CN108359224A - 一种具有缓释氮肥功效的全降解地膜及其制备方法 - Google Patents
一种具有缓释氮肥功效的全降解地膜及其制备方法 Download PDFInfo
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- CN108359224A CN108359224A CN201810148542.1A CN201810148542A CN108359224A CN 108359224 A CN108359224 A CN 108359224A CN 201810148542 A CN201810148542 A CN 201810148542A CN 108359224 A CN108359224 A CN 108359224A
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- slow
- nitrogen fertilizer
- release nitrogen
- degradable mulch
- lignin
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/18—Manufacture of films or sheets
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01G—HORTICULTURE; CULTIVATION OF VEGETABLES, FLOWERS, RICE, FRUIT, VINES, HOPS OR SEAWEED; FORESTRY; WATERING
- A01G13/00—Protecting plants
- A01G13/02—Protective coverings for plants; Coverings for the ground; Devices for laying-out or removing coverings
- A01G13/0256—Ground coverings
- A01G13/0268—Mats or sheets, e.g. nets or fabrics
- A01G13/0275—Films
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- C—CHEMISTRY; METALLURGY
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- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2367/00—Characterised by the use of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Derivatives of such polymers
- C08J2367/02—Polyesters derived from dicarboxylic acids and dihydroxy compounds
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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- C08J2467/00—Characterised by the use of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Derivatives of such polymers
- C08J2467/02—Polyesters derived from dicarboxylic acids and dihydroxy compounds
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2467/00—Characterised by the use of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Derivatives of such polymers
- C08J2467/04—Polyesters derived from hydroxy carboxylic acids, e.g. lactones
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
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Abstract
本发明公开了一种具有缓释氮肥功效的全降解地膜及其制备方法,其特征在于利用氨化改性的木质素与可完全生物降解塑料共混吹膜,制得缓释氮肥的全生物降解地膜。本发明有效利用了可再生的木质素资源,同时降低了地膜制备中石油基原材料的消耗,减少了生物炼制工业和不可降解地膜带来的环境污染问题,氨化木质素作为农作物的缓释氮肥还有助于提高氮肥利用率,改良土壤,因而具有良好的环境、资源和经济效益。
Description
技术领域
本发明属于农用薄膜技术领域,具体涉及一种具有缓释氮肥功效的全降解地膜及其制备方法。
背景技术
开发降解地膜是目前世界上解决地膜污染问题的主要方向,降解地膜的使用省去了回收和处理残膜的环节,给农业生产带来了极大的便利。传统的降解地膜是由聚乙烯(PE)复合光降解剂、淀粉等制备而成,一定时期内可以崩解成地膜碎片,但地膜碎片主要由难降解的PE构成,这些碎片将长期存在于土壤中,降低土壤质量和作物产量,同时危害生态环境,因此开发可完全降解的地膜已成为现今国内外的研究热点。多种聚酯类塑料如聚对苯二甲酸/己二酸丁二醇酯(PBAT)、聚乳酸(PLA)、聚碳酸亚丙酯(PPC)、聚丁二酸/己二酸丁二醇酯(PBSA)、聚羟基烷酸酯(PHA)、聚丁二酸丁二醇酯(PBS)等已被证明具有完全生物降解性能,在自然条件下可被多种微生物及动植物体内的酶分解代谢生成二氧化碳和水。但与传统地膜相比,该类塑料制备的地膜强度低、韧性差,而且成本较高,妨碍了其向市场的大规模推广应用。
木质素是植物中储量最大的天然芳香族高分子,作为生物炼制和造纸工业的副产物,具有廉价易得、生物可降解、易于衍生化等多重优点,然而只有不到2%的工业木质素被回收利用,其余的大量木质素被焚烧或丢弃,造成大量的资源浪费和环境污染。但是木质素本身具有土壤改良和植物防腐的功效,可以转化为高附加值产品应用于农林生产领域。将木质素进行氨化改性后用作肥料,氮元素会随着木质素的降解被缓慢释放出来,大大延长了肥效时间,显著地提高氮肥的有效利用率,同时有助于降低因施肥造成的地表水富营养化、地下水污染等环境问题。
将氨化木质素与可降解塑料共混挤出吹膜,可以增强地膜的力学性能。该方法得到的地膜仍然可以完全生物降解,不仅可以减少石油基材料的消耗和生物炼制工业污染物的排放,还大大降低地膜的成本。由于氨化木质素颜色较深,可以降低地膜的透光率,有利于抑制地面杂草的生长。
发明内容
本发明要解决的技术问题是提供一种具有缓释氮肥功效的全降解地膜,以解决现有技术存在的效果不佳等问题。
本发明还要解决的技术问题是提供上述具有缓释氮肥功效的全降解地膜的制备方法。
一种具有缓释氮肥功效的全降解地膜,它包括如下质量份数的组分:
其中,优选如下质量份数的组分:
其中,所述的可降解塑料为聚对苯二甲酸/己二酸丁二醇酯(PBAT)、聚乳酸(PLA)、聚碳酸亚丙酯(PPC)、聚丁二酸/己二酸丁二醇酯(PBSA)、聚羟基烷酸酯(PHA)和聚丁二酸丁二醇酯(PBS)中的任意一种或几种的组合,优选聚对苯二甲酸/己二酸丁二醇酯(PBAT)。
其中,所述的氨化木质素为碱木质素、酶解木质素、造纸木质素、有机溶剂木质素、木质素磺酸盐中的任意一种或几种的组合经氨化后得到,粒径为100~1000目。
其中,所述的氨化方法为:
向木质素中依次加入25~28wt%的氨水、蒸馏水和30wt%双氧水,80℃下连续搅拌反应1h,干燥后粉碎得到氨化木质素;其中,木质素、氨水、蒸馏水和双氧水的质量比为2:4:8:1。
其中,所述的增塑剂为癸二酸二丁酯、三乙酸甘油酯、聚乙二醇和柠檬酸酯类增塑剂中的任意一种或几种的组合;其中,柠檬酸酯类增塑剂包括柠檬酸三丁酯、乙酰柠檬酸三丁酯和柠檬酸三乙酯。
其中,所述的扩链剂为对苯二酚二羟乙基醚、间苯二酚二羟乙基醚、双酚A、1,4-丁二醇和二异氰酸酯类扩链剂中的任意一种或几种的组合;其中,二异氰酸酯类扩链剂包括二苯基甲烷二异氰酸酯和甲苯-2,4-二异氰酸酯。
其中,所述的抗氧化剂为丁基羟基茴香醚、二丁基羟基甲苯、叔丁基对苯二酚、季戊四醇双亚磷酸酯、3-(3,5-二叔丁基-4-羟基苯基)丙酸十八碳酸酯和硫代二丙酸双月桂酯中的任意一种或几种的组合。
其中,所述的热稳定剂为顺丁烯二酸酐和/或环氧大豆油。
其中,所述的润滑剂为季戊四醇硬脂酸酯、硬脂酸锌、硬脂酸钙和油酸酰胺中的任意一种或几种的组合。
进一步的,优选如下质量份数的组分:
进一步的,优选如下质量份数的组分:
上述缓释氮肥功效的全降解地膜的制备方法,它包括如下步骤:
将配方量的可降解塑料、氨化木质素、增塑剂、扩链剂、抗氧化剂、热稳定剂和润滑剂在高混机中充分混合后,经双螺杆造粒机挤出造粒,得到氨化木质素改性的塑料复合粒子;氨化木质素改性的塑料复合粒子经吹塑成膜,即得具有缓释氮肥功效的全降解地膜。
其中,高混机中,温度为100~110℃,转速为800~1000rpm,混合时间为10~20min;挤出造粒时,温度为120~180℃;吹塑成膜时,温度为120~150℃。
有益效果:
本发明采用降解过程中具有缓释氮肥功效的氨化木质素改性的生物降解塑料制备全生物降解地膜,既有效利用了可再生的木质素资源,减少了生物炼制和造纸工业带来的环境污染问题,又可以减少石油基材料的消耗和农业生产中的白色污染问题,还有助于提高氮肥利用率,改良土壤,节肥增产,因而具有良好的环境、资源和经济效益。氨化木质素的使用还有利于提高全降解地膜的力学性能,抑制杂草的生长。由于木质素廉价易得,可以有效降低地膜的生产成本,有利于向市场推广。
具体实施方式
根据下述实施例,可以更好地理解本发明。然而,本领域的技术人员容易理解,实施例所描述的内容仅用于说明本发明,而不应当也不会限制权利要求书中所详细描述的本发明。
实施例1
具体制备方法包括以下步骤:
(1)向10重量份碱木质素依次加入20份浓度为25~28wt%氨水、40份蒸馏水、5份浓度为30wt%的双氧水,在80℃下连续搅拌反应1小时,干燥粉碎得到氨化木质素;
(2)在高混机内加入50份PBAT、20份PLA、30份步骤(1)所述的氨化木质素、0.6份柠檬酸三乙酯、0.8份双酚A、0.3份叔丁基对苯二酚、0.5份环氧大豆油、0.2份油酸酰胺,在100℃下,以1000rpm的转速,混合15min,得到混合物料;
(3)将步骤(2)所述的混合物料经双螺杆挤出造粒,控制温度为150~160℃,得到氨化木质素改性的塑料复合粒子;
(4)将步骤(3)所述的复合粒子在140~150℃下进行吹塑成膜,得到具有缓释氮肥功效的全降解地膜。
实施例2
具体制备方法包括以下步骤:
(1)向10重量份酶解木质素依次加入20份浓度为25~28wt%氨水、40份蒸馏水、4份浓度为30wt%的双氧水,在60℃下连续搅拌反应2.5小时,干燥粉碎得到氨化木质素;
(2)在高混机内加入55份PBAT、25份PBS、20份步骤(1)所述的氨化木质素、0.6份三乙酸甘油酯、0.3份二苯基甲烷二异氰酸酯、0.4份二丁基羟基甲苯、0.6份顺丁烯二酸酐、0.15份硬脂酸钙,在105℃下,以1000rpm的转速,混合15min,得到混合物料;
(3)将步骤(2)所述的混合物料经双螺杆挤出造粒,控制温度为140~150℃,得到氨化木质素改性的塑料复合粒子;
(4)将步骤(3)所述的复合粒子在130~140℃下进行吹塑成膜,得到具有缓释氮肥功效的全降解地膜。
对比例1
将实施例1中的氨化木质素用同质量的PBAT代替,参照实施例1的步骤制备的地膜作为对比例1。
性能测试
采用万能拉力机对上述实施例1、2和对比例1材料的拉伸强度进行测定,并对上述材料进行生物堆肥降解实验,具体检测结果如表1所示。
表1
拉伸强度(MPa) | 6个月堆肥降解率(%) | |
实施例1 | 32 | >99% |
实施例2 | 29 | >99% |
对比例1 | 19 | >99% |
从表1所示的测试结果中可以看出,氨化木质素改性的地膜的拉伸强度得到了显著地增强,且符合完全降解的要求。
将实施例1、2和对比例1中的地膜进行盆栽实验,周期性地对土壤中氮元素含量进行测定(对比例1组中,在实验开始前施加市售硫酸铵,其氮元素含量和实施例1地膜中氮元素含量相同),氮肥缓释情况如表2所示。
表2
时间/天 | 0 | 30 | 60 | 90 |
实施例1(mg/kg) | 0 | 12.3 | 27.9 | 44.6 |
实施例2(mg/kg) | 0 | 10.9 | 24.5 | 38.9 |
对比例1(mg/kg) | 0 | 9.8 | 10.3 | 10.4 |
表2的结果表明本发明的地膜有缓释氮肥的功效,向土壤释放氮肥能持续90天,肥效时间长。
以上对本发明的具体实施例作了详细说明,但是本发明并不限于上述实施例,因此在不脱离本发明的精神和宗旨的前提下所作的变化和修改,都应涵盖在本发明的范围内。
Claims (10)
1.一种具有缓释氮肥功效的全降解地膜,其特征在于,它包括如下质量份数的组分:
2.根据权利要求1所述的具有缓释氮肥功效的全降解地膜,其特征在于,所述的可降解塑料为聚对苯二甲酸/己二酸丁二醇酯、聚乳酸、聚碳酸亚丙酯、聚丁二酸/己二酸丁二醇酯、聚羟基烷酸酯和聚丁二酸丁二醇酯中的任意一种或几种的组合。
3.根据权利要求1所述的具有缓释氮肥功效的全降解地膜,其特征在于,所述的氨化木质素为碱木质素、酶解木质素、造纸木质素、有机溶剂木质素、木质素磺酸盐中的任意一种或几种的组合经氨化后得到,粒径为100~1000目。
4.根据权利要求1所述的具有缓释氮肥功效的全降解地膜,其特征在于,所述的增塑剂为癸二酸二丁酯、三乙酸甘油酯、聚乙二醇和柠檬酸酯类增塑剂中的任意一种或几种的组合。
5.根据权利要求1所述的具有缓释氮肥功效的全降解地膜,其特征在于,所述的扩链剂为对苯二酚二羟乙基醚、间苯二酚二羟乙基醚、双酚A、1,4-丁二醇和二异氰酸酯类扩链剂中的任意一种或几种的组合。
6.根据权利要求1所述的具有缓释氮肥功效的全降解地膜,其特征在于,所述的抗氧化剂为丁基羟基茴香醚、二丁基羟基甲苯、叔丁基对苯二酚、季戊四醇双亚磷酸酯、3-(3,5-二叔丁基-4-羟基苯基)丙酸十八碳酸酯和硫代二丙酸双月桂酯中的任意一种或几种的组合。
7.根据权利要求1所述的具有缓释氮肥功效的全降解地膜,其特征在于,所述的热稳定剂为顺丁烯二酸酐和/或环氧大豆油。
8.根据权利要求1所述的具有缓释氮肥功效的全降解地膜,其特征在于,所述的润滑剂为季戊四醇硬脂酸酯、硬脂酸锌、硬脂酸钙和油酸酰胺中的任意一种或几种的组合。
9.权利要求1所述的具有缓释氮肥功效的全降解地膜的制备方法,其特征在于,它包括如下步骤:
将配方量的可降解塑料、氨化木质素、增塑剂、扩链剂、抗氧化剂、热稳定剂和润滑剂在高混机中充分混合后,经双螺杆造粒机挤出造粒,得到氨化木质素改性的塑料复合粒子;氨化木质素改性的塑料复合粒子经吹塑成膜,即得具有缓释氮肥功效的全降解地膜。
10.根据权利要求9所述的制备方法,其特征在于,高混机中,温度为100~110℃,转速为800~1000rpm,混合时间为10~20min;挤出造粒时,温度为120~180℃;吹塑成膜时,温度为120~150℃。
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