CN104194287A - Modified poly-adipic acid/butylene terephthalate composite material containing coconut shell flour and preparation method thereof - Google Patents
Modified poly-adipic acid/butylene terephthalate composite material containing coconut shell flour and preparation method thereof Download PDFInfo
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- CN104194287A CN104194287A CN201410418378.3A CN201410418378A CN104194287A CN 104194287 A CN104194287 A CN 104194287A CN 201410418378 A CN201410418378 A CN 201410418378A CN 104194287 A CN104194287 A CN 104194287A
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Abstract
The invention relates to a modified poly-adipic acid/butylene terephthalate composite material containing coconut shell flour and a preparation method thereof. The composite material is composed of the following components in parts by weight: 100 parts of poly-adipic acid/butylene terephthalate, 1-20 parts of coconut shell flour, 0.5-2 parts of lubricant and 0.1-1 part of heat stabilizer. The preparation method of the composite material comprises the following steps: preparing the modified coconut shell flour, proportioning according to the composite material composition, uniformly mixing by a high-speed mixer, and carrying out extrusion granulation on the mixture in a double screw extruder. By using the biodegradable polyester plastic poly-adipic acid/butylene terephthalate and waste coconut shell as the raw materials to prepare the composite material, the method can alleviate the environmental pollution caused by waste coconut shell and can perform the function of reinforcing the poly-adipic acid/butylene terephthalate composite material, thereby preparing the coconut shell flour modified poly-adipic acid/butylene terephthalate composite material with excellent mechanical properties.
Description
Technical field
The present invention relates to a kind of biodegradable polymer composite, relate in particular to poly-hexanodioic acid/butylene terephthalate matrix material of a kind of modification containing coconut shell flour and preparation method thereof.
Background technology
Be accompanied by the develop rapidly of global economy, countries in the world constantly increase progressively the demand of petroleum resources, and the application of petroleum base polymer materials is just progressively penetrated into the every field of national economy and human lives's all respects.Yet meanwhile oil crisis is increasingly serious, nondegradable petroleum-based plastics has also been brought serious problem of environmental pollution to countries in the world.In the face of shortage of resources and environmental pollution two large problems, exploitation has become the study hotspot of plastics and packet industry from the biodegradated polymer materal of renewable resources, realize especially the strategic choice of global economy Sustainable development.In a large amount of biodegradable synthesizing polymeric materials, poly-hexanodioic acid/butylene terephthalate is a kind of aliphatic/aromatic copolyester that has the excellent biodegradability of aliphatic polyester and the excellent mechanical property of aromatic polyester concurrently, and this copolyesters has good physical and the processing characteristics that can compare favourably with common plastics.With commodity polymer materials similar, the means such as poly-hexanodioic acid/butylene terephthalate also can be by injection moulding, extrude, blowing, mold pressing, casting film-forming and blown film are processed preparation.At present more external major companies will gather hexanodioic acid/butylene terephthalate and realize and commercially produce and release a series of related productss, as the Ecoflex commodity of BASF Aktiengesellschaft (BASF), the Eastar Bio commodity of U.S. Yi Shi Man (Eastman), the Biomax commodity of du pont company (Dupond) etc.Because poly-hexanodioic acid/butylene terephthalate has that recyclability, degradability, processability are superior, the advantage such as good toughness, high thermal resistance, mechanical property be superior, its goods are at industrial packaging, the fields such as agroforestry production are with a wide range of applications.But due to the existence of aromatic series segment, cause the degradation rate of poly-hexanodioic acid/butylene terephthalate relatively slow.Its tensile strength has not quite also limited the application of this material in the higher field of mechanical property requirements simultaneously.In addition, the cost of this material is relatively high, has limited the popularization of its marketization application.Therefore in order to improve the over-all properties of poly-hexanodioic acid/butylene terephthalate material and to reduce production costs, it is carried out to modification and seem particularly necessary.
Coconut belongs to Palmae cocoanut, is one of main woody oleiferous plants crop in torrid areas, and comprehensive utilization economic benefit is high, therefore enjoy the good reputation of " Bao Shu ".Coconut historical existing more than 2000 year in the plantation of China, its plantation region mainly concentrates on the southern provinces such as Hainan and Yunnan.Coconut almost spherical, is partly comprised of exocarp, mesocarp, endocarp, kind skin, kind benevolence (endosperm), embryo, Coconut Juice etc.The exocarp of coconut and mesocarp are commonly called as coconut palm clothing, account for the 33-35% of coconut total mass; Endocarp is commonly called as coconut husk, accounts for the 12-15% of coconut total mass, and the coconut husk of ripe coconut becomes brown, and quality is very hard.Utilize the hard quality of coconut husk, can be engraved as artwork or be processed into the apparatus such as musical instrument, bowl, spoon; Scientist's sight is just concentrating on coconut husk destructive distillation is being become to charcoal both at home and abroad, then high grade activated carbon is made in activated processing; Foreign study personnel also mix coconut shell flour in concrete, to alleviate concrete weight and to reduce the cost of buildings; Coconut shell flour also can be used as the filler of dark-coloured plastics and vulcanite goods.The main component of coconut shell flour is natural plant fibre, and quality is comparatively fine and close hard, has specific tenacity high, degradable, and the advantage such as wide material sources are cheap, thereby be subject to domestic and international scientist's extensive concern.At present, foreign study utilizes the correlation technique of coconut shell flour relatively ripe, and utilization ratio is relatively high.Foreign study person blows off agent and the fragrant dopant of ant etc. by the crushed material of coconut husk (coconut shell flour) for filler, agricultural chemicals thinner, surface liquid absorption agent, offset printing and asphaltic products. surface treatment agent, welding electrode surfacer, composite sheet weighting agent, mold agent, the piston of chemical fibre industry.CN 103030870 A disclose coated coconut shell flour particle particle blending foaming material of a kind of polyethylene/POM and preparation method thereof, and material light weight that the method makes is soft, intensity is high, rebound resilience good.CN 101186755 A disclose the preparation method of a kind of coconut palm clothing and thermoplastic plastic composite material, and the method has solved the problems such as the consistency of coconut fibre and thermoplastics and raw material process for treating surface.Ruan Lin light etc. (plastics, as can be seen here, used coir fibre making to meet material and have good market outlook by 04 phase in 2008.But at home, coconut shell flour still belongs to the waste in coconut carving artwork or the production of other ornament, and its comprehensive utilization ratio is lower.Be stacked in for a long time in physical environment, also can form very important ecological pressure.Therefore discarded coconut husk is finish-machined to coconut shell flour, it is recycled, the matrix material of developing renewable resources containing coconut shell flour has objective economic benefit and social value, present stage while, the cost of poly-hexanodioic acid/butylene terephthalate was also relatively high, and the introducing of coconut shell flour can reduce the production cost of this material product.Thereby develop this type of fully biodegradable, coconut shell flour modification cheaply gathers hexanodioic acid/butylene terephthalate matrix material and has significant social effect.
Summary of the invention
The object of this invention is to provide poly-hexanodioic acid/butylene terephthalate (PBAT) matrix material of a kind of modification containing coconut shell flour and preparation method thereof, in poly-hexanodioic acid/butylene terephthalate matrix, be written into coupling agent modified coconut shell flour, lubricant and thermo-stabilizer prepare containing the poly-hexanodioic acid/butylene terephthalate matrix material of coconut shell flour modification through extruding pelletization and injection moulding, the tensile strength that can solve above-mentioned single poly-hexanodioic acid/butylene terephthalate is little, degradation rate is slow, high in cost of production shortcoming, containing the poly-hexanodioic acid/butylene terephthalate matrix material of coconut shell flour modification, than single poly-hexanodioic acid/butylene terephthalate material, there is larger tensile strength and degradation rate faster, simultaneously, owing to introducing recoverable, reproducible coconut husk resource, therefore also there is the feature that production cost is low.
Poly-hexanodioic acid/butylene terephthalate matrix material of a kind of modification containing coconut shell flour and preparation method thereof, step comprises:
First aspect of the present invention is to provide the poly-hexanodioic acid/butylene terephthalate matrix material of a kind of modification containing coconut shell flour, and component comprises by weight:
100 parts of poly-hexanodioic acid/butylene terephthalate
Coconut shell flour 1-20 part.
Second aspect of the present invention is to provide a kind of preparation method of coupling agent modified coconut shell flour, and step comprises:
A. coconut husk is pulverized and obtained coconut shell flour, dry;
B. the coconut shell flour after drying in step a is mixed with ethanol, ultrasonicly disperse to such an extent that finely dispersed suspension adds coupling agent in described suspension; After being mixed with coupling agent, unit for uniform suspension refluxes; Separate solid, after being dried, makes coupling agent modified coconut shell flour.
Wherein, drying condition is: vacuum-drying;
Wherein, described vacuum-drying temperature is preferably 60-120 ℃, more preferably 70-100 ℃, more preferably 80-90 ℃.Wherein, coupling agent is any one in γ-aminopropyl triethoxysilane (KH550), titanic acid ester (NZD201).
Wherein, coupling agent is the 0.5-5% that consumption is preferably coconut shell flour weight, more preferably 0.5-1%.
Wherein, above-mentioned ethanol is dehydrated alcohol.
Wherein, the time of ultrasonic dispersion is preferably 5-15min, is preferably 8-10min.
Wherein, the temperature of backflow is for being preferably 70-120 ℃, more preferably 70-100 ℃, more preferably 80-100 ℃;
Wherein, the time of backflow is for being preferably 2-3h.
Wherein, the poly-hexanodioic acid/butylene terephthalate of every 100 weight parts, is used the coconut shell flour of coupling agent KH550 modification to be preferably 1-15 part, more preferably 1-10 part.
Wherein, the poly-hexanodioic acid/butylene terephthalate of every 100 weight parts, is used the coconut shell flour of coupling agent NZD201 modification to be preferably 1-15 part, more preferably 1-10 part.
The preparation method that three aspects of the present invention are to provide the poly-hexanodioic acid/butylene terephthalate matrix material of a kind of modification containing coconut shell flour, wherein, supplies raw materials by following weight fraction:
Described preparation method's step comprises:
Step 1. will be gathered hexanodioic acid/butylene terephthalate, coconut shell flour, lubricant, thermo-stabilizer mixing, obtain mixture;
Step 2. is granulated: by the granulating mixture in step a;
Step 3. injection moulding: by the granulation injection moulding in step b, obtain the poly-hexanodioic acid/butylene terephthalate matrix material of modification containing coconut shell flour.
Wherein, the molecular-weight average of poly-hexanodioic acid/butylene terephthalate is 3.6 * 10
4.
Wherein, lubricant is wherein any one or a few of the stearate such as Zinic stearas, calcium stearate, Magnesium Stearate, aluminum stearate, barium stearate.
Wherein, thermo-stabilizer is any one in MALEIC ANHYDRIDE, epoxy soybean oil.
Beneficial effect: of the present invention a kind of containing the poly-hexanodioic acid/butylene terephthalate matrix material of coconut shell flour modification, because coconut shell flour is through coupling agent modified processing, effectively improve the consistency between coconut shell flour and poly-hexanodioic acid/butylene terephthalate, can effectively improve the mechanical strength of poly-hexanodioic acid/butylene terephthalate.
Owing to take, gather hexanodioic acid/butylene terephthalate as body material, add natural coconut shell flour it is carried out to modification, what therefore finally make is completely green containing the poly-hexanodioic acid/butylene terephthalate matrix material of coconut shell flour modification, the material of totally biodegradable, meets the requirement of society Sustainable development.
One of raw material of the present invention coconut shell flour derives from the pericarp (such as the pericarp of the discarded coconut in south China area) of discarded coconut, introduce coconut shell flour and not only can reduce to gather the production cost containing the poly-hexanodioic acid/butylene terephthalate matrix material of coconut shell flour modification that hexanodioic acid/butylene terephthalate is matrix, and can effectively improve the added value of coconut husk, weaken and be piled up in the ecological pressure that environment causes because of coconut husk.
Technical process of the present invention is simple, and low production cost can be accomplished scale production.
Accompanying drawing explanation
Tensile strength and the elongation at break graphic representation of the poly-hexanodioic acid/butylene terephthalate matrix material of Fig. 1 Silane coupling agent KH550 modification coconut shell flour
Tensile strength and the elongation at break graphic representation of the poly-hexanodioic acid/butylene terephthalate matrix material of Fig. 2 titanate coupling agent NZD201 modification coconut shell flour modification
Embodiment
Below in conjunction with embodiment, the present invention is described in further detail.
Embodiment 1
Containing the poly-hexanodioic acid/butylene terephthalate matrix material of coconut shell flour modification, count by weight,
Step 1, the coconut husk of oven dry is placed in pulverizer and is ground into fritter, then with ball mill, wears into powder, crosses 100 mesh sieve, obtains coconut shell flour, is then placed in 80 ℃ of vacuum drying ovens and dries.A certain amount of above-mentioned 100 order coconut shell flours are mixed with 50ml dehydrated alcohol, and ultrasonic dispersion 10min obtains finely dispersed suspension; Silane coupling agent KH550 is dissolved in to 50ml dehydrated alcohol; Unit for uniform suspension is mixed to the 3h that refluxes at 80 ℃ with coupling agent solution; Be cooled to room temperature, through centrifugation, in 80 ℃ of vacuum drying ovens, dry.Make coupling agent modified coconut shell flour.
Step 2, lubricant stearic acid zinc, thermo-stabilizer MALEIC ANHYDRIDE, in 80 ℃ of vacuum drying poly-hexanodioic acid/butylene terephthalate and above-mentioned steps 1, made modification coconut shell flour joins normal temperature in high-speed mixer and mixes.
Step 3, the raw material mixing in step 2 is placed in twin screw extruder extruding pelletization, and extrusion temperature is 150 ℃, then applies injection moulding machine the injection moulding of matrix material particle is obtained to standard testing batten, standby.
Embodiment 2
Containing the poly-hexanodioic acid/butylene terephthalate matrix material of coconut shell flour modification, count by weight,
Above-mentioned a kind of preparation method containing the poly-hexanodioic acid/butylene terephthalate matrix material of coconut shell flour modification, with embodiment 1.
Embodiment 3
Containing the poly-hexanodioic acid/butylene terephthalate matrix material of coconut shell flour modification, count by weight,
Above-mentioned a kind of preparation method containing the poly-hexanodioic acid/butylene terephthalate matrix material of coconut shell flour modification, with embodiment 1.
Embodiment 4
Containing the poly-hexanodioic acid/butylene terephthalate matrix material of coconut shell flour modification, count by weight,
Described poly-hexanodioic acid/butylene terephthalate number-average molecular weight is 3.6 * 104;
Above-mentioned a kind of preparation method containing the poly-hexanodioic acid/butylene terephthalate matrix material of coconut shell flour modification, with embodiment 1.
Embodiment 5
Containing the poly-hexanodioic acid/butylene terephthalate matrix material of coconut shell flour modification, count by weight,
Above-mentioned a kind of preparation method containing the poly-hexanodioic acid/butylene terephthalate matrix material of coconut shell flour modification, with embodiment 1.
Embodiment 6
Containing the poly-hexanodioic acid/butylene terephthalate matrix material of coconut shell flour modification, count by weight,
Above-mentioned a kind of preparation method containing the poly-hexanodioic acid/butylene terephthalate matrix material of coconut shell flour modification, specifically comprises the steps:
Step 1, dry coconut husk is placed in pulverizer and is ground into fritter, then with ball mill, wears into powder, crosses 100 mesh sieves, obtains coconut shell flour, is then placed in 80 ℃ of vacuum drying ovens and dries.A certain amount of above-mentioned 100 order coconut shell flours are mixed with 50ml dehydrated alcohol, and ultrasonic dispersion 10min obtains finely dispersed suspension; Titanate coupling agent NZD201 is dissolved in to 50ml dehydrated alcohol; Unit for uniform suspension is mixed to the 3h that refluxes at 80 ℃ with coupling agent solution; Be cooled to room temperature, through centrifugation, in 80 ℃ of vacuum drying ovens, dry.Make coupling agent modified coconut shell flour.
Step 2, lubrication prescription calcium stearate, thermo-stabilizer epoxy soybean oil, in 80 ℃ of vacuum drying poly-hexanodioic acid/butylene terephthalate and above-mentioned steps 1, the titanate coupling agent NZD201 modification coconut shell flour of made oven dry joins normal temperature in high-speed mixer and mixes.
Step 3, the raw material mixing in step 2 is placed in twin screw extruder extruding pelletization, and extrusion temperature is 150 ℃, then applies injection moulding machine matrix material particle is injection molded into standard testing batten, standby.
Embodiment 7
Containing the poly-hexanodioic acid/butylene terephthalate matrix material of coconut shell flour modification, parts by weight meter, poly-
Above-mentioned a kind of preparation method containing the poly-hexanodioic acid/butylene terephthalate matrix material of coconut shell flour modification, with embodiment 6.
Embodiment 8
Containing the poly-hexanodioic acid/butylene terephthalate matrix material of coconut shell flour modification, count by weight,
Above-mentioned a kind of preparation method containing the poly-hexanodioic acid/butylene terephthalate matrix material of coconut shell flour modification, with embodiment 6.
Embodiment 9
Containing the poly-hexanodioic acid/butylene terephthalate matrix material of coconut shell flour modification, count by weight,
Above-mentioned a kind of preparation method containing the poly-hexanodioic acid/butylene terephthalate matrix material of coconut shell flour modification, with embodiment 6.
Embodiment 10
Containing the poly-hexanodioic acid/butylene terephthalate matrix material of coconut shell flour modification, count by weight,
Above-mentioned a kind of preparation method containing the poly-hexanodioic acid/butylene terephthalate matrix material of coconut shell flour modification, with embodiment 6.
Adopt universal electrical tension testing machine (SUN500 type, by Italian GALDABINI company, manufactured) tensile strength, the elongation at break containing the poly-hexanodioic acid/butylene terephthalate matrix material of coconut shell flour modification of the final gained of above-described embodiment 1-10 to be measured, it the results are shown in Table 1,2 and Fig. 1,2.
Table 1
Table 2
From above-mentioned table 1-2 and accompanying drawing 1-2, can find out, what this invention was prepared gathers hexanodioic acid/butylene terephthalate matrix material containing coconut shell flour modification, there is good mechanical property, and its tensile strength of material through modification has increase in various degree, meet the application requiring of general-purpose plastics, especially can reduce production costs, degradable, weaken the pressure that coconut husk causes environment as waste, and enhance productivity.
Above specific embodiments of the invention be have been described in detail, but it is just as example, the present invention is not restricted to specific embodiment described above.To those skilled in the art, any equivalent modifications that the present invention is carried out and alternative also all among category of the present invention.Therefore, equalization conversion and the modification done without departing from the spirit and scope of the invention, all should contain within the scope of the invention.
Claims (10)
1. containing the poly-hexanodioic acid/butylene terephthalate matrix material of modification of coconut shell flour, it is characterized in that, according to parts by weight, component comprises:
100 parts of poly-hexanodioic acid/butylene terephthalate;
Coconut shell flour 1-20 part.
2. matrix material according to claim 1, is characterized in that, also comprises lubricant, and described lubricant is selected from any one or a few in Zinic stearas, calcium stearate, barium stearate, aluminum stearate, Magnesium Stearate.
3. matrix material according to claim 1, is characterized in that, also comprises thermo-stabilizer, and described thermo-stabilizer is selected from any one in MALEIC ANHYDRIDE, epoxy soybean oil.
4. matrix material according to claim 1, is characterized in that, the molecular-weight average of poly-hexanodioic acid/butylene terephthalate is at least 3.6 * 10
4.
5. matrix material according to claim 1, is characterized in that, described coconut shell flour is coupling agent modified coconut shell flour, by following steps, is made:
A. coconut husk is pulverized and obtained coconut shell flour, dry;
B. the coconut shell flour after drying in step a is mixed with ethanol, ultrasonicly disperse to obtain finely dispersed suspension; In described suspension, add coupling agent; After being mixed with coupling agent, unit for uniform suspension refluxes; Separate solid, after being dried, makes coupling agent modified coconut shell flour.
6. matrix material according to claim 5, is characterized in that, described return time is 2-3 hour.
7. matrix material according to claim 5, is characterized in that, described coupling agent is selected from any one in γ-aminopropyl triethoxysilane, titanic acid ester.
8. matrix material according to claim 7, is characterized in that, described coupling agent consumption is the 0.5-5% of coconut shell flour weight.
9. a coupling agent modified coconut shell flour, is characterized in that, described coupling agent modified coconut shell flour, is made by following steps:
A. coconut husk is pulverized and obtained coconut shell flour, dry;
B. the coconut shell flour after drying in step a is mixed with ethanol, ultrasonicly disperse to obtain finely dispersed suspension; In described suspension, add coupling agent; After being mixed with coupling agent, unit for uniform suspension refluxes; Separate solid, after being dried, makes coupling agent modified coconut shell flour.
10. containing the modification of coconut shell flour, gather a preparation method for hexanodioic acid/butylene terephthalate matrix material, it is characterized in that, comprise the steps:
Step 1. will be gathered hexanodioic acid/butylene terephthalate, coconut shell flour, lubricant, thermo-stabilizer mixing, obtain mixture;
Step 2. is granulated: by the granulating mixture in step a;
Step 3. injection moulding: by the granulation injection moulding in step b, obtain the poly-hexanodioic acid/butylene terephthalate matrix material of modification containing coconut shell flour.
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Cited By (6)
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| CN106084677A (en) * | 2016-06-21 | 2016-11-09 | 上海东升新材料有限公司 | A kind of preparation method of chitin modification polyadipate/butylene terephthalate composite and products thereof |
| CN109957214A (en) * | 2017-12-14 | 2019-07-02 | 上海东升新材料有限公司 | A kind of nano-oxide and the modified polyadipate/butylene terephthalate composite material and preparation method of soybean protein isolate |
| CN110483956A (en) * | 2018-05-15 | 2019-11-22 | 上海昶法新材料有限公司 | One kind is containing the modified polyadipate/butylene terephthalate composite material and preparation method of banana bast fiber |
| CN112725933A (en) * | 2021-01-15 | 2021-04-30 | 邵阳阳光发品有限公司 | Flame-retardant composite fiber material for wig and preparation method thereof |
| CN112853535A (en) * | 2021-01-15 | 2021-05-28 | 邵阳阳光发品有限公司 | Composite fiber material for wig and preparation method thereof |
| CN115028977A (en) * | 2022-06-21 | 2022-09-09 | 惠州科碧尔生物新材料有限公司 | Blending modified sheet material prepared from natural biobased material and biodegradable raw material |
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| CN101186755A (en) * | 2007-11-20 | 2008-05-28 | 广州华工百川科技股份有限公司 | Method for preparing coconut shell and thermoplastic plastic composite material |
| CN101768333A (en) * | 2008-12-29 | 2010-07-07 | 中国林业科学研究院木材工业研究所 | Wood-plastic composite material and forming plate made of wood-plastic composite material |
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| CN101186755A (en) * | 2007-11-20 | 2008-05-28 | 广州华工百川科技股份有限公司 | Method for preparing coconut shell and thermoplastic plastic composite material |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106084677A (en) * | 2016-06-21 | 2016-11-09 | 上海东升新材料有限公司 | A kind of preparation method of chitin modification polyadipate/butylene terephthalate composite and products thereof |
| CN109957214A (en) * | 2017-12-14 | 2019-07-02 | 上海东升新材料有限公司 | A kind of nano-oxide and the modified polyadipate/butylene terephthalate composite material and preparation method of soybean protein isolate |
| CN109957214B (en) * | 2017-12-14 | 2022-03-15 | 上海东升新材料有限公司 | Nano oxide and soybean protein isolate modified poly (adipic acid)/butylene terephthalate composite material and preparation method thereof |
| CN110483956A (en) * | 2018-05-15 | 2019-11-22 | 上海昶法新材料有限公司 | One kind is containing the modified polyadipate/butylene terephthalate composite material and preparation method of banana bast fiber |
| CN112725933A (en) * | 2021-01-15 | 2021-04-30 | 邵阳阳光发品有限公司 | Flame-retardant composite fiber material for wig and preparation method thereof |
| CN112853535A (en) * | 2021-01-15 | 2021-05-28 | 邵阳阳光发品有限公司 | Composite fiber material for wig and preparation method thereof |
| CN112853535B (en) * | 2021-01-15 | 2021-12-21 | 邵阳阳光发品有限公司 | Composite fiber material for wig and preparation method thereof |
| CN112725933B (en) * | 2021-01-15 | 2022-01-18 | 邵阳阳光发品有限公司 | Flame-retardant composite fiber material for wig and preparation method thereof |
| CN115028977A (en) * | 2022-06-21 | 2022-09-09 | 惠州科碧尔生物新材料有限公司 | Blending modified sheet material prepared from natural biobased material and biodegradable raw material |
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Application publication date: 20141210 |