CN115316398B - 一种腐植酸型抗菌缓释除草剂及其制备方法 - Google Patents
一种腐植酸型抗菌缓释除草剂及其制备方法 Download PDFInfo
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- CN115316398B CN115316398B CN202211044419.8A CN202211044419A CN115316398B CN 115316398 B CN115316398 B CN 115316398B CN 202211044419 A CN202211044419 A CN 202211044419A CN 115316398 B CN115316398 B CN 115316398B
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- herbicide
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- carboxymethyl cellulose
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Classifications
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N57/00—Biocides, pest repellants or attractants, or plant growth regulators containing organic phosphorus compounds
- A01N57/18—Biocides, pest repellants or attractants, or plant growth regulators containing organic phosphorus compounds having phosphorus-to-carbon bonds
- A01N57/20—Biocides, pest repellants or attractants, or plant growth regulators containing organic phosphorus compounds having phosphorus-to-carbon bonds containing acyclic or cycloaliphatic radicals
-
- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N37/00—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom having three bonds to hetero atoms with at the most two bonds to halogen, e.g. carboxylic acids
- A01N37/44—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom having three bonds to hetero atoms with at the most two bonds to halogen, e.g. carboxylic acids containing at least one carboxylic group or a thio analogue, or a derivative thereof, and a nitrogen atom attached to the same carbon skeleton by a single or double bond, this nitrogen atom not being a member of a derivative or of a thio analogue of a carboxylic group, e.g. amino-carboxylic acids
- A01N37/50—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom having three bonds to hetero atoms with at the most two bonds to halogen, e.g. carboxylic acids containing at least one carboxylic group or a thio analogue, or a derivative thereof, and a nitrogen atom attached to the same carbon skeleton by a single or double bond, this nitrogen atom not being a member of a derivative or of a thio analogue of a carboxylic group, e.g. amino-carboxylic acids the nitrogen atom being doubly bound to the carbon skeleton
-
- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N43/00—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds
- A01N43/02—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with one or more oxygen or sulfur atoms as the only ring hetero atoms
- A01N43/04—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with one or more oxygen or sulfur atoms as the only ring hetero atoms with one hetero atom
- A01N43/14—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with one or more oxygen or sulfur atoms as the only ring hetero atoms with one hetero atom six-membered rings
- A01N43/16—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with one or more oxygen or sulfur atoms as the only ring hetero atoms with one hetero atom six-membered rings with oxygen as the ring hetero atom
-
- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01P—BIOCIDAL, PEST REPELLANT, PEST ATTRACTANT OR PLANT GROWTH REGULATORY ACTIVITY OF CHEMICAL COMPOUNDS OR PREPARATIONS
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01P—BIOCIDAL, PEST REPELLANT, PEST ATTRACTANT OR PLANT GROWTH REGULATORY ACTIVITY OF CHEMICAL COMPOUNDS OR PREPARATIONS
- A01P13/00—Herbicides; Algicides
-
- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01P—BIOCIDAL, PEST REPELLANT, PEST ATTRACTANT OR PLANT GROWTH REGULATORY ACTIVITY OF CHEMICAL COMPOUNDS OR PREPARATIONS
- A01P3/00—Fungicides
-
- C—CHEMISTRY; METALLURGY
- C05—FERTILISERS; MANUFACTURE THEREOF
- C05G—MIXTURES OF FERTILISERS COVERED INDIVIDUALLY BY DIFFERENT SUBCLASSES OF CLASS C05; MIXTURES OF ONE OR MORE FERTILISERS WITH MATERIALS NOT HAVING A SPECIFIC FERTILISING ACTIVITY, e.g. PESTICIDES, SOIL-CONDITIONERS, WETTING AGENTS; FERTILISERS CHARACTERISED BY THEIR FORM
- C05G3/00—Mixtures of one or more fertilisers with additives not having a specially fertilising activity
- C05G3/60—Biocides or preservatives, e.g. disinfectants, pesticides or herbicides; Pest repellants or attractants
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A50/00—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
- Y02A50/30—Against vector-borne diseases, e.g. mosquito-borne, fly-borne, tick-borne or waterborne diseases whose impact is exacerbated by climate change
Landscapes
- Life Sciences & Earth Sciences (AREA)
- Pest Control & Pesticides (AREA)
- Plant Pathology (AREA)
- Zoology (AREA)
- Engineering & Computer Science (AREA)
- Environmental Sciences (AREA)
- Wood Science & Technology (AREA)
- Chemical & Material Sciences (AREA)
- General Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Agronomy & Crop Science (AREA)
- Health & Medical Sciences (AREA)
- Dentistry (AREA)
- General Health & Medical Sciences (AREA)
- Organic Chemistry (AREA)
- Microbiology (AREA)
- Mycology (AREA)
- Agricultural Chemicals And Associated Chemicals (AREA)
Abstract
本发明涉及农药应用的技术领域,具体公开了一种腐植酸型抗菌缓释除草剂及其制备方法,缓释除草剂的制备方法包括以下步骤:将腐植酸溶解至去离子水中,并加入改性羧甲基纤维素钠、聚乙烯亚胺,在45‑55℃下搅拌得到混合液;将混合液升温后加入乙二醇反应,再加入除草剂、营养液反应后得到预制溶液,向预制溶液中加入致孔剂,超声分散后得到溶液A;将边搅拌边向FeCl3溶液中滴加溶液A,得到缓释凝胶球;将缓释凝胶球用去离子水洗涤后,经冷冻干燥得到缓释除草剂;且改性羧甲基纤维素钠由羧甲基纤维素钠经β‑二羰基化合物、胺类化合物改性得到,改性羧甲基纤维素钠具有席夫碱结构。本发明一种腐植酸型抗菌缓释除草剂能同时实现抗菌、除草,提高除草性能。
Description
技术领域
本发明涉及农药应用的技术领域,更具体地说,它涉及一种腐植酸型抗菌缓释除草剂及其制备方法。
背景技术
农田中广泛存在着杂草、细菌、真菌等物质,但是这些物质的存在会对农作物生长、乃至农田周边的环境带来很多的不利影响。
其中,杂草具有非常旺盛的生命力和繁殖力,通常会引起以下问题:1)侵占空间:杂草会占领地上和地下的空间,影响作物的光合作用,干扰作物生长,并且早期生产中,杂草的种子数量远远超过作物的播种量,加上出苗早,速度快,容易形成草荒;2)争夺养分:杂草会和作物争夺田地里的水分和营养成分,它们的根系极为庞大,本该属于作物的营养物质会被他们掠夺,导致作物前期生长不良,后期减产;3)传播病虫害:杂草是作物病害虫害的中间寄主,由于他们生命力旺盛,且多为两年生或多年生植物,所以病菌及害虫常常先在杂草上寄生或过冬,待作物长出后再继续为害;4)影响水利设施:杂草长满水渠后会使流速减缓,泥沙淤积,且为鼠类栖息提供条件,使渠坝受损;5)危害人体健康:部分杂草会产生毒素,当他们混入被收获的农作物中,会随着农产品进入市场,当人食用后可能会出中毒情况,家畜吃了具有毒性的杂草后也会中毒。
同样,一些细菌、真菌的存在也会带来许多危害,例如:1)斑点:植物由假单孢杆菌侵染引起的病害中,有相当数量呈斑点状,如水稻细菌性褐斑病、黄瓜细菌性角斑病、棉花细菌性角斑病等;2)叶枯:多数由黄单孢杆菌侵染引起,植物受侵染后最终导致叶片枯萎,如稻白叶枯病、黄瓜细菌性叶枯病、魔芋细菌性叶枯病等;3)青枯:一般由假单孢杆菌侵染植物维管束,阻塞输导通路,致使植物茎、叶枯萎,如番茄青枯病、马铃薯枯病、草莓青枯病等;4)溃疡:一般由黄单孢杆菌侵染植物所致,后期病斑木栓化,边缘隆起,中心凹陷呈溃疡状,如柑桔溃疡病、菜用大豆细菌性斑疹病、番茄果实细菌性斑疹病等;5)腐烂:多数由欧文氏杆菌侵染植物后引起腐烂,如白菜细菌性软腐病、茄科及葫芦科作物的细菌性软腐病、以及水稻基腐病等;6)畸型:由癌肿野杆菌侵染所致,使植物的根、根颈成侧根以及枝杆上造成畸形,呈瘤肿状,如菊花根癌病等。
由此可见,发展安全低毒高效的除草剂和抗菌剂对于农作物产量、环境保护、动植物及人的健康成长具有重要意义。
发明内容
为了同时实现除草和抗菌,以进一步提升除草性能,从而有效改善农作物生长环境,本发明提供一种腐植酸型抗菌缓释除草剂及其制备方法。
第一方面,本发明提供一种腐植酸型抗菌缓释除草剂的制备方法,采用以下技术方案:
一种腐植酸型抗菌缓释除草剂的制备方法,包括以下步骤:
1)采用溶胶凝胶法制备缓释凝胶材料:将腐植酸溶解至去离子水中得到基础溶液,向基础溶液中加入改性羧甲基纤维素钠、聚乙烯亚胺,并在45-55℃下搅拌20-30min得到混合液;将混合液升温至60-70℃后加入乙二醇,反应1-2h后再加入除草剂、营养液反应2-3h后得到预制溶液,向预制溶液中加入致孔剂,超声分散30-45min后得到溶液A;
且以腐植酸的质量为1份计,所述去离子水质量为25-30份,改性羧甲基纤维素钠质量为6-9份,聚乙烯亚胺质量为0.8-1份,乙二醇质量为0.3-0.6份,除草剂2-4份,营养液2-4份、致孔剂0.2-0.3份;
其中所述改性羧甲基纤维素钠由羧甲基纤维素钠经β-二羰基化合物、胺类化合物改性得到,且所述改性羧甲基纤维素钠具有席夫碱结构;
2)制备缓释凝胶球:将边搅拌边向FeCl3溶液中滴加溶液A,得到缓释凝胶球;
3)制备缓释除草剂:将缓释凝胶球用去离子水洗涤3-5次后,经冷冻干燥得到腐植酸型抗菌缓释除草剂。
进一步的,所述改性羧甲基纤维素钠由包括以下步骤的方法制备得到:
步骤一:将羧甲基纤维素钠溶于有机溶剂,在75-85℃下反应30-45min得到基础有机溶液;将基础有机溶液降温至50-65℃后加入催化剂,并恒温搅拌2-3h得到有机溶液;再将有机溶液升温至75-85℃后,逐滴加入β-二羰基化合物,搅拌4-5h后冷却,萃取得到样品后洗涤干燥粉碎得到固体;
且以羧甲基纤维素钠的质量为1份计,所述有机溶剂质量为25-30份,催化剂质量为0.5-1份,β-二羰基化合物质量为4-7份;
步骤二:将固体溶解至去离子水中后,加入对甲苯磺酸(TsOH)得到基液,在55-65℃下边搅拌边向基液中滴加胺类化合物,反应3-4h后冷却至室温,真空抽滤得到改性羧甲基纤维素钠;
且以产品质量为1份计,所述去离子水质量为20-30份,对甲苯磺酸质量为0.4-0.6份,胺类化合物质量为1-3份。
进一步的,所述步骤一中有机溶剂为二甲基乙酰胺(DMAC)、二甲基甲酰胺(DMF)、二甲基亚砜(DMSO)、丙酮、氯仿有机溶剂中的1种。
进一步的,所述步骤一中的催化剂为LiCl。
进一步的,所述步骤一中的β-二羰基化合物为乙酰乙酸叔丁酯、乙酰乙酸乙酯、乙酰丙酸甲酯、乙酰丙酸乙酯、乙酰丙酸丁酯中的一种。
进一步的,所述步骤二中的胺类化合物为乙酰胺、甲胺、苯胺、乙二胺、丙胺中的一种。
进一步的,所述制备缓释凝胶材料的步骤中,除草剂为磺酰脲类除草剂、有机磷类除草剂中的一种。
进一步的,所述制备缓释凝胶材料的步骤中,致孔剂为草木灰、碳酸钾、碳酸钙、聚乙二醇(PEG)、聚乙烯吡咯烷酮(PVP)中的一种或几种。
进一步的,所述制备缓释除草剂的步骤中,冷冻干燥时间为24h。
第二方面,本发明提供一种腐植酸型抗菌缓释除草剂,采用以下技术方案:
一种腐植酸型抗菌缓释除草剂,采用上述制备方法制备得到。
综上所述,本发明具有以下有益效果:
为了同时实现除草和抗菌、进一步提高除草剂的除草性能,本发明通过对羧甲基纤维素钠(CMC)的改性,旨在制备一种结构稳定性好、绿色环保缓释除草剂。
本发明一种腐植酸型抗菌缓释除草剂的制备方法中,首先将羧甲基纤维素钠乙酰乙酸化引入羰基,再将其与氨基反应,生成席夫碱化合物,得到改性羧甲基纤维素钠,改性后得到的改性羧甲基纤维素钠,具备席夫碱结构,而席夫碱具有抑菌、杀菌、抗肿瘤、抗病毒的生物活性,使得改性羧甲基纤维素钠在保持原有的性能的同时有了一定的抗菌能力;
再将改性羧甲基纤维素钠与腐植酸、聚乙烯亚胺、乙二醇等物质共混,同时加入除草剂、营养液等物质,充分混合均匀后滴入FeCl3溶液当中形成凝胶球,缓释凝胶球的抗菌性与除草性相互协同,使得制备得到的缓释除草剂同时达到更好的抗菌、除草作用。
农药进行人工的直接喷施会使人吸入农药对人体造成伤害,同时喷施的农药会随风飘散,引起空气污染等,并且一次性施用浓度高,可能会对作物造成伤害,浓度低则需要多次喷施费时费力。本发明中的缓释除草剂使用方便,不会随风飘散,制备所用材料均可降解,不会对环境造成污染,同时农药从凝胶体系当中缓慢释放出来,既不会浓度过高对作物产生危害,又避免了重复施药,节约人力物力。
本发明缓释农药中,凝胶球结构为改性羧甲基纤维素钠中所含有的羧基与FeCl3溶液中的铁离子交联形成三维网络结构,是一种具有大量孔隙的结构。本发明缓释农药制备过程中,将除草剂与改性羧甲基纤维素充分混和均匀,待凝胶球形成后除草剂镶即可嵌于三维网络结构的孔隙之中,再经过冷冻干燥后,使得除草剂紧密镶嵌其中。施用时凝胶球会吸收土壤中的水分,从而吸水溶胀,溶胀后的凝胶球将其中的除草剂释放出来,凝胶球缓慢吸水溶胀,从而除草剂缓慢的释放,达到缓释效果。以此,本发明制备得到的缓释农药在除草和抗菌的效果上,能够有效延长使用时间,达到更好的除草的效果。
如此,本发明一种腐植酸型抗菌缓释除草剂能够在有效除草的同时达到一定的抗菌性,从而进一步提升除草性能。
具体实施方式
以下结合实施例对本发明的具体内容做进一步详细解释说明,予以特别说明的是:以下实施例中未注明具体条件者,按照常规条件或制造商建议的条件进行,以下实施例中所用原料除特殊说明外均可来源于普通市售。
本发明中营养液由以下原料混合得到:四水硝酸钙0.4g/L,硝酸钾0.35g/L,磷酸二氢铵0.2g/L,七水硫酸镁0.15g/L,营养液中各原料具体用量根据植物需要进行调整。
实施例
实施例1
一种腐植酸型抗菌缓释除草剂的制备方法,包括以下步骤:
1)将1份羧甲基纤维素钠溶于25份二甲基乙酰胺(DMAC),置于三口烧瓶当中,在油浴中进行活化,温度控制在75℃,时长为30min;降温至50℃,加入0.5份LiCl,恒温下磁力搅拌2h;再升温至75℃,逐滴加入4份乙酰乙酸叔丁酯,搅拌4h后冷却,通过索氏提取法提取样品,并洗涤干燥粉碎备用;
2)将1份步骤1)中制备得到的产品充分溶解于20份去离子水中,并加入0.4份对甲苯磺酸(TsOH),在55℃下,缓慢滴入1份乙酰胺,边加边搅拌,反应3h后冷却至室温,真空抽滤,得到改性羧甲基纤维素钠;
3)采用溶胶凝胶法制备缓释凝胶材料,向1份腐植酸加25份去离子水充分溶解后加入6份改性羧甲基纤维素钠、0.8份聚乙烯亚胺,在45℃下,磁力搅拌机中搅拌20min,充分混合均匀、活化;升温至60℃,加入0.3份乙二醇,反应1h后加入2份苄嘧磺隆、2份营养液,再反应2h后加入0.2份草木灰,超声分散30min后,得到溶液A备用;
4)步骤3)中制备所得的溶液A缓慢滴加到FeCl3溶液当中,边滴边搅拌,得到缓释凝胶球。
5)将步骤4)中所制得的缓释凝胶球用去离子水洗涤3次后,经冷冻干燥24h,得到腐植酸型抗菌缓释除草剂。
实施例2
一种腐植酸型抗菌缓释除草剂的制备方法,包括以下步骤:
1)将1份羧甲基纤维素钠溶于30份二甲基乙酰胺(DMAC),置于三口烧瓶当中,在油浴中进行活化,温度控制在80℃,时长为30min;降温至60℃,加入1份LiCl,恒温下磁力搅拌3h;再升温至75℃,逐滴加入7份乙酰乙酸叔丁酯,搅拌5h后冷却,通过索氏提取法提取样品,并洗涤干燥粉碎备用;
2)将1份步骤1)中制备得到的产品充分溶解于30份去离子水中,并加入0.6份对甲苯磺酸(TsOH),在65℃下,缓慢滴入3份乙酰胺,边加边搅拌,反应4h后冷却至室温,真空抽滤,得到改性羧甲基纤维素钠;
3)采用溶胶凝胶法制备缓释凝胶材料,向1份腐植酸加30份去离子水充分溶解后加入9份改性羧甲基纤维素钠、1份聚乙烯亚胺,在55℃下,磁力搅拌机中搅拌30min,充分混合均匀、活化;升温至60℃,加入0.6份乙二醇,反应1h后加入4份草甘膦、4份营养液,再反应3h后加入0.3份碳酸钾,超声分散45min后,得到溶液A备用;
4)步骤3)中制备所得的溶液A缓慢滴加到FeCl3溶液当中,边滴边搅拌,得到缓释凝胶球;
5)将步骤4)中所制得的缓释凝胶球用去离子水洗涤5次后,经冷冻干燥24h,得到腐植酸型抗菌缓释除草剂。
实施例3
一种腐植酸型抗菌缓释除草剂的制备方法,包括以下步骤:
1)将1份羧甲基纤维素钠溶于27份二甲基甲酰胺(DMF),置于三口烧瓶当中,在油浴中进行活化,温度控制在75℃,时长为45min。降温至55℃,加入0.6份LiCl,恒温下磁力搅拌2h;再升温至75℃,逐滴加入5份乙酰乙酸乙酯,搅拌4h后冷却,通过索氏提取法提取样品,并洗涤干燥粉碎备用;
2)将1份步骤1)中制备得到的产品充分溶解于25份去离子水中,并加入0.4份对甲苯磺酸(TsOH),在55℃下,缓慢滴入1份乙二胺,边加边搅拌,反应3h后冷却至室温,真空抽滤,得到改性羧甲基纤维素钠;
3)采用溶胶凝胶法制备缓释凝胶材料,向1份腐植酸加27份去离子水充分溶解后加入6份改性羧甲基纤维素钠、1份聚乙烯亚胺,在50℃下,磁力搅拌机中搅拌30min,充分混合均匀、活化;升温至60℃,加入0.4份乙二醇,反应1h后加入3份苄嘧磺隆、2份营养液,再反应2h后加入0.2份碳酸钙,超声分散30min后,得到溶液A备用;
4)步骤3)中制备所得的溶液A缓慢滴加到FeCl3溶液当中,边滴边搅拌,得到缓释凝胶球;
5)将步骤4)中所制得的缓释凝胶球用去离子水洗涤5次后,经冷冻干燥24h,得到腐植酸型抗菌缓释除草剂。
实施例4
一种腐植酸型抗菌缓释除草剂的制备方法,包括以下步骤:
1)将1份羧甲基纤维素钠溶于28份二甲基亚砜(DMSO),置于三口烧瓶当中,在油浴中进行活化,温度控制在85℃,时长为30min;降温至65℃,加入0.7份LiCl,恒温下磁力搅拌2h;再升温至85℃,逐滴加入6份乙酰丙酸乙酯,搅拌4h后冷却,通过索氏提取法提取样品,并洗涤干燥粉碎备用;
2)将1份步骤1)中制备得到的产品充分溶解于30份去离子水中,并加入0.4份对甲苯磺酸(TsOH),在60℃下,缓慢滴入1份甲胺,边加边搅拌,反应4h后冷却至室温,真空抽滤,得到改性羧甲基纤维素钠;
3)采用溶胶凝胶法制备缓释凝胶材料,向1份腐植酸加25份去离子水充分溶解后加入7份改性羧甲基纤维素钠、1份聚乙烯亚胺,在50℃下,磁力搅拌机中搅拌25min,充分混合均匀、活化;升温至70℃,加入0.5份乙二醇,反应2h后加入3份草甘膦、4份营养液,再反应2h后加入0.2份致孔剂,超声分散45min后,得到溶液A备用;
4)步骤3)中制备所得的溶液A缓慢滴加到FeCl3溶液当中,边滴边搅拌,得到缓释凝胶球;
5)将步骤4)中所制得的缓释凝胶球用去离子水洗涤3次后,经冷冻干燥24h,得到腐植酸型抗菌缓释除草剂。
实施例5
一种腐植酸型抗菌缓释除草剂的制备方法,包括以下步骤:
1)将1份羧甲基纤维素钠溶于25份丙酮,置于三口烧瓶当中,在油浴中进行活化,温度控制在80℃,时长为40min;降温至55℃,加入0.6份LiCl,恒温下磁力搅拌2h;再升温至75℃,逐滴加入4份乙酰丙酸甲酯,搅拌4h后冷却,通过索氏提取法提取样品,并洗涤干燥粉碎备用;
2)将1份步骤1)中制备得到的产品充分溶解于28份去离子水中,并加入0.5份对甲苯磺酸(TsOH),在60℃下,缓慢滴入2份苯胺,边加边搅拌,反应3h后冷却至室温,真空抽滤,得到改性羧甲基纤维素钠;
3)采用溶胶凝胶法制备缓释凝胶材料,向1份腐植酸加26份去离子水充分溶解后加入8份改性羧甲基纤维素钠、0.9份聚乙烯亚胺,在50℃下,磁力搅拌机中搅拌25min,充分混合均匀、活化;升温至60℃,加入0.5份乙二醇,反应1h后加入2份苄嘧磺隆、3份营养液,再反应3h后加入0.2份聚乙二醇(PEG),超声分散30min后,得到溶液A备用;
4)步骤3)中制备所得的溶液A缓慢滴加到FeCl3溶液当中,边滴边搅拌,得到缓释凝胶球;
5)将步骤4)中所制得的缓释凝胶球用去离子水洗涤3次后,经冷冻干燥24h,得到腐植酸型抗菌缓释除草剂。
实施例6
一种腐植酸型抗菌缓释除草剂的制备方法,包括以下步骤:
1)将1份羧甲基纤维素钠溶于25份氯仿,置于三口烧瓶当中,在油浴中进行活化,温度控制在75℃,时长为38min;降温至60℃,加入0.7份LiCl,恒温下磁力搅拌2h;再升温至75℃,逐滴加入5份乙酰丙酸丁酯,搅拌5h后冷却,通过索氏提取法提取样品,并洗涤干燥粉碎备用;
2)将1份步骤1)中制备得到的产品充分溶解于25份去离子水中,并加入0.4份对甲苯磺酸(TsOH),在55℃下,缓慢滴入1份丙胺,边加边搅拌,反应3-4h后冷却至室温,真空抽滤,得到改性羧甲基纤维素钠;
3)采用溶胶凝胶法制备缓释凝胶材料,向1份腐植酸加29份去离子水充分溶解后加入8份改性羧甲基纤维素钠、1份聚乙烯亚胺,在50℃下,磁力搅拌机中搅拌30min,充分混合均匀、活化;升温至60℃,加入0.6份乙二醇,反应1h后加入3份草甘膦、2份营养液,再反应2h后加入0.2份聚乙烯吡咯烷酮(PVP),超声分散45min后,得到溶液A备用;
4)步骤3)中制备所得的溶液A缓慢滴加到FeCl3溶液当中,边滴边搅拌,得到缓释凝胶球;
5)将步骤4)中所制得的缓释凝胶球用去离子水洗5次后,经冷冻干燥24h,得到腐植酸型抗菌缓释除草剂。
性能检测
(一)一种腐植酸型抗菌缓释除草剂的除草应用测试
采用小杯法测试化合物的生物活性,反枝苋和狗尾草为供试植株:取同质量的实施例1-6置于pH=7.4的缓冲溶液中得到供试物溶液,将供试植物反枝苋和狗尾草种子清水浸泡24h,置于25℃培养箱中催芽至露白,选取大小一致的种子10颗置于小烧杯中。移取供试物溶液缓缓加入到小烧杯中,用保湿膜覆盖小烧杯并在保湿膜上随机扎孔,以保证透气性;将小烧杯置于24-26℃的光照培养箱中培养,10d后测定供试植株的根长和茎长。
实验设置有草甘膦作为供试物溶液的对照组。
表1不同实施例的除草活性
表1数据表明,本发明所制备得到的缓释农药有着良好的除草性能,提升了原有除草剂的除草效果。
(二)一种腐植酸型抗菌缓释除草剂的抗菌应用测试
测试采用滤纸片法:将上述实施例1-6所制除草剂放入分别放入加有菌种的培养皿中,于恒温培养箱中25℃恒温培养,7天后观察生长情况并测量抑制圈的大小(菌种生长形成多个菌落,每个菌落周围有一个不长菌落的透明圈,即为抑菌圈),以比较杀菌剂的毒力,所用菌种为金色葡萄球菌。
活性物对细菌抑制效果记载方法:5级:抑菌圈直径径大于20mm,有明显抑菌效果;4级:抑菌圈直径16~20mm,有较强抑菌效果;3级:抑菌圈直径13~16mm,有抑菌效果;2级:抑菌圈直径10~13mm,抑菌效果不明显;1级:抑菌圈直径7~10mm,抑菌效果微弱;0级:7mm(滤纸片直径),同于不含除草剂的空白对照。测量抑菌圈直径的方法是十字交叉测量2次,取平均值。
表2不同实施例的抑菌效果
表2数据表明,本发明所制备得到的缓释除草剂有抑菌效果,且抑菌效果较好,除草剂的抑菌性协同除草性,使得缓释除草剂整体的应用性能优于原有的除草剂。
由表1、表2的应用测试数据可知,实施例2中所制备的缓释除草剂效果最好,其改性羧甲基纤维素钠的反应方程如下:
以上内容是对本发明所作的进一步详细说明,不能认定本发明的具体实施方式仅限于此,对于本发明所属技术领域的普通技术人员来说,在不脱离本发明构思的前提下,还可以做出若干简单的推演或替换,都应当视为属于本发明由所提交的权利要求书确定保护范围。
Claims (3)
1.一种腐植酸型抗菌缓释除草剂的制备方法,其特征在于,包括以下步骤:
1)采用溶胶凝胶法制备缓释凝胶材料:将腐植酸溶解至去离子水中得到基础溶液,向基础溶液中加入改性羧甲基纤维素钠、聚乙烯亚胺,并在45-55℃下搅拌20-30min得到混合液;将混合液升温至60-70℃后加入乙二醇,反应1-2h后再加入除草剂、营养液反应2-3h后得到预制溶液,向预制溶液中加入致孔剂,超声分散30-45min后得到溶液A;除草剂为磺酰脲类除草剂、有机磷类除草剂中的一种;致孔剂为草木灰、碳酸钾、碳酸钙、聚乙二醇、聚乙烯吡咯烷酮中的一种或几种;
且以腐植酸的质量为1份计,所述去离子水质量为25-30份,改性羧甲基纤维素钠质量为6-9份,聚乙烯亚胺质量为0.8-1份,乙二醇质量为0.3-0.6份,除草剂2-4份,营养液2-4份、致孔剂0.2-0.3份;
其中所述改性羧甲基纤维素钠由羧甲基纤维素钠经β-二羰基化合物、胺类化合物改性得到,且所述改性羧甲基纤维素钠具有席夫碱结构;
所述改性羧甲基纤维素钠由包括以下步骤的方法制备得到:
步骤一:将羧甲基纤维素钠溶于有机溶剂,在75-85℃下反应30-45min得到基础有机溶液;将基础有机溶液降温至50-65℃后加入催化剂LiCl,并恒温搅拌2-3h得到有机溶液;再将有机溶液升温至75-85℃后,逐滴加入β-二羰基化合物,搅拌4-5h后冷却,萃取得到样品后洗涤干燥粉碎得到固体;β-二羰基化合物为乙酰乙酸叔丁酯、乙酰乙酸乙酯、乙酰丙酸甲酯、乙酰丙酸乙酯、乙酰丙酸丁酯中的一种;
且以羧甲基纤维素钠的质量为1份计,所述有机溶剂质量为25-30份,催化剂质量为0.5-1份,β-二羰基化合物质量为4-7份;有机溶剂为二甲基乙酰胺、二甲基甲酰胺、二甲基亚砜、丙酮、氯仿有机溶剂中的1种;
步骤二:将固体溶解至去离子水中后,加入对甲苯磺酸(TsOH)得到基液,在55-65℃下边搅拌边向基液中滴加胺类化合物,反应3-4h后冷却至室温,真空抽滤得到改性羧甲基纤维素钠;胺类化合物为乙酰胺、甲胺、苯胺、乙二胺、丙胺中的一种;
且以产品质量为1份计,所述去离子水质量为20-30份,对甲苯磺酸质量为0.4-0.6份,胺类化合物质量为1-3份;
2)制备缓释凝胶球:将边搅拌边向FeCl3溶液中滴加溶液A,得到缓释凝胶球;
3)制备缓释除草剂:将缓释凝胶球用去离子水洗涤3-5次后,经冷冻干燥得到腐植酸型抗菌缓释除草剂。
2.根据权利要求1所述的一种腐植酸型抗菌缓释除草剂的制备方法,其特征在于:所述制备缓释除草剂的步骤中,冷冻干燥时间为24h。
3.一种腐植酸型抗菌缓释除草剂,其特征在于:采用如权利要求1-2中任意一项的制备方法制备得到。
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