CN103484115A - Preparation method for blue fluorescent brightening agent - Google Patents
Preparation method for blue fluorescent brightening agent Download PDFInfo
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- CN103484115A CN103484115A CN201310435127.1A CN201310435127A CN103484115A CN 103484115 A CN103484115 A CN 103484115A CN 201310435127 A CN201310435127 A CN 201310435127A CN 103484115 A CN103484115 A CN 103484115A
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Abstract
The invention provides a preparation method for a blue fluorescent brightening agent. The blue fluorescent brightening agent is characterized in that the formula of the blue fluorescent brightening agent is composed of the following raw materials in parts by weight: 15-25 parts of calcium oxide, 20-30 parts of elemental sulfur, 12-25 parts of starch,1-5 parts of thorium nitrate and 1-5 parts of bismuth nitrate; the preparation process of the blue fluorescent brightening agent is as follows: putting a layer of carbon powder at the bottom of a crucible; uniformly mixing the raw materials, and then adding the mixture on the carbon powder; after drying at the temperature of 120 DEG C for 30 minutes, heating to the temperature of 1200 DEG C to 1300 DEG C under the condition of sealing; calcining for 10 to 15 minutes, so that the blue fluorescent brightening agent is obtained. The preparation method for the blue fluorescent brightening agent has the advantages that the process is simple, the preparation method is easy to control, the product quality is stable, the adaptability is strong, the energy conservation and environment protection are achieved, and the use is convenient.
Description
Technical field
The invention belongs to a kind of manufacture method of fluorescent material.
Background technology
Fluorescent material is to be coordinated through calcining and form with the trace active agent by metal (zinc, chromium) sulfide or rare earth oxide.Colourless or shallow white, be under UV-light (200～400nm) is irradiated, and according to the difference of metal in pigment and activator species, content, and presents versicolor visible ray (400～800nm).Inorganic fluorescent material; Inorganic fluorescent material be represented as rare earth luminescence and rare-earth luminescent material, its advantage is that receptivity is strong, turnover ratio is high, the narrowband emission of rare earth compounding central ion is conducive to panchromatic demonstration, and physicochemical property are stable.Because rare earth ion has abundant energy level and 4f transition of electron characteristic, make rare earth become luminous treasure-house, for high-tech area particularly provides the luminescent material of superior performance in the information communication field.At present, common inorganic fluorescent material is sulfide (as ZnS, the CaS) aluminate (SrAl2O4 with alkaline-earth metal, CaAl2O4, BaAl2O4) etc. as luminous host, using rare earth lanthanide [europium (Eu), samarium (Sm), erbium (Er), neodymium (Nd) etc.] as activator and co-activator.Traditional preparation method of inorganic phosphor is high temperature solid-state method, but the quick renewal along with new technology, the raising of luminescent material performance index need to overcome the intrinsic defect of classical synthetic method, some new methods are arisen at the historic moment, as combustion method, sol-gel processing [, hydrothermal deposition method, microwave method etc.In luminous field, the research of organic materials is subject to people's attention day by day.Because organic compound is of a great variety, adjustability is good, rich color, and purity of color is high, and molecular designing is relatively flexible.According to different molecular structures, luminous organic material can be divided into: (1) organic molecule luminescent material; (2) organic polymer luminescent material; (3) organic coordination compound luminescent material.These luminescent materials no matter on luminescence mechanism, physical and chemical performance, or have characteristics separately in application.Organic fluorescence materials; The organic molecule luminescent material is of a great variety, their multi-bands have conjugation heterocycle and various chromophore, structure is easy to adjust, and changes its conjugate length by introducing the unsaturated group such as ethylene linkage, phenyl ring and various chromophore, thereby compound optoelectronic character is changed.As oxadiazoles and derivatives class thereof, triazole and derivatives class thereof, rhodamine and derivatives class thereof, coumarin derivatives, 1,8-naphthalimide analog derivative, pyrazoline derivative, triphenylamine analog derivative, porphyrins, carbazole, pyrazine, thiazole derivative ， perylene analog derivative etc.They are widely used in the aspects such as optical electron device, DNA diagnosis, Optochemical sensor, dyestuff, white dyes, fluorescent coating, laser dyes [7], organic electroluminescence device (ELD).But the small molecules luminescent material is at solid-state lower easy generation Fluorescence-quenching, and the device that general adulterating method is made is easy accumulative crystallization again, and descend to device lifetime.Therefore numerous researchers is devoted to micromolecular research on the one hand, finds on the other hand the better luminescent material of performance, and high-molecular luminous material has just arisen at the historic moment.The organic polymer optical material is divided three classes usually: (1) side chain type: the small molecules luminophore is articulated on polymer side chain, (2) full conjugate backbone chain type: whole molecule is a large conjugated polymer system, (3) partly conjugated backbone chain type: luminescence center, on main chain, does not form a conjugated system but be spaced from each other between luminescence center.The high-molecular luminous material of studying at present is mainly conjugated polymers, as polyphenyl, Polythiophene, poly-fluorenes, poly-triphenylamine and derivative thereof etc.Also have poly-triphenylamine, polycarbazole, polypyrrole, poly-porphyrin [8] and derivative, multipolymer etc., study also often at present.Can also introduce polymer ends to luminophore or introduce in the middle of polymer chain, Kenneth P.Ghiggino etc. introduce RAFT reagent to fluorescent chromophore, by the RAFT polymerization, fluorescent chromophore are connected on polymkeric substance.From above various luminescence polymers, can find out, majority is the polymerization of main chain conjugation, and the main chain polymerization easily forms large conjugate area, but its solvability, meltbility all reduce, and processing is got up more difficult; And when luminophore being introduced to polymer ends or introducing in the middle of polymer chain, only have again end group luminous, and molecular weight can be very not large, if molecular weight is very large, luminophore content in polymkeric substance is low, and fluorescence is very weak.And the side chain polymer luminescent material is that the strong of main chain conjugated polymers supplemented.Along with scientific and technical progress, people are more and more to the research of fluorescence, and the range of application of fluorescent substance is more and more wider.Fluorescent substance, except as dyestuff, has also obtained application widely in fields such as pigment dyestuff, optical whitening agent, photooxidant, coating, chemistry and biochemical analysis, sun power trap, anti-fake mark, medicine spike and laser.The method of manufacturing fluorescent material of prior art, exist the technical process complexity wayward, the deficiency that cost is high.Through Chinese publication retrieval, there is no to find the scheme identical with the present invention.
Summary of the invention:
The object of the invention is to, for the deficiencies in the prior art, propose a kind of blue luminescence agent preparation method.
Blue luminescence agent preparation method of the present invention is characterized in that: composition of raw materials by weight, by calcium oxide 15-25 part, elemental sulfur 20-30 part, starch 12-25 part, thorium nitrate 99.99004323A8urity 1-5 part, bismuth nitric acid 1-5 part forms; Preparation process is: gets crucible and puts one deck powdered carbon in bottom, raw material is mixed and is added on powdered carbon, and under 120 ℃ after dry 30 minutes, under air-proof condition, 1200-1300 ℃ of calcining 10-15 minute that heat, the cooling product that obtains.
The present invention compared with prior art its beneficial effect is: have technique simple, be easy to control, constant product quality, strong adaptability, energy-conserving and environment-protective, the advantage such as easy to use.
Concrete embodiment:
Embodiment 1
Blue luminescence agent preparation method of the present invention is characterized in that: composition of raw materials by weight, by calcium oxide 15-25 part, elemental sulfur 20-30 part, starch 12-25 part, thorium nitrate 99.99004323A8urity 1-5 part, bismuth nitric acid 1-5 part forms; Preparation process is: gets crucible and puts one deck powdered carbon in bottom, raw material is mixed and is added on powdered carbon, and under 120 ℃ after dry 30 minutes, under air-proof condition, 1200-1300 ℃ of calcining 10-15 minute that heat, the cooling product that obtains.
Embodiment 2
Blue luminescence agent preparation method of the present invention is characterized in that: composition of raw materials by weight, by 15 parts, calcium oxide, 20 parts of elemental sulfurs, 12 parts of starch, 1 part of thorium nitrate 99.99004323A8urity, 1 part of composition of bismuth nitric acid; Preparation process is: gets crucible and puts one deck powdered carbon in bottom, raw material is mixed and is added on powdered carbon, and under 120 ℃ after dry 30 minutes, under air-proof condition, 1200-1300 ℃ of calcining 10-15 minute that heat, the cooling product that obtains.
Embodiment 3
Blue luminescence agent preparation method of the present invention is characterized in that: composition of raw materials by weight, by 25 parts, calcium oxide, 30 parts of elemental sulfurs, 25 parts of starch, 5 parts of thorium nitrate 99.99004323A8uritys, 5 parts of compositions of bismuth nitric acid; Preparation process is: gets crucible and puts one deck powdered carbon in bottom, raw material is mixed and is added on powdered carbon, and under 120 ℃ after dry 30 minutes, under air-proof condition, 1200-1300 ℃ of calcining 10-15 minute that heat, the cooling product that obtains.
Embodiment 4
Blue luminescence agent preparation method of the present invention is characterized in that: composition of raw materials by weight, by 20 parts, calcium oxide, 25 parts of elemental sulfurs, 20 parts of starch, 3 parts of thorium nitrate 99.99004323A8uritys, 3 parts of compositions of bismuth nitric acid; Preparation process is: gets crucible and puts one deck powdered carbon in bottom, raw material is mixed and is added on powdered carbon, and under 120 ℃ after dry 30 minutes, under air-proof condition, 1200-1300 ℃ of calcining 10-15 minute that heat, the cooling product that obtains.
Embodiment 5
Blue luminescence agent preparation method of the present invention is characterized in that: composition of raw materials by weight, by 25 parts, calcium oxide, 20 parts of elemental sulfurs, 12 parts of starch, 5 parts of thorium nitrate 99.99004323A8uritys, 1 part of composition of bismuth nitric acid; Preparation process is: gets crucible and puts one deck powdered carbon in bottom, raw material is mixed and is added on powdered carbon, and under 120 ℃ after dry 30 minutes, under air-proof condition, 1200-1300 ℃ of calcining 10-15 minute that heat, the cooling product that obtains.
Blue luminescence agent preparation method of the present invention, desired raw material all can be bought acquisition on market.There is technique simple, be easy to control, constant product quality, strong adaptability, energy-conserving and environment-protective, the advantage such as easy to use.Blue luminescence agent application of the present invention: can be general for making the ideal material of luminous printing ink, luminous paint, luminescent plastics, luminous printing paste.Luminous printing ink not only is applicable to the pattern and character of the various illumination effects of wire mark, as label, toy, calligraphy and painting, glass picture, non-setting adhesive etc., and because it has that transparency is high, the characteristics such as good film-forming property, coating be thin, can on the artworks such as all kinds of embossments, circular engravure (figure of buddha, vitrotype, plaster statue, tri-coloured glazed pottery), polymer picture, lamp decoration, spray or wire mark, under the prerequisite that does not affect its original decorations coloured silk or lines, greatly improve its added value.
Claims (1)
1. a blue luminescence agent preparation method is characterized in that: composition of raw materials by weight, by calcium oxide 15-25 part, elemental sulfur 20-30 part, starch 12-25 part, thorium nitrate 99.99004323A8urity 1-5 part, bismuth nitric acid 1-5 part forms; Preparation process is: gets crucible and puts one deck powdered carbon in bottom, raw material is mixed and is added on powdered carbon, and under 120 ℃ after dry 30 minutes, under air-proof condition, 1200-1300 ℃ of calcining 10-15 minute that heat, the cooling product that obtains.
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| CN201310435127.1A CN103484115A (en) | 2013-09-23 | 2013-09-23 | Preparation method for blue fluorescent brightening agent |
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| CN201310435127.1A CN103484115A (en) | 2013-09-23 | 2013-09-23 | Preparation method for blue fluorescent brightening agent |
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Citations (6)
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|---|---|---|---|---|
| GB245612A (en) * | 1925-05-18 | 1926-01-14 | Henry Montague Mines | Improvements in or relating to phosphorescent or luminous masses or compounds |
| CN1116647A (en) * | 1994-08-06 | 1996-02-14 | 深圳申海科技发展公司 | Photoluminescence powder |
| CN101130689A (en) * | 2007-10-15 | 2008-02-27 | 彩虹集团电子股份有限公司 | Method of producing green fluorescent powder |
| CN101168664A (en) * | 2007-11-30 | 2008-04-30 | 彩虹集团电子股份有限公司 | Method for preparing blue phosphor |
| CN101376807A (en) * | 2008-09-17 | 2009-03-04 | 彩虹集团电子股份有限公司 | Preparation of goldless green phosphor |
| JP2010059429A (en) * | 2009-10-26 | 2010-03-18 | Mitsubishi Chemicals Corp | Phosphor, luminescent device using the same, image display and illuminating device |
-
2013
- 2013-09-23 CN CN201310435127.1A patent/CN103484115A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB245612A (en) * | 1925-05-18 | 1926-01-14 | Henry Montague Mines | Improvements in or relating to phosphorescent or luminous masses or compounds |
| CN1116647A (en) * | 1994-08-06 | 1996-02-14 | 深圳申海科技发展公司 | Photoluminescence powder |
| CN101130689A (en) * | 2007-10-15 | 2008-02-27 | 彩虹集团电子股份有限公司 | Method of producing green fluorescent powder |
| CN101168664A (en) * | 2007-11-30 | 2008-04-30 | 彩虹集团电子股份有限公司 | Method for preparing blue phosphor |
| CN101376807A (en) * | 2008-09-17 | 2009-03-04 | 彩虹集团电子股份有限公司 | Preparation of goldless green phosphor |
| JP2010059429A (en) * | 2009-10-26 | 2010-03-18 | Mitsubishi Chemicals Corp | Phosphor, luminescent device using the same, image display and illuminating device |
Non-Patent Citations (4)
| Title |
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| 崔春芳，童凌峰，高洋编著: "《美术涂料与装饰技术手册》", 31 July 2010 * |
| 徐叙瑢主编: "《发光学与发光材料》", 30 April 2004 * |
| 王文广主编: "《塑料配方设计》", 31 December 1998 * |
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Application publication date: 20140101 |