CN102585799A - Chemiluminescent compositions, and production and use methods thereof - Google Patents

Chemiluminescent compositions, and production and use methods thereof Download PDF

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CN102585799A
CN102585799A CN2010102324577A CN201010232457A CN102585799A CN 102585799 A CN102585799 A CN 102585799A CN 2010102324577 A CN2010102324577 A CN 2010102324577A CN 201010232457 A CN201010232457 A CN 201010232457A CN 102585799 A CN102585799 A CN 102585799A
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compsn
agent
perylene dicarboximide
barkite
acvator
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P·S·宾德拉
M·A·克卢茨
S·P·霍奇森
R·潘尼尔
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MEIJIA HUIGUANG CO Ltd
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MEIJIA HUIGUANG CO Ltd
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Abstract

The invention relates to chemiluminescent compositions and production and use methods thereof. The chemiluminescent compositions described in the invention can be applied to various substrates usually sensitive to present chemiluminescent compositions. The invention also provides the methods for producing and using the chemiluminescent compositions.

Description

Chemical luminous composite and production thereof and method of use
Technical field
The present invention relates to chemical luminous composite (chemiluminescent compositions) and production and method of use.
Background technology
Chemical luminous composite utilizes two components system to produce light through chemical mode usually.Said two components it typically is the chemical solution form, are called " acvator (activator) " component and " barkite/salt (oxalate) " component.When the chemiluminescent light time of needs, acvator and barkite/salt are mixed.Activator component comprises peroxide cpd and catalyzer, and barkite/salt component comprises barkite.Said compsn also comprises fluorescent agent (fluorescer), and it can be present among one of said two kinds of components or both.Chemical luminous composite also comprises solvent or the solvent mixture that is used for activator component and is used for the solvent of barkite/salt component.The solvent that is used for said two components can be different, but miscible each other.
Chemical luminous composite typically is included in wherein and keeps in the device of two kinds of component physical sepn before activation through several different methods.Usually, said device is independently comprising each component and when the needs chemiluminescent light time of generation, is destroying the chamber so that two components are allowed to mutual blended form in the chamber.The example of a kind of extensive employing of this type device is " glo-stick (light stick) ".Here, the breakaway glass pipe-type bottles that will comprise a kind of sealing of component is encapsulated in the outer flexible receptacle that comprises another component, and this outer flexible receptacle also seals.Crooked said outer container causes said pipe-type bottles to break, thereby discharges said component and make two components mix and generation light.Although this method extensively adopts, but still is limited in the application-specific.
Summary of the invention
Described herein is to can be used for common chemical luminous composite to the responsive multiple base material of existing chemical luminous composite.The method of producing this chemical luminous composite also is provided.Advantage part of the present invention will illustrate in the following description and part will become obviously through said description, maybe can know through the practice of following aspect.Following advantage will and obtain through special key element of in appending claims, pointing out and combination realization thereof.The detailed description that should be understood that aforementioned general description and hereinafter all is merely exemplary and indicative, and nonrestrictive.
Embodiment
Before disclosing and describing compound of the present invention, compsn and/or method, should be understood that following aspect is not limited to specific compound, compound method or purposes, because it obviously can change.Should also be understood that term used herein is merely the description particular aspects, rather than be used for restriction.
In this specification sheets and following claim, should be defined as term with following implication with mentioning in a large number:
Mandatory declaration be that like what in specification sheets and appended claim, use, only if clear from context is pointed out contrary, otherwise singulative " a ", " an " and " the " comprise plural.Thereby for example " solvent " comprises the mixture of two kinds or more kinds of these kind solvents, or the like.
" optional " or " randomly " is meant the incident of describing subsequently or situation can take place or can not take place and this description comprises situation that said incident or situation take place and the situation that does not take place.For example, phrase " randomly comprises softening agent " and is meant and can exist or can not have softening agent.
In specification sheets and last claim, mention the weight part of element-specific in compsn or the goods or component, the weight relationships between element or component described in expression compsn or the goods and any other element or component, it is expressed with weight part.Therefore, in the formulation that comprises 2 parts by weight of component X and 5 parts by weight of component Y, X and Y exist with 2: 5 weight ratio, and no matter in this formulation, whether comprise other component, all exist with this ratio.
Only if there is opposite special instruction, otherwise the weight percentage of component is based on the prescription that comprises said component or the gross weight of compsn.
Described herein is chemical luminous composite and preparation and method of use.As hereinafter will discuss, depend on it and use that said compsn can be with the prepare of multiple different ingredients.Said compsn is made up of acvator and luminous agent (luminescer) usually.In one aspect, when compsn was powder, said chemical luminous composite comprised (i) water and at least a organic solvent; (ii) oxygenant and (iii) sequestrant, softening agent, thickening material, buffer reagent, catalyzer or its arbitrary combination; (iv) barkite or salt; (v) fluorescent agent (fluorescer); (many (a plurality of) solid particulate that vi) comprises one or more inorganic oxides, wherein component (i)-(vi) all not having the specificity that is attached on it combines unit (have a specific binding pair memberbonded to it).Component (i)-(iii) is generally the acvator part, and barkite/salt and fluorescent agent form said luminous agent.Said many solid particulates are scattered in the whole compsn to produce powder.Below describe the every kind of component and the solid particulate of acvator and luminous agent in detail.
Said acvator comprises water and at least a organic solvent.Water and additional organic solvents are used for promoting other solid of dissolve activating agent.In addition, said organic solvent can be used as thickening material.In one aspect, said organic solvent comprises polyvalent alcohol.Term " polyol " is defined as the compound with two or more hydroxyls in this article.The example of spendable polyvalent alcohol includes but not limited to glycerine and polyoxyethylene glycol among this paper.The amount of solvent can change according to the selected component that is used to produce acvator.In one aspect, the amount of water is the 1-10% of acvator weight, 2-8%, 2-6% or 2-4%.In one aspect of the method, organic solvent is up to 2% of acvator weight.
Said acvator comprises oxygenant.The effect of oxygenant below will be discussed.Usually, oxygenant is for reacting any compound of the barkite/salt in (that is oxidation) luminous agent.In one aspect, said oxygenant comprises hydrogen peroxide.In yet another aspect, said oxygenant comprises hydrogen peroxide precursor.Term used herein " hydrogen peroxide precursor " is defined as any compound of in-situ hydrogen peroxide.For example, hydrogen peroxide precursor can generate hydrogen peroxide with the water reaction.The example of hydrogen peroxide precursor includes but not limited to urea peroxide, hydrogen peroxide, sodiumperoxide, Sodium peroxoborate, peroxo-trisodium phosphate (sodium pyrophosphate peroxide) or its arbitrary combination.Can use USP 3,539 among this paper, disclosed oxygenant in 794 and 5,705,103, it is combined in here in full by reference.In one aspect, the amount of oxygenant is the 2-20% of acvator weight, or 5-15%, or 5-10%.
Said acvator also comprises one or more sequestrants.In one aspect, said sequestrant comprises polyamines and salt thereof.Term used herein " polyamines " is defined as has two or more replacements or any compound of substituted-amino (single, two, three or four) not.In one aspect, sequestrant comprises the EDTA disodium.On the other hand, the amount of sequestrant is less than 5% of acvator weight, less than 3%, less than 1%, less than 0.5% or less than 0.1%.
Said acvator can randomly comprise softening agent, thickening material, buffer reagent, catalyzer or its arbitrary combination.In one aspect, acvator comprises softening agent, thickening material, sequestrant, buffer reagent and catalyzer.Below describe each component in detail.
In one aspect, said softening agent comprises phthalic ester, adipic acid ester, trimellitate, sebate, benzoic ether, organophosphate, sulphonamide, citrate, vinyl halide (vinyl halide), vinylidene halide (vinylidene halide) or its arbitrary combination.On the other hand, said softening agent comprises bialkyl ortho phthalate.Term used herein " alkyl " is the saturated hydrocarbyl of 1-24 carbon atom of branching or non-branching, like methyl, ethyl, n-propyl, sec.-propyl, normal-butyl, isobutyl-, the tertiary butyl, amyl group, hexyl, heptyl, octyl group, decyl, tetradecyl, hexadecyl, eicosyl, tetracosyl etc." low alkyl group " group is the alkyl that comprises 1-6 carbon atom.In one aspect, softening agent is a dimethyl phthalate.In one aspect, the amount of softening agent is the 0.5-10% or the 1-5% of acvator weight.
But the quantum yield of the use enhanced chemiluminescence of catalyzer reaction.Can use USP 3,539 among this paper, disclosed catalyzer in 794 and 5,705,103, it is combined in here in full by reference.In one aspect, said catalyzer comprises quaternary ammonium compound, quaternary arsonium compound or quaternary phosphonium compound.On the other hand, said catalyzer comprises benzyl trialkyl ammonium compound or salicylate.To discuss like hereinafter, the character of the catalyzer of use and quantity can influence the time length and the intensity of chemiluminescence reaction.In one aspect, the amount of catalyzer is the 0.5-10% or the 1-5% of acvator weight.
Turn to said luminous agent (luminescer), said barkite/salt compound can be replacement or unsubstituted alkyl or aryl barkite or its salt.Term used herein " aryl " is any aromatic group based on carbon, includes but not limited to benzene, naphthalene etc.Term " aryl " also comprises " heteroaryl ", and said heteroaryl is defined as has the heteroatomic aromatic group of at least one intra-annular that is combined in aromatic group.Heteroatomic example includes but not limited to nitrogen, oxygen, sulphur and phosphorus.Said aryl can be replacement or unsubstituted.Said aryl can use one or more groups to replace, and said group includes but not limited to alkyl, alkynyl, thiazolinyl, aryl, halogen, nitro, amino, ester, ketone, aldehyde, hydroxyl, carboxylic acid or alkoxyl group.Term " alkyl " definition as above.
In one aspect, said barkite/salt compound is the solid of grind into powder subtly.This will guarantee that said barkite/salt is distributed in the whole acvator equably.In one aspect, the amount of barkite/salt compound is the 1-20% of said luminous agent weight, 5-10%, 5-20% or 5-15%.In one aspect, said barkite/salt compound comprises two (2,4; The 5-trichlorophenyl)-6-carbonyl pentyloxy phenyl) barkite (bis-(2,4,5-trichlorophenyl)-6-carbopentoxyphenyl) oxalate; CPPO) or two (2,4, the 5-trichlorophenyl) barkite (TCPO).
Second component of said luminous agent comprises fluorescent agent.Suitable fluorescent agent in visible-range (330nm-700nm) and in infra-red range (700nm-1000nm) have spectral emissions.By the chemical luminous composite wavelength of light emitted, promptly the color of the light of emission can change according to the specific fluorescent agent of adopting.In one aspect, can use the fluorescent agent of the four primaries light of the visible emitting spectrum in the table 1 among this paper.
Table 1
Color Fluorescent agent
Yellow 2-chloro-9, two (4-ethoxyl phenenyl) anthracenes of 10-; 1,5-two chloro-9, two (phenylacetylene base) anthracenes and 1 of 10-, 8-two chloro-9, two (phenylacetylene base) anthracenes of 10-
Red 1,7-two bromo-6,12-two phenoxys-N, N '-two (2-isopropyl phenyl)-3,4,9,10-perylene dicarboximide (perylenedicarboximide); 1,6,7,12-four phenoxys-N, N '-diethylammonium-3,4,9,10-perylene dicarboximide; 1,6,7,12-four (to fluorinated phenoxy)-N, N '-two (2, the 6-diisopropyl phenyl)-3,4,9,10-perylene dicarboximide; 1,6,7,12-four (adjacent fluorinated phenoxy)-N, N '-two (2, the 6-diisopropyl phenyl)-3,4,9,10-perylene dicarboximide; 1,6,7,12-four (adjacent chloro phenoxy)-N, N '-two (2, the 6-diisopropyl phenyl)-3,4,9,10-perylene dicarboximide; 1,6,7,12-four (to fluorinated phenoxy)-N, N '-two (2, the 6-diisopropyl phenyl)-3,4,9,10-perylene dicarboximide; 1,6,7,12-four (to tertiary butyl phenoxy)-N, N '-two (2, the 6-diisopropyl phenyl)-3,4,9,10-perylene dicarboximide; 1,6,7,12-four phenoxys)-N, N '-di neo-pentyl-3,4,9,10-perylene dicarboximide; 1,6,7,12-four (to the bromo phenoxy)-N, N '-two (2, the 6-diisopropyl phenyl)-3,4,9,10-perylene dicarboximide; 1,6,7,12-four phenoxys-N, N '-two (2, the 5-di-tert-butyl-phenyl)-3,4,9,10-perylene dicarboximide; 1,6,7,12-four phenoxys-N, N '-two (2, the 6-diisopropyl phenyl)-3,4,9,10-perylene dicarboximide;
Blue 2-chloro-9, two (4-ethoxyl phenenyl) anthracenes of 10-; 1-chloro-9, two (4-ethoxyl phenenyl) anthracenes of 10-
Green 9, two (phenylacetylene base) anthracenes of 10-; 2-ethyl-9, two (phenylacetylene base) anthracenes of 10-; 2-chloro-9, two (4-p-methoxy-phenyl) anthracenes of 10-; 1-chloro-9, two (phenylacetylene base) anthracenes of 10-
Orange 5,6,11,12-tetraphenyl tetracene
The example of radiative fluorescent agent includes but not limited to N in the IR scope, N '-two (2, the 5-di-tert-butyl-phenyl)-3,4,9,10-perylene dicarboximide, 16,17-butoxy violanthrone (violanthrone); 1-N, N-dibutylamino anthracene (abnthracene); Or iodate 6-methylacridine (6-methylacridinium iodide).
In some aspects, expectation obtains multiple different fluorescence color (fluorescent colors), does not still have the suitable fluorescent agent of available for this fluorescence color.Imagine two kinds or more fluorescent agents and can be used for compsn as herein described simultaneously, to obtain specific color.The selection of specific fluorescent agent and their relative concentration can produce multiple different colours.Table 2 has been listed some feasible combination of the fluorescent agent that sends following color of light: orange, pink, purple, dark green (turquoise) and white.
Table 2
Color/dyestuff The trade(brand)name of fluorescent chemicals/other title
Green 9, two (phenylacetylene base) anthracenes of 10-
Yellow 1,8-two chloro-9, two (phenylacetylene base) anthracenes of 10-
Red N, N '-two (2, the 5-di-tert-butyl-phenyl)-3,4,9,10-perylene dicarboximide
Blue 2-chloro-9, two (4-ethoxyl phenenyl) anthracenes of 10-
Orange 2-methyl isophthalic acid-anthraquinonyl amine
Pink The combination of redness and blue dyes
Purple The combination of redness and blue dyes
Dark green The combination of green and blue dyes
White The combination of redness, yellow and blue dyes
Infrared 16,17-butoxy violanthrone
In one aspect, but said fluorescent agent is the solid of fine grinding powdered.Similar with barkite/salt compound, this will guarantee that said fluorescent agent is uniformly distributed in the whole acvator.
Another component that is present in the powder as herein described comprises many solid particulates.Do not expect to accept the opinion constraint, the chemiluminescence reaction between said acvator and the luminous agent takes place in the surface of said solid particulate, and promptly it is a heterogeneous reaction.Depend on the selection of solid particulate, said particle can form chemical bond or can not form chemical bond with any component of existing in acvator and the luminous agent.In one aspect, said solid particulate be inert (promptly not with acvator and luminous agent in component form covalent linkage or non covalent bond).For example, the said solid particulate component of adsorption activation agent and luminous agent only.
In one aspect, said solid particulate comprises inorganic materials such as inorganic oxide, salt and element (elements).The example of inorganic oxide includes but not limited to silicon-dioxide, aluminum oxide, alkalimetal oxide, alkaline earth metal oxide, zeyssatite, zeolite or its arbitrary combination.Can use the multi-form of these materials among this paper.For example, can use fused silica or colloidal silica among this paper.The example of inorganic salt comprises carbonate, silicate and other natural or synthetic materials.Also imagine inorganic oxide and salt and can comprise other component.For example, zeyssatite comprises (elemental metals) silicon-dioxide of sodium, magnesium and iron for example that has the oligo-elements metal.
Also can use the mixture of inorganic oxide and salt.For example, zeolite is for comprising SiO 2, Al 2O 3And Na 2The aluminosilicate material of the mixture of O.The example that can be used for the zeolite among this paper includes but not limited to amicite; Euthalite; The red zeolite of sodium (barrerite); Bel's Burger stone; Silicon lithium aluminium stone; Burgers stone (boggsite); Brusterite; Chabazite; Clinoptilolite; Cowlesite; Dachiardite; Edingtonite; Epistilbite; Erionite; Faujusite; Ferrierite; Garranite; Gismondite; Sarcolite; Dagger-axe silicon sodium aluminium stone; Gonnardite; Goosecreekite; Harmotome; Herschelite; Heulandite; Lomontite; Levyne; Plumbous zeolite not; Mazzite; Merlinoite; Mesolite; The Meng Tesuo horse; Mordenite; Natrolite; Offretite (offretite); Secondary natrolite; Paulingite; Severe edema due to hypofunction of the spleen Si-Al-K stone (perlialite); Phillipsite; Pollux; Scolecite; The sodium dachiardite; Stellerite; Stilbite; Tetranatrolite; Thomsonite; Lack mud zeolite (tschernichite); Wairakite; Wellsite; Potassium chabazite (willhendersonite); Yugawaralite or its arbitrary combination.
The amount that is used to prepare the solid particulate of said powder can change; Yet it is present in the said powder with high quantity usually.The amount of the solid particulate that exists in the said powder can change the speed of reaction between the different components (for example oxygenant, barkite/salt, fluorescent agent) that exists in the powder, and it can finally change the aura time and intensity.The amount of solid particulate also can change the quality (texture) of said powder.For example, if expectation obtains " doing " powder, then can add more solid particulate.In one aspect, solid particulate is 50%-95%, 60%-95% or the 70%-90% of said powder weight.
The preparation of chemoluminescence powder is below described.The different components of acvator is mixed with various order each other, to produce homogeneous compositions.In one aspect, with solvent, sequestrant and oxygenant pre-mixing.Then, add inorganic materials.Here, also can add optional component such as thickening material.Said mixture mixing time enough is scattered in the whole powder to guarantee all components.At last, be added into fluorescent agent and barkite/salt in the mixture, to produce final chemoluminescence powder.For most of situation, powder is done; Yet owing to there is water, powder also can be moist slightly.The example process of producing said powder provides in embodiment 1 and 2.
In yet another aspect, can acvator and luminous agent be stored in the independent packaging before mixing each other.In one aspect, before using the chemoluminescence powder, acvator and luminous agent are remained in the independent packaging, wherein said packing do not allow air admission and with the component reaction of acvator and luminous agent.In this regard, the solid particulate with inorganic materials is incorporated in each packing.For example, can acvator and luminous agent be placed in (hermitically sealed) aluminium foil Blister Package (bubble packs) of independently stopping property sealing, to keep the storage time of acvator and luminous agent.When being time use chemoluminescence powder, acvator being released into the open container from said packing, and passing through vigorous stirring luminous agent and activator mix.So, be reflected in the open space (open air) and carry out, this chemical luminous composite with prior art is different.
The component that exists in acvator and the luminous agent reacts to each other when mixing, and produces visible or infrared light.Do not expect to accept opinion constraint, oxygenant (H for example 2O 2) react with barkite/salt compound, produce high reactive ring-type peroxide thing class (peroxy species).Then, this thing class fluorescence excitation agent.The fluorescent agent ballistic phonon of being excited (being quantity of radiant energy) turns back to stable ground state then.The color of the light of emission depends on that photon is from the frequency of fluorescent agent emission in the visible spectrum range.
Speed of reaction between the component of acvator and luminous agent especially can change through the rate of diffusion of oxygenant, barkite/salt compound and fluorescent agent in the control chemical luminous composite, and wherein said speed of reaction has determined the intensity and the time length of aura.For example, through regulating the concentration of solvent, softening agent, thickening material and sequestrant, can control aura intensity and time length especially.Thereby the compsn of describing among this paper can be launched coloured light 1 hour to 12 hours.
Because compsn as herein described does not use the organic solvent with smell and painted (staining) character that meets with opposition usually, so compsn as herein described can be applicable to numerous base materials.In addition, the toxicity of said compsn is much lower.As stated, said compsn can be applied to skin or hair partly.Alternatively, said composition can be applicable to clothing item or other base material.Powder as herein described is different from the chemical luminous composite that in other uses like analytical technology, uses.For example, compsn as herein described does not have like USP 6,251, and being attached to of limiting in 581 is used for producing the specificity binding partner (specific bindingpartners) (for example part) of any component of the powder of this paper.Usually, powder as herein described is prepared to use with the dry form that can directly apply to substrate surface.
In others, powder as herein described can be used for preparing moulded product (molded article).For example, can the wet form (like material mud (sludge), slurries (slurry) etc.) of powder be imported in the mould, and through in mould, applying water or the solvent that heat is removed remnants in drying at room temperature or to mould.The example that comprises the moulded product of chemical luminous composite described herein comprises chalk.A kind of example process of being produced chalk by chemical luminous composite is provided among the embodiment 2.Said chalk is used on paper or the rigid surface (like wall, floor etc.) and writes or draw, and wherein picture is luminous in the dark.
Because compsn described herein does not use the organic solvent that meets with opposition with smell and coloring property usually, so compsn as herein described can be applicable to a large amount of base materials.In addition, the toxicity of said compsn is much lower.Said compsn can be applied topically to skin or hair, and is easy to handle and need not extra security measures.
In one aspect, said chemical luminous composite is a gel.In one aspect, said chemical luminous composite is by comprising the method production that mixes following material:
A. acvator, it comprises that (i) comprises the solvent of water and at least a organic solvent, (ii) oxygenant and (iii) softening agent, thickening material, sequestrant, buffer reagent, catalyzer or its arbitrary combination; With
B. luminous agent, it comprises barkite/salt compound and fluorescent agent,
Wherein said compsn does not contain granulated material.
Can use any described acvator and luminous agent to produce said gel.Be different from above-mentioned powder, said acvator and luminous agent all do not comprise granulated material." granular " used herein is meant the material of the little solid particulate that comprises crystalline structure, and wherein said particle (1) is insoluble to or is slightly soluble in any liquid ingredient of chemical luminous system; Or (2) if dissolve in the liquid ingredient, and then said liquid ingredient exists with the amount of the measurement agent (metering agent) that is not enough to dissolve substantial part; Or (3) liquid ingredient not be for will significantly dissolve said particulate form, for example thickening material.For example, if with the thickening before introducing particle of said liquid, then this liquid ingredient is not with the form of significantly dissolving said granular particle.Gel described herein they be homogeneous and do not contain on above-mentioned solid particulate or the crystalline meaning, be uniform.
In embodiment 3 and the table 8 a kind of example process of producing said gel is provided.Mixing process is implemented in stainless steel device in several steps, to guarantee to form even gel.Under the situation of said gel, the amount of solvent also can change according to the component that being used to of selecting produced acvator.In one aspect, the amount of water is 40-85%, 45-80%, the 50-70% of acvator weight.On the other hand, said organic solvent is the 0.5-20% or the 1-15% of acvator weight.As discussed above, can be with said gel application in skin or hair and there is not safety worries.
In others, can use any chemical luminous composite described herein to prepare coating (paint).Can said compsn be mixed with many different coating, for example latex (latex) and oil-based paint.In others, because the nontoxic character of chemical luminous composite described herein, said coating can be the finger coating (finger paint) safe in utilization to children.A kind of example process of producing finger coating is provided among the embodiment 4.
Embodiment
Following examples are proposed; The complete open of compound, compsn and method how to produce and assess this paper record and require protection being provided to those of ordinary skills and describing, and said embodiment thinks and is merely exemplary and does not prepare to limit the contriver thinks their scope of invention.About number (for example amount, temperature etc.), guaranteed particularity as possible, yet should consider to exist some sum of errors deviations.Unless otherwise indicated, otherwise umber is meant weight part, temperature be in ℃ or be envrionment temperature and pressure equals or near barometric point (atmospheric).There are the variation and the combination of the reaction conditions can be used for optimizing the product purity that obtains by said method and productive rate in a large number, for example the solvent of concentration of component, expectation, solvent mixture, temperature, pressure and other reaction range and condition.Optimize these processing condition with only needing reasonable and conventional experiment.
Embodiment 1
Present embodiment is provided for the compsn of high aura intensity aura powder (high-glow intensity glowpowder).Table 3 and 4 provides the composition of producing acvator and luminous agent respectively.Table 5 has been listed the order of the high aura intensity aura powder that is used to produce time length 4-6 hour.Mixing process is implemented in stainless steel device to guarantee to form the powder of well blend in several steps.
Be the powder of production well blend, order 1 liquid ingredient is added in the stainless steel device with built-in homogenizer, and 2,000-2,500 RPM be heated to about 35 ℃, mix fully guaranteeing.One when being cooled to room temperature with this mixture, with regard to interpolation order 2.In abundant stirring, promptly under the 200-250RPM, interpolation is 3 composition in proper order then, and is each a small amount of, to guarantee the powder of well blend.The composition of the order of interpolation subsequently 4.
Order 4 is a luminous agent.The CPPO of powder type and fluorescent agent are mixed and grind to form thinner powder.The luminous agent powder is added in the activator powder, and under the quality control condition, stirs, to confirm (validate) reaction times and color.Observe the HS aura immediately, it lasts up to 6 hours.
Table 3: the concentration range and the composition that are used to have the HS aura powder activator of 4-6 hour aura time
No. The INCI title Function CAS number Concentration (w%)
1 Water (aqua) Solvent 7732-18-5 2.9-3.3
2 PEG-400 Wetting agent/solvent 25322-68-3 <1
3 Zeyssatite Absorption agent 61790-53-2 2-3
4 SiO 2 powder High area surface 7631-86-9 40-50
5 Urea peroxide Oxygenant 124-43-6 5-15
6 Dimethyl phthalate Solvent/softening agent 131-11-3 3-7
7 The EDTA disodium Chelating/viscosity controller 6381-92-6 <0.1
8 Aluminum oxide Inert granular material 1344-28-1 10-15
Amount to 65-95
Table 4: the concentration range of composition in the luminous agent powder
No. Trade(brand)name/other title Function CAS number Concentration (w %)
Fluorescent agent Dyestuff 0.2-0.3
Two (2,4, the 5-trichlorophenyl)-6-carbonyl pentyloxy phenyl) barkite (CPPO) Chemiluminescence compound 30431-54-0 5-15
SiO 2 powder High area surface 10-20
Aluminum oxide Inert granular material 5-10
Amount to 20-45
Table 5: the order of composition with HS aura powder of 4-6 hour aura time
SN Composition
1 Water, PEG-400, dimethyl phthalate, EDTA disodium, urea peroxide
2 Carbopol, zeyssatite
3 Aluminum oxide, SiO 2 powder
4 Fluorescent agent, CPPO
Embodiment 2
Present embodiment is provided for preparing the compsn of high aura intensity chalk.Table 6 and 7 is provided for producing the composition of acvator and luminous agent respectively.For producing chalk, acvator and fluorescent agent are added in the stainless steel device that comprises 10% weight water.Said stainless steel device has can be at the built-in whisking appliance of 200RPM running, to guarantee the mixing fully of material mud.In this mixture, add the terra alba (CAS number: of the very fine grainding of 30 weight % 99400-01-8) with the zeyssatite clay that is equal to the ground fine grainding of 20 weight % (CAS number: 61790-53-2), keep simultaneously stirring fully, i.e. 200RPM.Should expect then that mud was poured onto in the mould, excellent to form long 3 inches chalks with 0.5 inch of diameter.Said material mud spends 30 minutes in room temperature (promptly 22 ℃) and comes drying in mould.Said chalk be used in write or draw on paper or the crust and picture luminous in the dark.
Table 6: concentration range and composition with the HS aura chalk acvator that surpasses 12 hours aura time
Sequence number The INCI title Function CAS number Concentration (w%)
1 Water Solvent 7732-18-5 ?10-15
2 PEG-400 Wetting agent/solvent 25322-68-3 ?<1
3 Zeyssatite Absorption agent 61790-53-2 ?15-20
4 SiO 2 powder High area surface 7631-86-9 ?20-25
5 Urea peroxide Oxygenant 124-43-6 ?1.5-5
6 Dimethyl phthalate Solvent/softening agent 131-11-3 ?1-2.5
7 The EDTA disodium Chelating/viscosity controller 6381-92-6 ?<0.1
8 Aluminum oxide Inert granular material 1344-28-1 ?3.5-5
Amount to ?50-70
Table 7: the concentration range of composition in the luminous agent component of aura chalk
Sequence number Trade(brand)name/other title Function CAS number Concentration (w%)
Fluorescent agent Dyestuff 0.2-0.3
Two (2,4, the 5-trichlorophenyl)-6-carbonyl pentyloxy phenyl) barkite (CPPO) Chemiluminescence compound 30431-54-0 1.5-5
SiO 2 powder High area surface 7631-86-9 3.5-7
Aluminum oxide Inert granular material 1344-28-1 1.5-4
Amount to 7-15
Embodiment 3
Present embodiment is provided for the compsn of high aura intensity aura gel.Table 8 and 9 is provided for producing the composition of acvator and luminous agent respectively.Table 10 has been listed the order that is used to produce high aura intensity, short time length chemoluminescence gel.Mixing process is implemented in stainless steel device in several steps, to guarantee to form homogeneous gel.
For producing even gel, the solvent of order 1 is added in the stainless steel device with built-in homogenizer, and 2,000-2,500 RPM are heated to about 35 ℃, mix fully guaranteeing.In case this mixture is cooled to room temperature, add (added in increments) order 2 with regard to increment, to avoid caking.Then in abundant stirring, promptly 2,000-2,500RPM is with each a kind of composition of form interpolation order 3.The composition of the order of interpolation subsequently 4, it also is to add with each a kind of form.Keep stirring until forming even gel.At last, stir down at sweep buffering order 5 is added in the gel, and the adjusting mixing rate, be neutralized and evenly until gel.
Order 6 is a luminous agent.The CPPO of powder type and fluorescent agent are mixed and grind to form thinner powder.Then the luminous agent powder is added in the above-mentioned acvator gel, and under the quality control condition, stirs, to confirm reaction times and color.Observe the HS aura immediately, it lasts up to 6 hours.
Table 8: the concentration range and the composition that are used to have the HS aura acvator gel of 4-6 hour aura time
Sequence number The INCI title Function CAS number Concentration (w%)
1 Water Solvent 7732-18-5 50-75
2 PEG-400 Wetting agent/solvent 25322-68-3 1-5
3 Glycerine Wetting agent/solvent 56-81-5 5-10
4 Carbomer-940 Skin conditioner 9003-01-4 <1
5 Trolamine Buffer reagent 102-71-6 <1
6 Benzyltriethylammonium chloride Antistatic/catalyzer 56-37-1 <1
7 PVP?K90 Hair fixing agent/stiffening agent 9003-39-8 1-5
8 Urea peroxide Oxygenant 124-43-6 5-10
9 Dimethyl phthalate Solvent/softening agent 131-11-3 1-5
10 The EDTA disodium Chelating/viscosity controller 6381-92-6 <1
11 Natvosol Thickening material 9004-62-0 <1
Amount to 75-100
Table 9: the concentration range of composition in the luminous agent powder
Sequence number Trade(brand)name/other title Function CAS number Concentration (w%)
Fluorescent agent Dyestuff 0.2-0.3
Two (2,4, the 5-trichlorophenyl)-6-carbonyl pentyloxy phenyl) barkite (CPPO) Chemiluminescence compound 30431-54-0 5-10
Amount to 5-10
Table 10: the order of composition that is used to have the HS aura gel of 4-6 hour aura time
SN Composition
1 Water, glycerine, PEG-400, hydroxylated cellulose
2 Carbomer-940
3 Benzyltriethylammonium chloride, dimethyl phthalate, EDTA disodium, urea peroxide
4 PVP?K90,Fragrance(Manheimer?874072)
5 Trolamine
6 Fluorescent agent, CPPO
Embodiment 4
In the present embodiment, table 10 has been listed the order that is used to produce the chemoluminescence finger coating that hangs down aura intensity, long duration.Table 11 provides the composition that is used to produce acvator.Use the fluorescent agent in the table 9.Uniformly the solvent of finger coating through at first will order 1 is added in the stainless steel device with built-in homogenizer, and 2, and 000-2,500 RPM are heated to about 35 ℃ and produce guaranteeing to mix fully.When this mixture was cooled to room temperature, increment interpolation order 2 was to avoid caking.Then in abundant stirring, i.e. 2000-2,500RPM is with each a kind of composition of form interpolation order 3.Same subsequently composition with a kind of at every turn form interpolation order 4, and keep stirring until the uniform finger of formation coating.Then will order 5 buffer mixture stir and be added into down in the finger coating, and regulate mixing rate, until pointing that coating is neutralized and evenly at sweep.
Order 6 is a luminous agent.The CPPO of powder type and fluorescent agent are mixed and grind to form much thin powder.Then the luminous agent powder is added in the acvator gel of above preparation, and under the quality control condition, stirs, to confirm reaction times and color.Observe high-intensity relatively aura immediately, it lasts up to 18 hours.
Table 11: the concentration range and the composition that are used to have the low aura intensity finger coating acvator of 12-18 hour aura time
Sequence number The INCI title Function CAS number Concentration (w%)
1 Water Solvent 7732-18-5 ?50-75
2 PEG-400 Wetting agent/solvent 25322-68-3 ?1-5
3 Glycerine Wetting agent/solvent 56-81-5 ?5-10
4 Carbomer-940 Skin conditioner 9003-01-4 ?3-5
5 SS Catalyzer 1344-09-8 ?1-5
6 Dodecylbenzene sulfonate Emulsifying agent 1886-81-3 ?<1
7 PVP?K90 Stiffening agent 9003-39-8 ?1-3
8 Urea peroxide Oxygenant 124-43-6 ?5-10
9 Dimethyl phthalate Solvent/softening agent 131-11-3 ?1-3
10 The EDTA disodium Chelating/viscosity controller 6381-92-6 ?<1
Amount to ?75-100
Table 12: order with low strength finger coating composition of 12-18 hour aura time
SN Composition
1 Water, glycerine, PEG-400, Natvosol
2 Carbomer-940
3 SS, urea peroxide, dodecylbenzene sulfonate
4 PVP?K90,Fragrance(Manheimer?874072)
5 Dimethyl phthalate, EDTA disodium
6 Fluorescent agent, CPPO
In whole the application, with reference to many parts of open source literatures.Therefore, the disclosure of these open source literatures is incorporated among the application with their integral body by reference, to describe compound as herein described, compsn and method more all sidedly.
Can carry out various improvement and change to compound as herein described, compsn and method.The others of compound described herein, compsn and method will become obvious through detailed description and the practice of considering compound disclosed herein, compsn and method.Said detailed description and embodiment should be counted as exemplary.

Claims (14)

1. chemoluminescence powder, it comprises (i) water and at least a organic solvent; (ii) oxygenant and (iii) sequestrant; (iv) barkite/salt; (v) fluorescent agent; (the many solid particulates that vi) comprise one or more inorganic materials, wherein component (i)-(vi) all not having the specificity that is attached on it combines the unit.
2. the compsn of claim 1, wherein said organic solvent comprises polyvalent alcohol.
3. the compsn of claim 1, wherein said oxygenant comprises urea peroxide, hydrogen peroxide, sodiumperoxide, Sodium peroxoborate, peroxo-trisodium phosphate, hydrogen peroxide precursor or their arbitrary combination.
4. the compsn of claim 1, wherein said sequestrant comprises polyamines or its salt.
5. the compsn of claim 1; Wherein said compsn comprises that further softening agent and wherein said softening agent comprise phthalic ester, adipic acid ester, trimellitate, sebate, benzoic ether, organophosphate, sulphonamide, citrate, vinyl halide, vinylidene halide or their arbitrary combination.
6. the compsn of claim 1, wherein said barkite/salt compound comprise and replacing or unsubstituted aryl or alkyl barkite.
7. the compsn of claim 1, wherein said fluorescent agent comprises 2-chloro-9, two (4-ethoxyl phenenyl) anthracenes of 10-; 1,5-two chloro-9, two (phenylacetylene base) anthracenes and 1 of 10-, 8-two chloro-9, two (phenylacetylene base) anthracenes of 10-; Rubrene; 1,7-two bromo-6,12-two phenoxys-N, N '-two (2-isopropyl phenyl)-3,4,9,10-perylene dicarboximide; 1,6,7,12-four phenoxys-N, N '-diethylammonium-3,4,9,10-perylene dicarboximide; 1,6,7,12-four (to fluorinated phenoxy)-N, N '-two (2, the 6-diisopropyl phenyl)-3,4,9,10-perylene dicarboximide; 1,6,7,12-four (adjacent fluorinated phenoxy)-N, N '-two (2, the 6-diisopropyl phenyl)-3,4,9,10-perylene dicarboximide; 1,6,7,12-four (adjacent chloro phenoxy)-N, N '-two (2, the 6-diisopropyl phenyl)-3,4,9,10-perylene dicarboximide; 1,6,7,12-four (to fluorinated phenoxy)-N, N '-two (2, the 6-diisopropyl phenyl)-3,4,9,10-perylene dicarboximide; 1,6,7,12-four (to tertiary butyl phenoxy)-N, N '-two (2, the 6-diisopropyl phenyl)-3,4,9,10-perylene dicarboximide; 1,6,7,12-four phenoxys)-N, N '-di neo-pentyl-3,4,9,10-perylene dicarboximide; 1,6,7,12-four (to the bromo phenoxy)-N, N '-two (2, the 6-diisopropyl phenyl)-3,4,9,10-perylene dicarboximide; 1,6,7,12-four phenoxys-N, N '-two (2, the 5-di-tert-butyl-phenyl)-3,4,9,10-perylene dicarboximide; 1,6,7,12-four phenoxys-N, N '-two (2, the 6-diisopropyl phenyl)-3,4,9,10-perylene dicarboximide; 2-chloro-9, two (4-ethoxyl phenenyl) anthracenes of 10-; 1-chloro-9, two (4-ethoxyl phenenyl) anthracenes of 10-; 9, two (phenylacetylene base) anthracenes of 10-; N, N '-two (2, the 5-di-tert-butyl-phenyl)-3,4,9,10-perylene dicarboximide; 16,17-butoxy violanthrone; 1-N, N-dibutylamino anthracene; Or iodate 6-methylacridine
Figure DEST_PATH_FSB00000791917100021
, or their combination.
8. the compsn of claim 1, wherein said inorganic materials comprises inorganic salt, inorganic oxide, inorganic elements or their arbitrary combination.
9. the compsn of claim 11, wherein said inorganic oxide comprises silicon-dioxide, aluminum oxide, alkalimetal oxide, alkaline earth metal oxide, zeyssatite, zeolite or their arbitrary combination.
10. moulded product, it comprises the compsn that claim 1-9 is any.
11. the moulded product of claim 10, wherein said goods are chalk.
12. comprise the coating of chemical luminous composite, this chemical luminous composite comprises:
A. acvator, it comprises (i) solvent, comprises water and at least a organic solvent; (ii) oxygenant and (iii) softening agent, thickening material, sequestrant, buffer reagent, catalyzer or their arbitrary combination; With
B. luminous agent, it comprises barkite/salt compound and fluorescent agent,
Wherein said compsn does not contain granulated material.
13. the coating of claim 12, wherein said coating is finger coating.
14. the one-tenth cover material, it comprises
A. acvator, it comprises (i) solvent, comprises water and at least a organic solvent; (ii) oxygenant and (iii) sequestrant; (iv) first inorganic materials; And
B. luminous agent, it comprises (i) barkite/salt compound, (ii) fluorescent agent and (iii) second inorganic materials,
Wherein said component does not all have the specificity that is attached on it and combines the unit.
CN2010102324577A 2010-07-16 2010-07-16 Chemiluminescent compositions, and production and use methods thereof Pending CN102585799A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110229659A (en) * 2019-05-24 2019-09-13 中山大学 A kind of oxalate ester peroxide/hydrogel shines phase system and its preparation method and application

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2010001761A1 (en) * 2008-06-30 2010-01-07 アイオン株式会社 Sponge roller for cleaning

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2010001761A1 (en) * 2008-06-30 2010-01-07 アイオン株式会社 Sponge roller for cleaning

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110229659A (en) * 2019-05-24 2019-09-13 中山大学 A kind of oxalate ester peroxide/hydrogel shines phase system and its preparation method and application
CN110229659B (en) * 2019-05-24 2022-10-25 中山大学 Peroxyoxalate/hydrogel luminescent phase system and preparation method and application thereof

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