CN101880446A - Biodegradable plastic with antibacterial property and preparation method thereof - Google Patents
Biodegradable plastic with antibacterial property and preparation method thereof Download PDFInfo
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- CN101880446A CN101880446A CN 201010210513 CN201010210513A CN101880446A CN 101880446 A CN101880446 A CN 101880446A CN 201010210513 CN201010210513 CN 201010210513 CN 201010210513 A CN201010210513 A CN 201010210513A CN 101880446 A CN101880446 A CN 101880446A
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- 238000002360 preparation method Methods 0.000 title claims abstract description 8
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- 239000000975 dye Substances 0.000 claims abstract description 72
- 239000000284 extract Substances 0.000 claims abstract description 18
- 239000011159 matrix material Substances 0.000 claims abstract description 14
- 229920006238 degradable plastic Polymers 0.000 claims description 45
- 238000002156 mixing Methods 0.000 claims description 38
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- Compositions Of Macromolecular Compounds (AREA)
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Abstract
The invention provides a biodegradable plastic with antibacterial property and a preparation method thereof. The biodegradable plastic with antibacterial property comprises biodegradable plastic matrix and antibacterial plant source dyes which are dispersed in the biodegradable plastic matrix, wherein the mass ratio of the antibacterial plant source dyes to the biodegradable plastic matrix is (0.01-10):100. The invention simply and fast extracts various antibacterial plant source dyes and prepares the biodegradable plastic which is the effective constituent of the various antibacterial plant source dyes, so that the plastic not only is biodegradable but also has good antibacterial property. The biodegradable plastic changes the crystallization property of the existing plastic since the dyes play a part in nucleating agent, is more easily degraded after the plastic product is abandoned, is environment-friendly, and has the degradation rate which is more than 90% after being putted in compost, active sludge and soil for 6 months.
Description
[technical field]
The present invention relates to a kind of bio-degradable plastics, particularly relate to a kind of bio-degradable plastics with germ resistance.
[background technology]
Plastics on the China market are of a great variety at present, and are wherein most of based on polyvinyl chloride (PVC) raw material.These class plastics are difficult to degraded, and moulding processability is relatively poor, adds need add auxiliary agents such as pigment, softening agent, anti-aging agent man-hour, and these chemical are all toxic, have caused common hidden danger in use for the mankind and environment two aspects.Along with the raising day by day of awareness of safety, associated safety standard and relevant law are constantly revised by states such as European Union, the U.S., Japan and Russia.The phenomenon of being found the toxic substance content overproof in China's plastic goods happens occasionally, and has had a strong impact on Chinese international fame, causes enormous economic loss, has directly influenced the plastics outlet of China.Therefore, the application of Biodegradable material and functional type environmental-protection additive thereof becomes the outlet that addresses this problem.
[summary of the invention]
The purpose of this invention is to provide a kind of bio-degradable plastics, to solve above-mentioned the deficiencies in the prior art with germ resistance.
To achieve these goals, a kind of bio-degradable plastics with germ resistance of the present invention adopts following technical scheme:
A kind of bio-degradable plastics with germ resistance comprises bio-degradable plastics matrix and the germ resistance plant-sourced dyestuff that is scattered in wherein, and the mass ratio of described germ resistance plant-sourced dyestuff and described bio-degradable plastics matrix is (0.01-10): 100.
Described germ resistance plant-sourced dyestuff extracts from the plant that contains effective antimicrobial component, and the described plant that contains effective antimicrobial component comprises: madder, safflower, bush, pomegranate rind, onion, birchleaf pear, Stigma Croci, red sandalwood, northeast lithospermum erythrorrhizon, Asian puccoon, giant knotweed, hispid arthraxon, cape jasmine, smoke tree, glutinous rehmannia, tangerine peel, cork tree, barberry, turmeric, the root of large-flowered skullcap, root tuber of aromatic turmeric, rheum officinale, ginkgo, Potmarigold Calendula, Wild Chrysanthemum, Chinese scholartree, Zhe Shu, sandlwood, Herba Commelinae, woaded blue, indigo plant, acanthaceous indigo, wood is blue, Quercus acutissima, English walnut, arbor-vitae, purple perilla, Motherwort Herb, dark plum, giant knotweed, Turkey-galls, Salvia japonica Thunb., Chinese tallow tree, Herba Bidentis Tripartitae, five-leaved chaste tree, the barnyard grass persimmon, the beech willow, Chen, hazel, mulberry, lotus, tea, red bayberry, black soya bean, water caltrop, evergreen chinquapin, the potato gelsemium, Gnaphalium affine and Mongolian oak.
The extracting method of described germ resistance plant-sourced dyestuff is: the plant that will contain effective antimicrobial component is cleaned, dry, pulverizing; By mass parts, comminuted plants is by 1: solid-liquid ratio (1-50) with solvent at 25-75 ℃ of following ultrasonic extraction 0.1-15h, be cooled to room temperature after, suction filtration concentrates filtrate, lyophilize obtains Powdered germ resistance plant-sourced dyestuff; Described frequency of ultrasonic is 10-80KHz, and alternately the time is 30-60s; Described solvent is ethanol, acetone, Na
2CO
3, a kind of in chloroform, ethyl acetate or the propyl carbinol.
Described germ resistance plant-sourced dyestuff is the mixture of two or more germ resistance plant-sourced dyestuff.
Described germ resistance plant-sourced dyestuff is the mixture of two kinds of germ resistance plant-sourced dyestuffs, and its mass ratio is (1～50): 1.
Described bio-degradable plastics matrix is selected from the class among the terminal groups modification thing PBS multipolymer-COOH of the terminal groups modification thing PBS multipolymer-OH of terminal groups modification thing PBS-COOH, PBS multipolymer, PBS multipolymer of terminal groups modification thing PBS-OH, the PBS of PBS, PBS or PBS multipolymer; Described PBS multipolymer is synthetic by Succinic Acid, butyleneglycol and other diprotic acid or dibasic alcohol, and the molar fraction of PBS is 60-100% in the synthetic described PBS multipolymer; The glycol of synthetic PBS-OH, PBS multipolymer-OH and the mol ratio of diacid are a: b, b＜a≤3b; The glycol of synthetic PBS-COOH, PBS multipolymer-COOH and the mol ratio of diacid are c: d, c＜d≤3c.
To achieve these goals, a kind of preparation method with bio-degradable plastics of germ resistance of the present invention adopts following technical scheme:
The first step, the extraction of germ resistance plant-sourced dyestuff; The plant that will contain effective antimicrobial component is cleaned, dry, pulverizing; By mass parts, comminuted plants is by 1: solid-liquid ratio (1-50) with solvent at 25-75 ℃ of following ultrasonic extraction 0.1-15h, be cooled to room temperature after, suction filtration concentrates filtrate, lyophilize obtains Powdered germ resistance plant-sourced dyestuff; Second step, mixing; The master batch of bio-degradable plastics matrix is put into Banbury mixer and is heated, after treating complete fusion, the mass percent of mixing outward is that the germ resistance plant-sourced dyestuff of 0.01-10%, dispersion agent and the mass percent that mass percent is 0-10% are the coupling agent of 0-10%, at 80-160 ℃ of mixing 2-60min, treat to take off behind the naturally cooling and make the bio-degradable plastics that the present invention has germ resistance.
Carrying out mixing temperature behind the adding germ resistance plant-sourced dyestuff after the biodegradable plastic matrix fusion is 100-130 ℃.
The mass percent that adds dispersion agent is 0.01-8%, and the mass percent that adds coupling agent is 0.01-8%;
Described dispersion agent is selected from: low one's share of expenses for a joint undertaking wax, ionic polymer, stearates or polymer hyper-dispersant; Described coupling agent is selected from: silane coupling agent, titanate coupling agent, zirconium ester coupling agent, aluminate coupling agent or aluminium zirconium ester coupling agent.
Compared with prior art, the present invention has the following advantages:
(1) the present invention has extracted multiple germ resistance plant-sourced dyestuff by a kind of method of simple and fast, make the bio-degradable plastics with germ resistance of multiple interpolation germ resistance plant-sourced dyestuff effective constituent, it not only can biological degradation but also has good antibacterial property.
(2) in the bio-degradable plastics that the present invention makes with germ resistance, dyestuff plays the crystal property that the nucleator effect has changed plastics, after plastic prod goes out of use in the easier degraded, do not harm environment, place in compost, active sludge, soil that degradation rate all can reach more than 90% after 6 months.
(3) bio-degradable plastics with germ resistance that the present invention makes is a renewable resources, does not rely on Mineral resources such as oil, Sweet natural gas, and the source is abundant, and energy-conserving and environment-protective and relative low price, stable are the favorable substitutes of existing plastics.
[embodiment]
The present invention mainly may further comprise the steps:
The first step, from the plant that contains effective antimicrobial component, extract germ resistance plant-sourced dyestuff;
Second step, the germ resistance plant-sourced dyestuff that the first step is extracted and biodegradable plastics master batch are put into Banbury mixer and are carried out mixing to make the bio-degradable plastics that the present invention has germ resistance.
The extracting method of germ resistance plant-sourced dyestuff is in the first step: the plant that will contain effective antimicrobial component is cleaned, dry, pulverizing; By mass parts, comminuted plants is by 1: solid-liquid ratio (1-50) with solvent at 25-75 ℃ of following ultrasonic extraction 0.1-15h, be cooled to room temperature after, suction filtration concentrates filtrate, lyophilize obtains Powdered germ resistance plant-sourced dyestuff.The ultrasonic frequency of using in the first step is 10-80KHz, and alternately the time is 30-60s.The solvent that extracts usefulness in the first step adopts ethanol, acetone, Na
2CO
3, a kind of in chloroform, ethyl acetate or the propyl carbinol, foregoing ethanol is that volumetric concentration is the aqueous ethanolic solution of 0-100%, acetone is that volumetric concentration is the aqueous acetone solution of 0-100%, Na
2CO
3Be that massfraction is the Na of 0-2%
2CO
3The aqueous solution.
The plant that contains effective antimicrobial component in the first step of the present invention comprises: madder, safflower, bush, pomegranate rind, onion, birchleaf pear, Stigma Croci, red sandalwood, northeast lithospermum erythrorrhizon, Asian puccoon, giant knotweed, hispid arthraxon, cape jasmine, smoke tree, glutinous rehmannia, tangerine peel, cork tree, barberry, turmeric, the root of large-flowered skullcap, root tuber of aromatic turmeric, rheum officinale, ginkgo, Potmarigold Calendula, Wild Chrysanthemum, Chinese scholartree, Zhe Shu, sandlwood, Herba Commelinae, woaded blue, indigo plant, acanthaceous indigo, wood is blue, Quercus acutissima, English walnut, arbor-vitae, purple perilla, Motherwort Herb, dark plum, giant knotweed, Turkey-galls, Salvia japonica Thunb., Chinese tallow tree, Herba Bidentis Tripartitae, five-leaved chaste tree, the barnyard grass persimmon, the beech willow, Chen, hazel, mulberry, lotus, tea, red bayberry, black soya bean, water caltrop, evergreen chinquapin, the potato gelsemium, Gnaphalium affine and Mongolian oak.These plants all can extract germ resistance plant-sourced dyestuff.
The mixing step in second step is: the master batch of bio-degradable plastics is put into Banbury mixer heat, after treating complete fusion, the mass percent of mixing outward is that the germ resistance plant-sourced dyestuff of 0.01-10%, dispersion agent and the mass percent that mass percent is 0-10% are the coupling agent of 0-10%, at 80-160 ℃ of mixing 2-60min stirring and evenly mixing, treat to take off behind the naturally cooling and make the bio-degradable plastics that the present invention has germ resistance.
The bio-degradable plastics of using among the present invention mainly is terminal groups modification thing PBS-OH, PBS-COOH, PBS multipolymer-OH and the PBS multipolymer-COOH of poly butylene succinate (PBS), PBS multipolymer, PBS and PBS multipolymer; The PBS multipolymer is Succinic Acid, butyleneglycol and other diprotic acid or dibasic alcohol copolymerization and the product that generates, and wherein the molar fraction of PBS is 60-100%; The terminal groups modification thing of PBS, PBS multipolymer is the product that obtains behind the excessive synthetic down also purifying of two excessive acids or glycol, generate PBS-OH, PBS multipolymer-OH when glycol is excessive, the glycol of synthetic PBS-OH, PBS multipolymer-OH and the mol ratio of diacid can use a: b to represent, b＜a≤3b; Generate PBS-COOH, PBS multipolymer-COOH in the time of two excessive acids, the glycol of synthetic PBS-COOH, PBS multipolymer-COOH and the mol ratio of diacid can use c: d to represent, c＜d≤3c.
The dispersion agent that adds when mixing can be: low one's share of expenses for a joint undertaking wax, ionic polymer, stearates or polymer hyper-dispersant.
The coupling agent that adds when mixing can be: silane coupling agent, titanate coupling agent, zirconium ester coupling agent, aluminate coupling agent or aluminium zirconium ester coupling agent.
Below in conjunction with specific embodiment the present invention is described in further detail.
Embodiment one
The first step, the rheum officinale root is clean, dry, pulverizing; By mass parts, comminuted plants by 1: 1 solid-liquid ratio with ethanol at 45 ℃, ultrasonic frequency 10KHz～20KHz and with the time-interleaved ultrasonic extraction 1.6h down of 30s, after being cooled to room temperature, suction filtration concentrates filtrate, lyophilize obtains yellow powder shape germ resistance plant-sourced dyestuff;
Second step, Biodegradable material PBS master batch is put into Banbury mixer to be heated, after treating the complete fusion of above-mentioned PBS master batch, outer therein admixture amount per-cent is that rheum officinale germ resistance plant-sourced dyestuff, mass percent that 0.3% the first step extracts are that 0.15% dispersion agent EVA-3, mass percent are 0.15% coupling agent KH-550, at 110 ℃ of mixing 16min, make the material stirring and evenly mixing of adding, treat to take off behind the naturally cooling and just make bio-degradable plastics with germ resistance.
The effect of present embodiment is: the environmentally-friendly plastic proterties of the big yellow dye of interpolation that makes is for yellow; The antibacterium rate can reach 91%, the antifungal ability reaches more than 1 grade, and anti-microbial property is good; Elongation at break 387%, tensile strength 33.41MPa; Place in compost, active sludge, soil that degradation rate all can reach more than 90% after 6 months, of many uses after the forming process.
Embodiment two
The first step, the rheum officinale root is clean, dry, pulverizing; By mass parts, comminuted plants by 1: 50 solid-liquid ratio with acetone at 25 ℃, ultrasonic frequency 50KHz～80KHz and with the time-interleaved ultrasonic extraction 0.1h down of 30s, after being cooled to room temperature, suction filtration concentrates filtrate, lyophilize obtains yellow powder shape germ resistance plant-sourced dyestuff;
Second step, Biodegradable material PBS master batch is put into Banbury mixer to be heated, after treating the complete fusion of above-mentioned PBS master batch, outer therein admixture amount per-cent is that rheum officinale germ resistance plant-sourced dyestuff, mass percent that 0.01% the first step extracts are that 10% dispersing agent C H-2C, mass percent are 0.3% coupling agent TTOPP-38S, at 80 ℃ of mixing 25min, make the material stirring and evenly mixing of adding, treat to take off behind the naturally cooling and just make bio-degradable plastics with germ resistance.
The effect of present embodiment is: the environmentally-friendly plastic proterties of the big yellow dye of interpolation that makes is for yellow; The antibacterium rate can reach 94%, the antifungal ability reaches more than 1 grade, and anti-microbial property is good; Elongation at break 300%, tensile strength 32.77MPa; Place in compost, active sludge, soil that degradation rate all can reach more than 90% after 6 months, of many uses after the forming process.
Embodiment three
The first step, the rheum officinale root is clean, dry, pulverizing; By mass parts, comminuted plants by 1: 24 solid-liquid ratio with 0.2% Na
2CO
3At 60 ℃, ultrasonic frequency 35KHz～40KHz and with the time-interleaved down ultrasonic extraction 15h of 60s, be cooled to room temperature after, suction filtration concentrates filtrate, lyophilize obtains yellow powder shape germ resistance plant-sourced dyestuff.
Second step, Biodegradable material PBS-COOH master batch is put into Banbury mixer to be heated, after treating the complete fusion of above-mentioned PBS-COOH master batch, outer therein admixture amount per-cent is that rheum officinale germ resistance plant-sourced dyestuff, mass percent that 5% the first step extracts are that 8% dispersion agent 295A, mass percent are 4.2% coupling agent ModA, at 115 ℃ of mixing 40min, make the material stirring and evenly mixing of adding, treat to take off behind the naturally cooling and just make bio-degradable plastics with germ resistance.
The effect of present embodiment is: the environmentally-friendly plastic proterties of the big yellow dye of interpolation that makes is for yellow; The antibacterium rate can reach 93%, the antifungal ability reaches more than 1 grade, and anti-microbial property is good; Elongation at break 405%, tensile strength 21.32MPa; Place in compost, active sludge, soil that degradation rate all can reach more than 90% after 6 months, of many uses after the forming process.
Embodiment four
The first step, the rheum officinale root is clean, dry, pulverizing; By mass parts, comminuted plants by 1: 36 solid-liquid ratio with ethanol at 35 ℃, ultrasonic frequency 60KHz～70KHz and with the time-interleaved ultrasonic extraction 10h down of 40s, after being cooled to room temperature, suction filtration concentrates filtrate, lyophilize obtains yellow powder shape germ resistance plant-sourced dyestuff.
Second step, Biodegradable material PBS-COOH master batch is put into Banbury mixer to be heated, after treating the complete fusion of above-mentioned PBS-COOH master batch, outer therein admixture amount per-cent is that rheum officinale germ resistance plant-sourced dyestuff, mass percent that 10% the first step extracts are that 0.01% dispersion agent Zinic stearas, mass percent are 4% coupling agent DL-411-A, at 90 ℃ of mixing 37min, make the material stirring and evenly mixing of adding, treat to take off behind the naturally cooling and just make bio-degradable plastics with germ resistance.
The effect of present embodiment is: the environmentally-friendly plastic proterties of the big yellow dye of interpolation that makes is for yellow; The antibacterium rate can reach 90%, the antifungal ability reaches more than 1 grade, and anti-microbial property is good; Elongation at break 513%, tensile strength 35.76MPa; Place in compost, active sludge, soil that degradation rate all can reach more than 90% after 6 months, of many uses after the forming process.
Embodiment five
The first step, the rheum officinale root is clean, dry, pulverizing; By mass parts, comminuted plants by 1: 46 solid-liquid ratio with distilled water at 75 ℃, ultrasonic frequency 15KHz～75KHz and with the time-interleaved ultrasonic extraction 13h down of 30s, after being cooled to room temperature, suction filtration concentrates filtrate, lyophilize obtains yellow powder shape germ resistance plant-sourced dyestuff.
Second step, Biodegradable material PBS-OH master batch is put into Banbury mixer to be heated, after treating the complete fusion of above-mentioned PBS-OH master batch, outer therein admixture amount per-cent is that rheum officinale germ resistance plant-sourced dyestuff, mass percent that 0.3% the first step extracts are 10% coupling agent Z-6020, at 160 ℃ of mixing 2min, make the material stirring and evenly mixing of adding, treat to take off behind the naturally cooling and just make bio-degradable plastics with germ resistance.
The effect of present embodiment is: the environmentally-friendly plastic proterties of the big yellow dye of interpolation that makes is for yellow; The antibacterium rate can reach 94%, the antifungal ability reaches more than 1 grade, and anti-microbial property is good; Elongation at break 800%, tensile strength 49.01MPa; Place in compost, active sludge, soil that degradation rate all can reach more than 90% after 6 months, of many uses after the forming process.
Embodiment six
The first step, the rheum officinale root is clean, dry, pulverizing; By mass parts, will be comminuted plants by 1: 45 solid-liquid ratio with 75% aqueous ethanolic solution at 32 ℃, ultrasonic frequency 10KHz～45KHz and with the time-interleaved down ultrasonic extraction 15h of 30s, after being cooled to room temperature, suction filtration, filtrate is concentrated, and lyophilize obtains yellow powder shape germ resistance plant-sourced dyestuff.
Second step, Biodegradable material PBS-OH master batch is put into Banbury mixer to be heated, after treating the complete fusion of above-mentioned PBS-OH master batch, outer therein admixture amount per-cent is that rheum officinale germ resistance plant-sourced dyestuff, mass percent that 6.5% the first step extracts are 8% dispersion agent Luwax AF-29, at 150 ℃ of mixing 10min, make the material stirring and evenly mixing of adding, treat to take off behind the naturally cooling and just make bio-degradable plastics with germ resistance.
The effect of present embodiment is: the environmentally-friendly plastic proterties of the big yellow dye of interpolation that makes is for yellow; The antibacterium rate can reach 97%, the antifungal ability reaches more than 1 grade, and anti-microbial property is good; Elongation at break 587%, tensile strength 50.21MPa; Place in compost, active sludge, soil that degradation rate all can reach more than 90% after 6 months, of many uses after the forming process.
Embodiment seven
The first step, the rheum officinale root is clean, dry, pulverizing; By mass parts, will be comminuted plants by 1: 15 solid-liquid ratio with 50% aqueous acetone solution at 45 ℃, ultrasonic frequency 30KHz～80KHz and with the time-interleaved down ultrasonic extraction 5h of 45s, after being cooled to room temperature, suction filtration, filtrate is concentrated, and lyophilize obtains yellow powder shape germ resistance plant-sourced dyestuff.
Second step, Biodegradable material PBS multipolymer master batch is put into Banbury mixer to be heated, after treating the complete fusion of above-mentioned PBS multipolymer master batch, outer therein admixture amount per-cent is that rheum officinale germ resistance plant-sourced dyestuff, mass percent that 7% the first step extracts are 0.01% dispersing agent C MPS, at 160 ℃ of mixing 20min, make the material stirring and evenly mixing of adding, treat to take off behind the naturally cooling and just make bio-degradable plastics with germ resistance.
The effect of present embodiment is: the environmentally-friendly plastic proterties of the big yellow dye of interpolation that makes is for yellow; The antibacterium rate can reach 96%, the antifungal ability reaches more than 1 grade, and anti-microbial property is good; Elongation at break 765%, tensile strength 43.13MPa; Place in compost, active sludge, soil that degradation rate all can reach more than 90% after 6 months, of many uses after the forming process.
Embodiment eight
The first step, the rheum officinale root is clean, dry, pulverizing; By mass parts, comminuted plants by 1: 8 solid-liquid ratio with chloroform at 55 ℃, ultrasonic frequency 45KHz～75KHz and with the time-interleaved ultrasonic extraction 12h down of 30s, after being cooled to room temperature, suction filtration concentrates filtrate, lyophilize obtains yellow powder shape germ resistance plant-sourced dyestuff.
Second step, Biodegradable material PBS multipolymer master batch is put into Banbury mixer to be heated, after treating the complete fusion of above-mentioned PBS multipolymer master batch, outer therein admixture amount per-cent is that rheum officinale germ resistance plant-sourced dyestuff, mass percent that 3.5% the first step extracts are that 3.1% dispersion agent K-2, mass percent are 1.5% coupling agent TL-2B, at 130 ℃ of mixing 60min, make the material stirring and evenly mixing of adding, treat to take off behind the naturally cooling and just make bio-degradable plastics with germ resistance.
The effect of present embodiment is: the environmentally-friendly plastic proterties of the big yellow dye of interpolation that makes is for yellow; The antibacterium rate can reach 96%, the antifungal ability reaches more than 1 grade, and anti-microbial property is good; Elongation at break 432%, tensile strength 35.61MPa; Place in compost, active sludge, soil that degradation rate all can reach more than 90% after 6 months, of many uses after the forming process.
Embodiment nine
The first step, the rheum officinale root is clean, dry, pulverizing; By mass parts, comminuted plants by 1: 1 solid-liquid ratio with ethyl acetate at 30 ℃, ultrasonic frequency 65KHz～80KHz and with the time-interleaved ultrasonic extraction 15h down of 30s, after being cooled to room temperature, suction filtration concentrates filtrate, lyophilize obtains yellow powder shape germ resistance plant-sourced dyestuff.
Second step, the terminal groups modification thing PBS multipolymer-OH master batch of Biodegradable material PBS multipolymer is put into Banbury mixer and heated, after treating above-mentioned PBS multipolymer-complete fusion of OH master batch, outer therein admixture amount per-cent is that rheum officinale germ resistance plant-sourced dyestuff, mass percent that 4.5% the first step extracts are that 2.1% dispersion agent N-34, mass percent are 3.4% coupling agent KM-602, at 100 ℃ of mixing 50min, make the material stirring and evenly mixing of adding, treat to take off behind the naturally cooling and just make bio-degradable plastics with germ resistance.
The effect of present embodiment is: the environmentally-friendly plastic proterties of the big yellow dye of interpolation that makes is for yellow; The antibacterium rate can reach 96%, the antifungal ability reaches more than 1 grade, and anti-microbial property is good; Elongation at break 392%, tensile strength 21.63MPa; Place in compost, active sludge, soil that degradation rate all can reach more than 90% after 6 months, of many uses after the forming process.
Embodiment ten
The first step, the rheum officinale root is clean, dry, pulverizing; By mass parts, comminuted plants by 1: 12 solid-liquid ratio with propyl carbinol at 60 ℃, ultrasonic frequency 25KHz～75KHz and with the time-interleaved ultrasonic extraction 12h down of 40s, after being cooled to room temperature, suction filtration concentrates filtrate, lyophilize obtains yellow powder shape germ resistance plant-sourced dyestuff.
Second step, Biodegradable material PBS multipolymer-COOH master batch is put into Banbury mixer to be heated, after treating above-mentioned PBS multipolymer-complete fusion of COOH master batch, outer therein admixture amount per-cent is that rheum officinale germ resistance plant-sourced dyestuff, mass percent that 0.01% the first step extracts are that 3.5% dispersion agent stearic acid, mass percent are 8% coupling agent Zr-801, at 120 ℃ of mixing 31min, make the material stirring and evenly mixing of adding, treat to take off behind the naturally cooling and just make bio-degradable plastics with germ resistance.
The effect of present embodiment is: the environmentally-friendly plastic proterties of the big yellow dye of interpolation that makes is for yellow; The antibacterium rate can reach 96%, the antifungal ability reaches more than 1 grade, and anti-microbial property is good; Elongation at break 532%, tensile strength 27.55MPa; Place in compost, active sludge, soil that degradation rate all can reach more than 90% after 6 months, of many uses after the forming process.
Embodiment 11～20
Embodiment 11～20 replace with madder with the rheum officinale in the foregoing description one～ten; The environmentally-friendly plastic proterties of the interpolation madder that embodiment 11～20 make is a red powder; The antibacterium rate can reach 90%～93%, the antifungal ability reaches more than 1 grade, and anti-microbial property is good; Elongation at break 332～781%, tensile strength 22.64～49.48MPa; Place in compost, active sludge, soil that degradation rate all can reach more than 90% after 6 months, of many uses after the forming process.
Embodiment 21～30
Embodiment 21～30 replace with onion with the rheum officinale in the foregoing description one～ten; The environmentally-friendly plastic proterties of the interpolation onion dyestuff that embodiment 21～30 make is the orange powder; The antibacterium rate can reach 91%～95%, the antifungal ability reaches more than 1 grade, and anti-microbial property is good; Elongation at break 360～710%, tensile strength 26.07～49.09MPa; Place in compost, active sludge, soil that degradation rate all can reach more than 90% after 6 months, of many uses after the forming process.
Embodiment hentriaconta-40
Embodiment hentriaconta-～40 replace with onion with the rheum officinale in the foregoing description one～ten, then with the onion germ resistance plant-sourced dyestuff that extracts in the step 1 respectively with the rheum officinale germ resistance plant-sourced dyestuff that extracts according to the method among the embodiment one～ten, in mass ratio is (1～50): 1 ratio is composite, and then mixing with the terminal groups modification thing of the terminal groups modification thing of PBS, PBS multipolymer, PBS or PBS multipolymer.The environmentally-friendly plastic proterties of the composite dyestuff of interpolation that embodiment hentriaconta-～40 make is the orange powder; The antibacterium rate can reach 92%～95%, the antifungal ability reaches more than 1 grade, and anti-microbial property is good; Elongation at break 330～690%, tensile strength 21.07～47.09MPa; Place in compost, active sludge, soil that degradation rate all can reach more than 90% after 6 months, of many uses after the forming process.
Adopt the elongation and the tensile strength of standard GB 1040-1992 plastic tensile measurement of test method environmentally-friendly plastic in the above embodiment of the present invention.
Adopt the antibacterial effect of People's Republic of China's light industry standard QB/T 2591-2003 antibiotic plastic----anti-microbial property test method and antibacterial effect test and evaluation environmentally-friendly plastic in the above embodiment of the present invention.
The method of calculating degradation rate in the above embodiment of the present invention is: the environmentally-friendly plastic that makes is put into compost, active sludge, soil with the certain proportion size, every a recording quality loss of sampling (three parallel samples of each sample) in 7 days, serial sampling 6 months.The mass loss rate formula is: D=(m
0-m
t)/m
0* 100%; M wherein
0Original quality for the degraded cephacoria; m
tResidual mass for t days caudacorias of degraded.
Various germ resistance plant-sourced dyestuffs with effective antimicrobial component are with homogencous dyes or two or more composite dyestuff and PBS and the mixing environmentally-friendly plastic that makes of multipolymer Biodegradable material thereof among the present invention, and the addition of germ resistance plant-sourced dyestuff and the mass ratio of bio-degradable plastics matrix are (0.01-10): 100; The environmentally-friendly plastic of the interpolation germ resistance plant-sourced dyestuff that makes is riotous with colour; The antibacterium rate can reach 90%～98%, the antifungal ability reaches more than 1 grade, and anti-microbial property is good; Elongation at break 360～550%, tensile strength 32.87～47.28MPa; Place in compost, active sludge, soil that degradation rate all can reach more than 90% after 6 months, of many uses after the forming process.
The present invention is mixing with the Biodegradable materials such as terminal groups modification thing of the terminal groups modification thing of germ resistance plant-sourced dyestuff and PBS, PBS multipolymer, PBS or PBS multipolymer, remedy the drawback of synthetic dyestuff toxic organic compound matter discharging now, and given environmentally-friendly plastic better anti-bacterial effect and beautiful color.Germ resistance plant-sourced dyestuff is as effective antimicrobial component and nucleator, do not harm environment, and changed the degree of crystallinity of PBS and multipolymer Biodegradable material thereof, being beneficial to microorganism adheres in dyestuff crystallization place, make plastic prod after discarded, in the easier degraded, improve the elongation at break and the tensile strength of plastics greatly.Use germ resistance plant-sourced dyestuff can slowly discharge with the degradation process of degradable material, brings into play its anti-microbial property.Because these plastics are nontoxic, can be widely used in various products such as agricultural fishery goods, materials and equipments, food product containers, lotion container, seasickness bag, household supplies, stationery, leisure goods, wrapping material, body of a motor car inner and outer decorative parts, electronics/electric device, to guarantee human healthy living.The present invention is low with the method energy consumption that PBS, PBS multipolymer and the modified product thereof of germ resistance plant-sourced dyeing prepares environmentally-friendly plastic, save time, machine-shaping is convenient, and gives plastics with effects such as antibiotic, environmental protection, can be used for large-scale industrialization production.
Claims (10)
1. bio-degradable plastics with germ resistance, it is characterized in that: comprise bio-degradable plastics matrix and the germ resistance plant-sourced dyestuff that is scattered in wherein, the mass ratio of described germ resistance plant-sourced dyestuff and described bio-degradable plastics matrix is (0.01-10): 100.
2. the bio-degradable plastics that has germ resistance according to claim 1, it is characterized in that: described germ resistance plant-sourced dyestuff extracts from the plant that contains effective antimicrobial component, and the described plant that contains effective antimicrobial component comprises: madder, safflower, bush, pomegranate rind, onion, birchleaf pear, Stigma Croci, red sandalwood, northeast lithospermum erythrorrhizon, Asian puccoon, giant knotweed, hispid arthraxon, cape jasmine, smoke tree, glutinous rehmannia, tangerine peel, cork tree, barberry, turmeric, the root of large-flowered skullcap, root tuber of aromatic turmeric, rheum officinale, ginkgo, Potmarigold Calendula, Wild Chrysanthemum, Chinese scholartree, Zhe Shu, sandlwood, Herba Commelinae, woaded blue, indigo plant, acanthaceous indigo, wood is blue, Quercus acutissima, English walnut, arbor-vitae, purple perilla, Motherwort Herb, dark plum, giant knotweed, Turkey-galls, Salvia japonica Thunb., Chinese tallow tree, Herba Bidentis Tripartitae, five-leaved chaste tree, the barnyard grass persimmon, the beech willow, Chen, hazel, mulberry, lotus, tea, red bayberry, black soya bean, water caltrop, evergreen chinquapin, dye yam, Gnaphalium affine and Mongolian oak.
3. the bio-degradable plastics as having germ resistance as described in the claim 2, it is characterized in that: the extracting method of described germ resistance plant-sourced dyestuff is: the plant that will contain effective antimicrobial component cleans, dry, pulverize; By mass parts, comminuted plants is by 1: solid-liquid ratio (1-50) with solvent at 25-75 ℃ of following ultrasonic extraction 0.1-15h, be cooled to room temperature after, suction filtration concentrates filtrate, lyophilize obtains Powdered germ resistance plant-sourced dyestuff; Described frequency of ultrasonic is 10-80KHz, and alternately the time is 30-60s; Described solvent is ethanol, acetone, Na
2CO
3, a kind of in chloroform, ethyl acetate or the propyl carbinol.
4. the bio-degradable plastics as having germ resistance as described in the claim 3, it is characterized in that: described germ resistance plant-sourced dyestuff is the mixture of two or more germ resistance plant-sourced dyestuff.
5. the bio-degradable plastics as having germ resistance as described in the claim 4, it is characterized in that: described germ resistance plant-sourced dyestuff is the mixture of two kinds of germ resistance plant-sourced dyestuffs, and its mass ratio is (1～50): 1.
6. have the bio-degradable plastics of germ resistance according to claim 1, it is characterized in that: described bio-degradable plastics matrix is selected from the class among the terminal groups modification thing PBS multipolymer-COOH of the terminal groups modification thing PBS multipolymer-OH of terminal groups modification thing PBS-COOH, PBS multipolymer, PBS multipolymer of terminal groups modification thing PBS-OH, the PBS of PBS, PBS or PBS multipolymer; Described PBS multipolymer is synthetic by Succinic Acid, butyleneglycol and other diprotic acid or dibasic alcohol, and the molar fraction of PBS is 60-100% in the described PBS multipolymer of synthetic; The dibasic alcohol of synthetic PBS-OH, PBS multipolymer-OH and the mol ratio of diprotic acid are a: b, b＜a≤3b; The dibasic alcohol of synthetic PBS-COOH, PBS multipolymer-COOH and the mol ratio of diprotic acid are c: d, c＜d≤3c.
7. as having the preparation method of the bio-degradable plastics of germ resistance in the claim 1 to 6 as described in each, it is characterized in that it may further comprise the steps:
The first step, the extraction of germ resistance plant-sourced dyestuff; The plant that will contain effective antimicrobial component is cleaned, dry, pulverizing; By mass parts, comminuted plants is by 1: solid-liquid ratio (1-50) with solvent at 25-75 ℃ of following ultrasonic extraction 0.1-15h, be cooled to room temperature after, suction filtration concentrates filtrate, lyophilize obtains Powdered germ resistance plant-sourced dyestuff;
Second step, mixing; The master batch of bio-degradable plastics matrix is put into Banbury mixer and is heated, after treating complete fusion, the mass percent of mixing outward is that the germ resistance plant-sourced dyestuff of 0.01-10%, dispersion agent and the mass percent that mass percent is 0-10% are the coupling agent of 0-10%, at 80-160 ℃ of mixing 2-60min, treat to take off behind the naturally cooling and make the bio-degradable plastics that the present invention has germ resistance.
8. as having the preparation method of the bio-degradable plastics of germ resistance as described in the claim 7, it is characterized in that, add after the biodegradable plastic matrix fusion that to carry out mixing temperature behind the germ resistance plant-sourced dyestuff be 100-130 ℃.
9. as having the preparation method of the bio-degradable plastics of germ resistance as described in the claim 8, it is characterized in that the mass percent that adds dispersion agent is 0.01-8%, the mass percent that adds coupling agent is 0.01-8%.
10. as having the preparation method of the bio-degradable plastics of germ resistance as described in the claim 9, it is characterized in that described dispersion agent is selected from: low one's share of expenses for a joint undertaking wax, ionic polymer, stearates or polymer hyper-dispersant; Described coupling agent is selected from: silane coupling agent, titanate coupling agent, zirconium ester coupling agent, aluminate coupling agent or aluminium zirconium ester coupling agent.
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