CN108727634A - A method of extending luminescent plastic fluorescent lifetime - Google Patents
A method of extending luminescent plastic fluorescent lifetime Download PDFInfo
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- CN108727634A CN108727634A CN201810595938.0A CN201810595938A CN108727634A CN 108727634 A CN108727634 A CN 108727634A CN 201810595938 A CN201810595938 A CN 201810595938A CN 108727634 A CN108727634 A CN 108727634A
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- 239000004033 plastic Substances 0.000 title claims abstract description 55
- 229920003023 plastic Polymers 0.000 title claims abstract description 55
- 238000000034 method Methods 0.000 title claims abstract description 20
- 238000009825 accumulation Methods 0.000 claims abstract description 27
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 25
- 238000002360 preparation method Methods 0.000 claims abstract description 18
- 239000004594 Masterbatch (MB) Substances 0.000 claims abstract description 8
- 239000008187 granular material Substances 0.000 claims abstract description 7
- 239000002245 particle Substances 0.000 claims abstract description 7
- JIAARYAFYJHUJI-UHFFFAOYSA-L zinc dichloride Chemical compound [Cl-].[Cl-].[Zn+2] JIAARYAFYJHUJI-UHFFFAOYSA-L 0.000 claims description 24
- 239000000843 powder Substances 0.000 claims description 23
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims description 22
- 238000002156 mixing Methods 0.000 claims description 15
- 238000001035 drying Methods 0.000 claims description 14
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical class C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 claims description 13
- 239000007789 gas Substances 0.000 claims description 13
- 238000003756 stirring Methods 0.000 claims description 12
- 239000011592 zinc chloride Substances 0.000 claims description 12
- 235000005074 zinc chloride Nutrition 0.000 claims description 12
- 229910000019 calcium carbonate Inorganic materials 0.000 claims description 11
- 238000010792 warming Methods 0.000 claims description 11
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims description 10
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 10
- 238000010438 heat treatment Methods 0.000 claims description 9
- 238000009835 boiling Methods 0.000 claims description 8
- GFHNAMRJFCEERV-UHFFFAOYSA-L cobalt chloride hexahydrate Chemical compound O.O.O.O.O.O.[Cl-].[Cl-].[Co+2] GFHNAMRJFCEERV-UHFFFAOYSA-L 0.000 claims description 7
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 7
- 239000000654 additive Substances 0.000 claims description 6
- 230000000996 additive effect Effects 0.000 claims description 6
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 5
- 235000021355 Stearic acid Nutrition 0.000 claims description 5
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical class CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 claims description 5
- 239000001569 carbon dioxide Substances 0.000 claims description 5
- 229910002092 carbon dioxide Inorganic materials 0.000 claims description 5
- 238000006243 chemical reaction Methods 0.000 claims description 5
- 238000004821 distillation Methods 0.000 claims description 5
- 239000012153 distilled water Substances 0.000 claims description 5
- 239000008236 heating water Substances 0.000 claims description 5
- 239000005457 ice water Substances 0.000 claims description 5
- 239000012528 membrane Substances 0.000 claims description 5
- 239000012299 nitrogen atmosphere Substances 0.000 claims description 5
- JCXJVPUVTGWSNB-UHFFFAOYSA-N nitrogen dioxide Inorganic materials O=[N]=O JCXJVPUVTGWSNB-UHFFFAOYSA-N 0.000 claims description 5
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 claims description 5
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 claims description 5
- 238000004321 preservation Methods 0.000 claims description 5
- 239000010453 quartz Substances 0.000 claims description 5
- 239000000376 reactant Substances 0.000 claims description 5
- 230000035484 reaction time Effects 0.000 claims description 5
- 239000008117 stearic acid Substances 0.000 claims description 5
- 239000012065 filter cake Substances 0.000 claims description 4
- 235000019441 ethanol Nutrition 0.000 claims description 2
- 125000005909 ethyl alcohol group Chemical group 0.000 claims description 2
- 239000008246 gaseous mixture Substances 0.000 claims description 2
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 claims 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims 1
- -1 Hydrogen furans Chemical class 0.000 claims 1
- 239000001110 calcium chloride Substances 0.000 claims 1
- 229910001628 calcium chloride Inorganic materials 0.000 claims 1
- 229910052799 carbon Inorganic materials 0.000 claims 1
- 239000001257 hydrogen Substances 0.000 claims 1
- 229910052739 hydrogen Inorganic materials 0.000 claims 1
- 238000010521 absorption reaction Methods 0.000 abstract description 4
- 230000000694 effects Effects 0.000 abstract description 4
- 239000000463 material Substances 0.000 abstract description 4
- 238000003860 storage Methods 0.000 abstract description 3
- 239000013590 bulk material Substances 0.000 abstract description 2
- 238000001125 extrusion Methods 0.000 abstract description 2
- 229910044991 metal oxide Inorganic materials 0.000 abstract description 2
- 150000004706 metal oxides Chemical class 0.000 abstract description 2
- 239000000126 substance Substances 0.000 abstract description 2
- 239000000047 product Substances 0.000 description 7
- 230000000052 comparative effect Effects 0.000 description 6
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 description 4
- 239000004925 Acrylic resin Substances 0.000 description 3
- 229920000178 Acrylic resin Polymers 0.000 description 3
- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 description 3
- 238000002474 experimental method Methods 0.000 description 3
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
- 229920000180 alkyd Polymers 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- MKYBYDHXWVHEJW-UHFFFAOYSA-N N-[1-oxo-1-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)propan-2-yl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C(C(C)NC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)N1CC2=C(CC1)NN=N2 MKYBYDHXWVHEJW-UHFFFAOYSA-N 0.000 description 1
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- 229920006387 Vinylite Polymers 0.000 description 1
- 238000005282 brightening Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- 238000010304 firing Methods 0.000 description 1
- 230000003760 hair shine Effects 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- JDSHMPZPIAZGSV-UHFFFAOYSA-N melamine Chemical compound NC1=NC(N)=NC(N)=N1 JDSHMPZPIAZGSV-UHFFFAOYSA-N 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000003607 modifier Substances 0.000 description 1
- VIKNJXKGJWUCNN-XGXHKTLJSA-N norethisterone Chemical compound O=C1CC[C@@H]2[C@H]3CC[C@](C)([C@](CC4)(O)C#C)[C@@H]4[C@@H]3CCC2=C1 VIKNJXKGJWUCNN-XGXHKTLJSA-N 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 208000007578 phototoxic dermatitis Diseases 0.000 description 1
- 239000000049 pigment Substances 0.000 description 1
- 239000004597 plastic additive Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 239000004408 titanium dioxide Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/04—Ingredients treated with organic substances
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/02—Use of particular materials as binders, particle coatings or suspension media therefor
- C09K11/025—Use of particular materials as binders, particle coatings or suspension media therefor non-luminescent particle coatings or suspension media
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Luminescent Compositions (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The present invention relates to chemical material technical fields,Disclose a kind of method extending luminescent plastic fluorescent lifetime,The accumulation of energy agent being prepared is by the imperceptibility of organically-modified treated metal oxide further carries out particle size,So that specific surface area sharply increases,Produce the quantum effect that bulk material does not have,Luminous energy can greatly be stored,In luminous plastics mother granule preparation,Add the accumulation of energy agent being prepared,Master batch is obtained after twin-screw extrusion,It produces to obtain by mold required plastic products luminous,Fluorescent lifetime obtains 5-10 times and extends,The present invention improves the luminescent properties of plastics using the change of microstructure,Significantly improve absorption storage rate of the plastics to luminous energy,Substantially prolong fluorescent lifetime,It can be used for public arena night lighting,Warn the occasions such as the preparation of fluorescence clothes,It can realize the performance for improving luminescent plastic product and the realistic meaning for widening application field,It is a kind of technical solution being extremely worth of widely use.
Description
Technical field
The invention belongs to chemical material technical fields, and in particular to a method of extending luminescent plastic fluorescent lifetime.
Background technology
Plastics in production and life using very universal, and processing technology also comparative maturity.Luminescent plastic is that can produce
The plastics of raw aobvious luminous effect, typically mix transparent resin such as acrylic resin, vinylite, Da Mashu by luminous pigment
It is process in fat, alkyd resin, cyanurotriamide modified alkyd resin.Luminescenjt powder and plastics are combined into manufactured luminous modeling
Material, which is listed in, influences one of big invention of following ten.Although in contrast, the luminous intensity of luminescent plastic is smaller, however shining is
Electric energy and kinetic energy need not be provided, this will be a kind of novel plastic with specific function, special in energy saving, beautification life
The application of application scenario will be a quantum jump.
However the common problem that current luminescent plastic faces is accumulation of energy deficiency, optical energy attenuation speed is fast, hair
It is short between light time, it causes to utilize inconvenience.Existing plastic additive such as brightening agent has this very strong photosensitiveness so that light can not
Plastics inner is entered, fluorescent powder is unable to fully accumulation of energy, can lead to drastically reducing for luminous intensity, by the comprehensive of luminescent plastic
It can have a greatly reduced quality.
Invention content
The purpose of the present invention is for existing problem, provide a kind of method extending luminescent plastic fluorescent lifetime, show
Work improves absorption storage rate of the plastics to luminous energy, substantially prolongs fluorescent lifetime.
The present invention is achieved by the following technical solutions：
A method of extending luminescent plastic fluorescent lifetime, in luminous plastics mother granule preparation, add the accumulation of energy agent being prepared,
Accumulation of energy agent additive amount is the 0.24-0.28% of plastic master batch mass fraction, and the preparation method of the accumulation of energy agent includes the following steps：
（1）0.14-0.16 moles of cobalt chloride hexahydrate is weighed, is placed in large beaker, 15-18 milliliters of tetrahydrofurans, ice water is added
Bath lower stirring 20-30 minutes, 1.5-2.0 milliliters of triethylamines and 5-6 milliliters of distilled water are placed in small beaker and are stirred and evenly mixed, then
It is added in large beaker, is warming up to 40-50 DEG C, after stirring 1-2 hours, sealed, be placed in quiet in 70-80 DEG C of baking oven using sealed membrane
It sets 3-4 hours；
（2）0.2-0.3 moles of calcium carbonate is weighed, is pulverized, is mixed with 0.15-0.18 moles of zinc chloride powder, is added to four
In mouth flask, 70-80 milliliters of ether are added into flask, heating water bath stirs 15-20 minutes, to 40-45 DEG C by 0.5-0.8
Gram stearic acid is dissolved in 20-25 milliliters of absolute ethyl alcohols, is added drop-wise in four-hole boiling flask by separatory funnel after mixing, is heated up
It to 85-90 DEG C, is reacted under stiring, the reaction time is 60-80 minutes；
（3）By step（1）It stands object to take out, by step（2）Reactant after reaction, which is poured into, to be stood in object beaker, ice bath
It is cooled to 4-6 DEG C, is persistently stirred 30-40 minutes, mixing speed is 400-500 revs/min, is then allowed to stand 3-4 hours and is taken out
Filter obtains filter cake and is placed in baking oven to dry, and the powder after drying is placed into as in quartz boat in tube furnace, is passed through gaseous mixture
Body, setting heating rate is 3.0-3.5 DEG C/min, is warming up to 380-400 DEG C, stops heating and heat preservation 2-3 after reaching target temperature
Cooled to room temperature after hour, obtains having glossiness powder.
It is further described as to said program, step（1）The tetrahydrofuran is air-distillation under nitrogen atmosphere
It obtains within 2-3 hours.
It is further described as to said program, step（2）The calcium carbonate and zinc chloride powder particle size exist
Between 100-120 mesh.
It is further described as to said program, step（3）The drying time is 5-6 hours, and drying temperature is
100-110℃。
It is further described as to said program, step（3）The mixed gas is nitrogen and carbon dioxide according to body
Product is than being 5-6:1 ratio mixing, gas flow are 2.0-2.5 cubes m/h.
The present invention has the following advantages compared with prior art：It is insufficient in order to solve accumulation of energy in existing luminescent plastic processing, when shining
Between short problem, the present invention provides a kind of methods extending luminescent plastic fluorescent lifetime, and the accumulation of energy agent being prepared will be organic
Metal oxide after modification further carries out the imperceptibility of particle size so that specific surface area sharply increases, and produces
The quantum effect that bulk material does not have can greatly store luminous energy, and in luminous plastics mother granule preparation, addition is prepared
Accumulation of energy agent, master batch is obtained after twin-screw extrusion, produces to obtain required plastic products luminous, fluorescent lifetime by mold
It obtains 5-10 times to extend, the present invention improves the luminescent properties of plastics using the change of microstructure, significantly improves plastics pair
The absorption storage rate of luminous energy, substantially prolongs fluorescent lifetime, can be used for public arena night lighting, the preparation etc. of warning fluorescence clothes
Occasion can realize the performance for improving luminescent plastic product and the realistic meaning for widening application field, be a kind of extremely worth
The technical solution promoted the use of.
Specific implementation mode
To make the purpose of the present invention, technical solution and effect clearer, clear and definite, with reference to specific embodiment to this hair
It is bright to be described further, it should be understood that the specific embodiments described herein are merely illustrative of the present invention, is not used to limit
Technical solution provided by the present invention.
Embodiment 1
A method of extending luminescent plastic fluorescent lifetime, in luminous plastics mother granule preparation, add the accumulation of energy agent being prepared,
Accumulation of energy agent additive amount is the 0.24% of plastic master batch mass fraction, and the preparation method of the accumulation of energy agent includes the following steps：
（1）0.14 mole of cobalt chloride hexahydrate is weighed, is placed in large beaker, 15 milliliters of tetrahydrofurans are added, are stirred under ice-water bath
20 minutes, 1.5 milliliters of triethylamines and 5 milliliters of distilled water are placed in small beaker and are stirred and evenly mixed, are then added in large beaker, risen
Temperature after stirring 1 hour, is sealed using sealed membrane to 40 DEG C, is placed in 70 DEG C of baking ovens and stands 3 hours；
（2）0.2 mole of calcium carbonate is weighed, is pulverized, mixes, is added in four-hole boiling flask with 0.15 mole of zinc chloride powder,
70 milliliters of ether are added into flask, heating water bath stirs 15 minutes to 40 DEG C, 0.5 gram of stearic acid is dissolved in 20 milliliters of nothings
It in water-ethanol, is added drop-wise in four-hole boiling flask by separatory funnel after mixing, is warming up to 85 DEG C, is reacted under stiring,
Reaction time is 60 minutes；
（3）By step（1）It stands object to take out, by step（2）Reactant after reaction, which is poured into, to be stood in object beaker, ice bath
4 DEG C are cooled to, is persistently stirred 30 minutes, mixing speed is 400 revs/min, is then allowed to stand 3 hours and is filtered, obtains filter cake
It is placed in baking oven and dries, the powder after drying is placed into as in quartz boat in tube furnace, is passed through mixed gas, setting heating
Speed is 3.0 DEG C/min, is warming up to 380 DEG C, reaches and stops heating and heat preservation cooled to room temperature after 2 hours after target temperature,
Obtain having glossiness powder.
It is further described as to said program, step（1）The tetrahydrofuran is air-distillation 2 under nitrogen atmosphere
What hour obtained.
It is further described as to said program, step（2）The calcium carbonate and zinc chloride powder particle size exist
Between 100-120 mesh.
It is further described as to said program, step（3）The drying time is 5 hours, drying temperature 100
℃。
It is further described as to said program, step（3）The mixed gas is nitrogen and carbon dioxide according to body
Product is than being 5:1 ratio mixing, gas flow are 2.0 cubes ms/h.
Embodiment 2
A method of extending luminescent plastic fluorescent lifetime, in luminous plastics mother granule preparation, add the accumulation of energy agent being prepared,
Accumulation of energy agent additive amount is the 0.26% of plastic master batch mass fraction, and the preparation method of the accumulation of energy agent includes the following steps：
（1）0.15 mole of cobalt chloride hexahydrate is weighed, is placed in large beaker, 16 milliliters of tetrahydrofurans are added, are stirred under ice-water bath
25 minutes, 1.8 milliliters of triethylamines and 5.5 milliliters of distilled water are placed in small beaker and are stirred and evenly mixed, are then added in large beaker,
45 DEG C are warming up to, after stirring 1.5 hours, is sealed using sealed membrane, is placed in 75 DEG C of baking ovens and stands 3.5 hours；
（2）0.25 mole of calcium carbonate is weighed, is pulverized, mixes, is added in four-hole boiling flask with 0.16 mole of zinc chloride powder,
75 milliliters of ether are added into flask, heating water bath stirs 18 minutes to 42 DEG C, 0.6 gram of stearic acid is dissolved in 22 milliliters of nothings
It in water-ethanol, is added drop-wise in four-hole boiling flask by separatory funnel after mixing, is warming up to 88 DEG C, is reacted under stiring,
Reaction time is 70 minutes；
（3）By step（1）It stands object to take out, by step（2）Reactant after reaction, which is poured into, to be stood in object beaker, ice bath
5 DEG C are cooled to, is persistently stirred 35 minutes, mixing speed is 450 revs/min, is then allowed to stand 3.5 hours and is filtered, is filtered
Cake is placed in baking oven and dries, and the powder after drying is placed into as in quartz boat in tube furnace, is passed through mixed gas, and setting rises
Warm speed is 3.3 DEG C/min, is warming up to 390 DEG C, and stopping heating and heat preservation naturally cooling to after 2.5 hours after reaching target temperature
Room temperature obtains having glossiness powder.
It is further described as to said program, step（1）The tetrahydrofuran is air-distillation under nitrogen atmosphere
It obtains within 2.5 hours.
It is further described as to said program, step（2）The calcium carbonate and zinc chloride powder particle size exist
Between 100-120 mesh.
It is further described as to said program, step（3）The drying time is 5.5 hours, drying temperature 105
℃。
It is further described as to said program, step（3）The mixed gas is nitrogen and carbon dioxide according to body
Product is than being 5.5:1 ratio mixing, gas flow are 2.2 cubes ms/h.
Embodiment 3
A method of extending luminescent plastic fluorescent lifetime, in luminous plastics mother granule preparation, add the accumulation of energy agent being prepared,
Accumulation of energy agent additive amount is the 0.28% of plastic master batch mass fraction, and the preparation method of the accumulation of energy agent includes the following steps：
（1）0.16 mole of cobalt chloride hexahydrate is weighed, is placed in large beaker, 18 milliliters of tetrahydrofurans are added, are stirred under ice-water bath
30 minutes, 2.0 milliliters of triethylamines and 6 milliliters of distilled water are placed in small beaker and are stirred and evenly mixed, are then added in large beaker, risen
Temperature after stirring 2 hours, is sealed using sealed membrane to 50 DEG C, is placed in 80 DEG C of baking ovens and stands 4 hours；
（2）0.3 mole of calcium carbonate is weighed, is pulverized, mixes, is added in four-hole boiling flask with 0.18 mole of zinc chloride powder,
80 milliliters of ether are added into flask, heating water bath stirs 20 minutes to 45 DEG C, 0.8 gram of stearic acid is dissolved in 25 milliliters of nothings
It in water-ethanol, is added drop-wise in four-hole boiling flask by separatory funnel after mixing, is warming up to 90 DEG C, is reacted under stiring,
Reaction time is 80 minutes；
（3）By step（1）It stands object to take out, by step（2）Reactant after reaction, which is poured into, to be stood in object beaker, ice bath
6 DEG C are cooled to, is persistently stirred 40 minutes, mixing speed is 500 revs/min, is then allowed to stand 4 hours and is filtered, obtains filter cake
It is placed in baking oven and dries, the powder after drying is placed into as in quartz boat in tube furnace, is passed through mixed gas, setting heating
Speed is 3.5 DEG C/min, is warming up to 400 DEG C, reaches and stops heating and heat preservation cooled to room temperature after 3 hours after target temperature,
Obtain having glossiness powder.
It is further described as to said program, step（1）The tetrahydrofuran is air-distillation 3 under nitrogen atmosphere
What hour obtained.
It is further described as to said program, step（2）The calcium carbonate and zinc chloride powder particle size exist
Between 100-120 mesh.
It is further described as to said program, step（3）The drying time is 5-6 hours, drying temperature 110
℃。
It is further described as to said program, step（3）The mixed gas is nitrogen and carbon dioxide according to body
Product is than being 6:1 ratio mixing, gas flow are 2.5 cubes ms/h.
Comparative example 1
With differing only in for embodiment 1, the accumulation of energy agent additive amount is the 0.30% of plastic master batch mass fraction, remaining holding
Unanimously.
Comparative example 2
With differing only in for embodiment 2, in the preparation of the accumulation of energy agent, step is omitted（1）In cobalt chloride hexahydrate is changed
Property process, directly adds cobalt chloride hexahydrate, remaining is consistent.
Comparative example 3
With differing only in for embodiment 3, in the preparation of the accumulation of energy agent, step is omitted（2）In to calcium carbonate and zinc chloride
Modifying process directly adds calcium carbonate and zinc chloride, remaining is consistent.
Comparative example 4
With differing only in for embodiment 3, in the preparation process of the accumulation of energy agent, step（2）Target temperature is 350 DEG C, remaining
It is consistent.
Contrast experiment
The method for using embodiment 1-3 and comparative example 1-4 respectively improves the fluorescent lifetime of luminescent plastic, to add nanometer titanium dioxide
The method of silica modifier as a control group, using acrylic resin as plastic body, fluorescent powder dosage and acrylic resin it
Between mass ratio be 5:1, keep the consistent processing of remaining ingredient in addition to accumulation of energy agent to prepare luminescent plastic plank, 50 milli of plastic plate length
Rice, it is 10 millimeters wide, it is 5 millimeters thick, keep irrelevant variable consistent in experiment, luminescent material be tested for the property, when measuring different
Between after plastics brightness value（mcd/m2）, the results are shown in table below：
（It is 1000lx that exciting light, which shines, in experiment, and firing time is 10 minutes.）
The present invention improves the luminescent properties of plastics using the change of microstructure, significantly improves plastics and is deposited to the absorption of luminous energy
Storage rate, substantially prolongs fluorescent lifetime, can be used for public arena night lighting, the occasions such as preparation of warning fluorescence clothes, Neng Goushi
It now improves the performance of luminescent plastic product and widens the realistic meaning of application field, be a kind of skill being extremely worth of widely use
Art scheme.
Claims (5)
1. a kind of method extending luminescent plastic fluorescent lifetime, which is characterized in that in luminous plastics mother granule preparation, prepared by addition
Obtained accumulation of energy agent, accumulation of energy agent additive amount are the 0.24-0.28% of plastic master batch mass fraction, the preparation method of the accumulation of energy agent
Include the following steps：
（1）0.14-0.16 moles of cobalt chloride hexahydrate is weighed, is placed in large beaker, 15-18 milliliters of tetrahydrofurans, ice water is added
Bath lower stirring 20-30 minutes, 1.5-2.0 milliliters of triethylamines and 5-6 milliliters of distilled water are placed in small beaker and are stirred and evenly mixed, then
It is added in large beaker, is warming up to 40-50 DEG C, after stirring 1-2 hours, sealed, be placed in quiet in 70-80 DEG C of baking oven using sealed membrane
It sets 3-4 hours；
（2）0.2-0.3 moles of calcium carbonate is weighed, is pulverized, is mixed with 0.15-0.18 moles of zinc chloride powder, is added to four
In mouth flask, 70-80 milliliters of ether are added into flask, heating water bath stirs 15-20 minutes, to 40-45 DEG C by 0.5-0.8
Gram stearic acid is dissolved in 20-25 milliliters of absolute ethyl alcohols, is added drop-wise in four-hole boiling flask by separatory funnel after mixing, is heated up
It to 85-90 DEG C, is reacted under stiring, the reaction time is 60-80 minutes；
（3）By step（1）It stands object to take out, by step（2）Reactant after reaction, which is poured into, to be stood in object beaker, ice bath
It is cooled to 4-6 DEG C, is persistently stirred 30-40 minutes, mixing speed is 400-500 revs/min, is then allowed to stand 3-4 hours and is taken out
Filter obtains filter cake and is placed in baking oven to dry, and the powder after drying is placed into as in quartz boat in tube furnace, is passed through gaseous mixture
Body, setting heating rate is 3.0-3.5 DEG C/min, is warming up to 380-400 DEG C, stops heating and heat preservation 2-3 after reaching target temperature
Cooled to room temperature after hour, obtains having glossiness powder.
2. a kind of method extending luminescent plastic fluorescent lifetime as described in claim 1, which is characterized in that step（1）Described four
Hydrogen furans obtains for air-distillation 2-3 hours under nitrogen atmosphere.
3. a kind of method extending luminescent plastic fluorescent lifetime as described in claim 1, which is characterized in that step（2）The carbon
Sour calcium and zinc chloride powder particle size are between 100-120 mesh.
4. a kind of method extending luminescent plastic fluorescent lifetime as described in claim 1, which is characterized in that step（3）The baking
The dry time is 5-6 hours, and drying temperature is 100-110 DEG C.
5. a kind of method extending luminescent plastic fluorescent lifetime as described in claim 1, which is characterized in that step（3）It is described mixed
It according to volume ratio is 5-6 that close gas, which be nitrogen and carbon dioxide,:1 ratio mixing, gas flow be 2.0-2.5 cubic metres/it is small
When.
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| CN114231284A (en) * | 2021-12-24 | 2022-03-25 | 广东翔龙科技股份有限公司 | Preparation method of active heavy calcium carbonate applied to rare earth self-luminous material |
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