CN105385014B - A kind of light altering film for agriculture and preparation method and application - Google Patents
A kind of light altering film for agriculture and preparation method and application Download PDFInfo
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- CN105385014B CN105385014B CN201510916840.7A CN201510916840A CN105385014B CN 105385014 B CN105385014 B CN 105385014B CN 201510916840 A CN201510916840 A CN 201510916840A CN 105385014 B CN105385014 B CN 105385014B
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Abstract
The invention belongs to agricultural light-light conversion field of functional materials, disclose a kind of light altering film for agriculture by the use of nitride red fluorescent powder as light conversion agent and preparation method and application.The light altering film for agriculture mainly includes light conversion agent master batch and film matrix, and wherein light conversion agent master batch is made of the component of following mass fraction：Nitride red light conversion agent 10~50%；Auxiliary agent 1~10%；Surplus is master batch matrix.The nitride light conversion agent and the Spectral matching needed for photosynthesis of plant of the present invention is good, it is co-doped with simultaneously by trivalent rare earth ions and cation is replaced, obtain excellent red long-afterglow luminescent properties, can under conditions of night or without sunlight the long period blood orange light needed for photosynthesis of plant is persistently provided, extend photosynthesis of plant.Master batch is made in the nitride light conversion agent and is used further to manufacture agricultural film, light conversion agent can be carried out pre-dispersed, improves dispersibility of the nitride light conversion agent in film matrix, when applied to agriculture field, achieving the effect that increasing of quality and production.
Description
Technical field
The invention belongs to agricultural light-light conversion field of functional materials, more particularly to a kind of light altering film for agriculture and preparation method thereof
With application.
Background technology
Agricultural rare-earth shines-and light conversion agent is also referred to as agricultural light conversion agent.Agricultural light conversion agent is processed to be used in combination for light altering film for agriculture
When proportion of crop planting, the plant growth that is partially converted to useless or harmful to plant growth in sunlight can be needed what is absorbed
Light；In addition, the light conversion agent with apparent twilight sunset effect, under field conditions (factors) for light deficiency when can still make the photosynthetic work of greenhouse implants
With efficiently carrying out.Therefore, agricultural light conversion agent and light altering film for agriculture are as a kind of high-tech agriculture for effectively improving chamber crop yield
Industry light filling material under the background for having been unable to meet modern society's demand in traditional agriculture tillage system reform, increasingly becomes current light
The new trend that power technology is applied in agriculture field.
The light of heterogeneity is different to the growth of plant.The blue violet light of 400~480nm of wavelength can be by chlorophyll, class
Carrotene absorbs strongly, and the cauline leaf of plant is promoted to grow；The blood orange light of 600~700nm of wavelength can be promoted by Chlorophyll absorption
The fruit growth of plant；The green-yellow light of 500~600nm of wavelength is to photosynthesis almost without contribution；And 315~400nm of wavelength
Except the light near 360nm, to promoting fruit coloring, remaining can make plant become short near ultraviolet ray, and blade becomes beneficial in addition to
It is thick；The ultraviolet light of 290~315nm of wavelength is all harmful to most plants, can promote agricultural film degeneration and wane.Ideal conversion film can
By light that is being harmful to plant growth and can not absorbing be converted to blue violet light that the green element of Photosynthesis can be absorbed and utilized and
Blood orange light so as to change the light quality of the light through light altering film for agriculture, promotes absorption of the plant to nutrients such as nitrogen, phosphorus, potassium, zinc,
The blade area of plant and expansion degree are improved, increases the plant height of plant and petiole length, thus increases the content of leaf chlorophyll,
The photosynthate content in blade is increased, promotes plant growth.
So far, it can be used to process light altering film for agriculture and can preferably promote the critical material light conversion agent of crop growth,
Although having had made some progress, there are still it is many problem of：(1) containing trivalent europium ion (Eu3+) organic ligand rare earth turn
Photo etching can absorb 240~420nm ultraviolet lights, launches the blood orange light of 580~630nm, advantage is original intensity height, to carrying
Full period yield and the quality effect of high crop are notable, but it only absorbs ultraviolet light and emission spectrum is narrow, the absorbing wavelength with plant
Matching is poor, the easy photodissociation under sunlight, and cost is higher；(2) Anthraquinones, Pyrazine or acridine fluorochrome,
Advantage is not only to absorb ultraviolet light but also absorb green-yellow light, but its emission spectrum and the Wavelength matched property of plant absorption are poor, of high cost,
And the short strength retrogression of fluorescence lifetime is fast；(3) containing europium (Eu2+) alkaline earth sulfide inorganic rare earth light conversion agent, can inhale
The blood orange light or absorb ultraviolet light and green-yellow light simultaneously that 280~400nm ultraviolet light emissions in receipts natural light go out, transmitting is blue
Purple light, blood orange light, and it is with wide emission band, emission spectrum is opposite with spectrum needed for photosynthesis of plant coincide with
And turn the advantages of light intensity decays are slower, but its original intensity is not so good as organic RE light conversion agent, and easy deliquescence in air, illumination
Under it is oxidizable.
Rear-earth-doped nitride phosphor is because of its structural stability height, and excitation wavelength range is wide, and launch wavelength is adjustable, physics
Property is stablized, and luminous efficiency is high, and the excellent performance such as nontoxic receives the very big concern of scientific circles and LED industry circle.It is and existing
Patent and pertinent literature there are no using such nitride red fluorescent powder as Light Conversion Agent Used in Agricultural Films.
Invention content
In order to overcome the shortcomings and deficiencies of the prior art described above, primary and foremost purpose of the invention is that providing one kind turns light agriculture
Film.The light altering film for agriculture using nitride red fluorescent powder as light conversion agent, can by the purple light (200~400nm) in sunlight and
Green-yellow light (400~550nm) for accounting for solar spectrum energy larger proportion etc. is converted to the blood orange light that can promote crop growth
(550~800nm).
Another object of the present invention is to provide the preparation method of above-mentioned light altering film for agriculture.
It is still another object of the present invention to provide above-mentioned light altering film for agriculture agriculture field application.
The purpose of the present invention is realized by following proposal：
A kind of light altering film for agriculture mainly includes light conversion agent master batch and film matrix, and wherein light conversion agent master batch is by following quality point
Several component compositions：
Nitride red light conversion agent 10~50%
Auxiliary agent 1~10%
Master batch matrix surplus.
The structural formula of the nitride red light conversion agent can be M2-xSi5N8:XRE or M1-yAlSiN3:One kind in yRE
Or it is a variety of, wherein：0<x<2,0<y<0.5；M can be at least one of Mg, Ca, Sr, Ba, Zn and Cd；RE can be Eu or Eu with
At least one of five kinds of rare earth metals of Tm, Nd, Er, Ho, Dy.
Preferably, the M is at least one of alkaline-earth metal Ca, Sr or Ba；The RE is Eu or Eu and Tm,
At least one of tri- kinds of thuliums of Nd, Dy.
It is furthermore preferred that the M is two or more in alkaline-earth metal Ca, Sr or Ba.
The nitride red light conversion agent can be prepared by following methods：By chemical formula from alkaline-earth metal simple substance powder
Corresponding raw material simple substance is weighed in end, aluminium powder, silica flour and rare earth metal powder, is ground to be uniformly mixed, under an inert atmosphere 800
~1000 DEG C of 1~2h of melting, obtain presoma；After 1~2h of ball milling, by presoma in N21400~1600 DEG C of roastings under atmosphere
3~6h obtains required nitride red light conversion agent.
As synthesis M2-xSi5N8:During xRE, the molar ratio of alkaline-earth metal powder used, silica flour and rare earth metal powder is
(2-x):5:X, wherein 0<x<2；As synthesis M1-yAlSiN3:During yRE, alkaline-earth metal powder, aluminium powder, silica flour and rare earth used
The molar ratio of metal powder is (1-y):1:1:Y, wherein 0<y<0.5.
Preferably, as synthesis M2-xSi5N8:During xRE, alkaline-earth metal powder used, silica flour and rare earth metal powder rub
You are than being 1.96:5:0.04；As synthesis M1-yAlSiN3:During yRE, alkaline-earth metal powder used, aluminium powder, silica flour and rare earth gold
The molar ratio for belonging to powder is 0.96:1:1:0.04.
In order to preferably realize the present invention, the product after roasting is cooled down, is ground, pickling, washing, drying waited
Journey can obtain nitride red light conversion agent after purification.
The cooling, which preferably refers to, to be cooled to room temperature.
The acid can be one kind in nitric acid, hydrochloric acid and sulfuric acid, and preferably volume fraction is 10% nitric acid.
The master batch matrix can gather for low density polyethylene (LDPE), linear low density polyethylene, medium density polyethylene, high density
At least one of ethylene, polypropylene, ethylene-vinyl acetate resin and polyvinyl chloride.
The auxiliary agent can be polyethylene wax, vinyl bis-stearamides, zinc stearate, stearic acid pentaerythritol ester, gather
At least one of ethylene glycol, titanate coupling agent and aluminate coupling agent.
The film matrix can gather for low density polyethylene (LDPE), linear low density polyethylene, medium density polyethylene, high density
At least one of ethylene, polypropylene, ethylene-vinyl acetate resin and polyvinyl chloride, film matrix and master batch matrix can be with
It is identical to can also be different.
Preferably, above-mentioned film matrix is at least one of low density polyethylene (LDPE) and linear low density polyethylene.
In the light altering film for agriculture, nitride red light conversion agent quality can be the 0.01~20% of light altering film for agriculture quality.
Preferably, in the light altering film for agriculture, nitride red light conversion agent quality is the 0.5~2% of light altering film for agriculture quality.
The dosage of the film matrix is the 50~97% of light altering film for agriculture quality.
Preferably, the dosage of the film matrix is the 90~97% of light altering film for agriculture quality.
A kind of preparation method of the light altering film for agriculture, mainly includes the following steps that：
(1) by nitride red light conversion agent, master batch matrix and auxiliary agent after mixing, it is made through double screw extruder extrusion
Grain, obtains light conversion agent master batch；
(2) the light conversion agent master batch obtained in film matrix and step (1) is uniformly mixed, processing film forming obtains light altering film for agriculture.
Extruding pelletization described in step (1) is 100~400r/ through rotating speed preferably under 130~180 DEG C of operation temperature
The double screw extruder of min squeezes out, air-cooled granulation.
Processing film forming described in step (2) can be used including the progress such as rolling process and extrusion molding.
The light altering film for agriculture can effectively absorb the ultraviolet portion being harmful in sunlight to plant growth, and being converted into can promote
It into the blood orange light part of photosynthesis of plant, applied to agriculture field, can achieve the effect that increasing of quality and production, there is very high economy
Value.
The present invention mechanism be：
Representative nitride red fluorescent powder such as M2Si5N8:Eu、MAlSiN3:Eu has wider excitation band, exciting light
200~550nm of spectrum covering；Emission spectrum can cover 550~700nm, relatively be suitble to the spectrum needed for photosynthesis of plant；Lead to simultaneously
It crosses trivalent rare earth ions to be co-doped with replacing with cation, can also obtain excellent red long-afterglow luminescent properties, it can be in night or nothing
The long period persistently provides the blood orange light needed for photosynthesis of plant under conditions of sunlight.The present invention passes through this is nitride red
Master batch is first made in light conversion agent, is used further to manufacture agricultural film, can be pre-dispersed to the progress of nitride red light conversion agent, and it is red to improve nitride
Dispersibility of the color light conversion agent in film matrix, dust pollution when reducing execute-in-place.Nitride red light conversion agent is mixed into agriculture
In film so that film, which has, turns light effect, and good with photosynthesis of plant Spectral matching.
The present invention is had the following advantages and advantageous effect relative to the prior art：
(1) the nitride red light conversion agent sample particle size uniformity that the present invention is prepared with alloyage, dispersibility preferably, have
There are wide excitation (200~550nm) and emission band (550~700nm), can effectively absorb ultraviolet light and portion to plant pest
Divide green-yellow light, the blood orange light needed for plant growth is provided, it is preferable with photosynthesis of plant Spectral matching.Meanwhile nitride is red
Color light conversion agent also has that initial luminous brightness is high, and physicochemical properties are stable, not oxidizable under the slow and illumination that turns light intensity decays
The advantages that.
(2) it is co-doped with replacing with cationic moiety by trivalent rare earth ions, the nitride red light conversion agent of synthesis also obtains
Excellent red long-afterglow luminescent properties, can persistently provide Plant Light for a long time under the conditions of night or illumination are insufficient
The required blood orange light of cooperation extends the photosynthesis of plant time.
(3) it due to the excellent characteristics of luminescence of nitride red light conversion agent and nontoxic, can be directly used for preparing light conversion agent master batch
And light altering film for agriculture, reduce the step of being reprocessed to light conversion agent.Nitride red light conversion agent is first made master batch to be used further to manufacture
Agricultural film can carry out light conversion agent at pre-dispersed, dispersibility of the raising nitride feux rouges light conversion agent in film matrix, reduction scene
Dust pollution during operation.Nitride red light conversion agent is mixed in agricultural film so that film, which has, turns light effect, and and plant photosynthesis
Action spectrum matching is good；In the implantation methods that light altering film for agriculture is used to apply carbon dioxide simultaneously, matter is increased to plant yield-increasing and is played
Preferably effect, it is disease-free, without insect pest, without chemical pesticide, quality is good, improves yield etc., with obvious effects, there is very high warp
Ji value, there is large-scale promotion prospect.
Description of the drawings
Fig. 1 is the excitation and emission spectra figure of the nitride red light conversion agent prepared by embodiment 1,2,3,4 and 7.
Fig. 2 is that the light altering film for agriculture prepared by embodiment 12~14,16 and 19 turns light spectrum to sunlight.
Specific embodiment
With reference to embodiment and attached drawing, the present invention is described in further detail, but embodiments of the present invention are unlimited
In this.
Agents useful for same of the present invention is commercially available.
Embodiment 1：Nitride red light conversion agent Ca1.96Si5N8:The preparation of 0.04Eu
According to stoichiometric ratio, 1.96mol calcium powders, 5mol silica flours, 0.04mol europium powder are accurately weighed, and in agate mortar
Middle grinding 20min；Make raw material after mixing, be fitted into boron nitride crucible and be placed in melting in high temperature furnace；Melt stage, indifferent gas
Atmosphere is argon gas atmosphere, air-flow velocity 100mL/min, and high temperature furnace rises to 900 DEG C with the heating rate of 50 DEG C/min, heat preservation
1.5h.After high temperature furnace natural cooling room temperature, powder sample is transferred to tube furnace by gained presoma through ball mill by wet process ball milling 1h
Middle roasting；Firing stage, protective atmosphere are nitrogen atmosphere, and air-flow velocity 80mL/min, tube furnace is with the heating speed of 5 DEG C/min
Degree rises to 1450 DEG C, keeps the temperature 4h, is cooled to 550 DEG C with 5 DEG C of cooling rate later, cools to room temperature with the furnace.After roasting
After product grinding is thin, with nitric acid acidwashing of the percent by volume for 10%, deionization washing, 2~4 times repeatedly, mesh is obtained after dry
Mark nitride red light conversion agent.
Embodiment 2：Nitride red light conversion agent Sr1.96Si5N8:The preparation of 0.04Eu
According to stoichiometric ratio, 1.96mol strontiums powder, 5mol silica flours, 0.04mol europium powder are accurately weighed, and in agate mortar
Middle grinding 20min；Make raw material after mixing, be fitted into boron nitride crucible and be placed in melting in high temperature furnace；Melt stage, indifferent gas
Atmosphere is argon gas atmosphere, air-flow velocity 100mL/min, and high temperature furnace rises to 900 DEG C with the heating rate of 50 DEG C/min, heat preservation
1.5h.After high temperature furnace natural cooling room temperature, powder sample is transferred to tube furnace by gained presoma through ball mill by wet process ball milling 1h
Middle roasting；Firing stage, protective atmosphere are nitrogen atmosphere, and air-flow velocity 80mL/min, tube furnace is with the heating speed of 5 DEG C/min
Degree rises to 1450 DEG C, keeps the temperature 4h, is cooled to 550 DEG C with 5 DEG C of cooling rate later, cools to room temperature with the furnace.After roasting
After product grinding is thin, with nitric acid acidwashing of the percent by volume for 10%, deionization washing, 2~4 times repeatedly, mesh is obtained after dry
Mark nitride red light conversion agent.
Embodiment 3：Nitride red light conversion agent Ba1.96Si5N8:The preparation of 0.04Eu
According to stoichiometric ratio, 1.96mol barium powder, 5mol silica flours, 0.04mol europium powder are accurately weighed, and in agate mortar
Middle grinding 20min；Make raw material after mixing, be fitted into boron nitride crucible and be placed in melting in high temperature furnace；Melt stage, indifferent gas
Atmosphere is argon gas atmosphere, air-flow velocity 100mL/min, and high temperature furnace rises to 900 DEG C with the heating rate of 50 DEG C/min, heat preservation
1.5h.After high temperature furnace natural cooling room temperature, powder sample is transferred to tube furnace by gained presoma through ball mill by wet process ball milling 1h
Middle roasting；Firing stage, protective atmosphere are nitrogen atmosphere, and air-flow velocity 80mL/min, tube furnace is with the heating speed of 5 DEG C/min
Degree rises to 1450 DEG C, keeps the temperature 4h, is cooled to 550 DEG C with 5 DEG C of cooling rate later, cools to room temperature with the furnace.After roasting
After product grinding is thin, with nitric acid acidwashing of the percent by volume for 10%, deionization washing, 2~4 times repeatedly, mesh is obtained after dry
Mark nitride red light conversion agent.
Embodiment 4：Nitride red light conversion agent CaSr0.96Si5N8:The preparation of 0.04Eu
According to stoichiometric ratio, 1mol calcium powders, 0.96mol strontiums powder, 5mol silica flours, 0.04mol europium powder are accurately weighed, and
20min is ground in agate mortar；Make raw material after mixing, be fitted into boron nitride crucible and be placed in melting in high temperature furnace；Melt rank
Section, inert atmosphere are argon gas atmosphere, air-flow velocity 100mL/min, and high temperature furnace rises to 900 with the heating rate of 50 DEG C/min
DEG C, keep the temperature 1.5h.After high temperature furnace natural cooling room temperature, gained presoma shifts powder sample through ball mill by wet process ball milling 1h
To tubular type kiln roasting；Firing stage, protective atmosphere are nitrogen atmosphere, and air-flow velocity 80mL/min, tube furnace is with 5 DEG C/min
Heating rate rise to 1450 DEG C, keep the temperature 4h, be cooled to 550 DEG C with 5 DEG C of cooling rate later, cool to room temperature with the furnace.It will
It is 2~4 times repeatedly, dry with nitric acid acidwashing of the percent by volume for 10%, deionization washing after product grinding carefully after roasting
After obtain target nitride red light conversion agent.
Embodiment 5：Nitride red light conversion agent Sr0.96BaSi5N8:The preparation of 0.04Eu
According to stoichiometric ratio, 0.96mol strontiums powder, 1mol barium powder, 5mol silica flours, 0.04mol europium powder are accurately weighed, and
20min is ground in agate mortar；Make raw material after mixing, be fitted into boron nitride crucible and be placed in melting in high temperature furnace；Melt rank
Section, inert atmosphere are argon gas atmosphere, air-flow velocity 100mL/min, and high temperature furnace rises to 900 with the heating rate of 50 DEG C/min
DEG C, keep the temperature 1.5h.After high temperature furnace natural cooling room temperature, gained presoma shifts powder sample through ball mill by wet process ball milling 1h
To tubular type kiln roasting；Firing stage, protective atmosphere are nitrogen atmosphere, and air-flow velocity 80mL/min, tube furnace is with 5 DEG C/min
Heating rate rise to 1450 DEG C, keep the temperature 4h, be cooled to 550 DEG C with 5 DEG C of cooling rate later, cool to room temperature with the furnace.It will
It is 2~4 times repeatedly, dry with nitric acid acidwashing of the percent by volume for 10%, deionization washing after product grinding carefully after roasting
After obtain target nitride red light conversion agent.
Embodiment 6：Nitride red light conversion agent SrSi5N8:The preparation of 1Eu
According to stoichiometric ratio, 1mol strontiums powder, 5mol silica flours, 1mol europium powder are accurately weighed, and ground in agate mortar
20min；Make raw material after mixing, be fitted into boron nitride crucible and be placed in melting in high temperature furnace；Melt stage, inert atmosphere are argon
Gas atmosphere, air-flow velocity 100mL/min, high temperature furnace rise to 900 DEG C with the heating rate of 50 DEG C/min, keep the temperature 1.5h.High temperature
After stove natural cooling room temperature, powder sample is transferred to tubular type kiln roasting by gained presoma through ball mill by wet process ball milling 1h；Roasting
Burning stage, protective atmosphere are nitrogen atmosphere, air-flow velocity 80mL/min, and tube furnace is risen to the heating rate of 5 DEG C/min
1450 DEG C, 4h is kept the temperature, 550 DEG C is cooled to 5 DEG C of cooling rate later, cools to room temperature with the furnace.Product after roasting is ground
After levigate, with nitric acid acidwashing of the percent by volume for 10%, deionization washing, 2~4 times repeatedly, target nitridation is obtained after dry
Object red light conversion agent.
Embodiment 7：Nitride red light conversion agent Ca0.96AlSiN3:The preparation of 0.04Eu
According to stoichiometric ratio, 0.96mol calcium powders, 1mol aluminium powders, 1mol silica flours, 0.04mol europium powder are accurately weighed, and
20min is ground in agate mortar；Make raw material after mixing, be fitted into boron nitride crucible and be placed in melting in high temperature furnace；Melt rank
Section, inert atmosphere are argon gas atmosphere, air-flow velocity 100mL/min, and high temperature furnace rises to 900 with the heating rate of 50 DEG C/min
DEG C, keep the temperature 1.5h.After high temperature furnace natural cooling room temperature, gained presoma shifts powder sample through ball mill by wet process ball milling 1h
To tubular type kiln roasting；Firing stage, protective atmosphere are nitrogen atmosphere, and air-flow velocity 80mL/min, tube furnace is with 5 DEG C/min
Heating rate rise to 1550 DEG C, keep the temperature 4h, be cooled to 550 DEG C with 5 DEG C of cooling rate later, cool to room temperature with the furnace.It will
It is 2~4 times repeatedly, dry with nitric acid acidwashing of the percent by volume for 10%, deionization washing after product grinding carefully after roasting
After obtain target nitride red light conversion agent.
Embodiment 8：Nitride red light conversion agent Ca0.5Sr0.46AlSiN3:The preparation of 0.04Eu
According to stoichiometric ratio, accurately weigh 0.5mol calcium powders, 0.46mol strontiums powder, 1mol aluminium powders, 1mol silica flours,
0.04mol europium powder, and 20min is ground in agate mortar；Make raw material after mixing, be packed into boron nitride crucible and be placed in high temperature
It is melted in stove；Melt stage, inert atmosphere are argon gas atmosphere, and air-flow velocity 100mL/min, high temperature furnace is with the liter of 50 DEG C/min
Warm speed rises to 900 DEG C, keeps the temperature 1.5h.After high temperature furnace natural cooling room temperature, gained presoma, will through ball mill by wet process ball milling 1h
Powder sample is transferred to tubular type kiln roasting；Firing stage, protective atmosphere are nitrogen atmosphere, and air-flow velocity 80mL/min is managed
Formula stove rises to 1550 DEG C with the heating rate of 5 DEG C/min, keeps the temperature 4h, 550 DEG C is cooled to later with 5 DEG C of cooling rate, with stove
It is cooled to room temperature.By the product grinding after roasting it is thin after, washed with nitric acid acidwashing that percent by volume is 10%, deionization, instead
It is 2~4 times multiple, obtain target nitride red light conversion agent after dry.
Embodiment 9：Nitride red light conversion agent Ca1.96Si5N8:The preparation of 0.02Eu, 0.02Tm
According to stoichiometric ratio, 1.96mol calcium powders, 5mol silica flours, 0.02mol europiums powder, 0.02mol thulium powder are accurately weighed,
And 20min is ground in agate mortar；Make raw material after mixing, be fitted into boron nitride crucible and be placed in melting in high temperature furnace；It is molten
Melt the stage, inert atmosphere is argon gas atmosphere, air-flow velocity 100mL/min, and high temperature furnace is risen to the heating rate of 50 DEG C/min
900 DEG C, keep the temperature 1.5h.After high temperature furnace natural cooling room temperature, gained presoma turns powder sample through ball mill by wet process ball milling 1h
Move to tubular type kiln roasting；Firing stage, protective atmosphere are nitrogen atmosphere, air-flow velocity 80mL/min, tube furnace with 5 DEG C/
The heating rate of min rises to 1450 DEG C, keeps the temperature 4h, is cooled to 550 DEG C with 5 DEG C of cooling rate later, cools to room temperature with the furnace.
After the product grinding carefully after roasting, with nitric acid acidwashing of the percent by volume for 10%, deionization washing, 2~4 times repeatedly, do
Target nitride red light conversion agent is obtained after dry.
Embodiment 10：Nitride red light conversion agent Ca1.96Si5N8:The preparation of 0.01Eu, 0.02Tm, 0.01Dy
According to stoichiometric ratio, accurately weigh 1.96mol calcium powders, 5mol silica flours, 0.01mol europiums powder, 0.02mol thuliums powder,
0.01mol dysprosium powder, and 20min is ground in agate mortar；Make raw material after mixing, be packed into boron nitride crucible and be placed in high temperature
It is melted in stove；Melt stage, inert atmosphere are argon gas atmosphere, and air-flow velocity 100mL/min, high temperature furnace is with the liter of 50 DEG C/min
Warm speed rises to 900 DEG C, keeps the temperature 1.5h.After high temperature furnace natural cooling room temperature, gained presoma, will through ball mill by wet process ball milling 1h
Powder sample is transferred to tubular type kiln roasting；Firing stage, protective atmosphere are nitrogen atmosphere, and air-flow velocity 80mL/min is managed
Formula stove rises to 1450 DEG C with the heating rate of 5 DEG C/min, keeps the temperature 4h, 550 DEG C is cooled to later with 5 DEG C of cooling rate, with stove
It is cooled to room temperature.By the product grinding after roasting it is thin after, washed with nitric acid acidwashing that percent by volume is 10%, deionization, instead
It is 2~4 times multiple, obtain target nitride red light conversion agent after dry.
Embodiment 11：Nitride red light conversion agent CaSr0.96Si5N8:The preparation of 0.02Eu, 0.02Tm
According to stoichiometric ratio, accurately weigh 1mol calcium powders, 0.96mol strontiums powder, 5mol silica flours, 0.02mol europiums powder,
0.02mol thulium powder, and 20min is ground in agate mortar；Make raw material after mixing, be packed into boron nitride crucible and be placed in high temperature
It is melted in stove；Melt stage, inert atmosphere are argon gas atmosphere, and air-flow velocity 100mL/min, high temperature furnace is with the liter of 50 DEG C/min
Warm speed rises to 900 DEG C, keeps the temperature 1.5h.After high temperature furnace natural cooling room temperature, gained presoma, will through ball mill by wet process ball milling 1h
Powder sample is transferred to tubular type kiln roasting；Firing stage, protective atmosphere are nitrogen atmosphere, and air-flow velocity 80mL/min is managed
Formula stove rises to 1450 DEG C with the heating rate of 5 DEG C/min, keeps the temperature 4h, 550 DEG C is cooled to later with 5 DEG C of cooling rate, with stove
It is cooled to room temperature.By the product grinding after roasting it is thin after, washed with nitric acid acidwashing that percent by volume is 10%, deionization, instead
It is 2~4 times multiple, obtain target nitride red light conversion agent after dry.
Embodiment 12：The preparation of light altering film for agriculture
Take the nitride red light conversion agent 150kg of the embodiment of the present invention 1, low density polyethylene (LDPE) (LDPE Q210, Chinese stone
Change Shanghai Petrochemical Co. Ltd.) 50kg, linear low density polyethylene (LLDPE YLF-1802, Sinopec Yangtze
Petrochemical industry Co., Ltd) 100kg, vinyl bis-stearamides (EBS, Dongguan Ding Hai plastic cement Chemical Co., Ltd.) 5kg, sequentially
Be added to high-speed mixer, after being stirred evenly with high-speed mixer, operation temperature at 130~180 DEG C, through rotating speed for 100~
The double screw extruder of 400r/min squeezes out, and air-cooled granulation is prepared into master batch.
Take the master batch 30kg prepared by the present embodiment, low density polyethylene (LDPE) (LDPE Q210, Sinopec Shanghai oil
Work limited company) 305kg, (LLDPE YLF-1802, Sinopec Yangtze petrochemical industry are limited for linear low density polyethylene
Company) 405kg, after mixing with inflation film manufacturing machine blown film, required light altering film for agriculture is obtained, gained film thickness is 90 microns.Wherein
Inflation film manufacturing machine melting temperature is 180 DEG C, and die head temperature is 160 DEG C.
Embodiment 13：The preparation of light altering film for agriculture
Take the nitride red light conversion agent 70kg prepared by the embodiment of the present invention 2, high density polyethylene (HDPE) (HHM5502, China
Maoming branch company of petrochemical industry limited company) 100kg, stearic acid pentaerythritol ester (PTES, Guangzhou Chuan Jinxin chemical industry section
Skill Co., Ltd) 8kg, high-speed mixer is sequentially added to, after being stirred evenly with high-speed mixer, in 130~180 DEG C of operation
Temperature is squeezed out through the double screw extruder that rotating speed is 100~400r/min, and air-cooled granulation is prepared into master batch.
Take the light conversion master batch 30kg prepared by the present embodiment, low density polyethylene (LDPE) (LDPE Q210, Sinopec Shanghai stone
Oily chemical inc) 260kg, linear low density polyethylene (LLDPE YLF-1802, Sinopec Yangtze petrochemical industry
Co., Ltd) 500kg, after mixing with inflation film manufacturing machine blown film, required light altering film for agriculture is obtained, gained film thickness is 90 microns.
Wherein inflation film manufacturing machine melting temperature is 180 DEG C, and die head temperature is 160 DEG C.
Embodiment 14：The preparation of light altering film for agriculture
Take the nitride red light conversion agent 100kg prepared by the embodiment of the present invention 3, polypropylene (EPC30R-H, China Petroleum
Chemical inc Maoming branch company) 220kg, polyethylene glycol (PEG400, Guangzhou Chang Hong Chemical Co., Ltd.s) 13kg,
High-speed mixer is sequentially added to, after being stirred evenly with high-speed mixer, operation temperature at 130~180 DEG C is through rotating speed
The double screw extruder of 100~400r/min squeezes out, and air-cooled granulation is prepared into master batch.
Take the light conversion master batch 30kg prepared by the present embodiment, low density polyethylene (LDPE) (LDPE Q210, Sinopec Shanghai stone
Oily chemical inc) 400kg, linear low density polyethylene (LLDPE YLF-1802, Sinopec Yangtze petrochemical industry
Co., Ltd) 460kg, after mixing with inflation film manufacturing machine blown film to get required light altering film for agriculture, gained film thickness is 90 micro-
Rice.Wherein inflation film manufacturing machine melting temperature is 180 DEG C, and die head temperature is 160 DEG C.
Embodiment 15：The preparation of light altering film for agriculture
Take the nitride red light conversion agent 100kg used in the embodiment of the present invention 4, polyvinyl chloride (SG-5, Xingjiang Tianye Co.'s (collection
Group) Co., Ltd) 400kg, titanate coupling agent (ZJ-130, Guangzhou Zhong Jie Chemical Industry Science Co., Ltd) 5.5kg sequentially throw
Be added to high-speed mixer, after being stirred evenly with high-speed mixer, operation temperature at 130~180 DEG C, through rotating speed for 100~
The double screw extruder of 400r/min squeezes out, and air-cooled granulation is prepared into master batch.
Take the light conversion master batch 60kg prepared by the present embodiment, low density polyethylene (LDPE) (LDPE Q210, Sinopec Shanghai stone
Oily chemical inc) 270kg, linear low density polyethylene (LLDPE YLF-1802, Sinopec Yangtze petrochemical industry
Co., Ltd) 300kg, after mixing with inflation film manufacturing machine blown film to get required light altering film for agriculture, gained film thickness is 90 micro-
Rice.Wherein inflation film manufacturing machine melting temperature is 180 DEG C, and die head temperature is 160 DEG C.
Embodiment 16：The preparation of light altering film for agriculture
Take the nitride red light conversion agent 20kg of the embodiment of the present invention 7, low density polyethylene (LDPE) (LDPE Q210, Sinopec
Shanghai Petrochemical Co. Ltd.) 50kg, linear low density polyethylene (LLDPE YLF-1802, Sinopec Yangtze stone
Oily Chemical Co., Ltd.) 110kg, zinc stearate (DZ-101, new east station of Guangzhou political affairs Chemical Co., Ltd.) 20kg, it is sequentially added at a high speed
Mixing machine, after being stirred evenly with high-speed mixer, operation temperature at 130~180 DEG C through rotating speed is 100~400r/min's
Double screw extruder squeezes out, and air-cooled granulation is prepared into master batch.
Take the light conversion master batch 30kg prepared by the present embodiment, low density polyethylene (LDPE) (LDPE Q210, Sinopec Shanghai stone
Oily chemical inc) 270kg, linear low density polyethylene (LLDPE YLF-1802, Sinopec Yangtze petrochemical industry
Co., Ltd) 300kg, after mixing with inflation film manufacturing machine blown film to get required light altering film for agriculture, gained film thickness is 90 micro-
Rice.Wherein inflation film manufacturing machine melting temperature is 180 DEG C, and die head temperature is 160 DEG C.
Embodiment 17：The preparation of light altering film for agriculture
Take the nitride red light conversion agent 100kg of the embodiment of the present invention 9, low density polyethylene (LDPE) (LDPE Q210, Chinese stone
Change Shanghai Petrochemical Co. Ltd.) 50kg, linear low density polyethylene (LLDPE YLF-1802, Sinopec Yangtze
Petrochemical industry Co., Ltd) 100kg, aluminate coupling agent (SG-AL821, the auspicious Chemical Co., Ltd. in Guangzhou City) 10kg, sequentially
Be added to high-speed mixer, after being stirred evenly with high-speed mixer, operation temperature at 130~180 DEG C, through rotating speed for 100~
The double screw extruder of 400r/min squeezes out, and air-cooled granulation is prepared into master batch.
Take the light conversion master batch 10kg prepared by the present embodiment, low density polyethylene (LDPE) (LDPE Q210, Sinopec Shanghai stone
Oily chemical inc) 90kg, linear low density polyethylene (LLDPE YLF-1802, Sinopec Yangtze petrochemical industry
Co., Ltd) 100kg, after mixing with inflation film manufacturing machine blown film to get required light altering film for agriculture, gained film thickness is 90 micro-
Rice.Wherein inflation film manufacturing machine melting temperature is 180 DEG C, and die head temperature is 160 DEG C.
Embodiment 18：The preparation of light altering film for agriculture
The nitride red light conversion agent 100kg of the embodiment of the present invention 11 is taken, (2604A adds ethylene-vinyl acetate resin
Put on airs AT) 150kg, aluminate coupling agent (SG-AL821, the auspicious Chemical Co., Ltd. in Guangzhou City) 10kg, it is sequentially added at a high speed
Mixing machine, after being stirred evenly with high-speed mixer, operation temperature at 130~180 DEG C through rotating speed is 100~400r/min's
Double screw extruder squeezes out, and air-cooled granulation is prepared into master batch.
Take the light conversion master batch 30kg prepared by the present embodiment, low density polyethylene (LDPE) (LDPE Q210, Sinopec Shanghai stone
Oily chemical inc) 305kg, linear low density polyethylene (LLDPE YLF-1802, Sinopec Yangtze petrochemical industry
Co., Ltd) 405kg, after mixing with inflation film manufacturing machine blown film to get required light altering film for agriculture, gained film thickness is 90 micro-
Rice.Wherein inflation film manufacturing machine melting temperature is 180 DEG C, and die head temperature is 160 DEG C.
Embodiment 19：The preparation of light altering film for agriculture
Take the nitride red light conversion agent 0kg of the embodiment of the present invention 5, low density polyethylene (LDPE) (LDPE Q210, Sinopec
Shanghai Petrochemical Co. Ltd.) 50kg, linear low density polyethylene (LLDPE YLF-1802, Sinopec Yangtze stone
Oily Chemical Co., Ltd.) 100kg, polyethylene wax (DT-200N, Guangzhou Duo Feng Chemical Co., Ltd.s) 5kg be sequentially added to height
Fast mixing machine.After being stirred evenly with high-speed mixer, operation temperature at 130~180 DEG C through rotating speed is 100~400r/min
Double screw extruder squeeze out, air-cooled granulation is prepared into master batch.
Take the light conversion master batch 30kg prepared by the present embodiment, low density polyethylene (LDPE) (LDPE Q210, Sinopec Shanghai stone
Oily chemical inc) 200kg, linear low density polyethylene (LLDPE YLF-1802, Sinopec Yangtze petrochemical industry
Co., Ltd) 600kg, after mixing with inflation film manufacturing machine blown film to get required light altering film for agriculture, gained film thickness is 90 micro-
Rice.Wherein inflation film manufacturing machine melting temperature is 180 DEG C, and die head temperature is 160 DEG C.
Fig. 1 is the excitation and emission spectra figure of nitride light conversion agent prepared in embodiment 1,2,3,4 and 7, wherein swashing
Hair wavelength is 450nm, and launch wavelength is respectively 603nm, 623nm, 580nm, 647nm and 690nm, has wider excitation
(200~50nm) and emission band (550~800nm), it is preferable with photosynthesis of plant Spectral matching.
Fig. 2 is that the light altering film for agriculture prepared by embodiment 12~14,16 and 19 turns light spectrum to sunlight.It can by spectrogram
Know, absorbing wavelength ranging from 200~450nm of the light altering film for agriculture prepared by embodiment 12~14,16 and 19 turns optical wavelength range
For 550~800nm, effectively the purple light (200~400nm) in sunlight and green-yellow light (400~550nm) part can be turned
Turn to wide-band spectrum, predominantly blood orange light (550~800nm), with photosynthesis of plant needed for Spectral matching it is preferable, can pole
The earth promotes photosynthesis of plant；In addition, nitride red light conversion agent is incorporated into film matrix, can improve to a certain extent
The intensity of illumination of film is crossed, improves the intensity of illumination of plant absorption.
Table 1 is the practical function data of light altering film for agriculture made from embodiment 13,17,18 and 19：Since in July, 2014 to
In September, 2014 is stopped, and has carried out the experimental tests of two batches of vegetables of mulching plant, the comparison film of use is respectively the embodiment of the present invention
13rd, light altering film for agriculture made from 17 and 18 and the comparison blank film obtained of embodiment 19.Experimental result is as shown in table 1.
The practical function data of 1 light altering film for agriculture of table
From table 1 it follows that the use of light altering film for agriculture can effectively facilitate vegetables precocity and reach effect of increasing production, and work as institute
Light conversion agent in light altering film for agriculture be co-doped with through trivalent rare earth ions or cation replace, twilight sunset effect can be improved so that
Vegetables precocity and effect of increasing production are more preferable.
Above-described embodiment is the preferable embodiment of the present invention, but embodiments of the present invention are not by above-described embodiment
Limitation, other any Spirit Essences without departing from the present invention with made under principle change, modification, replacement, combine, simplification,
Equivalent substitute mode is should be, is included within protection scope of the present invention.
Claims (8)
1. a kind of light altering film for agriculture, it is characterised in that：Including light conversion agent master batch and film matrix, wherein, light conversion agent master batch is by following
The component composition of mass fraction：
Nitride red light conversion agent 10~50%
Auxiliary agent 1~10%
Master batch matrix surplus；
The structural formula of the nitride red light conversion agent is M2-xSi5N8:XRE or M1-yAlSiN3:It is one or more in yRE,
Wherein：0 ＜ x ＜, 2,0 ＜ y ＜ 0.5；M is at least one of Ca, Sr and Ba；RE is in Eu and two kinds of rare earth metals of Tm, Dy
It is at least one.
2. light altering film for agriculture according to claim 1, it is characterised in that：
In the light altering film for agriculture, the quality of nitride red light conversion agent is the 0.01~20% of light altering film for agriculture quality；Film base
The dosage of body is the 50~97% of light altering film for agriculture quality.
3. light altering film for agriculture according to claim 1, it is characterised in that：
In the light altering film for agriculture, the quality of nitride red light conversion agent is the 0.5~2% of light altering film for agriculture quality；Film matrix
Dosage be light altering film for agriculture quality 90~97%.
4. light altering film for agriculture according to claim 1, it is characterised in that：
The nitride red light conversion agent is prepared by following methods：According to chemical formula from alkaline-earth metal elemental powders, aluminium
Corresponding raw material simple substance is weighed in powder, silica flour and rare earth metal powder, is ground to be uniformly mixed, under an inert atmosphere 800~
1~2h is melted at 1000 DEG C, obtains presoma；After 1~2h of ball milling, by gained presoma in N21400~1600 DEG C of roastings under atmosphere
3~6h is burnt, obtains required nitride red light conversion agent；
As synthesis M2-xSi5N8:During xRE, the molar ratio of alkaline-earth metal powder used, silica flour and rare earth metal powder is (2-x):
5:X, wherein 0 ＜ x ＜ 2；
As synthesis M1-yAlSiN3:During yRE, alkaline-earth metal powder used, aluminium powder, silica flour and rare earth metal powder molar ratio be
(1-y):1:1:Y, wherein 0 ＜ y ＜ 0.5.
5. light altering film for agriculture according to claim 1, it is characterised in that：
The master batch matrix for low density polyethylene (LDPE), linear low density polyethylene, medium density polyethylene, high density polyethylene (HDPE),
At least one of polypropylene, ethylene-vinyl acetate resin and polyvinyl chloride；
The auxiliary agent for polyethylene wax, vinyl bis-stearamides, zinc stearate, stearic acid pentaerythritol ester, polyethylene glycol,
At least one of titanate coupling agent and aluminate coupling agent；
The film matrix for low density polyethylene (LDPE), linear low density polyethylene, medium density polyethylene, high density polyethylene (HDPE),
At least one of polypropylene, ethylene-vinyl acetate resin and polyvinyl chloride.
6. a kind of preparation method according to Claims 1 to 5 any one of them light altering film for agriculture, it is characterised in that including following step
Suddenly：
(1) by nitride red light conversion agent, master batch matrix and auxiliary agent after mixing, through double screw extruder extruding pelletization,
Obtain light conversion agent master batch；
(2) the light conversion agent master batch of gained in film matrix, step (1) is uniformly mixed, processing film forming obtains light altering film for agriculture.
7. the preparation method of light altering film for agriculture according to claim 6, it is characterised in that：
Extruding pelletization described in step (1) refers under 130~180 DEG C of operation temperature through rotating speed as 100~400r/min's
Double screw extruder squeezes out, air-cooled granulation；
Processing film forming described in step (2) refers to using rolling process or extrusion molding progress.
8. Claims 1 to 5 any one of them light altering film for agriculture is in the application of agriculture field.
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| CN105713288B (en) * | 2016-03-30 | 2017-12-26 | 华南农业大学 | One kind turns light conversion farm film and preparation method and application |
| CN106318382A (en) * | 2016-08-24 | 2017-01-11 | 甘肃稀土新材料股份有限公司 | Nitride red steady persistence material and preparing method thereof |
| CN106349543B (en) * | 2016-08-30 | 2018-07-10 | 四川省有色冶金研究院有限公司 | A kind of compounding rare earth application conversion film and preparation method thereof |
| CN106554453B (en) * | 2016-10-12 | 2018-10-09 | 沈阳大学 | A kind of agricultural light conversion film material and preparation method thereof |
| CN107474830A (en) * | 2017-06-26 | 2017-12-15 | 浙江转喆科技有限公司 | A kind of light conversion agent and preparation method thereof and agricultural blue conversion film and preparation method thereof |
| CN107488451A (en) * | 2017-06-26 | 2017-12-19 | 浙江转喆科技有限公司 | A kind of light conversion agent and preparation method thereof and agricultural red conversion film and preparation method thereof |
| CN109263216A (en) * | 2018-08-27 | 2019-01-25 | 上海骊塑商贸有限公司 | A kind of scattering energy saving film that self-adaptive temperature is adjusted |
| CN111302315B (en) * | 2020-03-16 | 2023-02-17 | 昆明学院 | Preparation method and application of nitrogen-carbon-based light conversion agent, light conversion plastic film and preparation method thereof |
| KR20220155312A (en) * | 2020-03-30 | 2022-11-22 | 덴카 주식회사 | Phosphor powder, composite, light emitting device and method for producing phosphor powder |
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