CN108456291B - Shape memory type energy-absorbing protective moisture-permeable composite material and preparation method thereof - Google Patents

Shape memory type energy-absorbing protective moisture-permeable composite material and preparation method thereof Download PDF

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CN108456291B
CN108456291B CN201810066609.7A CN201810066609A CN108456291B CN 108456291 B CN108456291 B CN 108456291B CN 201810066609 A CN201810066609 A CN 201810066609A CN 108456291 B CN108456291 B CN 108456291B
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component
parts
composite material
shape memory
moisture
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CN108456291A (en
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刘世勇
盖静
戴江臻
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Chengdu Dekeli Polymer Materials Co ltd
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Chengdu Dekeli Polymer Materials Co ltd
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Abstract

The invention discloses a shape memory type energy-absorbing protective moisture-permeable composite material and a preparation method thereof, wherein the shape memory energy-absorbing protective moisture-permeable composite material is prepared by mixing an A component and a B component, and the weight ratio of the A component to the B component is 5-500: 100; the component A is polyurethane resin with moisture permeability and shape memory functions, and the component B is boron modified organic silicon resin with shear thickening functions. In the invention, the component A can provide support for the composite material, help the composite material to be molded and moisture permeable, and recover the original shape of the composite material by heating after the composite material is deformed, and the component B can absorb energy and harden when being subjected to violent impact, thereby providing excellent protective performance of the composite material.

Description

Shape memory type energy-absorbing protective moisture-permeable composite material and preparation method thereof
Technical Field
The invention belongs to the field of polymer composite materials, and relates to a shape memory type energy-absorbing protective moisture-permeable composite material and a preparation method thereof.
Background
The shear thickening material is characterized in that when the strain rate of external stress is greater than the critical shear rate, the viscosity or modulus of the material is rapidly increased, and the material is rapidly changed from a soft state to a hard solid state, so that the energy absorption and protection effects are achieved. Shear thickening materials mainly include two major classes, one is a particle colloid composed of nanoparticles and a liquid dispersion medium, and the other is a molecular colloid represented by boron-modified silicone resin. Patent publication No. CN 101871748A discloses a soft stab-resistant and bulletproof material, which uses particle colloid to provide energy-absorbing protection effect, but the particle colloid cannot be molded and generally needs to be sealed for use, and nanoparticles therein gradually agglomerate and settle, so that the protection effect is lost, while the molecular colloid does not need to be sealed, the performance is stable, and more attention is gradually paid, such as shear thickening materials disclosed in patent publication No. CN 104862975B, CN 102037088A, CN 102926211B and the like. Although the molecular colloid can be shaped, the shaping performance is poor, and the deformation can be caused by small stress, so the patents tend to be used for the impregnated fabric, which solves the problem of easy deformation of the material, but limits the application range of the material, and the boron modified organic silicon resin has poor moisture permeability, is unfavorable for the human body to wear after being impregnated with the fabric, and reduces the wearing comfort. In addition, although the shear thickening material and part of high-performance fabrics have better bulletproof effect, the stab-resistant effect is poorer, and the bulletproof material still has defects in the aspect of protective performance.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide a shape memory type energy-absorbing protection moisture-permeable composite material and a preparation method thereof.
The purpose of the invention is realized by the following technical scheme: a shape memory type energy-absorbing protective moisture-permeable composite material comprises a component A and a component B, wherein the weight ratio of the component A to the component B is 5-500: 100;
the component A is polyurethane resin with moisture permeability and shape memory functions;
the component B is boron modified organic silicon resin with a shear thickening function.
Preferably, the weight ratio of the A component to the B component is 30-200: 100.
A preparation method of a shape memory type energy-absorbing protective moisture-permeable composite material is provided, wherein the energy-absorbing protective moisture-permeable composite material is prepared by mixing a component A and a component B;
the weight ratio of the component A to the component B is 5-500:100, the component A is polyurethane resin with moisture permeability and shape memory functions, and the component B is boron modified organic silicon resin with shear thickening functions.
Preferably, the weight ratio of the A component to the B component is 30-200: 100.
Preferably, the preparation of the component A comprises the following steps, wherein the raw materials are calculated according to the parts by mass:
adding 100 parts of polyglycol with the molecular mass of 2000-6000 into a sealed dispersion kettle, sequentially adding 8-40 parts of diisocyanate, 0-0.1 part of catalyst, 0.5-5 parts of micromolecule chain extender and 10-15 parts of hydrophilic chain extender, reacting for 4-6 hours, controlling the temperature to be 70-90 ℃, then cooling to 30 ℃, adding 0-12 parts of neutralizing agent for neutralization, adding deionized water for stirring and emulsifying, and then adding 0.5-5 parts of rear chain extender to prepare aqueous polyurethane emulsion with the solid content of 20-30%;
and (3) spray drying the aqueous polyurethane emulsion to obtain the component A.
Preferably, the polyglycol comprises at least one of polycarbonate diol, polycaprolactone diol and poly adipic acid diol ester diol;
the diisocyanate comprises at least one of toluene diisocyanate, diphenylmethane diisocyanate, hydrogenated diphenylmethane diisocyanate, isophorone diisocyanate and hexamethylene diisocyanate;
the catalyst comprises at least one of an organobismuth catalyst and an organosilver catalyst;
the small molecular chain extender comprises at least one of 1, 4-butanediol, 1, 4-cyclohexanedimethanol, ethylene glycol and 1, 6-hexanediol;
the hydrophilic chain extender comprises at least one of 2, 2-dimethylolpropionic acid, 2- (2-aminoethyl) aminoethanesulfonic acid sodium salt and alpha, omega-polypropylene glycol-diamine-sulfopropyl sodium salt;
the neutralizing agent comprises at least one of triethylamine, dimethylethanolamine and 2-amino-2-methyl-1-propanol;
the rear chain extender comprises at least one of ethylenediamine, hexamethylenediamine, methylcyclohexanediamine and hydrazine hydrate.
Preferably, the sealed dispersion kettle is a sealed dispersion kettle with a temperature control and dispersion device.
Preferably, the preparation of the component B comprises the following steps, wherein the raw materials are calculated according to the parts by mass:
taking 100 parts of polysiloxane, adding 5-20 parts of boride into the polysiloxane, controlling the temperature at 120-300 ℃, and reacting for 2-6 hours to obtain the component B.
Preferably, the polysiloxane is a polydimethylsiloxane bearing at least two silanol functional groups.
Preferably, the boride is at least one of boric acid, boric oxide and pyroboric acid.
The invention has the beneficial effects that:
(1) the energy-absorbing protective moisture-permeable composite material with the shape memory function provided by the invention takes the shape memory polyurethane resin with hydrophilic groups and the boron modified organic silicon resin as main raw materials, and the introduction of the hydrophilic groups endows the composite material with certain moisture permeability, so that the use comfort of the composite material when the composite material is used as a human body wearing material is improved;
(2) the shape memory polyurethane material used in the invention has good molding and shaping properties, and the polyurethane material can be molded at will when the temperature is raised, and can be shaped after being cooled, so that the composite material has strong applicability and wide application range, can be used for civil purposes such as fracture external fixation materials, motion protection materials, automobile anti-collision materials and the like, and can also be matched with high-performance fibers and the like to be used for military purposes such as bulletproof clothes, bulletproof helmets and the like;
(3) the shape memory polyurethane material used in the invention has excellent strength and toughness at normal temperature, and can provide a certain stab-resistant effect when used as a protective material;
(4) the boron modified organic silicon resin material used in the invention has excellent energy absorption effect and is instantly hardened when being rapidly impacted, thereby providing good protection effect for the composite material;
(5) the shape memory polyurethane provided by the invention can recover the original shape after being heated again, so that the composite material is endowed with certain repairability when being damaged, and the composite material can be repeatedly utilized and can be remixed and molded after being completely damaged, thereby avoiding the waste of resources and the pollution and damage to the environment.
Detailed Description
The technical solutions of the present invention will be described clearly and completely with reference to the following embodiments, and it should be understood that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be obtained by a person skilled in the art without inventive effort based on the embodiments of the present invention, are within the scope of the present invention.
Example 1
The embodiment provides a shape memory type energy-absorbing protective moisture-permeable composite material, which is prepared by mixing a component A and a component B, wherein the component A is 50 parts of polyurethane resin, and the component B is 100 parts of boron modified organic silicon resin material.
The component A polyurethane resin is prepared by the following steps in sequence:
adding 100 parts of polycaprolactone diol with the relative molecular mass of 6000 into a sealed dispersion kettle with a heating, temperature-controlling and dispersing device, adding 8 parts of hexamethylene diisocyanate and 0.1 part of organic silver catalyst, reacting at 90 ℃ for 2 hours, then adding 0.5 part of 1, 4-cyclohexanedimethanol, reacting for 1 hour, adding 10 parts of alpha, omega-polypropylene glycol-diamine-sulfopropyl sodium salt serving as a hydrophilic chain extender, reacting for 1 hour, cooling to 30 ℃, adding deionized water, stirring at a high speed for emulsification, and then adding 0.5 part of ethylenediamine to prepare a waterborne polyurethane emulsion with the solid content of 20%;
and (3) spray drying the aqueous polyurethane emulsion to obtain the polyurethane resin with moisture permeability and shape memory functions.
The B component boron modified organic silicon resin is prepared by the following steps:
100 parts of dihydroxy polydimethylsiloxane (NEWTECH-1381, NyBorie chemical Co., Ltd.) is taken and added with 5 parts of boric acid to react for 2 hours at 300 ℃ to obtain the B component boron modified organic silicon resin.
The composite material provided by the embodiment has an excellent energy absorption and protection effect, has a certain shape memory function, and is endowed with good moisture permeability by introducing the sodium sulfonate group.
Example 2
The embodiment provides a shape memory type energy-absorbing protective moisture-permeable composite material, which is prepared by mixing a component A and a component B, wherein the component A is 5 parts of polyurethane resin, and the component B is 100 parts of boron modified organic silicon resin material.
The component A polyurethane resin is prepared by the following steps in sequence:
adding 100 parts of polycarbonate diol with the relative molecular mass of 2000 into a sealed dispersion kettle with a heating, temperature-controlling and dispersing device, adding 40 parts of toluene diisocyanate, reacting for 2 hours at 70 ℃, then adding 5 parts of 1, 6-hexanediol, reacting for 1 hour, adding 13 parts of hydrophilic chain extender 2, 2-dimethylolpropionic acid, reacting for 3 hours, cooling to 30 ℃, adding 10 parts of triethylamine, neutralizing, adding deionized water, stirring at high speed, emulsifying, and then adding 5 parts of methylcyclohexanediamine to prepare a waterborne polyurethane emulsion with the solid content of 30%;
and (3) spray drying the aqueous polyurethane emulsion to obtain the polyurethane resin with moisture permeability and shape memory functions.
The B component boron modified organic silicon resin is prepared by the following steps:
100 parts of dihydroxy polydimethylsiloxane (NEWTECH-1384, NyBorie chemical Co., Ltd.) is taken and added with 20 parts of pyroboric acid to react for 6 hours at 160 ℃ to obtain the B component boron modified organic silicon resin.
Example 3
The embodiment provides a shape memory type energy-absorbing protective moisture-permeable composite material, which is prepared by mixing a component A and a component B, wherein the component A is 200 parts of polyurethane resin, and the component B is 100 parts of boron modified organic silicon resin material.
The component A polyurethane resin is prepared by the following steps in sequence:
adding 100 parts of poly (glycol adipate) diol with the relative molecular mass of 3000 into a sealed dispersion kettle with a heating, temperature-controlling and dispersing device, adding 38 parts of isophorone diisocyanate, 0.07 part of organic bismuth catalyst to react for 2 hours at 85 ℃, then adding 1 part of 1, 4-butanediol to react for 0.5 hour, adding 15 parts of hydrophilic chain extender 2, 2-dimethylolpropionic acid to react for 3 hours, cooling to 30 ℃, adding 12 parts of triethylamine to neutralize, adding deionized water to stir at high speed for emulsification after neutralization is completed, and then adding 1 part of hexamethylenediamine to prepare aqueous polyurethane emulsion with the solid content of 30%;
and (3) spray drying the aqueous polyurethane emulsion to obtain the polyurethane resin with moisture permeability and shape memory functions.
The B component boron modified organic silicon resin is prepared by the following steps:
100 parts of dihydroxy polydimethylsiloxane (NEWTECH-1385, NyBorie chemical Co., Ltd.) is taken and added with 10 parts of boric acid to react for 5 hours at 140 ℃ to obtain the B component boron modified organic silicon resin.
Example 4
The embodiment provides a shape memory type energy-absorbing protective moisture-permeable composite material, which is prepared by mixing a component A and a component B, wherein the component A is 500 parts of polyurethane resin, and the component B is 100 parts of boron modified organic silicon resin material.
The component A polyurethane resin is prepared by the following steps in sequence:
adding 100 parts of polycaprolactone diol with the relative molecular mass of 4000 into a sealed dispersion kettle with a heating, temperature-controlling and dispersing device, adding 35 parts of diphenylmethane diisocyanate, 0.03 part of organic bismuth catalyst, reacting at 60 ℃ for 2 hours, then adding 0.6 part of 1, 4-butanediol, reacting for 0.5 hour, adding 11 parts of hydrophilic chain extender 2, 2-dimethylolpropionic acid, reacting for 3 hours, cooling to 30 ℃, adding 9 parts of triethylamine for neutralization, adding deionized water after neutralization, stirring at high speed for emulsification, and then adding 1.2 parts of hydrazine hydrate (80% aqueous solution) to prepare aqueous polyurethane emulsion with the solid content of 25%;
and (3) spray drying the aqueous polyurethane emulsion to obtain the polyurethane resin with moisture permeability and shape memory functions.
The B component boron modified organic silicon resin is prepared by the following steps:
100 parts of dihydroxy polydimethylsiloxane (NEWTECH-1385, Nyglass chemical Co., Ltd.) is taken and added with 8 parts of boric acid to react for 4 hours at 120 ℃ to obtain the B component boron modified organic silicon resin.
The foregoing is illustrative of the preferred embodiments of this invention, and it is to be understood that the invention is not limited to the precise form disclosed herein and that various other combinations, modifications, and environments may be resorted to, falling within the scope of the concept as disclosed herein, either as described above or as apparent to those skilled in the relevant art. And that modifications and variations may be effected by those skilled in the art without departing from the spirit and scope of the invention as defined by the appended claims.

Claims (6)

1. A shape memory type energy-absorbing protective moisture-permeable composite material is characterized by comprising a component A and a component B, wherein the weight ratio of the component A to the component B is 30-200: 100;
the component A is polyurethane resin with moisture permeability and shape memory functions;
the component B is boron modified organic silicon resin with a shear thickening function;
the preparation of the component A comprises the following steps, wherein the raw materials are calculated according to parts by mass:
adding 100 parts of polyglycol with the relative molecular mass of 2000-6000 into a sealed dispersion kettle, sequentially adding 8-40 parts of diisocyanate, 0-0.1 part of catalyst, 0.5-5 parts of micromolecule chain extender and 10-15 parts of hydrophilic chain extender, reacting for 4-6 hours, controlling the temperature to be 70-90 ℃, then cooling to 30 ℃, adding 0-12 parts of neutralizing agent for neutralization, adding deionized water for stirring and emulsifying, and then adding 0.5-5 parts of rear chain extender to prepare aqueous polyurethane emulsion with the solid content of 20-30%;
spray drying the aqueous polyurethane emulsion to obtain a component A;
the polyglycol comprises at least one of polycarbonate diol, polycaprolactone diol and poly adipic acid diol ester diol;
the preparation of the component B comprises the following steps, wherein the raw materials are calculated according to parts by mass:
taking 100 parts of polysiloxane, adding 5-20 parts of boride into the polysiloxane, controlling the temperature at 120-300 ℃, and reacting for 2-6 hours to obtain the component B.
2. A preparation method of a shape memory type energy-absorbing protective moisture-permeable composite material is characterized in that the energy-absorbing protective moisture-permeable composite material is prepared by mixing a component A and a component B;
the weight ratio of the component A to the component B is 30-200: 100, the component A is polyurethane resin with moisture permeability and shape memory functions, and the component B is boron modified organic silicon resin with shear thickening function;
the preparation of the component A comprises the following steps, wherein the raw materials are calculated according to parts by mass:
adding 100 parts of polyglycol with the relative molecular mass of 2000-6000 into a sealed dispersion kettle, sequentially adding 8-40 parts of diisocyanate, 0-0.1 part of catalyst, 0.5-5 parts of micromolecule chain extender and 10-15 parts of hydrophilic chain extender, reacting for 4-6 hours, controlling the temperature to be 70-90 ℃, then cooling to 30 ℃, adding 0-12 parts of neutralizing agent for neutralization, adding deionized water for stirring and emulsifying, and then adding 0.5-5 parts of rear chain extender to prepare aqueous polyurethane emulsion with the solid content of 20-30%;
spray drying the aqueous polyurethane emulsion to obtain a component A;
the polyglycol comprises at least one of polycarbonate diol, polycaprolactone diol and poly adipic acid diol ester diol;
the preparation of the component B comprises the following steps, wherein the raw materials are calculated according to parts by mass:
taking 100 parts of polysiloxane, adding 5-20 parts of boride into the polysiloxane, controlling the temperature at 120-300 ℃, and reacting for 2-6 hours to obtain the component B.
3. The method for preparing the shape memory type energy-absorbing, protective and moisture permeable composite material according to claim 2, wherein the diisocyanate comprises at least one of toluene diisocyanate, diphenylmethane diisocyanate, hydrogenated diphenylmethane diisocyanate, isophorone diisocyanate, and hexamethylene diisocyanate;
the catalyst comprises at least one of an organobismuth catalyst and an organosilver catalyst;
the small molecular chain extender comprises at least one of 1, 4-butanediol, 1, 4-cyclohexanedimethanol, ethylene glycol and 1, 6-hexanediol;
the hydrophilic chain extender comprises at least one of 2, 2-dimethylolpropionic acid, 2- (2-aminoethyl) aminoethanesulfonic acid sodium salt and alpha, omega-polypropylene glycol-diamine-sulfopropyl sodium salt;
the neutralizing agent comprises at least one of triethylamine, dimethylethanolamine and 2-amino-2-methyl-1-propanol;
the rear chain extender comprises at least one of ethylenediamine, hexamethylenediamine, methylcyclohexanediamine and hydrazine hydrate.
4. The method for preparing the shape memory type energy-absorbing protective moisture-permeable composite material according to claim 2, wherein the sealed dispersion kettle is a sealed dispersion kettle with a temperature control and dispersion device.
5. The method for preparing a shape memory type energy-absorbing protective moisture-permeable composite material according to claim 2, wherein the polysiloxane is polydimethylsiloxane with at least two silanol functional groups.
6. The method for preparing the shape memory type energy-absorbing protective moisture-permeable composite material according to claim 2, wherein the boride is at least one of boric acid, boron oxide and pyroboric acid.
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