CN1317537A - Single-base dual-energy light-transforming agent and its preparing prcess and application - Google Patents
Single-base dual-energy light-transforming agent and its preparing prcess and application Download PDFInfo
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Abstract
A single-base dual-function light-transforming agent uses the sulfide of alkali-earth metal as matrix, Eu and Cu ions as co-activating agent and other metal ions as sensing agent, and has a formula Mg1-m-n-kCamSrnBakS: Eu2+, yCu+, 2RE2, qTM, where RE is one or two of Y, La, Ce, Pr, Nd, Sm, Gd, Tb, Dy, Ho, Er, Tm, Yb and Lu and TM is one or two of Bi, Sb, Mn and Pb. It is prepared through mixing the sulfates of Mg, Ca, SR, Ba, or Cu with the oxides of Eu, RE, or TM and high-temp solid-phase reaction. It can transfer the near ultraviolet light and green light to blue and red light to promote photosynthesis of plant.
Description
The invention belongs to the technical field of luminescent materials, and relates to an agricultural film single-base dual-energy light conversion agent capable of simultaneously converting ultraviolet light and green light in sunlight into blue light and red light capable of effectively promoting plant growth, and a manufacturing method and an application method thereof.
Sunlight is a necessary condition for plant growth, but not all bands of light in the sunlight are beneficial to plant growth, and the effect of light on plants is closely related to the quality of light, namely spectral composition. Each plant should have its specific optimal growth spectrum. The plant can grow fast, increase yield and improve quality under the optimal growth action spectrum condition. However, the spectrum of sunlight incident normally to the ground is not the optimum spectrum for crop growth. Therefore, the research on the optimal action spectrum of the crop growth and the artificial simulation thereof have important academic value and practical significance.
Based on the general rule that chlorophyll (chla, chlb) has strong absorption for blue light and red light and little absorption for ultraviolet light and green light, some luminescent materials capable of absorbing ultraviolet light to emit blue light (or red light) and absorbing green light to emit red light have been used to improve crop lighting conditions. Russia, Japan, China, Korea, etc. have been reported. Particularly, in recent years, research reports about light conversion agents in China are increasing, and the researches prove that the light conversion performance of the luminescent material can be used for improving the illumination condition of crops, namely increasing the blue light irradiation or red light irradiation degree of plants; the farmland experiment also shows that the increase of the irradiation intensity of the red (blue) light of the crops can lead the roots of the crops to be developed, the stems and leaves to be flourishing, the yield and income increase and the quality to be superior.
Researches show that light, magnetism and gas have the effects of promoting the growth of plants and inhibiting certain diseases and insect pests. Therefore, scientists have considered light, magnetism and gas as fertilizers, which are called light fertilizer, magnetic fertilizer and gas fertilizer, respectively, and this is a new type of environmental-friendly fertilizer following "chemical fertilizer". The effect of inhibiting plant diseases and insect pests is regarded as a physical insect prevention effect and can be regarded as a physical pesticide. The single-base dual-energy rare earth light conversion agent has the functions of fertilizer efficiency and pesticide effect, and gives new significance to the agricultural film.
The light conversion film is used for cultivating crops, the sunlight which is given to people by nature and can be enjoyed is fully utilized, so that chemical materials and pesticides are reduced to be finally cancelled, high-efficiency ecological agriculture is really realized, and green food is developed.
CN1105040A, CN1122814A and CN1132219A all describe the application of rare earth europium organic complexes in agricultural films, and the invention utilizes the europium organic complexes to convert near ultraviolet light into orange red light. However, in this invention, red light is only used as effective light for plant cultivation, and the effectiveness of blue light on plants is not considered, so that the action of chlorophyll a, b and carotenes using blue light is inhibited, which may cause adverse effects. Plant pigments have two absorption types as shown below, and in the formation of photomorphogenetic response, pft type having a plant growth promoting effect is subjected to mutual light conversion by pr type R and light (light centered at 670 nm) and fr light (light centered at 725 nm), and it is known that not only the intensity of light but also the light quality have an important influence on the growth and development of plants.
CN1072945A describes the application of a kind of fluorescent pigment as a light conversion agent in agricultural films, and the invention converts near ultraviolet light and green light into blue light and red light respectively by two kinds of fluorescent pigments. The fluorescent dye is characterized by comprising a fluorescent dye (A) with the maximum absorption of 350-450 nm, preferably 370-430 nm, the maximum luminescence of 380-520 nm, preferably 400-460 nm, and a fluorescent dye (B) with the maximum absorption of 460-580nm, preferably 480-550nm, the maximum luminescence of 540-800nm, and the maximum emission of 570-700nm, wherein the luminescence spectrum of (A) and the absorption spectrum of (B) are partially overlapped. The invention realizes the simultaneous conversion of near ultraviolet light and green light into blue light and red light by two light conversion materials.
The invention aims to provide a single-base dual-energy rare earth light conversion agent which can convert one part of near ultraviolet light into blue light, convert the other part of the near ultraviolet light into red light and simultaneously convert the green light into the red light. The term "single-radical dual-energy" as used herein means that a single-matrix compound has the function of simultaneously converting ultraviolet light and green light and simultaneously emitting blue light and red light, with the result that after sunlight irradiated onto the wavelength conversion material of the present invention is transmitted, the near-ultraviolet light and green light are reduced, while the blue light and red light are increased.
The object of the present inventionis achieved in the following manner. The single-matrix dual-function light conversion agent takes alkaline earth metal sulfide as a matrix and rare earth ions Eu2+And transition metal ion Cu+The composition formula of the co-excitation lingual agent is as follows:
Mg1-m-n-kCamSrnBakS:xEu2+,yCu+zRE2, qTM wherein: RE = Y, La, Ce, Pr, Nd, Sm, Gd, Tb, Dy, Ho, Er, Tm, Yb, Lu,
TM = Bi, one or two of Sb, Mn and Pb,
0≤m≤1.0, 0≤n≤1.0, 0≤k≤1.0
0≤x≤2×10-3％； 0≤y≤5×10-3％
0≤z≤1×10-4％； 0≤q≤1×10-4% single-base dual-energy rare earth light conversion agent, the maximum excitation wavelength is in the region of 300-350nm and 480-580nm, and the maximum emission wavelength is in the region of 420-450nm and 620-680 nm. That is, the mono-based dual energy means that one compound absorbs ultraviolet light and green light at the same time and emits blue light and red light at the same time. The light conversion mechanism of the invention is that one part of near ultraviolet light is converted into blue light and the other part is converted into red light through the luminescence and sensitization of rare earth ions and transition metal ions in alkaline earth metal sulfide, and simultaneously, the green light is converted into the red light. The alkaline earth metal sulfide may be a monobasic alkaline earth metal sulfide, or a dibasic alkaline earth metal sulfide or a tribasic alkaline earth metal sulfide.
By adjusting Mg1-m-n-kCamSrnBakThe species and the content of the cations in the S, the species and the content of the activator ions regulate the matching between the excitation spectrum of the light conversion agent and the reflection spectrum of the plants, and the matching between the emission spectrum of the light conversion agent and the absorption spectrum of the plants. The Stokes shift (difference between the maximum luminescence wavelength and the maximum absorption wavelength) of the single-base dual-energy rare earth light conversion agent is not large to a certain extent, so that the Stokes shift of the invention is at least 50 nm.
In the composition formula, when y =0, the single-base dual-energy light conversion agent is changed into a red light agent, the maximum excitation wavelength of the red light agent is in the region of 280-350nm and 480-580nm, and the maximum emission wavelength is in the region of 620-680 nm.
When x =0 in the general formula, the single-base dual-energy light conversion agent is changed into a blue light agent, the maximum excitation wavelength of the blue light agent is in the range of 270-350nm, and the maximum emission wavelength is in the range of 420-450 nm. The red light agent and the blue light agent are two limit types of the double-energy light conversion agent.
The invented manufacturing method of single-base dual-energy light conversion agent is (1) according to the composition in general formula of single-base dual-energy light conversion agent the sulfates of Mg, Ca, Sr, Ba and Cu and Eu are calculated2+Weight of RE, TM oxides; (2) push button Calculating the weight of the reducing agent activated carbon by a reaction equation; (3) adding 5-10% (weight percentage) of fluxing agent: such as alkali metal sulfates, alkaline earth metal halides, and ammonium halides. (4) After the raw materials are uniformly mixed, the single-base dual-energy light conversion agent is synthesized by adopting a high-temperature solid-phase reaction in one step, wherein the synthesis temperature is 1100-1200 ℃, and the burning time is 1-3 hours.
The following are non-limiting examples of the synthesis of the single-base dual-energy rare earth light conversion agent of the present invention:
example 1: the single-base dual-energy light conversion agent (A) CaS, Cu, Eu, Tb and Bi
The specific synthetic steps are as follows: the product is synthesized by adopting high-temperature solid-phase reaction. Weighing CaSO according to stoichiometric ratio4136.14g,CuSO4798mg,Eu2O3176mg,Tb4O718.6mg,Bi2O346.4mg,NH4Cl1.07g and active carbon 176.29g (or raw materials are prepared according to the proportion). After the mixture is ground evenly, the mixture is put into a quartz crucible or a corundum crucible, and a quartz test tube is put into a high-temperature furnace with weak reducing gas and burned for 2 hours at the temperature of 1100-1200 ℃. And gradually cooling to obtain the sample.
The characteristic excitation spectrum and emission spectrum of the single-base dual-energy rare earth light conversion agent (A) are shown in figures 1 and 2. FIGS. 1 and 2 show that the single-base dual-energy rare earth light conversion agent (C) can convert near-ultraviolet light and green light into blue light and red light simultaneously.
Example 2: single-base dual-energy rare-earth light conversion agent (B) Ca0.6Mg0.4S:Cu,Eu,Tb,Bi
The specific synthetic steps are as follows: the product is synthesized by adopting high-temperature solid-phase reaction. Weighing CaSO according to stoichiometric ratio481.684g,MgSO448.124g,CuSO4798mg,Eu2O3176mg,Tb4O718.6mg,Bi2O346.4mg,Na2SO42.38g,NH4Cl1.07g and active carbon 176.29g (or raw materials are prepared according to the proportion). After the mixture is evenly ground, the mixture is put into a quartz crucible or a corundum crucible and is burnt for 2 hours at the temperature of 1100-1200 ℃. And gradually cooling to obtain the sample.
The characteristic excitation spectrum and emission spectrum of the single-base dual-energy rare earth light conversion agent (B) are shown in figures 1 and 2. FIGS. 1 and 2 show that the single-base dual-energy rare earth light conversion agent (B) can simultaneously convert near-ultraviolet light and green light into blue light and red light.
Example 3: single-base dual-energy rare-earth light conversion agent (C) Ca0.5Sr0.5S:Cu,Eu,Ce,Mn
The specific synthetic steps are as follows: the product is synthesized by adopting high-temperature solid-phase reaction. Weighing CaSO according to stoichiometric ratio468.078g,SrSO491.81g,CuSO4798mg,Eu2O3176mg,Tb4O718.6mg,Bi2O346.4mg,Na2SO42.38g,CaF21.18g,NH4Cl1.07g and active carbon 176.29g (or raw materials are prepared according to the proportion). After the mixture is evenly ground, the mixture is put into a quartz crucible or a corundum crucible and is burnt for 2 hours at 1100-1200 ℃. And gradually cooling to obtain the sample.
The characteristic excitation spectrum and emission spectrum of the single-base dual-energy light conversion agent (C) are shown in FIGS. 1 and 2. FIGS. 1 and 2 show that the single-base dual-energy rare earth light conversion agent (C) can convert near-ultraviolet light and green light into blue light and red light simultaneously.
Example 4: red light agent (D) CaS Eu, Dy, Bi
The specific synthetic steps are as follows: the product is synthesized by adopting high-temperature solid-phase reaction. Weighing CaSO according to stoichiometric ratio4136.14g,Eu2O3176mg,CeO217.21mg,Dy2O337.3mg,Na2SO42.38g,CaF21.18g,NH4Cl1.07g and active carbon 176.29g (or raw materials are prepared according to the proportion). After the mixture is evenly ground, the mixture is put into a quartz crucible or a corundum crucible and is burnt for 2 hours at the temperature of 1100-1200 ℃. And gradually cooling to obtain the sample.
The characteristic excitation spectrum and emission spectrum of red light agent (D) are shown in fig. 3. FIG. 3 shows that red (D) can convert near UV light and green light simultaneously to red light.
Example 5: bluing agent (E) CaS, Cu, Er, Bi
The specific synthetic steps are as follows: the product is synthesized by adopting high-temperature solid-phase reaction. Weighing CaSO according to stoichiometric ratio4136.14g,CuSO4798mg,Er2O319.13mg,Bi2O346.4mg,Na2SO42.38g,CaF21.18g,NH4Cl1.07g and active carbon 176.29g (or raw materials are prepared according to the proportion). After the mixture is evenly ground, the mixture is put into a quartz crucible or a corundum crucible and is burnt for 2 hours at the temperature of 1100-1200 ℃. And gradually cooling to obtain the sample.
The characteristic excitation spectrum and emission spectrum of the bluing agent (E) are shown in fig. 4. Fig. 4 shows that red (E) converts near uv light to blue light.
The light conversion agent can be used for being melted with plastic raw materials to prepare agricultural plastic products with various functions:
1. double-energy light conversion master batch (I).
Example (c): 96Kg of polyethylene and 4Kg of dual-energy light conversion agent (A) are mixed, dispersed, melted and extruded into granules, thus obtaining the dual-energy light conversion master batch.
2. And (3) a dual-energy light-conversion antifogging master batch (II).
Example (c): 86Kg of polyethylene, 4Kg of dual-energy light conversion agent (A) and 4Kg of dehazing agent FY-1 or FY-210 Kg of polyethylene are mixed, dispersed, melted and extruded into particles to obtain the dual-energy light conversion antifogging master batch.
3. Multifunctional master batch (III).
Example (c): polyethylene 46Kg, dual-energy light conversion agent (A)4Kg, dehazing agent FY-1 or FY-210 Kg, dripping agent 10Kg, light stabilizer Chmmassorb944LD 5Kg, heat insulating agent CaCO325Kg, mixing, dispersing, melting, extruding and granulating to obtain the multifunctional master batch. The multifunctional master batch has the functions of light conversion, fog prevention and heat preservation.
The single-base dual-energy rare earth light conversion agent can be used for preparing agricultural plastic products with various functions: the double-energy light conversion rare earth master batch is added into high molecular resin according to 0.1-1.0% of the effective concentration of a light conversion agent and is applied to manufacturing light conversion agricultural films, agricultural greenhouse light conversion plates and other materials applied to plant cultivation.
4. Agricultural film
Example (c): 25Kg of light conversion master batch and 975Kg of polyethylene are mixed, dispersed, melted, extruded and blown to obtain the double-energy light conversion agricultural film with various thicknesses, which is superior to the common plastic film for greenhouses.
5. Dual-energy light conversion plate
Example (c): 10Kg of light conversion master batch (I) and 990Kg of polyethylene are mixed, dispersed, melted and extruded to form the double-energy light conversion plate with various thicknesses, which is used for replacing common glass for greenhouses.
6. The single-base dual-energy light conversion agent spraying liquid is used as a light functional additive to be directly sprayed on plants.
Example (c): 1.0Kg of single-base dual-energy light conversion agent, 5.0Kg of polyacrylic resin, 10.0Kg of ethanol and 984Kg of water, the polyacrylic resin is fully dissolved in the ethanol, the light conversion agent is added, the mixture is fully stirred, and then the water is added for dilution. The prepared light conversion agent spray liquid is directly sprayed on the leaf surfaces of plants by a spraying device, and the photosynthesis of the plants can be promoted.
The dual-energy light conversion agricultural film and the dual-energy light conversion plate are used in greenhouse gardening, and are found to have at least one of the following functions:
temperature increasing and adjusting: the temperature in the greenhouse can be increased in low-temperature seasons to prevent crops from being frozen, and the temperature in the greenhouse can be reduced in high-temperature seasons to prevent crops from being burnt.
High-quality precocity: can make crops mature earlier and optimize the quality.
And (3) increasing yield and income: can increase the single yield of crops andincrease the income.
And (3) disease and pest prevention: the red light has a preventive effect on pests such as insects and whiteflies, so that the use of pesticides in the greenhouse film can be greatly reduced.
The effect of the present invention can be confirmed in fig. 5 and table 1. And (4) conclusion:
1. the present invention relates to a single-base double-energy light conversion agent which is an alkaline earth metal sulfide rare earth luminescent material.
2. The alkaline earth metal sulfide may be a monobasic alkaline earth metal sulfide, a dibasic alkaline earth metal sulfide or a tribasic alkaline earth metal sulfide
3. The chemical composition of single-base dual-energy light conversion agent is mainly characterized by that it uses alkaline earth metal sulfide as matrix and uses rare earth ion Eu2+And transition metal ion Cu+Is a co-activator and the other metal ions are sensitizers.
4. The main characteristics of the excitation spectrum of the single-base dual-energy light conversion agent are that the strongest excitation wavelength is in an ultraviolet region of 330nm and a green region of 540 nm. Namely, the single-base dual-energy rare earth light conversion agent can be simultaneously excited by ultraviolet light and green light.
5. The main characteristics of the excitation spectrum of the single-base dual-energy light conversion agent are that the strongest emission wavelength is in a blue light region of 430nm and a red light region of 650 nm. Namely, the single-base dual-energy rare earth light conversion agent simultaneously emits blue light and red light.
6. The single-base dual-energy light conversion agent can convert near ultraviolet light and green light in the spectrum ofartificial light sources used in sunlight, plant workshops and the like into blue light and orange-red light which are effective for plant growth.
7. The single-base dual-energy light conversion agent can convert ultraviolet light with low photosynthesis efficiency and centered at 300nm into blue light with 430nm as the center and red light with 650nm as the center.
8. The single-base dual-energy light conversion agent can convert green light with low photosynthesis efficiency and with the center of 550nm into red light with the center of 650 nm.
9. The agricultural products processed by the single-base dual-energy light conversion agent are particularly suitable for crops cultivated in low-temperature and low-illumination areas.
10. The agricultural product processed by the single-base dual-energy light conversion agent can prevent diseases and insect pests.
11. The agricultural products processed by the single-base dual-energy rare earth light conversion agent can make crops mature earlier and optimize the quality.
12. The agricultural products processed by the single-base dual-energy rare earth light conversion agent can be used for crops.
13. The invention can also be used in the fields of building materials, industrial arts and the like.
Description of the drawings:
FIG. 1: excitation spectrum of light conversion agent of the invention
FIG. 2: emission spectrum of light conversion agent of the invention
FIG. 3: excitation and emission spectra of red agents
FIG. 4: excitation spectrum and emission spectrum of bluing agent
FIG. 5: relationship diagram of temperature and air temperature in plastic film greenhouse
TABLE 1 agricultural test investigation of light conversion films
| Variety of test | Membranes | Test area (m2) | Time of sowing (moon/day) | Time of transplantation (moon/day) | Time of initial picking (moon/day) | Growth period (sky) | Actual cell yield (Kg) | Reduced yield per mu (Kg) | Increase of yield (％) |
| Cucumber (Cucumis sativus) Bean Water spinach | R W R W R W R W R W R W R W R W | 35.0 8.0 0.3 0.3 36.0 30.0 0.23 0.23 0.27 0.27 23.0 23.0 0.1 0.1 0.03 0.03 | 3/8 3/8 3/9 3/9 4/11 4/11 / / 2/5 2/5 4/8 4/2 4/1 4/1 4/10 4/10 | 4/10 4/10 4/13 4/13 4/19 4/19 4/4 4/4 4/13 4/13 / / / / / / | 5/15 5/21 5/21 5/23 6/9 6/14 5/17 5/17 5/29 6/7 5/4 5/1 4/25 4/25 5/16 5/24 | 68 74 73 75 59 64 43 43 115 124 26 29 24 24 36 44 | 366.5 63.7 1800 1500 143 75 271 224 650 525 218 156 105 76 68 49 | 6984.4 5311.0 6000.0 5000.0 2649.0 1667.5 1178.3 974.0 2407.0 1944.6 6322.0 4524.0 1050.0 760.0 1360.0 980.0 | +31.5 +20.0 +58.9 +21.0 +23.8 +39.7 +32.8 +38.8 |
TABLE 1
| Variety of test | Membranes | Test area (m2) | During sowingWorkshop (moon/day) | Time of transplantation (moon/day) | Time of initial picking (moon/day) | Growth period (sky) | Actual cell yield (Kg) | Yield per mu is increased (Kg) (％) |
| Luffa cylindrica Eggplant Chili pepper | R W R W R W R W R W R W | 233.5 200.1 44.0 44.0 0.6 0.6 0.1 0.1 0.09 0.09 50.0 50.0 | 3/4 3/4 3/20 3/20 / / / / 2/5 2/5 3/2 3/2 | 4/13 4/13 4/13 4/13 4/26 4/26 4/29 4/22 4/12 4/12 5/10 5/10 | 6/1 6/7 5/30 5/31 6/1 6/4 6/12 6/12 5/20 5/24 6/7 6/7 | 89 95 71 72 36 39 44 51 106 110 97 97 | 957.5 663.5 57.1 46.9 548 445 386 313 95 73 16.45 14.85 | 2735.7 2211.7 +23.7 865.2 710.6 +21.8 915.2 741.8 +23.4 3860.0 3130.0 +23.3 1055.6 811.1 +30.1 2193 198.0 +10.8 |
*R: a light conversion film W: common film
Claims (8)
1. A single-base dual-energy light conversion agent is characterized by that it uses alkaline earth metal sulfide as matrix and rare earth ion Eu2+And transition metal ion Cu+The metal ions are taken as coactivators, and other metal ions are taken as sensitizers, and the general formula of the composition is as follows:
Mg1-m-n-kCamSrnBakS:xEu2+,yCu+zRE2, qTM wherein: RE = Y, La, Ce, Pr, Nd, Sm, Gd, Tb, Dy, Ho, Er, Tm, Yb, Lu,
TM = one or two of Bi, Sb, Mn, Pb
0≤m≤1.0, 0≤n≤1.0, 0≤k≤1.0
0≤x≤2×10-3％； 0≤y≤5×10-3％
0≤z≤1×10-4％； 0≤q≤1×10-4% single-base dual-energy rare earth light conversion agent, the maximum excitation wavelength is in the region of 300-350nm and 480-580nm, and the maximum emission wavelength is in the region of 420-450nm and 620-680 nm.
2. The mono-based bi-energy light conversion agent according to claim 1, characterized in that the alkaline earth metal sulfide can be a monobasic alkaline earth metal sulfide, or a dibasic alkaline earth metal sulfide or a tribasic alkaline earth metal sulfide.
3. The single-base dual-energy light conversion agent according to claim 1, wherein the single-base dual-function light conversion agent has a stokes shift (difference between the maximum light emission wavelength and the maximum absorption wavelength) of at least 50 nm.
4. A method for producing the mono-based bi-energy light conversion agent according to claim 1, characterized in that (1) sulfates of Mg, Ca, Sr, Ba, Cu and Eu are calculated according to the composition in the general formula of the mono-based bi-energy light conversion agent2+Weight of RE, TM oxides; (2) push button
5. The method for using the single-base dual-energy light conversion agent as claimed in claim 1, which can be used for melting with plastic raw materials to form a master batch of agricultural plastic products with various functions.
6. The method for applying the mono-based dual-energy light conversion agent according to claim 5, wherein the method can be used for preparing a dual-energy light conversion master batch (I), a dual-energy light conversion anti-fog master batch (II) and a multifunctional master batch (III) with light conversion, anti-fog and heat preservation functions.
7. The method of using mono-based bi-energy light conversion agent as claimed in claim 5 or 6, which can be used to make agricultural plastic products with various functions: the double-energy light conversion rare earth master batch is added into high molecular resin according to 0.1-1.0% of the effective concentration of a light conversion agent and is applied to manufacturing light conversion agricultural films, agricultural greenhouse light conversion plates and other materials applied to plant cultivation.
8. A method of using the mono-based bi-energy light conversion agent of claim 1, wherein the agent can be applied as a light functional adjuvant by spraying directly on plants.
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2001
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