CN101654532A - Nanometer material modified polyethylene agricultural film and its preparing method - Google Patents
Nanometer material modified polyethylene agricultural film and its preparing method Download PDFInfo
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- CN101654532A CN101654532A CN 200910195425 CN200910195425A CN101654532A CN 101654532 A CN101654532 A CN 101654532A CN 200910195425 CN200910195425 CN 200910195425 CN 200910195425 A CN200910195425 A CN 200910195425A CN 101654532 A CN101654532 A CN 101654532A
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Abstract
Provided is a nanometer material modified polyethylene agricultural film in the polyethylene technical field. which comprises following components in mass ratio: 91.5-99.3 parts of polyethylene resin,0.2-1.5 parts of inorganic nanocomposite, 0.1-1 part of antioxidant, 0.1-1 part of light stabilizing agent and 0.3-5 parts of processing auxiliary agent. The provided agricultural film has excellentphysical and mechanical performance and weatherability and can be produced into high quality agricultural warmhouse booth film.
Description
Technical field
What the present invention relates to is film of a kind of technical field of nano material and preparation method thereof, specifically is a kind of nanometer material modified polyethylene agricultural film and preparation method thereof.
Background technology
Along with Agricultural Development, agripast has become and has promoted the more requisite important production means of high-efficient development of agricultural.Northern China severe winter to early spring, the sunshine duration is short, free air temperature is low, is to improve crop yield, and the demand of the agricultural booth film of excellent performance is continued to increase.It is raw material that tradition agricultural booth film mainly adopts polyvinyl chloride (PVC) RESINS.Though polyvinyl chloride film is than weather-resistant, owing to contain a large amount of softening agent, the softening agent volatilization adds that polyvinyl chloride (PVC) RESINS itself should degrade in processing and the use, can cause environmental pollution.And the polyvinyl chloride low-temperature performance is bad, is easy to again when temperature is higher relax, and easily adsorbs dust and density of film is bigger, and the unit surface cost is higher, and is not easy to store, replaced by polyethylene film gradually in recent years.
But polyvinyl resin is because of existing two keys in its molecular chain, easily oxidative degradation causes it in storage, moulding, use under action of ultraviolet radiation, and recurring structure changes along with the prolongation of time, the deterioration of physico-mechanical properties occurs.The method for preparing the weathering resistance agricultural film that adopts both at home and abroad is mainly and adds the light inlet stabilization additives at present, applies anti-aging coating, inorganic material-modified weathering resistance etc.And add the method for photostabilizer in present stage this area, for example add oxidation inhibitor and photostabilizer etc. and be that the anti-photoaging of macromolecular material is the most general, most convenient, most economical method.
Through the retrieval of prior art is found: put down in writing among the Chinese patent literature CN1056696A to utilize to cooperate in the UV light stabilizing agent formed and the phenolic antioxidant adding polyvinyl resin and prepare weatherability film by hindered amines, triazines, benzophenone light stabilizer.Though organic photostabilizer has many good qualities, it is mainly organism, does not have the ability of long-acting ultraviolet light; It is that the coating of 1-1.2mm is made the agricultural film material by apply a layer thickness in the polyethylene basic unit of film that Chinese patent literature CN101381469A has put down in writing a kind of, the composition of coating comprises PVA, phosphoric acid, urea and water, and the film of making has high toughness and good ageing resistance.But this method preparation technology is comparatively complicated, the shortcoming that the film of making exists anti-aging coating to come off easily; Chinese patent literature CN1502654A has put down in writing a kind of polythene material, by in polyvinyl resin, adding nanometer grade calcium carbonate, improved the physical and mechanical properties of surface polyethylene coating film, and since light shield improved effect that nano-calcium carbonate had the ageing-resistant performance of mulch film.But because the adding of lime carbonate makes the transparency of film reduce, and, make the ageing-resistant performance of film fail to be significantly improved because of not adding auxiliary organic photostabilizer; Chinese patent literature CN1718625A has put down in writing a kind of nanometer treatment process, by adopting nanometer SiO
2Shed Film of Polyolefin is carried out modification handle, reach the adding of metallocene linear low density of polyethylene, improved the mechanical property and the ageing-resistant performance of canopy film.Its preparation method who adopts is for preparing nanometer SiO earlier
2The ageing-resistant composite canopy film masterbatch of modified metallocene is mixed with weathering resistance canopy film with itself and polyolefin resin again.Its technology is comparatively complicated, and in preparation process, nanometer SiO
2Reunite easily and cause the reduction of antiageing effect.
Summary of the invention
The present invention is directed to the prior art above shortcomings, a kind of nanometer material modified polyethylene agricultural film and preparation method thereof is provided, have excellent physical mechanical property, weather resistance, can be made into fine agricultural greenhouse awning film.
The present invention is achieved by the following technical solutions:
The present invention relates to nanometer material modified polyethylene agricultural film, its component and mass ratio are followed successively by: polyvinyl resin 91.5-99.3 part, inorganic nano composite material 0.2-1.5 part, oxidation inhibitor 0.1-1 part, photostabilizer 0.1-1 part and processing aid 0.3-5 part.
Described inorganic nano composite material is meant through surface treatment and the composite nanometer titanium dioxide composite material of making or nanometer silicon dioxide composite material or its combination.
Described surface treatment agent is a kind of or its combination in stearic acid and salt, titanate coupling agent, aluminate coupling agent or the silane coupling agent.
The component of described oxidation inhibitor and mass percentage content thereof are phenolic antioxidant 25%-30% and phosphite ester kind antioxidant 70%-75%;
Described phenolic antioxidant is four [β-(3, the 5-di-tert-butyl-hydroxy phenyl) propionic acid] pentaerythritol ester or β-positive octadecanol esters of (3, the 5-di-tert-butyl-hydroxy phenyl) propionic acid;
Described phosphite ester kind antioxidant is three (2, the 4-di-tert-butyl-phenyl) phosphorous acid ester.
Described photostabilizer is hindered amine as light stabilizer or benzotriazole light stabilizer or its combination;
Described hindered amine light stabilizer is a 4-benzoyloxy-2,2,6, the 6-tetramethyl piperidine;
Described benzotriazole light stabilizer is 2-(2 '-hydroxyl-3 ', 5 '-two uncle's phenyl)-5-chlorination benzotriazole.
The component of described processing aid and mass percentage content thereof are lubricant 17%-33% and modifier 67%-83%;
Described lubricant is a kind of or its combination in stearic amide, stearin, amine hydroxybenzene, hydroxyl stearylamide or stearic acid and the salt thereof;
Described modifier is a kind of or its combination in paraffin, whiteruss or the polyethylene wax.
The present invention relates to the preparation method of above-mentioned nanometer material modified polyethylene agricultural film, may further comprise the steps:
The first step, nano-powder is carried out making inorganic nano composite material after drying treatment and the ball-milling processing successively;
Described nano-powder is meant TiO
2Powder or SiO
2Powder or its combination, the median size of this nano-powder is 10-90nm;
Described drying treatment is meant: nano-powder was placed under 80-120 ℃ the condition dry 2-4 hour;
Described ball-milling processing is meant: with dried nano-powder and surface treatment agent by 1: 1-5: 1 quality is mixed to be placed on than proportioning and is carried out ground and mixed reaction 15-30 minute in the ball mill.
Described surface treatment agent is a kind of or its combination in stearic acid and salt, titanate coupling agent, aluminate coupling agent or the silane coupling agent.
Second goes on foot, 0.2-1.5 weight part inorganic nano composite material is carried out placing superhigh speed mixing machine to carry out in the lump pre-mixing 3-10 minute with 91.5-99.3 weight account polyethylene resin, 0.1-1 weight part oxidation inhibitor, 0.1-1 weight part photostabilizer and 0.3-5 weight part processing aid after redrying is handled, and makes film raw material;
Described redrying is handled and is meant: inorganic nano composite material was placed under 70-110 ℃ the condition dry 1-3 hour;
The 3rd goes on foot, film raw material is placed on the forcing machine make the polyethylene film that thickness is 0.1-0.2mm by inflation film process;
Described inflation film process is meant: 150-230 ℃ of blow temperatures of setting, blow-up ratio are 1: 2-1: 3, pulling speed is that 3-6m/min, engine speed are that 80-110rpm is a polyethylene film with film raw material blowing.
Compared with prior art the present invention has the following advantages:
Overcome the shortcoming of the easy photoaging of agricultural film, wide band, the ability of long-acting shielding ultraviolet rays and the synergy that organic photostabilizer blocks film degradation with aging reaction chain by the performance inorganic nano composite material increase substantially the weather-proof ability of film;
Solved the problem that organic uv absorbers easily lost efficacy,, made most of ultraviolet ray can not enter film inside, and organic photostabilizer is effectively protected by the wide band of performance inorganic nano composite material, the ability of long-acting shielding ultraviolet rays;
Improved mechanical properties in films,, made film obtain excellent comprehensive mechanical properties by the synergy of inorganic nano composite material and processing aid;
Given film the good feature of environmental protection, can reduce the usage quantity of organic photostabilizer behind the use inorganic nano composite material, reduce the environmentally harmful product that the especially organic photostabilizer degraded of film matrix resin back produces, therefore aspect environment protection, also had an advantage;
The preparation method is simple, uses traditional film production equipment to finish, and has avoided being equipped with specific equipment for producing the weather resistant agricultural film, has reduced facility investment.
Embodiment
Below embodiments of the invention are elaborated: present embodiment is being to implement under the prerequisite with the technical solution of the present invention, provided detailed embodiment and concrete operating process, but protection scope of the present invention is not limited to following embodiment.
Embodiment 1:
The first step, be 1 part of nano-TiO of 20-30nm with median size
2Drying is 4 hours under 100 ℃ condition, with 0.5 part of nano-TiO that drying is good
220 minute finish surface treatment and composite make inorganic nano composite material by 1: 1 proportioning in the reaction of ball mill high speed ground and mixed with 0.5 part of silane coupling agent;
Second step, with inorganic nano composite material under 100 ℃ condition dry 3 hours, with 0.2 part inorganic nano composite material and 98.6 parts polyvinyl resin, 0.1 part four [β-(3, the 5-di-tert-butyl-hydroxy phenyl) propionic acid] pentaerythritol ester, 0.3 part three (2, the 4-di-tert-butyl-phenyl) phosphorous acid ester, 2-(2 '-hydroxyl-3 ' of 0.2 part, 5 '-two uncle's phenyl)-and 5-chlorination benzotriazole, 0.1 part amine hydroxybenzene, 0.5 part polyethylene wax carried out pre-mixing 10 minutes, and pre-mixing speed is 1300rpm;
The 3rd step, material that premix is got togather by the complete processing of inflation film process, are made the polyethylene film that thickness is about 0.1mm on forcing machine; Processing temperature 150-230 ℃, blow-up ratio is 1: 2-1: 3, and pulling speed is 3-6m/min, engine speed is 80-110rpm.
According to GB/T 13022-91 plastics---film stretching method for testing performance, QB/T1130-91 plastics right-angle tearing method for testing performance, film is made into the standard batten, then according to GB/T 16422.3-1999 plastics laboratory light source exposure test method the 3rd part: fluorescent ultraviolet lamp, adopt fluorescent ultraviolet lamp climatic test machine that film standard testing sample was carried out the weather accelerated deterioration 700 hours.
Embodiment 2: concrete preparation method is with embodiment 1, material proportion and proportioning thereof are as follows: polyethylene 98.6 weight parts, titanium dioxide powder 0.16 weight part, silicon-dioxide powdery 0.04 weight part, titanate coupling agent 0.1 weight part, four [β-(3, the 5-di-tert-butyl-hydroxy phenyl) propionic acid] pentaerythritol ester 0.1 weight part, three (2, the 4-di-tert-butyl-phenyl) phosphorous acid ester 0.3 weight part, 4-benzoyloxy-2,2,6,6-tetramethyl piperidine 0.1 weight part, amine hydroxybenzene 0.1 weight part and polyethylene wax 0.5 weight part.
According to GB/T 13022-91 plastics---film stretching method for testing performance, QB/T1130-91 plastics right-angle tearing method for testing performance, film is made into the standard batten, then according to GB/T 16422.3-1999 plastics laboratory light source exposure test method the 3rd part: fluorescent ultraviolet lamp, adopt fluorescent ultraviolet lamp climatic test machine that film standard testing sample was carried out the weather accelerated deterioration 700 hours.
Embodiment 3: concrete preparation method is with embodiment 1, material proportion is as follows: polyethylene 91.5 weight parts, titanium dioxide powder 0.5 weight part, silicon-dioxide powdery 0.5 weight part, titanate coupling agent 0.5 weight part, four [β-(3, the 5-di-tert-butyl-hydroxy phenyl) propionic acid] pentaerythritol ester 0.3 weight part, three (2, the 4-di-tert-butyl-phenyl) phosphorous acid ester 0.7 weight part, 4-benzoyloxy-2,2,6,6-tetramethyl piperidine 1 weight part, amine hydroxybenzene 1 weight part and polyethylene wax 4 weight parts.
According to GB/T 13022-91 plastics---film stretching method for testing performance, QB/T1130-91 plastics right-angle tearing method for testing performance, film is made into the standard batten, then according to GB/T 16422.3-1999 plastics laboratory light source exposure test method the 3rd part: fluorescent ultraviolet lamp, adopt fluorescent ultraviolet lamp climatic test machine that film standard testing sample was carried out the weather accelerated deterioration 700 hours.
Embodiment 4: concrete preparation method is with embodiment 1, material proportion is as follows: polyethylene 99.3 weight parts, titanium dioxide powder 0.1 weight part, silane coupling agent 0.1 weight part, β-(3, the 5-di-tert-butyl-hydroxy phenyl) positive octadecanol ester 0.03 weight part of propionic acid, three (2, the 4-di-tert-butyl-phenyl) phosphorous acid ester 0.07 weight part, 2-(2 '-hydroxyl-3 ', 5 '-two uncle's phenyl)-5-chlorination benzotriazole 0.1 weight part, amine hydroxybenzene 0.1 weight part and polyethylene wax 0.2 weight part.
According to GB/T 13022-91 plastics---film stretching method for testing performance, QB/T1130-91 plastics right-angle tearing method for testing performance, film is made into the standard batten, then according to GB/T 16422.3-1999 plastics laboratory light source exposure test method the 3rd part: fluorescent ultraviolet lamp, adopt fluorescent ultraviolet lamp climatic test machine that film standard testing sample was carried out the weather accelerated deterioration 700 hours.
Comparative Examples: prepare no nano material and add the modified polyethylene film, concrete preparation method is with embodiment 1, material proportion is as follows: polyethylene 97.4 weight parts, four [β-(3, the 5-di-tert-butyl-hydroxy phenyl) propionic acid] pentaerythritol ester 0.1 weight part, three (2, the 4-di-tert-butyl-phenyl) phosphorous acid ester 0.3 weight part, 4-benzoyloxy-2,2,6,6-tetramethyl piperidine 0.2 weight part, amine hydroxybenzene 0.5 weight part and polyethylene wax 1.5 weight parts.
According to GB/T 13022-91 plastics---film stretching method for testing performance, QB/T1130-91 plastics right-angle tearing method for testing performance, film is made into the standard batten, then according to GB/T 16422.3-1999 plastics laboratory light source exposure test method the 3rd part: fluorescent ultraviolet lamp, adopt fluorescent ultraviolet lamp climatic test machine that film standard testing sample was carried out the weather accelerated deterioration 700 hours.
Implementation result is analyzed:
To the nanometer material modified polyethylene film of accelerated deterioration after 700 hours respectively and the mechanical property contrast of not adding nano-material modified polyethylene film following (every group of batten got 10 battens tests flawless and other flaws and averaged):
Table 1 performance comparison table
More than test shows, through the polyethylene agricultural film tensile strength of nano-material modified mistake, elongation at break, angle tear strength all than add modified polyethylene agricultural film height without nano material.In sum, nanometer material modified polyethylene agricultural film preparation technology of the present invention is simple, does not need expensive specific equipment, has solved organic photostabilizer easily degraded and the easy problem that lost efficacy of ultraviolet radiation absorption, overcome the easy aged shortcoming of polyethylene agricultural film, possessed excellent weathering resistance.
Claims (10)
1, a kind of nanometer material modified polyethylene agricultural film, it is characterized in that the component and the mass ratio of this film are followed successively by: polyvinyl resin 91.5-99.3 part, inorganic nano composite material 0.2-1.5 part, oxidation inhibitor 0.1-1 part, photostabilizer 0.1-1 part and processing aid 0.3-5 part.
2, nanometer material modified polyethylene agricultural film according to claim 1 is characterized in that, the component of described oxidation inhibitor and mass percentage content thereof are phenolic antioxidant 25%-30% and phosphite ester kind antioxidant 70%-75%.
3, nanometer material modified polyethylene agricultural film according to claim 2, it is characterized in that, described phenolic antioxidant is four [β-(3, the 5-di-tert-butyl-hydroxy phenyl) propionic acid] pentaerythritol ester or β-positive octadecanol esters of (3, the 5-di-tert-butyl-hydroxy phenyl) propionic acid; Described phosphite ester kind antioxidant is three (2, the 4-di-tert-butyl-phenyl) phosphorous acid ester.
4, nanometer material modified polyethylene agricultural film according to claim 1 is characterized in that, described photostabilizer is hindered amine as light stabilizer or benzotriazole light stabilizer or its combination.
5, nanometer material modified polyethylene agricultural film according to claim 4 is characterized in that, described hindered amine light stabilizer is a 4-benzoyloxy-2,2,6, the 6-tetramethyl piperidine; Described benzotriazole light stabilizer is 2-(2 '-hydroxyl-3 ', 5 '-two uncle's phenyl)-5-chlorination benzotriazole.
6, nanometer material modified polyethylene agricultural film according to claim 1 is characterized in that, the component of described processing aid and mass percentage content thereof are lubricant 17%-33% and modifier 67%-83%.
7, nanometer material modified polyethylene agricultural film according to claim 6 is characterized in that, described lubricant is a kind of or its combination in stearic amide, stearin, amine hydroxybenzene, hydroxyl stearylamide or stearic acid and the salt thereof; Described modifier is a kind of or its combination in paraffin, whiteruss or the polyethylene wax.
8, the preparation method of nanometer material modified polyethylene agricultural film according to claim 1 is characterized in that, may further comprise the steps:
The first step, nano-powder is carried out making inorganic nano composite material after drying treatment and the ball-milling processing successively;
Second goes on foot, 0.2-1.5 weight part inorganic nano composite material is carried out placing superhigh speed mixing machine to carry out in the lump pre-mixing 3-10 minute with 91.5-99.3 weight account polyethylene resin, 0.1-1 weight part oxidation inhibitor, 0.1-1 weight part photostabilizer and 0.3-5 weight part processing aid after redrying is handled, and makes film raw material;
The 3rd goes on foot, film raw material is placed on the forcing machine make the polyethylene film that thickness is 0.1-0.2mm by inflation film process.
9, the preparation method of nanometer material modified polyethylene agricultural film according to claim 8 is characterized in that, described nano-powder is meant TiO
2Powder or SiO
2Powder or its combination, the median size of this nano-powder is 10-90nm.
10, the preparation method of nanometer material modified polyethylene agricultural film according to claim 8, it is characterized in that described inflation film process is meant: 150-230 ℃ of blow temperatures of setting, blow-up ratio are 1: 2-1: 3, pulling speed is that 3-6m/min, engine speed are that 80-110rpm is a polyethylene film with film raw material blowing.
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102250403A (en) * | 2011-06-27 | 2011-11-23 | 上海工程技术大学 | Multifunctional agricultural thin film and preparation method thereof |
| CN103601945A (en) * | 2013-10-14 | 2014-02-26 | 太湖华强科技有限公司 | Modified polyethylene agricultural film |
| CN104530554A (en) * | 2015-01-31 | 2015-04-22 | 黄山永新股份有限公司 | Calcium-carbonate-filling-modified linear low density polyethylene film and preparation method thereof |
| CN104530546A (en) * | 2014-12-22 | 2015-04-22 | 山东农业大学 | Special anti-reflection reinforced master batch for agricultural greenhouse film and preparation method of anti-reflection reinforced master batch |
| CN105131402A (en) * | 2015-09-25 | 2015-12-09 | 安徽江淮汽车股份有限公司 | PE (Polyethylene) composite material and preparation method thereof |
| CN106220950A (en) * | 2016-07-30 | 2016-12-14 | 程志刚 | A kind of light and thin type agricultural film and preparation method thereof |
| CN106437089A (en) * | 2016-11-22 | 2017-02-22 | 江苏欧圣木业有限公司 | PE-containing wear-resisting and high-strength laminate flooring |
| CN106854315A (en) * | 2016-11-30 | 2017-06-16 | 徐丹峰 | The greenhouse film and preparation method of a kind of high intensity |
| WO2017140172A1 (en) * | 2016-02-17 | 2017-08-24 | 黄秀茹 | Additive for use in polymer, additive composition and polymeric composition of the additive, and uses thereof as light stabilizer |
| CN107474353A (en) * | 2017-06-26 | 2017-12-15 | 浙江转喆科技有限公司 | A kind of conversion film and preparation method thereof |
| CN107488449A (en) * | 2017-06-26 | 2017-12-19 | 浙江转喆科技有限公司 | Lower conversion light conversion agent and preparation method thereof and lower transformation of blue conversion film and preparation method thereof |
| CN107488453A (en) * | 2017-06-26 | 2017-12-19 | 浙江转喆科技有限公司 | Upper conversion light conversion agent and preparation method thereof and upper conversion conversion film and preparation method thereof |
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2009
- 2009-09-10 CN CN 200910195425 patent/CN101654532A/en active Pending
Cited By (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102250403B (en) * | 2011-06-27 | 2012-12-19 | 上海工程技术大学 | Multifunctional agricultural thin film and preparation method thereof |
| CN102250403A (en) * | 2011-06-27 | 2011-11-23 | 上海工程技术大学 | Multifunctional agricultural thin film and preparation method thereof |
| CN103601945B (en) * | 2013-10-14 | 2016-05-18 | 太湖华强科技有限公司 | A kind of modified polyethylene agricultural film |
| CN103601945A (en) * | 2013-10-14 | 2014-02-26 | 太湖华强科技有限公司 | Modified polyethylene agricultural film |
| CN104530546A (en) * | 2014-12-22 | 2015-04-22 | 山东农业大学 | Special anti-reflection reinforced master batch for agricultural greenhouse film and preparation method of anti-reflection reinforced master batch |
| CN104530554A (en) * | 2015-01-31 | 2015-04-22 | 黄山永新股份有限公司 | Calcium-carbonate-filling-modified linear low density polyethylene film and preparation method thereof |
| CN105131402A (en) * | 2015-09-25 | 2015-12-09 | 安徽江淮汽车股份有限公司 | PE (Polyethylene) composite material and preparation method thereof |
| WO2017140172A1 (en) * | 2016-02-17 | 2017-08-24 | 黄秀茹 | Additive for use in polymer, additive composition and polymeric composition of the additive, and uses thereof as light stabilizer |
| CN106220950A (en) * | 2016-07-30 | 2016-12-14 | 程志刚 | A kind of light and thin type agricultural film and preparation method thereof |
| CN106437089A (en) * | 2016-11-22 | 2017-02-22 | 江苏欧圣木业有限公司 | PE-containing wear-resisting and high-strength laminate flooring |
| CN106854315A (en) * | 2016-11-30 | 2017-06-16 | 徐丹峰 | The greenhouse film and preparation method of a kind of high intensity |
| CN107474353A (en) * | 2017-06-26 | 2017-12-15 | 浙江转喆科技有限公司 | A kind of conversion film and preparation method thereof |
| CN107488449A (en) * | 2017-06-26 | 2017-12-19 | 浙江转喆科技有限公司 | Lower conversion light conversion agent and preparation method thereof and lower transformation of blue conversion film and preparation method thereof |
| CN107488453A (en) * | 2017-06-26 | 2017-12-19 | 浙江转喆科技有限公司 | Upper conversion light conversion agent and preparation method thereof and upper conversion conversion film and preparation method thereof |
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Application publication date: 20100224 |