CN105968583A - Preparation method of calcium molybdate/europium doped polypropylene luminescent material - Google Patents
Preparation method of calcium molybdate/europium doped polypropylene luminescent material Download PDFInfo
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- CN105968583A CN105968583A CN201610547446.5A CN201610547446A CN105968583A CN 105968583 A CN105968583 A CN 105968583A CN 201610547446 A CN201610547446 A CN 201610547446A CN 105968583 A CN105968583 A CN 105968583A
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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- C09K2211/00—Chemical nature of organic luminescent or tenebrescent compounds
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Abstract
The invention discloses a preparation method of a calcium molybdate/europium doped polypropylene luminescent material, belonging to the technical field of luminescence. The preparation method aims to solve the problems of abundant energy waste and the like caused by short service life of the energy-saving lamp due to poor high-temperature quenching resistance, low luminous efficacy and other defects in the traditional rare-earth material at present. The method comprises the following steps: carrying out reaction on the raw material europium oxide and hydrochloric acid to obtain europium chloride hexahydrate, carrying out reaction with phenanthroline and an alpha-thenoyltrifluoroacetone chloroformic solution to obtain a rare-earth complex fluorophore, blending the rare-earth complex fluorophore with calcium carbonate, molybdenum oxide and ammonia hydrogen phosphate, carrying out ball milling, carrying out microwave heating to obtain the calcium molybdate/europium complex fluorescent powder, carrying out high-temperature melting with polypropylene, and carrying out injection molding to obtain the calcium molybdate/europium doped polypropylene luminescent material. The method solves the problems of poor high-temperature quenching resistance and low luminous efficacy in the traditional rare-earth material, prolongs the service life of the energy-saving lamp, and greatly saves the energy consumption.
Description
Technical field
The invention discloses the preparation method of the polypropylene luminescent material of a kind of calcium molybdate/europium doping, belong to field of luminescent technology.
Background technology
Owing to the ion of rare earth element has special electron structure and abundant energy level quantity, make it a huge mine of luminescent materials.In the various luminescent materials of human development, rare earth element plays an important role, the rare earth luminous category almost covering whole solid luminescence.Rare earth luminescent material industry belongs to technology-intensive type industry.The production of rare earth luminescent material is to have merged the multi-disciplinary comprehensive process technology such as crystallology, Solid-state Chemistry, surface chemistry, colorimetry, gas discharge, and the successful research and development of product and market are thrown in and set up in substantial amounts of technological reserve and experience accumulation.During technology leads the industry development of the market competition; enterprise must have independent research and innovation ability; personalization technology solution can be quickly formed for customer demand; to meet that rare earth luminescent material downstream industry is complicated and changeable, differentiation and scale the market demand deposited, could be established in the market competition and seeking development.For an industry with relatively high-tech barrier, the cultivation of independent research and development capacity is a long term accumulation and the process persistently put into, it is difficult to realized by simple introduction production technology or purchase sophisticated equipment.
The application of rare earth luminescent material can bring environmental protection and energy saving, color color developing good and long-life effect to light source, is conducive to promoting the update illuminating display field product.At present, China's rare earth luminescent material industry is immediately following international rare earth luminescent material research and development and the trend of application, and establishes good market interaction mechanism, basic material indispensable during becoming energy-saving illumination and Electronic Development of Information Industry between downstream industry.In addition to above-mentioned field, rare earth luminescent material is also extensively used for promoting plant growing, ultraviolet disinfection, health care, noctilucence to show and simulates special source and the production of equipment such as full spectrum light source of nature light, and application is continuously available expansion.The quality of the most domestic rare earth material and external top standard there is also bigger gap, prominent show as non-refractory quencher, the deterioration of non-uvioresistant, granularity is big, light efficiency is low, heat stability and the line of resistance to hydrargyrum bombardment ability, the defect such as cause produced electricity-saving lamp light efficiency low and the life-span is shorter.
Summary of the invention
The technical problem that present invention mainly solves: electricity-saving lamp that defect causes is short for service life for the most traditional rare earth material non-refractory quencher, light efficiency be low etc., cause the problem such as a large amount of wastes of the energy, it is provided that the preparation method of the polypropylene luminescent material of a kind of calcium molybdate/europium doping；The present invention is with europium oxide as raw material, six chloride hydrate europiums are prepared with hydrochloric acid reaction, react with Phen, α-thenoyltrifluoroacetone chloroformic solution again, prepare rare-earth complex fluorogen, then being blended with calcium carbonate, molybdenum oxide, phosphoric acid hydrogen ammonia ball milling, microwave heating prepares calcium molybdate/europium complex fluorescent material, last and polypropylene high-temperature fusion, injection mo(u)lding, prepares the polypropylene luminescent material of calcium molybdate/europium doping；The problem that the present invention compensate for traditional rare earth material non-refractory quencher, light efficiency is low, extends the service life of electricity-saving lamp, is greatly saved the consumption of the energy.
In order to solve above-mentioned technical problem, the technical solution adopted in the present invention is:
(1) 0.8 ~ 1.0mmol europium oxide is weighed, adding 30 ~ 50mL mass fraction is in 30% hydrochloric acid, it is completely dissolved to europium oxide with 200 ~ 300r/min stirring mixing, it is placed on Rotary Evaporators evaporation and concentration to there being white powder to separate out, proceed to 60 ~ 65 DEG C of drying baker are vacuum dried 10 ~ 12h, take out, obtain six chloride hydrate europiums；
(2) 1.5 ~ 1.8mmol α-thenoyltrifluoroacetone and 0.5 ~ 0.6mmol Phen are weighed, add in 100 ~ 120mL chloroform, and be 1mol/L six chloride hydrate europium-ethanol solution by 5 ~ 6ml molar concentration, drop in chloroform with 0.3 ~ 0.5mL/min, dripping complete follow-up continuous stirring 10 ~ 12h, sucking filtration, with ethanol and chloroform filter cake 1 ~ 2 time, proceed to 90 ~ 95 DEG C of vacuum drying ovens are dried 8 ~ 10h, obtain rare-earth complex fluorogen；
(3) 10 ~ 12mmol calcium carbonate, 10 ~ 12mmol molybdenum oxide are weighed, 5 ~ 6mmol phosphoric acid hydrogen ammonia, above-mentioned rare-earth complex fluorogen, in addition ball mill after ball milling 20 ~ 30min, move in microwave oven, with 560W microwave heating 30 ~ 40min, naturally cool to room temperature, take out, obtain calcium molybdate/europium complex fluorescent material；
(4) calcium molybdate/europium complex fluorescent material of the above-mentioned preparation of 0.15 ~ 0.20g is weighed, add in 14 ~ 15g polypropylene, it is placed in melting mixing in 230 ~ 240 DEG C of blended instrument uniform, it is cooled to 40 ~ 50 DEG C, and inject a mixture in injection instrument, under 1 ~ 2MPa pressure, keep temperature 1 ~ 2h, prepare the polypropylene luminescent material of calcium molybdate/europium doping.
The application process of the present invention is: first the polypropylene luminescent material deionized water of the calcium molybdate present invention prepared/europium doping carries out washing 2 ~ 3 times, it is placed in the baking oven of 40 ~ 45 DEG C drying, to be buckled in it inside glass lamp shade, and fluorescent lamp is energized, after testing, its light efficiency can reach 100 ~ 140lm W, color rendering index commonly reaches 80 ~ 100, life-span is up to 10000 ~ 14000h, and stability is preferable, efficient and energy-conserving and environment-protective.
The invention has the beneficial effects as follows:
(1) preparation method of the present invention is simple, and fluorescence lifetime is up to 10000 ~ 14000h, high temperature resistant, can bear great-power electronic bundle, high-energy radiation and the effect of strong ultraviolet light, and range of application is more extensive；
(2) colour developing number improves 50%, stability is preferable, energy-conserving and environment-protective, it is to avoid the waste of many energy；
(3) this preparation method is workable, and course of reaction is easy to operate, and condition is easily controlled, and reaction efficiency is high, it is simple to industrialized production.
Detailed description of the invention
First 0.8 ~ 1.0mmol europium oxide is weighed, adding 30 ~ 50mL mass fraction is in 30% hydrochloric acid, it is completely dissolved to europium oxide with 200 ~ 300r/min stirring mixing, it is placed on Rotary Evaporators evaporation and concentration to there being white powder to separate out, proceed to 60 ~ 65 DEG C of drying baker are vacuum dried 10 ~ 12h, take out, obtain six chloride hydrate europiums；Weigh 1.5 ~ 1.8mmol α-thenoyltrifluoroacetone and 0.5 ~ 0.6mmol Phen, add in 100 ~ 120mL chloroform, and be 1mol/L six chloride hydrate europium-ethanol solution by 5 ~ 6ml molar concentration, drop in chloroform with 0.3 ~ 0.5mL/min, dripping complete follow-up continuous stirring 10 ~ 12h, sucking filtration, with ethanol and chloroform filter cake 1 ~ 2 time, proceed to 90 ~ 95 DEG C of vacuum drying ovens are dried 8 ~ 10h, obtain rare-earth complex fluorogen；Weigh 10 ~ 12mmol calcium carbonate, 10 ~ 12mmol molybdenum oxide, 5 ~ 6mmol phosphoric acid hydrogen ammonia, above-mentioned rare-earth complex fluorogen, in addition ball mill after ball milling 20 ~ 30min, move in microwave oven, with 560W microwave heating 30 ~ 40min, naturally cool to room temperature, take out, obtain calcium molybdate/europium complex fluorescent material；Weigh the calcium molybdate/europium complex fluorescent material of the above-mentioned preparation of 0.15 ~ 0.20g, add in 14 ~ 15g polypropylene, it is placed in melting mixing in 230 ~ 240 DEG C of blended instrument uniform, it is cooled to 40 ~ 50 DEG C, and inject a mixture in injection instrument, under 1 ~ 2MPa pressure, keep temperature 1 ~ 2h, prepare the polypropylene luminescent material of calcium molybdate/europium doping.
Example 1
First weighing 0.8mmol europium oxide, adding 30mL mass fraction is in 30% hydrochloric acid, is completely dissolved to europium oxide with 200r/min stirring mixing, it is placed on Rotary Evaporators evaporation and concentration to there being white powder to separate out, proceed to 60 DEG C of drying baker are vacuum dried 10h, take out, obtain six chloride hydrate europiums；Weigh 1.5mmol α-thenoyltrifluoroacetone and 0.5mmol Phen, add in 100mL chloroform, and be 1mol/L six chloride hydrate europium-ethanol solution by 5ml molar concentration, drop in chloroform with 0.3mL/min, dripping complete follow-up continuous stirring 10h, sucking filtration, with ethanol and chloroform filter cake 1 time, proceed to 90 DEG C of vacuum drying ovens are dried 8h, obtain rare-earth complex fluorogen；Weighing 10mmol calcium carbonate, 10mmol molybdenum oxide, 5mmol phosphoric acid hydrogen ammonia, above-mentioned rare-earth complex fluorogen, in addition ball mill after ball milling 20min, move in microwave oven, with 560W microwave heating 30min, naturally cool to room temperature, take out, obtain calcium molybdate/europium complex fluorescent material；Weigh the calcium molybdate/europium complex fluorescent material of the above-mentioned preparation of 0.15g, add in 14g polypropylene, be placed in melting mixing in 230 DEG C of blended instrument uniform, it is cooled to 40 DEG C, and injects a mixture in injection instrument, under 1MPa pressure, keep temperature 1h, prepare the polypropylene luminescent material of calcium molybdate/europium doping.
The application process of the present invention is: first the polypropylene luminescent material deionized water of the calcium molybdate present invention prepared/europium doping carries out washing 2 times, it is placed in the baking oven of 40 DEG C drying, to be buckled in it inside glass lamp shade, and fluorescent lamp is energized, after testing, its light efficiency can reach 100lm W, color rendering index commonly reaches 80, life-span is up to 10000h, and stability is preferable, efficient and energy-conserving and environment-protective.
Example 2
First weighing 0.9mmol europium oxide, adding 40mL mass fraction is in 30% hydrochloric acid, is completely dissolved to europium oxide with 250r/min stirring mixing, it is placed on Rotary Evaporators evaporation and concentration to there being white powder to separate out, proceed to 63 DEG C of drying baker are vacuum dried 11h, take out, obtain six chloride hydrate europiums；Weigh 1.6mmol α-thenoyltrifluoroacetone and 0.55mmol Phen, add in 110mL chloroform, and be 1mol/L six chloride hydrate europium-ethanol solution by 5.5ml molar concentration, drop in chloroform with 0.4mL/min, dripping complete follow-up continuous stirring 11h, sucking filtration, with ethanol and chloroform filter cake 1.5 times, proceed to 93 DEG C of vacuum drying ovens are dried 9h, obtain rare-earth complex fluorogen；Weighing 11mmol calcium carbonate, 11mmol molybdenum oxide, 5.5mmol phosphoric acid hydrogen ammonia, above-mentioned rare-earth complex fluorogen, in addition ball mill after ball milling 25min, move in microwave oven, with 560W microwave heating 35min, naturally cool to room temperature, take out, obtain calcium molybdate/europium complex fluorescent material；Weigh the calcium molybdate/europium complex fluorescent material of the above-mentioned preparation of 0.17g, add in 14.5g polypropylene, it is placed in melting mixing in 235 DEG C of blended instrument uniform, it is cooled to 45 DEG C, and inject a mixture in injection instrument, under 1.5MPa pressure, keep temperature 1.5h, prepare the polypropylene luminescent material of calcium molybdate/europium doping.
The application process of the present invention is: first the polypropylene luminescent material deionized water of the calcium molybdate present invention prepared/europium doping carries out washing 2.5 times, it is placed in the baking oven of 43 DEG C drying, to be buckled in it inside glass lamp shade, and fluorescent lamp is energized, after testing, its light efficiency can reach 120lm W, color rendering index commonly reaches 90, life-span is up to 12000h, and stability is preferable, efficient and energy-conserving and environment-protective.
Example 3
First weighing 1.0mmol europium oxide, adding 50mL mass fraction is in 30% hydrochloric acid, is completely dissolved to europium oxide with 300r/min stirring mixing, it is placed on Rotary Evaporators evaporation and concentration to there being white powder to separate out, proceed to 65 DEG C of drying baker are vacuum dried 12h, take out, obtain six chloride hydrate europiums；Weigh 1.8mmol α-thenoyltrifluoroacetone and 0.6mmol Phen, add in 120mL chloroform, and be 1mol/L six chloride hydrate europium-ethanol solution by 6ml molar concentration, drop in chloroform with 0.5mL/min, dripping complete follow-up continuous stirring 12h, sucking filtration, with ethanol and chloroform filter cake 2 times, proceed to 95 DEG C of vacuum drying ovens are dried 10h, obtain rare-earth complex fluorogen；Weighing 12mmol calcium carbonate, 12mmol molybdenum oxide, 6mmol phosphoric acid hydrogen ammonia, above-mentioned rare-earth complex fluorogen, in addition ball mill after ball milling 30min, move in microwave oven, with 560W microwave heating 40min, naturally cool to room temperature, take out, obtain calcium molybdate/europium complex fluorescent material；Weigh the calcium molybdate/europium complex fluorescent material of the above-mentioned preparation of 0.20g, add in 15g polypropylene, be placed in melting mixing in 240 DEG C of blended instrument uniform, it is cooled to 50 DEG C, and injects a mixture in injection instrument, under 2MPa pressure, keep temperature 2h, prepare the polypropylene luminescent material of calcium molybdate/europium doping.
The application process of the present invention is: first the polypropylene luminescent material deionized water of the calcium molybdate present invention prepared/europium doping carries out washing 3 times, it is placed in the baking oven of 45 DEG C drying, to be buckled in it inside glass lamp shade, and fluorescent lamp is energized, after testing, its light efficiency can reach 140lm W, color rendering index commonly reaches 100, life-span is up to 14000h, and stability is preferable, efficient and energy-conserving and environment-protective.
Claims (1)
1. the preparation method of the polypropylene luminescent material of calcium molybdate/europium doping, it is characterised in that concrete preparation process is:
(1) 0.8 ~ 1.0mmol europium oxide is weighed, adding 30 ~ 50mL mass fraction is in 30% hydrochloric acid, it is completely dissolved to europium oxide with 200 ~ 300r/min stirring mixing, it is placed on Rotary Evaporators evaporation and concentration to there being white powder to separate out, proceed to 60 ~ 65 DEG C of drying baker are vacuum dried 10 ~ 12h, take out, obtain six chloride hydrate europiums；
(2) 1.5 ~ 1.8mmol α-thenoyltrifluoroacetone and 0.5 ~ 0.6mmol Phen are weighed, add in 100 ~ 120mL chloroform, and be 1mol/L six chloride hydrate europium-ethanol solution by 5 ~ 6ml molar concentration, drop in chloroform with 0.3 ~ 0.5mL/min, dripping complete follow-up continuous stirring 10 ~ 12h, sucking filtration, with ethanol and chloroform filter cake 1 ~ 2 time, proceed to 90 ~ 95 DEG C of vacuum drying ovens are dried 8 ~ 10h, obtain rare-earth complex fluorogen；
(3) 10 ~ 12mmol calcium carbonate, 10 ~ 12mmol molybdenum oxide are weighed, 5 ~ 6mmol phosphoric acid hydrogen ammonia, above-mentioned rare-earth complex fluorogen, in addition ball mill after ball milling 20 ~ 30min, move in microwave oven, with 560W microwave heating 30 ~ 40min, naturally cool to room temperature, take out, obtain calcium molybdate/europium complex fluorescent material；
(4) calcium molybdate/europium complex fluorescent material of the above-mentioned preparation of 0.15 ~ 0.20g is weighed, add in 14 ~ 15g polypropylene, it is placed in melting mixing in 230 ~ 240 DEG C of blended instrument uniform, it is cooled to 40 ~ 50 DEG C, and inject a mixture in injection instrument, under 1 ~ 2MPa pressure, keep temperature 1 ~ 2h, prepare the polypropylene luminescent material of calcium molybdate/europium doping.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108441210A (en) * | 2018-04-18 | 2018-08-24 | 青岛大学 | A kind of preparation method and products thereof of graphene oxide/rare-earth complex luminescent material |
| CN110845764A (en) * | 2019-11-27 | 2020-02-28 | 安徽江淮汽车集团股份有限公司 | Preparation method of modified molybdenum trioxide, polyolefin composite material and preparation method thereof |
| CN112992424A (en) * | 2021-02-19 | 2021-06-18 | 中国科学院长春应用化学研究所 | Method for directly preparing silver nanowire/europium-doped calcium molybdate composite luminescent transparent conductive film |
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2016
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108441210A (en) * | 2018-04-18 | 2018-08-24 | 青岛大学 | A kind of preparation method and products thereof of graphene oxide/rare-earth complex luminescent material |
| CN110845764A (en) * | 2019-11-27 | 2020-02-28 | 安徽江淮汽车集团股份有限公司 | Preparation method of modified molybdenum trioxide, polyolefin composite material and preparation method thereof |
| CN112992424A (en) * | 2021-02-19 | 2021-06-18 | 中国科学院长春应用化学研究所 | Method for directly preparing silver nanowire/europium-doped calcium molybdate composite luminescent transparent conductive film |
| CN112992424B (en) * | 2021-02-19 | 2021-11-12 | 中国科学院长春应用化学研究所 | Method for directly preparing silver nanowire/europium-doped calcium molybdate composite luminescent transparent conductive film |
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Application publication date: 20160928 |