm) was changed by placing it in a mixed gas (250mL of a 4.8% hydrogen, 10% oxygen, 85.2% nitrogen mixture) over time as shown in Table 9:
TABLE 9
Time of day 15min 30min 100min 240min
Hydrogen gas concentration (%) 3.2 1.9 0.2 0
The hydrogen concentration of the resulting flexible film (0.2g,350 μm) was changed after various times in a mixed gas (250mL of a mixed gas of 1% hydrogen, 5% oxygen and 94% nitrogen) as shown in Table 10:
watch 10
Time per hour 2 6 10 16 24
Hydrogen gas concentration (%) 0.72 0.64 0.40 0.09 0
Example 6
Weighing 20g of polydimethylsiloxane (3500cst) containing 5% of vinyl, putting the polydimethylsiloxane into a 250mL plastic beaker, then adding 0.2g of hydrogen-containing silicone oil, 8g of boric acid powder (200 meshes) and 2.0g of Pd @ C catalyst, stirring uniformly, adding 0.05g of 2 wt% of card type catalyst, quickly stirring uniformly, pouring the mixture into a stainless steel disc, and curing at 60 ℃ for 15h to obtain the flexible film. And heating the film for 3h at 200 ℃ in a nitrogen atmosphere to obtain the porous flexible film material.
The resulting porous flexible film (0.2g,610 μm) was placed in a mixed gas (250mL of a 4.8% hydrogen, 10% oxygen, 85.2% nitrogen mixture) for various times, and the hydrogen concentration of the system was varied as shown in Table 11:
TABLE 11
Time of day 15min 30min 100min 240min
Hydrogen gas concentration (%) 4.3 3.1 0.4 0
The resulting porous flexible film (0.2g,610 μm) was placed in a mixed gas (250mL of a 1% hydrogen, 5% oxygen, 94% nitrogen mixture) and the change in hydrogen concentration of the system over time was as shown in Table 12:
TABLE 12
Time per hour 2 6 10 16 24
Hydrogen gas concentration (%) 0.79 0.61 0.33 0.07 0

Claims (10)

1. The polymer film material with the hydrogen absorption function is characterized by comprising the following raw materials: a water absorbent, a noble metal catalyst, and a polymer matrix.
2. The polymeric film material having a hydrogen absorbing function as claimed in claim 1, wherein the weight ratio of the water absorbent particles to the polymer matrix is in the range of 2.3 to 0.5%, and the noble metal catalyst is used in an amount of 0.05 to 1% by weight.
3. A polymer film material having a hydrogen absorbing function as claimed in claim 1, wherein the water absorbing agent is a water absorbing agent for absorbing water by generating bound water, or a water absorbing agent for a porous material for absorbing water by a porous adsorption method, or a water absorbing agent for an organic inorganic material for absorbing water by a chemical reaction method.
4. The polymer film material having a hydrogen absorbing function as claimed in claim 3, wherein the water absorbent for absorbing water by generating bound water comprises CaCl2、MgSO4、K2CO3And Na2SO4(ii) a Water absorption by porous absorption methodThe water absorbent of the collected porous material comprises a molecular sieve, attapulgite, a porous organic framework material and a porous inorganic framework material; a water-absorbing agent for organic and inorganic materials which absorbs water by means of a chemical reaction, comprising B2O3Organic boric anhydride, organic boric acid ester and P2O5。
5. The polymer thin film material having a hydrogen absorbing function according to claim 1, wherein the noble metal catalyst is Pt, Pd, or Au and a support thereof.
6. The polymer film material with hydrogen absorption function as claimed in claim 1, wherein the polymer matrix is a thermoplastic elastomer material or a thermosetting elastomer material, the thermoplastic elastomer material is a thermoplastic elastomer material with a block structure, and the thermosetting rubber material is a rubber material which can be formed by thermal vulcanization.
7. The polymer film material with hydrogen absorption function as claimed in claim 6, wherein the thermoplastic elastomer material is SBS or polyurethane, and the thermosetting rubber material is silicone rubber, ethylene propylene diene monomer, nitrile rubber or natural rubber.
8. The preparation method of the polymer film material with the hydrogen absorption function is characterized by uniformly mixing a water absorbent, a polymer matrix and a noble metal catalyst, and preparing thermoplastic and thermosetting hydrogen absorption materials with different structures and application forms by a physical and chemical forming method.
9. The method for preparing a polymer film material having a hydrogen absorbing function according to claim 8, wherein: the mixing method is open milling, banburying, solution or melt compounding.
10. The method for preparing a polymer film material having a hydrogen absorbing function according to claim 8, wherein: the molding method is a hot pressing, coating, extruding or blow molding method.
CN202011242689.0A 2020-11-09 2020-11-09 Polymer film material with hydrogen absorption function and preparation method thereof Pending CN112341822A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113069877A (en) * 2021-04-13 2021-07-06 南京华东电子真空材料有限公司 High-air-suction-rate environment-friendly hydrogen and water absorbent
CN115232429A (en) * 2022-07-06 2022-10-25 中国工程物理研究院材料研究所 Self-supporting flexible dehydrogenation material, film, preparation method and application thereof

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO1999063298A1 (en) * 1998-06-03 1999-12-09 Marconi Aerospace Defense Systems, Inc. Hydrogen absorbing rubber
CN108636449A (en) * 2018-04-26 2018-10-12 西南科技大学 The preparation method of the compound hydrogen-absorbing material of the graphene-supported nano Pd catalyst of alkynyl
CN109384976A (en) * 2018-11-23 2019-02-26 西南科技大学 A kind of flexibility disappears the preparation method of hydrogen thin-film material
CN110951262A (en) * 2019-11-25 2020-04-03 中国工程物理研究院总体工程研究所 Preparation method of novel polysiloxane type hydrogen-absorbing polymer film material

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO1999063298A1 (en) * 1998-06-03 1999-12-09 Marconi Aerospace Defense Systems, Inc. Hydrogen absorbing rubber
CN108636449A (en) * 2018-04-26 2018-10-12 西南科技大学 The preparation method of the compound hydrogen-absorbing material of the graphene-supported nano Pd catalyst of alkynyl
CN109384976A (en) * 2018-11-23 2019-02-26 西南科技大学 A kind of flexibility disappears the preparation method of hydrogen thin-film material
CN110951262A (en) * 2019-11-25 2020-04-03 中国工程物理研究院总体工程研究所 Preparation method of novel polysiloxane type hydrogen-absorbing polymer film material

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113069877A (en) * 2021-04-13 2021-07-06 南京华东电子真空材料有限公司 High-air-suction-rate environment-friendly hydrogen and water absorbent
CN115232429A (en) * 2022-07-06 2022-10-25 中国工程物理研究院材料研究所 Self-supporting flexible dehydrogenation material, film, preparation method and application thereof
CN115232429B (en) * 2022-07-06 2023-10-27 中国工程物理研究院材料研究所 Self-supporting flexible hydrogen eliminating material, thin film, and preparation method and application thereof

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