CN106543651A - A kind of bagasse is modified the method and its product of polyadipate/butylene terephthalate composite - Google Patents

A kind of bagasse is modified the method and its product of polyadipate/butylene terephthalate composite Download PDF

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Publication number
CN106543651A
CN106543651A CN201510599995.2A CN201510599995A CN106543651A CN 106543651 A CN106543651 A CN 106543651A CN 201510599995 A CN201510599995 A CN 201510599995A CN 106543651 A CN106543651 A CN 106543651A
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China
Prior art keywords
bagasse
polyadipate
butylene terephthalate
whisker
composite
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Pending
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CN201510599995.2A
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Chinese (zh)
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施晓旦
郝鲁峰
孙振军
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Shanghai Dongsheng New Material Co Ltd
Shandong Dongsheng New Material Co Ltd
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Shanghai Dongsheng New Material Co Ltd
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Abstract

The invention provides a kind of method of the modified polyadipate/butylene terephthalate composite of bagasse, wherein, using 100 parts of polyadipate/butylene terephthalates, 1-20 part bagasse fibres, 5-10 part whiskers, 0.5-2 part lubricants, 0.1-1 part heat stabilizers are modified reaction, including step:Alkali process are carried out to bagasse first, then according to above-mentioned mass fraction charging reaction, then uniformly mixed with high speed blender, then blend is placed in double screw extruder carries out extruding pelletization.The present invention adopts Biodegradable polyester plastics polyadipate/butylene terephthalate and bagasse to prepare composite, the twice laid of bagasse not only can be realized, and enhancing polyadipate/butylene terephthalate material mechanical performance, and effectively reduces cost can be played a part of together with whisker.

Description

A kind of bagasse is modified the method and its product of polyadipate/butylene terephthalate composite
Technical field
The present invention relates to fully biodegradable field of polymer composite material, more particularly to a kind of bagasse is modified The method of polyadipate/butylene terephthalate composite, and the product prepared according to the method.
Background technology
Polyadipate/butylene terephthalate is that one kind has aliphatic polyester excellent biodegradability energy and virtue concurrently The aliphatic/aromatic copolymerization of fragrant adoption ester excellent mechanical performance, with good processing characteristics, The fields such as industrial packaging, agriculture and forestry production are with a wide range of applications.But, its tensile strength less, is limited Application of the material in the higher field of mechanical property requirements is made.Additionally, the cost of the material is of a relatively high, limit The popularization of its marketization application is made.Therefore in order to improve the comprehensive of polyadipate/butylene terephthalate material Close performance and reduce production cost, need to be modified which.
Garbage of the bagasse as industrial sucrose, is generally intended for use primarily in fuel, farmers''s compost of sugar refinery's boiler With the Feed Manufacturing of domestic animal etc..Natural plant fibre has the excellent spies such as inexpensive light weight, specific strength and specific modulus height Property, particularly Plant fiber belong to Renewable resource, can be with the characteristic of natural degradation so as to good work Industry application prospect.But, bagasse fibre has between the easy moisture absorption, fiber/base material interfacial bond property very again The shortcomings of difference.The interface performance for improving composite in order to process by fibre modification and the mechanics for improving material Performance, the present invention carry out alkali process to fiber and can obtain good effect.
The content of the invention
In order to overcome above-mentioned problems of the prior art, a first aspect of the present invention, there is provided a kind of Bagasse is modified the method for polyadipate/butylene terephthalate composite, wherein, the reaction for using Thing according to the mass fraction, including:
The method comprising the steps of:
(1) in being 1~5% alkali liquor by bagasse immersion mass concentration, with 1: 20 solid-liquid weight than mixing, 2~3h is processed at 25 DEG C, then Jing washes dealkalize, acid bath dealkalize, is washed to neutrality, bagasse is obtained after being dried Fiber is standby;
(2) whisker is mixed with 50ml dehydrated alcohol, ultrasonic disperse 10min obtains finely dispersed suspension; By in gamma-aminopropyl-triethoxy-silane coupling agent (KH550) or titanate coupling agent (NZD-201) Kind, by the 0.5% of whisker mass fraction, it is dissolved in 50ml dehydrated alcohol;By unit for uniform suspension and coupling agent solution Mix homogeneously flows back at 80 DEG C 3h;Room temperature is cooled to, is centrifuged, dried in 80 DEG C of vacuum drying ovens;
(3) will be above-mentioned whisker, bagasse fibre and polyadipate/butylene terephthalate, lubricant, heat steady Determine agent together, be placed in high speed blender and mixed;
(4) after mix homogeneously, extruding pelletization in double screw extruder is placed in, that is, obtains target product composite.
Preferably, the number-average molecular weight of the polyadipate/butylene terephthalate is 3.6 × 104
Preferably, the one kind during the whisker is selected from calcium sulfate crystal whiskers or magnesium sulfate crystal whisker.
Preferably, the one kind during the lubricant is selected from zinc stearate or calcium stearate.
Preferably, the one kind during the heat stabilizer is selected from maleic anhydride or epoxy soybean oil.
A second aspect of the present invention, there is provided the modified polyadipate of bagasse prepared by a kind of foundation said method/ Butylene terephthalate composite.
The present invention adopts Biodegradable polyester plastics polyadipate/butylene terephthalate and bagasse to prepare Composite, not only can realize the twice laid of bagasse, and can play enhancing poly- together with whisker The effect of adipic acid/butylene terephthalate material mechanical performance, and effectively reduce production cost.
Specific embodiment
With reference to specific embodiment, the present invention is further elaborated, but the present invention is not limited to following enforcement Mode.
A first aspect of the present invention, there is provided a kind of
Bagasse is modified the method for polyadipate/butylene terephthalate composite, wherein, use Reactant according to the mass fraction, including:
The method comprising the steps of:
(1) in being 1~5% alkali liquor by bagasse immersion mass concentration, with 1: 20 solid-liquid weight than mixing, 2~3h is processed at 25 DEG C, then Jing washes dealkalize, acid bath dealkalize, is washed to neutrality, bagasse is obtained after being dried Fiber is standby;
(2) whisker is mixed with 50ml dehydrated alcohol, ultrasonic disperse 10min obtains finely dispersed suspension; By in gamma-aminopropyl-triethoxy-silane coupling agent (KH550) or titanate coupling agent (NZD-201) Kind, by the 0.5% of whisker mass fraction, it is dissolved in 50ml dehydrated alcohol;By unit for uniform suspension and coupling agent solution Mix homogeneously flows back at 80 DEG C 3h;Room temperature is cooled to, is centrifuged, dried in 80 DEG C of vacuum drying ovens;
(3) will be above-mentioned whisker, bagasse fibre and polyadipate/butylene terephthalate, lubricant, heat steady Determine agent together, be placed in high speed blender and mixed;
(4) after mix homogeneously, extruding pelletization in double screw extruder is placed in, that is, obtains target product composite.
Preferably, the number-average molecular weight of the polyadipate/butylene terephthalate is 3.6 × 104
Preferably, the one kind during the whisker is selected from calcium sulfate crystal whiskers or magnesium sulfate crystal whisker.
Preferably, the one kind during the lubricant is selected from zinc stearate or calcium stearate.
Preferably, the one kind during the heat stabilizer is selected from maleic anhydride or epoxy soybean oil.
A second aspect of the present invention, there is provided the modified polyadipate of bagasse prepared by a kind of foundation said method/ Butylene terephthalate composite.
Embodiment 1
Prepare the modified polyadipate/butylene terephthalate composite of bagasse:Add by following mass fraction Enter corresponding reactant:
Above-mentioned formula is reacted according to the following steps:
(1) in being 4% alkali liquor by bagasse immersion mass concentration first, with 1: 20 solid-liquid weight than mixing, 2h is processed at 25 DEG C, then Jing washes dealkalize, acid bath dealkalize, is washed to neutrality, obtains bagasse fine after being dried Dimension is standby.
(2) whisker is mixed with 50ml dehydrated alcohol, ultrasonic disperse 10min obtains finely dispersed suspension; Gamma-aminopropyl-triethoxy-silane coupling agent (KH550) is pressed into the 0.5% of whisker mass fraction, 50ml is dissolved in Dehydrated alcohol;Unit for uniform suspension is mixed homogeneously into the 3h that flows back at 80 DEG C with coupling agent solution;It is cooled to room temperature, It is centrifuged, dries in 80 DEG C of vacuum drying ovens.
(3) by above-mentioned whisker, Caulis Sacchari sinensis fiber and polyadipate/butylene terephthalate, lubricant, thermally-stabilised Agent together, is placed in high speed blender and is mixed;
(4) after mix homogeneously, extruding pelletization in double screw extruder is placed in, that is, obtains target product composite;
(5) a small amount of above-mentioned composite particles are taken, Jing injection mo(u)ldings are obtained standard testing batten, standby, to treat Stretching detection.
Embodiment 2
Prepare the modified polyadipate/butylene terephthalate composite of bagasse:Add by following mass fraction Enter corresponding reactant:
Above-mentioned formula is reacted according to the following steps:
(1) in being 3% alkali liquor by bagasse immersion mass concentration first, with 1: 20 solid-liquid weight than mixing, 3h is processed at 25 DEG C, then Jing washes dealkalize, acid bath dealkalize, is washed to neutrality, obtains bagasse fine after being dried Dimension is standby.
(2) whisker is mixed with 50ml dehydrated alcohol, ultrasonic disperse 10min obtains finely dispersed suspension; Titanate coupling agent (NZD-201) is pressed into the 0.5% of whisker mass fraction, 50ml dehydrated alcohol is dissolved in;Will Unit for uniform suspension mixs homogeneously the 3h that flows back at 80 DEG C with coupling agent solution;Room temperature is cooled to, is centrifuged, Dry in 80 DEG C of vacuum drying ovens;
(3) by above-mentioned whisker, Caulis Sacchari sinensis fiber and polyadipate/butylene terephthalate, lubricant, thermally-stabilised Agent together, is placed in high speed blender and is mixed;
(4) after mix homogeneously, extruding pelletization in double screw extruder is placed in, that is, obtains target product composite;
(5) a small amount of above-mentioned composite particles are taken, Jing injection mo(u)ldings are obtained standard testing batten, standby, to treat Stretching detection.
Embodiment 3
Prepare the modified polyadipate/butylene terephthalate composite of bagasse:Add by following mass fraction Enter corresponding reactant:
Above-mentioned formula is reacted according to the following steps:
(1) in being 2.5% alkali liquor by bagasse immersion mass concentration first, with 1: 20 solid-liquid weight than mixed Close, 3h is processed at 25 DEG C, then Jing washes dealkalize, acid bath dealkalize, is washed to neutrality, Caulis Sacchari sinensis is obtained after being dried Slag fiber is standby.
(2) whisker is mixed with 50ml dehydrated alcohol, ultrasonic disperse 10min obtains finely dispersed suspension;Will Gamma-aminopropyl-triethoxy-silane coupling agent (KH550) presses the 0.5% of whisker mass fraction, be dissolved in 50ml without Water-ethanol;Unit for uniform suspension is mixed homogeneously into the 3h that flows back at 80 DEG C with coupling agent solution;It is cooled to room temperature, It is centrifuged, dries in 80 DEG C of vacuum drying ovens;
(3) by above-mentioned whisker, Caulis Sacchari sinensis fiber and polyadipate/butylene terephthalate, lubricant, thermally-stabilised Agent together, is placed in high speed blender and is mixed;
(4) after mix homogeneously, extruding pelletization in double screw extruder is placed in, that is, obtains target product composite;
(5) a small amount of above-mentioned composite particles are taken, Jing injection mo(u)ldings are obtained standard testing batten, standby, to treat Stretching detection.
Embodiment 4
Prepare the modified polyadipate/butylene terephthalate composite of bagasse:Add by following mass fraction Enter corresponding reactant:
Above-mentioned formula is reacted according to the following steps:
(1) in being 2% alkali liquor by bagasse immersion mass concentration first, with 1: 20 solid-liquid weight than mixing, 3h is processed at 25 DEG C, then Jing washes dealkalize, acid bath dealkalize, is washed to neutrality, obtains bagasse fine after being dried Dimension is standby.
(2) whisker is mixed with 50ml dehydrated alcohol, ultrasonic disperse 10min obtains finely dispersed suspension; Titanate coupling agent (NZD-201) is pressed into the 0.5% of whisker mass fraction, 50ml dehydrated alcohol is dissolved in;Will Unit for uniform suspension mixs homogeneously the 3h that flows back at 80 DEG C with coupling agent solution;Room temperature is cooled to, is centrifuged, Dry in 80 DEG C of vacuum drying ovens;
(3) by above-mentioned whisker, Caulis Sacchari sinensis fiber and polyadipate/butylene terephthalate, lubricant, thermally-stabilised Agent together, is placed in high speed blender and is mixed;
(4) after mix homogeneously, extruding pelletization in double screw extruder is placed in, that is, obtains target product composite;
(5) a small amount of above-mentioned composite particles are taken, Jing injection mo(u)ldings are obtained standard testing batten, standby, to treat Stretching detection.
Stretching detection
With unmodified polyadipate/butylene terephthalate consumption/part as comparative example, drawn using universal electrical Force tester (SUN500 types, by Italian GALDABINI companies manufacture) to above-described embodiment 1-4 most The tensile strength of preparation-obtained batten, elongation at break are measured eventually, and which is the results are shown in Table shown in 1:
Tensile strength/MPa Elongation at break/%
Embodiment 1 41.5 321.4
Embodiment 2 36.4 361.8
Embodiment 3 39.2 348.6
Embodiment 4 29.0 333.5
Comparative example 22.1 316.0
Table 1
, polyadipate/to benzene two modified through bagasse fibre is can be seen that by the data result of table 1 The mechanical property of formic acid fourth diester is obviously improved.
Above the specific embodiment of the present invention has been described in detail, but, which is intended only as example, this It is bright to be not restricted to particular embodiments described above.To those skilled in the art, it is any to the present invention The equivalent modifications for carrying out and replacement are also all among scope of the invention.Therefore, in the essence without departing from the present invention The impartial conversion made under god and scope and modification, should all cover within the scope of the invention.

Claims (6)

1. the method for the modified polyadipate/butylene terephthalate composite of a kind of bagasse, wherein, use Reactant according to the mass fraction, including:
The method comprising the steps of:
(1) in being 1~5% alkali liquor by bagasse immersion mass concentration, with 1: 20 solid-liquid weight than mixing, 2~3h is processed at 25 DEG C, then Jing washes dealkalize, acid bath dealkalize, is washed to neutrality, bagasse is obtained after being dried Fiber is standby;
(2) whisker is mixed with 50ml dehydrated alcohol, ultrasonic disperse 10min obtains finely dispersed suspension; By in gamma-aminopropyl-triethoxy-silane coupling agent (KH550) or titanate coupling agent (NZD-201) Kind, by the 0.5% of whisker mass fraction, it is dissolved in 50ml dehydrated alcohol;By unit for uniform suspension and coupling agent solution Mix homogeneously flows back at 80 DEG C 3h;Room temperature is cooled to, is centrifuged, dried in 80 DEG C of vacuum drying ovens;
(3) will be above-mentioned whisker, bagasse fibre and polyadipate/butylene terephthalate, lubricant, heat steady Determine agent together, be placed in high speed blender and mixed;
(4) after mix homogeneously, extruding pelletization in double screw extruder is placed in, that is, obtains target product composite.
2. method according to claim 1, it is characterised in that the polyadipate/butylene terephthalate Number-average molecular weight be 3.6 × 104
3. method according to claim 1, it is characterised in that the whisker is selected from calcium sulfate crystal whiskers or sulphuric acid One kind in magnesium whisker.
4. method according to claim 1, it is characterised in that the lubricant is selected from zinc stearate or Hard Fat One kind in sour calcium.
5. method according to claim 1, it is characterised in that the heat stabilizer is selected from maleic anhydride Or the one kind in epoxy soybean oil.
6. the modified polyadipate/p-phthalic acid fourth two of bagasse for being prepared according to any one of the claims method Ester composite.
CN201510599995.2A 2015-09-18 2015-09-18 A kind of bagasse is modified the method and its product of polyadipate/butylene terephthalate composite Pending CN106543651A (en)

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Cited By (7)

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CN109666266A (en) * 2017-10-13 2019-04-23 上海东升新材料有限公司 One kind is containing the modified polyadipate/butylene terephthalate composite material and preparation method of bi-component fibres
CN110483955A (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 pina fibre
CN110498653A (en) * 2019-09-27 2019-11-26 浙江寰龙环境科技有限公司 A kind of water-permeable brick and its preparation process of high-intensitive high infiltration
CN110540741A (en) * 2019-09-23 2019-12-06 济南圣泉集团股份有限公司 Degradable composite material and preparation method and application thereof
CN112358712A (en) * 2020-12-07 2021-02-12 深圳市裕同包装科技股份有限公司 Bagasse fiber/PHA (polyhydroxyalkanoate) completely-degradable composite material and preparation method thereof
WO2021199839A1 (en) * 2020-03-30 2021-10-07 宇部マテリアルズ株式会社 Biodegradable resin composition
CN114437524A (en) * 2022-02-07 2022-05-06 天津科技大学 Preparation method of sugarcane cellulose-based degradable composite material

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CN101914241A (en) * 2010-08-04 2010-12-15 孙卫东 Formula of special material for cases of electrocars and motorcycles
CN103421286A (en) * 2013-08-08 2013-12-04 华南理工大学 High temperature resistant and degradable polylactic acid wood plastic material and preparation method thereof
CN105820522A (en) * 2016-04-01 2016-08-03 安徽理工大学 Calcium sulfate whisker reinforced and toughened polylactic acid composite and preparation method thereof

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CN101914241A (en) * 2010-08-04 2010-12-15 孙卫东 Formula of special material for cases of electrocars and motorcycles
CN103421286A (en) * 2013-08-08 2013-12-04 华南理工大学 High temperature resistant and degradable polylactic acid wood plastic material and preparation method thereof
CN105820522A (en) * 2016-04-01 2016-08-03 安徽理工大学 Calcium sulfate whisker reinforced and toughened polylactic acid composite and preparation method thereof

Cited By (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109666266A (en) * 2017-10-13 2019-04-23 上海东升新材料有限公司 One kind is containing the modified polyadipate/butylene terephthalate composite material and preparation method of bi-component fibres
CN110483955A (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 pina fibre
CN110540741A (en) * 2019-09-23 2019-12-06 济南圣泉集团股份有限公司 Degradable composite material and preparation method and application thereof
CN110498653A (en) * 2019-09-27 2019-11-26 浙江寰龙环境科技有限公司 A kind of water-permeable brick and its preparation process of high-intensitive high infiltration
WO2021199839A1 (en) * 2020-03-30 2021-10-07 宇部マテリアルズ株式会社 Biodegradable resin composition
JPWO2021199839A1 (en) * 2020-03-30 2021-10-07
CN115315484A (en) * 2020-03-30 2022-11-08 宇部材料工业株式会社 Biodegradable resin composition
JP7421635B2 (en) 2020-03-30 2024-01-24 宇部マテリアルズ株式会社 Biodegradable resin composition
CN112358712A (en) * 2020-12-07 2021-02-12 深圳市裕同包装科技股份有限公司 Bagasse fiber/PHA (polyhydroxyalkanoate) completely-degradable composite material and preparation method thereof
CN114437524A (en) * 2022-02-07 2022-05-06 天津科技大学 Preparation method of sugarcane cellulose-based degradable composite material
CN114437524B (en) * 2022-02-07 2023-09-19 天津科技大学 Preparation method of sugarcane cellulose-based degradable composite material

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