CN108034199A - High filled biodegradable radiation cross-linked foam material and preparation method thereof - Google Patents

High filled biodegradable radiation cross-linked foam material and preparation method thereof Download PDF

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Publication number
CN108034199A
CN108034199A CN201711196162.7A CN201711196162A CN108034199A CN 108034199 A CN108034199 A CN 108034199A CN 201711196162 A CN201711196162 A CN 201711196162A CN 108034199 A CN108034199 A CN 108034199A
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weight
parts
high filled
linked foam
filled biodegradable
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于彦存
韩常玉
董丽松
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Changchun Institute of Applied Chemistry of CAS
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Changchun Institute of Applied Chemistry of CAS
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    • C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
    • C08J9/04—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent
    • C08J9/06—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent by a chemical blowing agent
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    • C08J9/10—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent by a chemical blowing agent developing nitrogen, the blowing agent being a compound containing a nitrogen-to-nitrogen bond
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    • C08J9/104—Hydrazines; Hydrazides; Semicarbazides; Semicarbazones; Hydrazones; Derivatives thereof
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    • C08J2367/00—Characterised by the use of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Derivatives of such polymers
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Abstract

High filled biodegradable radiation cross-linked foam material and preparation method thereof, belongs to polymer and its processing technique field.Solve and how a kind of excellent physical properties are provided, water-fast, durability is good, expansion ratio is higher, the problem of can regulating and controlling the foamed material of mechanical property in a wide range.The foamed material of the present invention includes 60 100 parts by weight polyadipate mutual-phenenyl two acid bromide two alcohol esters, 0 40 parts by weight of filler, 0.5 15 parts by weight of blowing agent, 0.01 5 parts by weight blowing promotors and 0.1 10 parts by weight of crosslinking agent.Wherein, crosslinking agent is the one or more in vinyl trimethylsilane, vinyltriethoxysilane, vinyl three (β methoxy ethoxies) silane.The foamed material possesses the advantages of excellent physical properties, water-tolerant, durability are good, expansion ratio is higher, and is foamed by dosing corresponding filler, can regulate and control the mechanical property of expanded material in a wide range.

Description

High filled biodegradable radiation cross-linked foam material and preparation method thereof
Technical field
The invention belongs to polymer and its processing technique field, and in particular to a kind of high filled biodegradable crosslinking with radiation Foamed material and preparation method thereof.
Background technology
Foam of polymers is a kind of special heterogeneous material, it is to be collectively formed by solid polymer with gas phase, be with Polymeric material of the plastics for solvent and containing a large amount of bubbles, therefore the composite plastic using gas as filler can also be regarded as Material.Compared with pure plastics, it has many excellent performances, it is such as light, specific strength is high, absorbable shock loading, it is heat-insulated and every Sound performance is good etc..Thus it is widely applied in the field such as industry, agricultural, building, communications and transportation.
Foamed material is mainly with foam of polymers such as polyethylene (PE) foam, polypropylene (PP) foam, polystyrene at present (PS) based on foam, polyvinyl chloride (PVC) foam and polyurethane (PU), this kind of foamed material volume is big, recycling is difficult, in nature It is non-degradable under environment, serious environmental problem is brought, is exacerbated " white pollution ".Therefore, light of environmental concerns, open energetically Degradable foamed material is sent out and promotes to be closed be subject to worldwide academia and industrial quarters instead of conventional polymer foamed material Note.Compared with universal foam material, degradable foamed material mechanical performance currently on the market is poor, and water resistance is poor, product Durability is poor.
Polyadipate-mutual-phenenyl two acid bromide two alcohol ester, is made by adipic acid and terephthalic acid (TPA) and butanediol through polycondensation, it The materials such as carbon dioxide and water, environmental sound can be finally degraded under the action of bacterium or enzyme.And due to synthesis Raw materials used to be easy to get relatively, synthesis technique is also easy relative to microbe fermentation method etc., so having in cost obvious excellent Gesture.It is hopeful to substitute general polyethylene or polypropylene and enter general-purpose plastics field, it is dirty caused by environment alleviates conventional plastic Dye.BASF Aktiengesellschaft has been realized in the industrialization production of polyadipate-mutual-phenenyl two acid bromide two alcohol ester, trade nameBe BASF AG production a kind of biodegradable plastic truly because it Only with can rot in several weeks in soil or in fertilizer, and it will not leave behind any residue.Therefore, it is prepared into sending out After foam material, the pollution problem that traditional expanded material is brought can be effectively solved.BASF AG is in the market in 1998 This product is released, since it possesses very excellent quality so that it become in world markets occupy leading position Artificial creature's degradable material.At home, Ye You many enterprises realize polyadipate-mutual-phenenyl two acid bromide two alcohol ester's industrialization Production.
Although polyadipate-mutual-phenenyl two acid bromide two alcohol ester possesses excellent degradability, widely should obtain With, but as people are for the raising of the pursuit of product quality, the performance requirement of foamed material has not been contented just to merely Its feature of environmental protection, people, which are more desirable to it, can have both excellent comprehensive performance, such as physical property, water resistance, durability, and be Meet different application demand, to the controllability of material property also there is certain vision.
The content of the invention
It is an object of the invention to solve how to provide a kind of excellent physical properties, water-tolerant, durable in the prior art Property is good, expansion ratio is higher, can regulate and control in a wide range expanded material mechanical property high filled biodegradable Radiation cross-linked foam material and preparation method thereof.
It is as follows that the present invention solves the technical solution that above-mentioned technical problem is taken：
High filled biodegradable radiation cross-linked foam material and preparation method thereof, including：
The crosslinking agent is vinyl trimethylsilane, vinyltriethoxysilane, (the 'beta '-methoxy ethoxy of vinyl three Base) one or more mixing in any proportion in silane；
The filler is one kind in starch, cellulose, lignin, silica, talcum powder, montmorillonite, calcium carbonate.
Preferably, composition and parts by weight are：
Preferably, the foaming agent for azodicarbonamide, Barium azodicarboxylate, diisopropyl azodiformate, N, One or more mixing in any proportion in N- dinitrosopentamethlyene tetramines, 4,4 '-oxobenzenesulfonyl hydrazide.
Preferably, the blowing promotor is that the one or more in zinc oxide, zinc stearate, calcium stearate press any ratio The mixing of example.
Above-mentioned high filled biodegradable radiation cross-linked foam material and preparation method thereof, step is as follows：
Step 1: weighing each raw material by composition and parts by weight, add in extruder and carry out mixing granulator, mixing granulator temperature For 80-170 DEG C, the obtained mixing granulator material extrusion sheet on sheet extruder, sheet thickness 0.5-3.0mm, extrusion temperature Spend for 100-170 DEG C；
Step 2: at room temperature in air, crosslinking with radiation is carried out to blend sheet, irradiation dose 0.5-9KGy, obtains Precrosslink material；
Step 3: by precrosslink material, 2-48h is further crosslinked in 50-80 DEG C of hot bath, obtains crosslinking material；
Step 4: crosslinking material is foamed, temperature is 190-250 DEG C, time 1-20min, and obtaining high filling can Biodegradable radiation cross-linked foam material.
Preferably, mixing granulator is completed in double screw extruder, and the equipment of extrusion sheet is extruded for single screw rod sheet material Machine.
Preferably, ionized radiation source is60Co sources or electron accelerator.
Preferably, crosslinking material foams in vertical or horizontal foaming furnace.
Compared with prior art, beneficial effects of the present invention are：
High filled biodegradable radiation cross-linked foam material and preparation method thereof of the present invention possess excellent physical properties, The advantages of water-tolerant, durability are good, expansion ratio is higher, and foamed by dosing corresponding filler, can be very The mechanical property of regulation and control expanded material, such as compressive strength, compression modulus etc., allow it to meet more to apply in wide scope Field, after testing, the apparent density of foamed material of the invention is 50-500Kg/m3, tensile strength 1.10-2.64MPa, Elongation at break is 370-560%, compressive strength 0.45-5.56MPa.
The preparation method of the high filled biodegradable radiation cross-linked foam material of the present invention and preparation method thereof, which uses, to be contained Have the silane of vinyl as crosslinking agent, realize under low radiation dose to polyadipate-mutual-phenenyl two acid bromide two alcohol ester and its Blend carries out cross-linking radiation, reduces RADIATION PROCESSING cost, meanwhile, it can accelerate this after molecule interchain introduces silica chemical bond The biodegradation rate of a little biodegradable foamed materials；
The preparation method of the high filled biodegradable radiation cross-linked foam material of the present invention uses cross-linking radiation and hydro-thermal Crosslinking combines, it is ensured that material meets the needs of foaming, and obtained excellent physical properties, water-tolerant, durability are good, expansion ratio Higher foamed plastics, and further reduce dose of radiation；
The preparation method of the high filled biodegradable radiation cross-linked foam material of the present invention uses cross-linking radiation at room temperature, It is easy to operate.
Embodiment
In order to further appreciate that the present invention, the preferred embodiments of the invention are retouched with reference to embodiment State, but it is to be understood that these descriptions are intended merely to further illustrate the spy of the present invention and are weighed just with advantage rather than to the present invention The limitation that profit requires.
The high filled biodegradable radiation cross-linked foam material of the present invention, by 60-100 parts by weight polyadipate-to benzene Dioctyl phthalate butanediol ester, 0-40 parts by weight of filler, 0.5-15 parts by weight of blowing agent, 0.01-5 parts by weight blowing promotor and 0.1- 10 parts by weight of crosslinking agent form.
Wherein, polyadipate-mutual-phenenyl two acid bromide two alcohol ester's parts by weight are preferably 70-90, more preferably 75-85.Filling Thing is one kind in starch, cellulose, lignin, silica, talcum powder, montmorillonite, calcium carbonate, and parts by weight are preferably 10- 35, more preferably 15-25.Foaming agent is azodicarbonamide, Barium azodicarboxylate, diisopropyl azodiformate, N, N- bis- Five methine tetramine of nitroso, 4, one or more mixing in any proportion in 4 '-oxobenzenesulfonyl hydrazide, parts by weight are excellent Elect 5-10 as, more preferably 6-9, especially preferably 8.Blowing promotor for zinc oxide, zinc stearate, one kind in calcium stearate or A variety of mixing in any proportion, parts by weight are preferably 3-5, more preferably 3.5-4.Crosslinking agent for vinyl trimethylsilane, One or more in any proportion mixed in vinyltriethoxysilane, vinyl three ('beta '-methoxy ethyoxyl) silane Close, parts by weight are preferably 4-9, more preferably 5.5-8, especially preferably 6-7.
The preparation method of the high filled biodegradable radiation cross-linked foam material of the present invention, step are as follows：
Step 1: weighing each raw material by composition and parts by weight, add in double screw extruder and carry out mixing granulator, mixing is made Grain temperature is 80-170 DEG C, obtained mixing granulator material extrusion sheet on single screw rod sheet extruder, sheet thickness 0.5- 3.0mm, preferably 1mm, extrusion temperature are 100-170 DEG C；
Step 2: at room temperature in air, crosslinking with radiation is carried out to blend sheet, irradiation dose 0.5-9KGy, obtains Precrosslink material；
Step 3: by precrosslink material, 2-48h is further crosslinked in 50-80 DEG C of hot bath, obtains crosslinking material；
Step 4: crosslinking material is foamed in vertical or horizontal foaming furnace, temperature is 190-250 DEG C, time 1- 20min, is preferably 220-240 DEG C, time 4-10min, obtains high filled biodegradable radiation cross-linked foam material.
The further details of explanation present invention of embodiment will be passed through below.But the invention is not limited in these examples.
Embodiment 1
High filled biodegradable radiation cross-linked foam material：By 100 weight of polyadipate-mutual-phenenyl two acid bromide two alcohol ester Part, 5 parts by weight of azodicarbonamide, 1 parts by weight of zinc oxide and 0.5 parts by weight of vinyl trimethylsilane composition.
The preparation of above-mentioned high filled biodegradable radiation cross-linked foam material：Each raw material is taken by proportioning, adds twin-screw Extruder carries out mixing granulator, and mixing granulator temperature is 80-170 DEG C, and obtained pellet is extruded into sheet material using single screw extrusion machine, Extrusion temperature is 100-170 DEG C, sheet thickness 1.0mm.Then use electron accelerator, at room temperature in air to sheet material into Row pre-irradiation, irradiation dose 9KGy, the sheet material after pre-irradiated is crosslinked, is further crosslinked 2h in 80 DEG C of hot bath.Most Foam afterwards in vertical-foaming stove, blowing temperature is 220 DEG C, and foamed time 4min, obtains foamed material.
The foamed material obtained to embodiment 1 carries out performance detection, and testing result is as shown in table 1.
Embodiment 2
High filled biodegradable radiation cross-linked foam material：By by 60 weight of polyadipate-mutual-phenenyl two acid bromide two alcohol ester Measure part, 40 parts by weight of starch, 0.5 weight of 5 parts by weight of azodicarbonamide, 1 parts by weight of zinc oxide and vinyltriethoxysilane Measure part composition.
The preparation of above-mentioned high filled biodegradable radiation cross-linked foam material：Each raw material is taken by proportioning, adds twin-screw Extruder carries out mixing granulator, and mixing granulator temperature is 80-170 DEG C, and obtained pellet is extruded into sheet material using single screw extrusion machine, Extrusion temperature is 100-170 DEG C, sheet thickness 1.0mm.Then use electron accelerator, at room temperature in air to sheet material into Row pre-irradiation, irradiation dose 9KGy, the sheet material after pre-irradiated is crosslinked, is further crosslinked 36h in 60 DEG C of hot bath.Most Foam afterwards in vertical-foaming stove, blowing temperature is 230 DEG C, and foamed time 4min, obtains foamed material.
The foamed material obtained to embodiment 2 carries out performance detection, and testing result is as shown in table 1.
Embodiment 3
High filled biodegradable radiation cross-linked foam material：By by 90 weight of polyadipate-mutual-phenenyl two acid bromide two alcohol ester Measure part, 10 parts by weight of starch, 4,4 '-oxobenzenesulfonyl hydrazide, 15 parts by weight, 2 parts by weight of calcium stearate and the (β-first of vinyl three Epoxide ethyoxyl) silane 0.1 parts by weight composition.
The preparation of above-mentioned high filled biodegradable radiation cross-linked foam material：Each raw material is taken by proportioning, adds twin-screw Extruder carries out mixing granulator, and mixing granulator temperature is 80-170 DEG C, and obtained pellet is extruded into sheet material using single screw extrusion machine, Extrusion temperature is 100-170 DEG C, sheet thickness 1.5mm.Using60Co sources, carry out pre-irradiation in air to sheet material at room temperature, Irradiation dose is 8KGy, the sheet material after pre-irradiated is crosslinked, and 30h is further crosslinked in 70 DEG C of hot bath.Finally vertical Foam in foaming furnace, blowing temperature is 250 DEG C, and foamed time 1min, obtains foamed material.
The foamed material obtained to embodiment 3 carries out performance detection, and testing result is as shown in table 1.
Embodiment 4
High filled biodegradable radiation cross-linked foam material：By by 80 weight of polyadipate-mutual-phenenyl two acid bromide two alcohol ester Measure part, 20 parts by weight of cellulose, 2 weight of 10 parts by weight of azodicarbonamide, 2 parts by weight of stearic acid and vinyltriethoxysilane Measure part composition.
The preparation of above-mentioned high filled biodegradable radiation cross-linked foam material：Each raw material is taken by proportioning, adds twin-screw Extruder carries out mixing granulator, and mixing granulator temperature is 80-170 DEG C, and obtained pellet is extruded into sheet material using single screw extrusion machine, Extrusion temperature is 100-170 DEG C, sheet thickness 2.0mm.Using electron accelerator, sheet material is carried out in air at room temperature pre- Irradiation, irradiation dose 7KGy, the sheet material after pre-irradiated is crosslinked, is further crosslinked 10h in 80 DEG C of hot bath.Finally exist Foam in vertical-foaming stove, blowing temperature is 220 DEG C, and foamed time 4min, obtains foamed material.
The foamed material obtained to embodiment 4 carries out performance detection, and testing result is as shown in table 1.
Embodiment 5
High filled biodegradable radiation cross-linked foam material：By by 70 weight of polyadipate-mutual-phenenyl two acid bromide two alcohol ester Measure part, 30 parts by weight of cellulose, 12 parts by weight of Barium azodicarboxylate, 5 parts by weight of zinc stearate and vinyl trimethylsilane 10 Parts by weight form.
The preparation of above-mentioned high filled biodegradable radiation cross-linked foam material：Each raw material is taken by proportioning, adds twin-screw Extruder carries out mixing granulator, and mixing granulator temperature is 80-170 DEG C, and obtained pellet is extruded into sheet material using single screw extrusion machine, Extrusion temperature is 100-170 DEG C, sheet thickness 0.5mm.Using electron accelerator, sheet material is carried out in air at room temperature pre- Irradiation, irradiation dose 0.5KGy, the sheet material after pre-irradiated is crosslinked, is further crosslinked 2h in 80 DEG C of hot bath.Finally Foam in vertical-foaming stove, blowing temperature is 240 DEG C, and foamed time 3min, obtains foamed material.
The foamed material obtained to embodiment 5 carries out performance detection, and testing result is as shown in table 1.
Embodiment 6
High filled biodegradable radiation cross-linked foam material：By by 75 weight of polyadipate-mutual-phenenyl two acid bromide two alcohol ester Measure part, 25 parts by weight of lignin, N, 10 parts by weight of N- dinitrosopentamethlyene tetramines, 1 parts by weight of zinc stearate and vinyl Three ('beta '-methoxy ethyoxyl) silane, 8 parts by weight form.
The preparation of above-mentioned high filled biodegradable radiation cross-linked foam material：Each raw material is taken by proportioning, adds twin-screw Extruder carries out mixing granulator, and mixing granulator temperature is 80-170 DEG C, and obtained pellet is extruded into sheet material using single screw extrusion machine, Extrusion temperature is 100-170 DEG C, sheet thickness 1.5mm.Using60Co sources, carry out pre-irradiation in air to sheet material at room temperature, Irradiation dose is 9KGy, the sheet material after pre-irradiated is crosslinked, and 8h is further crosslinked in 70 DEG C of hot bath.Finally in vertical hair Foam in bubble stove, blowing temperature is 210 DEG C, and foamed time 10min, obtains foamed material.
The foamed material obtained to embodiment 6 carries out performance detection, and testing result is as shown in table 1.
Embodiment 7
High filled biodegradable radiation cross-linked foam material：By by 95 weight of polyadipate-mutual-phenenyl two acid bromide two alcohol ester Measure part, 5 parts by weight of lignin, 10 parts by weight of azodicarbonamide, 1 parts by weight of stearic acid and (the 'beta '-methoxy ethoxy of vinyl three Base) silane 0.05 parts by weight composition.
The preparation of above-mentioned high filled biodegradable radiation cross-linked foam material：Each raw material is taken by proportioning, adds twin-screw Extruder carries out mixing granulator, and mixing granulator temperature is 80-170 DEG C, and obtained pellet is extruded into sheet material using single screw extrusion machine, Extrusion temperature is 100-170 DEG C, sheet thickness 0.5mm.Using electron accelerator, sheet material is carried out in air at room temperature pre- Irradiation, irradiation dose 6KGy, the sheet material after pre-irradiated is crosslinked, is further crosslinked 6h in 80 DEG C of hot bath.Finally exist Foam in vertical-foaming stove, blowing temperature is 220 DEG C, and foamed time 4min, obtains foamed material.
The foamed material obtained to embodiment 7 carries out performance detection, and testing result is as shown in table 1.
Embodiment 8
High filled biodegradable radiation cross-linked foam material：By by 60 weight of polyadipate-mutual-phenenyl two acid bromide two alcohol ester Measure part, 40 parts by weight of silica, 10 parts by weight of azodicarbonamide, 5 parts by weight of zinc oxide and vinyltriethoxysilane 2 Parts by weight form.
The preparation of above-mentioned high filled biodegradable radiation cross-linked foam material：Each raw material is taken by proportioning, adds twin-screw Extruder carries out mixing granulator, and mixing granulator temperature is 80-170 DEG C, and obtained pellet is extruded into sheet material using single screw extrusion machine, Extrusion temperature is 100-170 DEG C, sheet thickness 1.0mm.Using electron accelerator, sheet material is carried out in air at room temperature pre- Irradiation, irradiation dose 8KGy, the sheet material after pre-irradiated is crosslinked, is further crosslinked 40h in 60 DEG C of hot bath.Finally exist Foam in vertical-foaming stove, blowing temperature is 240 DEG C, and foamed time 2min, obtains foamed material.
The foamed material obtained to embodiment 8 carries out performance detection, and testing result is as shown in table 1.
Embodiment 9
High filled biodegradable radiation cross-linked foam material：By by 85 weight of polyadipate-mutual-phenenyl two acid bromide two alcohol ester Measure part, 5 parts by weight of silica 1,15 parts by weight of diisopropyl azodiformate, 0.01 parts by weight of zinc stearate and vinyl three 3 parts by weight of ('beta '-methoxy ethyoxyl) silane form.
The preparation of above-mentioned high filled biodegradable radiation cross-linked foam material：Each raw material is taken by proportioning, adds twin-screw Extruder carries out mixing granulator, and mixing granulator temperature is 80-170 DEG C, and obtained pellet is extruded into sheet material using single screw extrusion machine, Extrusion temperature is 100-170 DEG C, sheet thickness 2.5mm.Using electron accelerator, sheet material is carried out in air at room temperature pre- Irradiation, irradiation dose 9KGy, the sheet material after pre-irradiated is crosslinked, is further crosslinked 4h in 80 DEG C of hot bath.Finally exist Foam in vertical-foaming stove, blowing temperature is 200 DEG C, and foamed time 12min, obtains foamed material.
The foamed material obtained to embodiment 9 carries out performance detection, and testing result is as shown in table 1.
Embodiment 10
High filled biodegradable radiation cross-linked foam material：By by 65 weight of polyadipate-mutual-phenenyl two acid bromide two alcohol ester Measure part, 35 parts by weight of talcum powder, 8 weight of 5 parts by weight of Barium azodicarboxylate, 1 parts by weight of zinc stearate and vinyl trimethylsilane Measure part composition.
The preparation of above-mentioned high filled biodegradable radiation cross-linked foam material：Each raw material is taken by proportioning, adds twin-screw Extruder carries out mixing granulator, and mixing granulator temperature is 80-170 DEG C, and obtained pellet is extruded into sheet material using single screw extrusion machine, Extrusion temperature is 100-170 DEG C, sheet thickness 0.5mm.Using electron accelerator, sheet material is carried out in air at room temperature pre- Irradiation, irradiation dose 2KGy, the sheet material after pre-irradiated is crosslinked, is further crosslinked 12h, in level in 70 DEG C of hot bath Foam in foaming furnace, blowing temperature is 250 DEG C, and foamed time 1min, obtains foamed material.
The foamed material obtained to embodiment 10 carries out performance detection, and testing result is as shown in table 1.
Embodiment 11
High filled biodegradable radiation cross-linked foam material：By by 75 weight of polyadipate-mutual-phenenyl two acid bromide two alcohol ester Measure part, 25 parts by weight of talcum powder, N, 10 parts by weight of N- dinitrosopentamethlyene tetramines, 3 parts by weight of stearic acid and vinyl three 0.2 parts by weight of Ethoxysilane form.
The preparation of above-mentioned high filled biodegradable radiation cross-linked foam material：Each raw material is taken by proportioning, adds twin-screw Extruder carries out mixing granulator, and mixing granulator temperature is 80-170 DEG C, and obtained pellet is extruded into sheet material using single screw extrusion machine, Extrusion temperature is 100-170 DEG C, sheet thickness 1mm.Using electron accelerator, pre- spoke is carried out to sheet material in air at room temperature According to irradiation dose 9KGy, the sheet material after pre-irradiated is crosslinked, is further crosslinked 2h in 80 DEG C of hot bath, is sent out in level Foam in bubble stove, blowing temperature is 190 DEG C, and foamed time 20min, obtains foamed material.
The foamed material obtained to embodiment 11 carries out performance detection, and testing result is as shown in table 1.
Embodiment 12
High filled biodegradable radiation cross-linked foam material：By by 90 weight of polyadipate-mutual-phenenyl two acid bromide two alcohol ester Measure part, 10 parts by weight of montmorillonite, three ethoxy of 15 parts by weight of diisopropyl azodiformate, 5 parts by weight of calcium stearate and vinyl 10 parts by weight of base silane form.
The preparation of above-mentioned high filled biodegradable radiation cross-linked foam material：Each raw material is taken by proportioning, adds twin-screw Extruder carries out mixing granulator, and mixing granulator temperature is 80-170 DEG C, and obtained pellet is extruded into sheet material using single screw extrusion machine, Extrusion temperature is 100-170 DEG C, sheet thickness 0.5mm.Using electron accelerator, sheet material is carried out in air at room temperature pre- Irradiation, irradiation dose 0.5KGy, the sheet material after pre-irradiated is crosslinked, is further crosslinked 6h, in water in 70 DEG C of hot bath Foam in flat foaming furnace, blowing temperature is 220 DEG C, and foamed time 1min, obtains foamed material.
The foamed material obtained to embodiment 12 carries out performance detection, and testing result is as shown in table 1.
Embodiment 13
High filled biodegradable radiation cross-linked foam material：By by 70 weight of polyadipate-mutual-phenenyl two acid bromide two alcohol ester Measure part, 30 parts by weight of montmorillonite, 15 parts by weight of azodicarbonamide, 5 parts by weight of stearic acid and (the 'beta '-methoxy ethoxy of vinyl three Base) silane 6 parts by weight composition.
The preparation of above-mentioned high filled biodegradable radiation cross-linked foam material：Each raw material is taken by proportioning, adds twin-screw Extruder carries out mixing granulator, and mixing granulator temperature is 80-170 DEG C, and obtained pellet is extruded into sheet material using single screw extrusion machine, Extrusion temperature is 100-170 DEG C, sheet thickness 0.5mm.Using electron accelerator, sheet material is carried out in air at room temperature pre- Irradiation, irradiation dose 5KGy, the sheet material after pre-irradiated is crosslinked, is further crosslinked 20h, in level in 60 DEG C of hot bath Foam in foaming furnace, blowing temperature is 220 DEG C, and foamed time 2min, obtains foamed material.
The foamed material obtained to embodiment 13 carries out performance detection, and testing result is as shown in table 1.
Embodiment 14
High filled biodegradable radiation cross-linked foam material：By by 85 weight of polyadipate-mutual-phenenyl two acid bromide two alcohol ester Measure part, 15 parts by weight of calcium carbonate, N, 15 parts by weight of N- dinitrosopentamethlyene tetramines, 5 parts by weight of zinc oxide and vinyl three 10 parts by weight of ('beta '-methoxy ethyoxyl) silane form.
The preparation of above-mentioned high filled biodegradable radiation cross-linked foam material：Each raw material is taken by proportioning, adds twin-screw Extruder carries out mixing granulator, and mixing granulator temperature is 80-170 DEG C, and obtained pellet is extruded into sheet material using single screw extrusion machine, Extrusion temperature is 100-170 DEG C, sheet thickness 0.5mm.Using electron accelerator, sheet material is carried out in air at room temperature pre- Irradiation, irradiation dose 9KGy, the sheet material after pre-irradiated is crosslinked, is further crosslinked 8h, in level in 70 DEG C of hot bath Foam in foaming furnace, blowing temperature is 220 DEG C, and foamed time 2min, obtains foamed material.
The foamed material obtained to embodiment 14 carries out performance detection, and testing result is as shown in table 1.
Embodiment 15
High filled biodegradable radiation cross-linked foam material：By by 75 weight of polyadipate-mutual-phenenyl two acid bromide two alcohol ester Measure part, 25 parts by weight of calcium carbonate, 10 weight of 10 parts by weight of azodicarbonamide, 5 parts by weight of zinc oxide and vinyltriethylsilane Measure part composition.
The preparation of above-mentioned high filled biodegradable radiation cross-linked foam material：Each raw material is taken by proportioning, adds twin-screw Extruder carries out mixing granulator, and mixing granulator temperature is 80-170 DEG C, and obtained pellet is extruded into sheet material using single screw extrusion machine, Extrusion temperature is 100-170 DEG C, sheet thickness 0.5mm.Using electron accelerator, sheet material is carried out in air at room temperature pre- Irradiation, irradiation dose 9KGy, the sheet material after pre-irradiated is crosslinked, is further crosslinked 10h, in level in 70 DEG C of hot bath Foam in foaming furnace, blowing temperature is 200 DEG C, and foamed time 12min, obtains foamed material.
The foamed material obtained to embodiment 15 carries out performance detection, and testing result is as shown in table 1.
Comparative example 1
High filled biodegradable radiation cross-linked foam material：By by 75 weight of polyadipate-mutual-phenenyl two acid bromide two alcohol ester Measure part, 25 parts by weight of calcium carbonate, 10 parts by weight of azodicarbonamide, 5 parts by weight of zinc oxide and Triallyl isocyanurate 10 Parts by weight form.
The preparation of above-mentioned high filled biodegradable radiation cross-linked foam material：Each raw material is taken by proportioning, adds twin-screw Extruder carries out mixing granulator, and mixing granulator temperature is 80-170 DEG C, and obtained pellet is extruded into sheet material using single screw extrusion machine, Extrusion temperature is 100-170 DEG C, sheet thickness 0.5mm.Using electron accelerator, sheet material is carried out in air at room temperature pre- Irradiation, irradiation dose 9KGy, the sheet material after pre-irradiated is crosslinked, is further crosslinked 10h, in level in 70 DEG C of hot bath Foam in foaming furnace, blowing temperature is 200 DEG C, and foamed time 12min, obtains foamed material.
Comparative example 2
High filled biodegradable radiation cross-linked foam material：By by 75 weight of polyadipate-mutual-phenenyl two acid bromide two alcohol ester Measure part, 25 parts by weight of calcium carbonate, 10 parts by weight of azodicarbonamide, 5 parts by weight of zinc oxide and Triallyl isocyanurate 10 Parts by weight form.
The preparation of above-mentioned high filled biodegradable radiation cross-linked foam material：Each raw material is taken by proportioning, adds twin-screw Extruder carries out mixing granulator, and mixing granulator temperature is 80-170 DEG C, and obtained pellet is extruded into sheet material using single screw extrusion machine, Extrusion temperature is 100-170 DEG C, sheet thickness 0.5mm.Using electron accelerator, sheet material is carried out in air at room temperature pre- Irradiation, irradiation dose 100KGy.Foam in horizontal foaming furnace, blowing temperature is 200 DEG C, foamed time 12min, can not Prepare foamed material.
To the apparent density of the biodegradable radiation cross-linked foam material of embodiment 1-15 and comparative example 2, expansion ratio, drawing Intensity, elongation at break, compressive strength and durability is stretched to be detected.Wherein, apparent density by GB-T-6343-2009 into Row detection；Tensile strength and elongation at break use the method in GB/T6344-1996 to be detected；Compressive strength uses GB/ Method in T8813-2008 is detected；The method that durability uses is detected.Testing result is as shown in table 1.
The performance of the biodegradable radiation cross-linked foam material of table 1 embodiment 1-15 and comparative example 1-2
As it can be seen from table 1 crosslinking agent only using the present invention, could the excellent foam material of two steps crosslinking processability Material, crosslinking agent of the prior art can not be crosslinked (comparative example 1) using low irradiation dose, and high filling of the invention can biology Degraded radiation cross-linked foam material possesses the advantages of excellent physical properties, durability are good, expansion ratio is higher, not less than existing skill In art using big irradiation dose crosslinking prepare foamed material technology (comparative example 2), and by with the degradable height of other biological Molecule, such as polylactic acid, carbon dioxide-epoxy propane copolymer, poly butylene succinate carry out blending foaming, can be very The mechanical property of regulation and control expanded material in wide scope.
The water resistance of the foamed material of embodiment 1-15 is detected, detection method is：By high filled biodegradable Radiation cross-linked foam material soaks 15 days in 80 DEG C waters.After testing, after soaking 30 days, the table of foamed material of the invention See well, without significant change, tensile strength is reduced without obvious.Illustrate the foamed material water-tolerant of the present invention.

Claims (8)

1. high filled biodegradable radiation cross-linked foam material, it is characterised in that including：
The crosslinking agent is vinyl trimethylsilane, vinyltriethoxysilane, vinyl three ('beta '-methoxy ethyoxyl) One or more mixing in any proportion in silane；
The filler is one kind in starch, cellulose, lignin, silica, talcum powder, montmorillonite, calcium carbonate.
2. high filled biodegradable radiation cross-linked foam material according to claim 1, it is characterised in that composition and weight Part it is：
3. high filled biodegradable radiation cross-linked foam material, it is characterised in that the foaming agent is azodicarbonamide, idol Nitrogen dioctyl phthalate barium, diisopropyl azodiformate, N, in N- dinitrosopentamethlyene tetramines, 4,4 '-oxobenzenesulfonyl hydrazide One or more mixing in any proportion.
4. high filled biodegradable radiation cross-linked foam material, it is characterised in that the blowing promotor is zinc oxide, stearic acid One or more mixing in any proportion in zinc, calcium stearate.
5. the preparation method of the high filled biodegradable crosslinking with radiation described in claim 1-4 any one, it is characterised in that Step is as follows：
Step 1: weighing each raw material by composition and parts by weight, add in extruder and carry out mixing granulator, mixing granulator temperature is 80-170 DEG C, obtained mixing granulator material extrusion sheet on sheet extruder, sheet thickness 0.5-3.0mm, extrusion temperature For 100-170 DEG C；
Step 2: at room temperature in air, crosslinking with radiation is carried out to blend sheet, irradiation dose 0.5-9KGy, is pre-payed Join material；
Step 3: by precrosslink material, 2-48h is further crosslinked in 50-80 DEG C of hot bath, obtains crosslinking material；
Step 4: crosslinking material is foamed, temperature is 190-250 DEG C, time 1-20min, and obtaining high filling can biology Degraded radiation cross-linked foam material.
6. the preparation method of high filled biodegradable crosslinking with radiation according to claim 5, it is characterised in that mixing is made Grain is completed in double screw extruder, and the equipment of extrusion sheet is single screw rod sheet extruder.
7. the preparation method of high filled biodegradable crosslinking with radiation according to claim 5, it is characterised in that ionization spoke The source of penetrating is60Co sources or electron accelerator.
8. the preparation method of high filled biodegradable crosslinking with radiation according to claim 5, it is characterised in that cross-linking agent Material foams in vertical or horizontal foaming furnace.
CN201711196162.7A 2017-11-25 2017-11-25 High filled biodegradable radiation cross-linked foam material and preparation method thereof Withdrawn CN108034199A (en)

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CN114369267A (en) * 2022-03-22 2022-04-19 北京林业大学 Ternary composite film material and preparation method and application thereof
CN114369267B (en) * 2022-03-22 2022-05-17 北京林业大学 Ternary composite film material and preparation method and application thereof

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Application publication date: 20180515