CN104277391B - A kind of humic acids/polyvinyl alcohol blending modified degradable solid-state mulch film - Google Patents
A kind of humic acids/polyvinyl alcohol blending modified degradable solid-state mulch film Download PDFInfo
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- CN104277391B CN104277391B CN201410485532.9A CN201410485532A CN104277391B CN 104277391 B CN104277391 B CN 104277391B CN 201410485532 A CN201410485532 A CN 201410485532A CN 104277391 B CN104277391 B CN 104277391B
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- humic acids
- polyvinyl alcohol
- mulch film
- plasticizer
- degradable solid
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- 239000004021 humic acid Substances 0.000 title claims abstract description 49
- 239000004372 Polyvinyl alcohol Substances 0.000 title claims abstract description 45
- 229920002451 polyvinyl alcohol Polymers 0.000 title claims abstract description 45
- 238000002156 mixing Methods 0.000 title claims abstract description 32
- 239000002362 mulch Substances 0.000 title claims abstract description 26
- 239000004014 plasticizer Substances 0.000 claims abstract description 12
- 238000010792 warming Methods 0.000 claims abstract description 10
- 239000007822 coupling agent Substances 0.000 claims abstract description 9
- 238000010438 heat treatment Methods 0.000 claims abstract description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000003431 cross linking reagent Substances 0.000 claims abstract description 7
- 239000000314 lubricant Substances 0.000 claims abstract description 7
- 238000006243 chemical reaction Methods 0.000 claims abstract description 6
- 239000000843 powder Substances 0.000 claims abstract description 6
- 230000008961 swelling Effects 0.000 claims abstract description 6
- 238000002360 preparation method Methods 0.000 claims abstract 5
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 18
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims description 18
- 239000008188 pellet Substances 0.000 claims description 10
- 238000003756 stirring Methods 0.000 claims description 10
- ZFOZVQLOBQUTQQ-UHFFFAOYSA-N Tributyl citrate Chemical compound CCCCOC(=O)CC(O)(C(=O)OCCCC)CC(=O)OCCCC ZFOZVQLOBQUTQQ-UHFFFAOYSA-N 0.000 claims description 8
- 239000000203 mixture Substances 0.000 claims description 6
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical group [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 claims description 5
- CJZGTCYPCWQAJB-UHFFFAOYSA-L calcium stearate Chemical compound [Ca+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O CJZGTCYPCWQAJB-UHFFFAOYSA-L 0.000 claims description 5
- 239000008116 calcium stearate Substances 0.000 claims description 5
- 235000013539 calcium stearate Nutrition 0.000 claims description 5
- 238000003490 calendering Methods 0.000 claims description 5
- 229910000077 silane Inorganic materials 0.000 claims description 5
- HQKMJHAJHXVSDF-UHFFFAOYSA-L magnesium stearate Chemical compound [Mg+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O HQKMJHAJHXVSDF-UHFFFAOYSA-L 0.000 claims description 4
- VILCJCGEZXAXTO-UHFFFAOYSA-N 2,2,2-tetramine Chemical compound NCCNCCNCCN VILCJCGEZXAXTO-UHFFFAOYSA-N 0.000 claims description 3
- 229910021538 borax Inorganic materials 0.000 claims description 3
- 239000004328 sodium tetraborate Substances 0.000 claims description 3
- 235000010339 sodium tetraborate Nutrition 0.000 claims description 3
- 229960001124 trientine Drugs 0.000 claims description 3
- PESZCXUNMKAYME-UHFFFAOYSA-N Citroflex A-4 Chemical compound CCCCOC(=O)CC(O)(C(=O)OCCCC)C(C(C)=O)C(=O)OCCCC PESZCXUNMKAYME-UHFFFAOYSA-N 0.000 claims description 2
- MQIUGAXCHLFZKX-UHFFFAOYSA-N Di-n-octyl phthalate Natural products CCCCCCCCOC(=O)C1=CC=CC=C1C(=O)OCCCCCCCC MQIUGAXCHLFZKX-UHFFFAOYSA-N 0.000 claims description 2
- BJQHLKABXJIVAM-UHFFFAOYSA-N bis(2-ethylhexyl) phthalate Chemical compound CCCCC(CC)COC(=O)C1=CC=CC=C1C(=O)OCC(CC)CCCC BJQHLKABXJIVAM-UHFFFAOYSA-N 0.000 claims description 2
- 235000019359 magnesium stearate Nutrition 0.000 claims description 2
- 229920002554 vinyl polymer Polymers 0.000 claims description 2
- 238000005516 engineering process Methods 0.000 description 5
- 238000000034 method Methods 0.000 description 5
- 239000002689 soil Substances 0.000 description 4
- 238000012271 agricultural production Methods 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- -1 polyethylene Polymers 0.000 description 3
- 241001465754 Metazoa Species 0.000 description 2
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 2
- 229920002521 macromolecule Polymers 0.000 description 2
- 229920003023 plastic Polymers 0.000 description 2
- 239000004033 plastic Substances 0.000 description 2
- 239000002985 plastic film Substances 0.000 description 2
- 229920006255 plastic film Polymers 0.000 description 2
- 125000004151 quinonyl group Chemical group 0.000 description 2
- GPLIMIJPIZGPIF-UHFFFAOYSA-N 2-hydroxy-1,4-benzoquinone Chemical compound OC1=CC(=O)C=CC1=O GPLIMIJPIZGPIF-UHFFFAOYSA-N 0.000 description 1
- QJZYHAIUNVAGQP-UHFFFAOYSA-N 3-nitrobicyclo[2.2.1]hept-5-ene-2,3-dicarboxylic acid Chemical compound C1C2C=CC1C(C(=O)O)C2(C(O)=O)[N+]([O-])=O QJZYHAIUNVAGQP-UHFFFAOYSA-N 0.000 description 1
- 239000004698 Polyethylene Substances 0.000 description 1
- 229920002472 Starch Polymers 0.000 description 1
- 239000012675 alcoholic extract Substances 0.000 description 1
- 125000003368 amide group Chemical group 0.000 description 1
- 230000004071 biological effect Effects 0.000 description 1
- 150000001720 carbohydrates Chemical class 0.000 description 1
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 1
- 239000003245 coal Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 150000002085 enols Chemical class 0.000 description 1
- 239000003337 fertilizer Substances 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- 239000003864 humus Substances 0.000 description 1
- 238000003973 irrigation Methods 0.000 description 1
- 230000002262 irrigation Effects 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N phenol group Chemical group C1(=CC=CC=C1)O ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 229920000573 polyethylene Polymers 0.000 description 1
- 229920000915 polyvinyl chloride Polymers 0.000 description 1
- 239000004800 polyvinyl chloride Substances 0.000 description 1
- 102000004169 proteins and genes Human genes 0.000 description 1
- 108090000623 proteins and genes Proteins 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 239000008107 starch Substances 0.000 description 1
- 235000019698 starch Nutrition 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
Abstract
The invention discloses the preparation method and applications of a kind of humic acids/polyvinyl alcohol blending modified degradable solid-state mulch film.It is by PVA and water by the mass ratio of 1:1～3 be stirred at room temperature swelling after be warming up to 80～100 DEG C, add plasticizer, be warming up to 150～180 DEG C of reactions 0.5～1h, obtain the PVA colloidal sol of pre-plasticising.Humic acids powder is weighed by the mass ratio of PVA:HA=1:0.8～1.5, HA in mass ratio: plasticizer: coupling agent=1:0.1～0.3:0.01～0.04 mixing, heating 0.5～1h must melt magma, add it in pre-plasticising PVA colloidal sol, add cross-linking agent and lubricant, 180～200 DEG C of mixing rear pelletizes, are blow molded or roll, and obtain humic acids/polyvinyl alcohol blending modified degradable solid-state mulch film.This mulch film has good mechanical property and degradability, with low cost, and suit large area to popularize application.
Description
Technical field
The present invention relates to a kind of humic acids/polyvinyl alcohol blending modified degradable solid-state mulch film, belong to agricultural production application field.
Background technology
For realizing the purpose of agricultural production and income, utilize plastic film to carry out culture underglass technology and used by vast farmers.But common agricultural plastic ground membrane is mainly polyethylene or polyvinyl chloride macromolecular compound; this material has the physical property of excellence; but it is difficult to degraded under field conditions (factors); recycling it is difficult to after using; " white pollution " problem of residual is difficult to solve, and safety and the sustainable development of agricultural production in serious threat, and farmland mulch to be reduced remains; protect the fields ecological environment, and the most viable method eliminating plastic film " white pollution " is exploitation and uses degradable mulch.
Humic acids (HA) is a kind of organic macromolecule compound being widely present in nature, is the main component of humus in rich soil, exists in a large number in coal, marsh, pond, irrigation canals and ditches mud.Containing multiple functional groups such as alcoholic extract hydroxyl group, phenolic hydroxyl group, hydroxyquinone, enol base, quinonyl, half quinonyl, methoxyl group, amido, carboxyls in humic acids molecular structure, humic acids derives from animals and plants remains, existing saccharide and protein-based construction unit, also there is substantial amounts of photoactivatable groups, have and can be converted into the characteristic of fertilizer after degradable and degraded.Owing to humic acids has good chemistry and biological activity, the research of humic acids mulch film and application also result in the very big concern of people.But owing to humic acids itself does not have thermoplasticity, also without definite melting point, thus the current research about humic acids mulch film and report are only limitted to humic acids liquid-state mulch film, and owing to technology and the problem operated with do not obtain large scale application always.
Summary of the invention
Present Research for humic acids mulch film, the present invention proposes one and utilizes polyvinyl alcohol (PVA) and humic acids (HA) to carry out blending and modifying, thus prepare the new solution of humic acids/polyvinyl alcohol degradable solid-state mulch film, make product more can meet actual application needs.
It is an object of the invention to provide a kind of method preparing humic acids/polyvinyl alcohol blending modified degradable solid-state mulch film.
The purpose of the present invention is achieved through the following technical solutions:
(1) by polyvinyl alcohol with water by polyvinyl alcohol: the mass ratio of water=1:1～3 mixes, then after being stirred at room temperature swelling 1～2 h, it is warming up to 80～100 DEG C, add the plasticizer of 0.1～0.3 times of polyvinyl alcohol weight, being continuously heating to 150～180 DEG C of stirring reaction 0.5～1 h, the polyvinyl alcohol colloidal sol obtaining pre-plasticising is standby.
(2) by polyvinyl alcohol: the mass ratio of humic acids=1:0.8～1.5 weighs the humic acids powder of 200～400 mesh, again by humic acids: plasticizer: the mass ratio of coupling agent=1:0.1～0.3:0.01～0.04 weighs plasticizer and coupling agent, by load weighted humic acids, plasticizer and coupling agent mix, stirring, then heating 0.5～1 h must melt magma, melted magma is joined in the pre-Plasticised Polyvinyl alcosol that step (1) prepares, and humic acids in mass ratio: the ratio of cross-linking agent: lubricant=100:0.3～0.5:0.1～0.4 adds cross-linking agent and lubricant, pelletize after 180～200 DEG C of mixing 15～60 min, obtain the pellet of blending and modifying.
(3) pellet step (2) obtained is in 180～200 DEG C of extrusion-blown modlings or calendering, obtains humic acids/polyvinyl alcohol blending modified degradable solid-state mulch film.
The plasticizer used is one or more in ethylene glycol, glycerol, tributyl citrate, tributyl 2-acetylcitrate, dioctyl phthalate；
The coupling agent used is silane coupler；
The cross-linking agent used is Borax, N, one or more in N '-methylene acrylamide, triethylene tetramine；
The lubricant used is one or more in calcium stearate or magnesium stearate.
The invention have the advantages that
(1) by by after polyvinyl alcohol and humic acids pre-plasticising respectively, the Particular craft technology of blending and modifying has prepared degradable humic acids solid-state mulch film product again, compared with original humic acids liquid-state mulch film, more meet tradition plastic mulching cultivation technology needs, it is easier to accept for wide farmers.
(2) humic acid material wide material sources, are the animal and plant resources rotted, and compared with starch based degradable mulch, price is the cheapest, there is not the problem striving grain with people.
(3) it is not introduced into environmentally harmful chemical drugs, environmental-protection fully-degradable can be realized, typically can realize degradable after using 3-5 month.
Detailed description of the invention
Embodiment
1
:
1) taking PVA 20 kg, add 30 kg water, after being stirred at room temperature swelling 1 h, be warming up to 80～100 DEG C, add mixture 3 kg that volume ratio is 1:1 ethylene glycol and glycerol, be warming up to 160 DEG C of stirring reaction 0.5 h, the PVA colloidal sol obtaining pre-plasticising is standby.
2) take and be crushed to HA powder 20 kg of 300 mesh, add ethylene glycol and glycerol mixture 3 kg that volume ratio is 1:1, silane coupler 0.3 kg, after stirring Hybrid Heating 0.5 h, join in the pre-plasticising PVA colloidal sol that step (1) prepares, and add Borax 0.08 kg and calcium stearate 0.04 kg, pelletize after 180 DEG C of mixing 30 min, obtain the pellet of blending and modifying.
3) by above-mentioned pellet in 180～200 DEG C of extrusion-blown modlings or calendering, humic acids/polyvinyl alcohol blending modified degradable solid-state mulch film is obtained.
After tested, the humic acids/polyvinyl alcohol blending modified degradable solid-state mulching film stretching intensity prepared is 4.28 MPa, and elongation at break is 267.6%, and soil buries method degraded 50% and needs about 70 days.
Embodiment
2
:
1) taking PVA 20 kg, add 40 kg water, after being stirred at room temperature swelling 1 h, be warming up to 80～100 DEG C, add 3 kg tributyl citrate, be warming up to 160 DEG C of stirring reaction 0.5 h, the PVA colloidal sol obtaining pre-plasticising is standby.
2) take and be crushed to HA powder 30 kg of 400 mesh, add tributyl citrate 3 kg, silane coupler 0.4 kg, after stirring Hybrid Heating 0.5 h, join in the pre-plasticising PVA colloidal sol that step (1) prepares, and add N, N '-methylene acrylamide 0.09kg and calcium stearate 0.04 kg, pelletize after 180 DEG C of mixing 30 min, obtains the pellet of blending and modifying.
3) by above-mentioned pellet in 180～200 DEG C of extrusion-blown modlings or calendering, humic acids/polyvinyl alcohol blending modified degradable solid-state mulch film is obtained.
After tested, the humic acids/polyvinyl alcohol blending modified degradable solid-state mulching film stretching intensity prepared is 3.52 MPa, and elongation at break is 156.8%, and soil buries method degraded 50% and needs about 60 days.
Embodiment
3
:
1) taking PVA 20 kg, add 30 kg water, after being stirred at room temperature swelling 1 h, be warming up to 80～100 DEG C, add mixture 3 kg that volume ratio is 1:1 ethylene glycol and glycerol, be warming up to 170 DEG C of stirring reaction 0.5 h, the PVA colloidal sol obtaining pre-plasticising is standby.
2) take and be crushed to HA powder 16 kg of 300 mesh, add mixture 3 kg that volume ratio is 1:1 ethylene glycol and glycerol, silane coupler 0.3 kg, after stirring Hybrid Heating 0.5 h, join in the pre-plasticising PVA colloidal sol that step (1) prepares, and add triethylene tetramine 0.06 kg and calcium stearate 0.04 kg, pelletize after 190 DEG C of mixing 30 min, obtain the pellet of blending and modifying.
3) by above-mentioned pellet in 180～200 DEG C of extrusion-blown modlings or calendering, humic acids/polyvinyl alcohol blending modified degradable solid-state mulch film is obtained.
After tested, the humic acids/polyvinyl alcohol blending modified degradable solid-state mulching film stretching intensity prepared is 5.66 MPa, and elongation at break is 324.8%, and soil buries method degraded 50% and needs about 80 days.
Claims (4)
1. the preparation method of humic acids/polyvinyl alcohol blending modified degradable solid-state mulch film, it is characterised in that: comprise the steps:
(1) by polyvinyl alcohol with water by polyvinyl alcohol: the mass ratio of water=1:1～3 mixes, then after being stirred at room temperature swelling 1～2 h, it is warming up to 80～100 DEG C, add the plasticizer of 0.1～0.3 times of polyvinyl alcohol weight, being continuously heating to 150～180 DEG C of stirring reaction 0.5～1 h, the polyvinyl alcohol colloidal sol obtaining pre-plasticising is standby；
(2) by polyvinyl alcohol: the mass ratio of humic acids=1:0.8～1.5 weighs the humic acids powder of 200～400 mesh, again by humic acids: plasticizer: the mass ratio of coupling agent=1:0.1～0.3:0.01～0.04 weighs plasticizer and coupling agent, by load weighted humic acids, plasticizer and coupling agent mix, stirring, then heating 0.5～1 h must melt magma, melted magma is joined in the pre-Plasticised Polyvinyl alcosol that step (1) prepares, and humic acids in mass ratio: the ratio of cross-linking agent: lubricant=100:0.3～0.5:0.1～0.4 adds cross-linking agent and lubricant, pelletize after 180～200 DEG C of mixing 15～60 min, obtain the pellet of blending and modifying；
(3) pellet step (2) obtained is in 180～200 DEG C of extrusion-blown modlings or calendering, obtains humic acids/polyvinyl alcohol blending modified degradable solid-state mulch film；
The cross-linking agent that wherein step (2) uses is Borax, N, one or more in N '-methylene acrylamide, triethylene tetramine.
The preparation method of a kind of humic acids the most as claimed in claim 1/polyvinyl alcohol blending modified degradable solid-state mulch film, it is characterised in that: the plasticizer of use is one or more in ethylene glycol, glycerol, tributyl citrate, tributyl 2-acetylcitrate, dioctyl phthalate.
The preparation method of a kind of humic acids the most as claimed in claim 1/polyvinyl alcohol blending modified degradable solid-state mulch film, it is characterised in that: the coupling agent of use is silane coupler.
The preparation method of a kind of humic acids the most as claimed in claim 1/polyvinyl alcohol blending modified degradable solid-state mulch film, it is characterised in that: the lubricant of use is one or more in calcium stearate or magnesium stearate.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410485532.9A CN104277391B (en) | 2014-09-22 | 2014-09-22 | A kind of humic acids/polyvinyl alcohol blending modified degradable solid-state mulch film |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201410485532.9A CN104277391B (en) | 2014-09-22 | 2014-09-22 | A kind of humic acids/polyvinyl alcohol blending modified degradable solid-state mulch film |
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| CN104277391A CN104277391A (en) | 2015-01-14 |
| CN104277391B true CN104277391B (en) | 2016-08-17 |
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Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104672700B (en) * | 2015-02-04 | 2017-02-08 | 南京悠谷知识产权服务有限公司 | Polyvinyl chloride material and preparation method thereof |
| CN107141674B (en) * | 2017-05-24 | 2020-05-22 | 浙江理工大学 | Polyvinyl alcohol and phosphoric acid compound blended film and preparation method thereof |
| CN110294909B (en) * | 2019-06-20 | 2022-03-22 | 江苏省农业科学院 | Method for preparing water-resistant bioplastic from biomass hydrolysis residues |
| CN110615958A (en) * | 2019-08-16 | 2019-12-27 | 山东森工新材料科技有限公司 | Humic acid composite gel material and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101481508A (en) * | 2008-01-11 | 2009-07-15 | 山东科技大学 | Humic acid multifunctional degradable black mulch film |
| CN101589681A (en) * | 2009-07-10 | 2009-12-02 | 李保华 | Completely degraded plastic film and production method thereof |
| CN103373879A (en) * | 2013-07-10 | 2013-10-30 | 湖南中烟工业有限责任公司 | Degradable solid mulching film special for tobacco and preparation method of degradable solid mulching film |
| CN104017316A (en) * | 2014-05-30 | 2014-09-03 | 新疆大学 | Composite material containing polyvinyl alcohol and soapstone modified with quaternary ammonium salt of fulvic acid, and preparation method, products and applications of the composite material |
-
2014
- 2014-09-22 CN CN201410485532.9A patent/CN104277391B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101481508A (en) * | 2008-01-11 | 2009-07-15 | 山东科技大学 | Humic acid multifunctional degradable black mulch film |
| CN101589681A (en) * | 2009-07-10 | 2009-12-02 | 李保华 | Completely degraded plastic film and production method thereof |
| CN103373879A (en) * | 2013-07-10 | 2013-10-30 | 湖南中烟工业有限责任公司 | Degradable solid mulching film special for tobacco and preparation method of degradable solid mulching film |
| CN104017316A (en) * | 2014-05-30 | 2014-09-03 | 新疆大学 | Composite material containing polyvinyl alcohol and soapstone modified with quaternary ammonium salt of fulvic acid, and preparation method, products and applications of the composite material |
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Inventor after: Zhang Xiru Inventor after: Peng Hongying Inventor after: Sui Yan Inventor after: Luo Zhigang Inventor after: Wen Jiwu Inventor after: Hu Ronghua Inventor before: Sui Yan Inventor before: Luo Zhigang Inventor before: Wen Jiwu Inventor before: Hu Ronghua |
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Effective date of registration: 20150916 Address after: The North Industrial Park of Ji'an city of Jiangxi province Xingan County 331300 Applicant after: JIANGXI SHUANGJIA TECHNOLOGY DEVELOPMENT CO., LTD. Address before: 343009 Ji'an City, Jiangxi province Qingyuan District School Road No. 28 Applicant before: Jinggangshan University |
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Denomination of invention: A degradable solid mulching film modified by humic acid / polyvinyl alcohol blend Effective date of registration: 20201218 Granted publication date: 20160817 Pledgee: Jiangxi Xingan Rural Commercial Bank Co.,Ltd. Pledgor: Jiangxi Shuangjia Technology Co.,Ltd. Registration number: Y2020980009525 |