CN108727531A - Advertisement light emitting word photoelectric functional method for glass preparation and its product - Google Patents

Advertisement light emitting word photoelectric functional method for glass preparation and its product Download PDF

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Publication number
CN108727531A
CN108727531A CN201810505209.1A CN201810505209A CN108727531A CN 108727531 A CN108727531 A CN 108727531A CN 201810505209 A CN201810505209 A CN 201810505209A CN 108727531 A CN108727531 A CN 108727531A
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China
Prior art keywords
parts
luminescent powder
photoelectric functional
light emitting
temperature
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CN201810505209.1A
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Chinese (zh)
Inventor
周小二
周心刚
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Anhui Xintao Optoelectronics Technology Co Ltd
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Anhui Xintao Optoelectronics Technology Co Ltd
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Priority to CN201810505209.1A priority Critical patent/CN108727531A/en
Publication of CN108727531A publication Critical patent/CN108727531A/en
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    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08FMACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F220/00Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
    • C08F220/02Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
    • C08F220/10Esters
    • C08F220/12Esters of monohydric alcohols or phenols
    • C08F220/14Methyl esters, e.g. methyl (meth)acrylate
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B29WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29CSHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C39/00Shaping by casting, i.e. introducing the moulding material into a mould or between confining surfaces without significant moulding pressure; Apparatus therefor
    • B29C39/02Shaping by casting, i.e. introducing the moulding material into a mould or between confining surfaces without significant moulding pressure; Apparatus therefor for making articles of definite length, i.e. discrete articles
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08FMACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F2/00Processes of polymerisation
    • C08F2/44Polymerisation in the presence of compounding ingredients, e.g. plasticisers, dyestuffs, fillers

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  • Chemical & Material Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • Luminescent Compositions (AREA)

Abstract

The invention discloses advertisement light emitting word photoelectric functional method for glass preparation and its product, main preparation process includes pre-polymerization material, moulding, polymerization, post-processing, and product includes following component according to the mass fraction:105 ~ 140 parts of methyl methacrylate, 3 ~ 7 parts of azodiisobutyronitrile, 1 ~ 3 part of n-butanol, 15 ~ 25 parts of hexahydrophthalic anhydride, modified 8 ~ 18 parts of luminescent powder, 3 ~ 8 parts of stearic acid sodium, 0.1 ~ 1 part of two contracting omega-diol diacrylate, 0.5 ~ 1.5 part of triaryl hexafluorophosphoric acid sulfosalt.Photoelectric functional method for glass preparation of the present invention is simple and practical, solve the problems, such as that luminescent powder is difficult to be uniformly distributed in methyl methacrylate and long-term is easy precipitation agglomerate, and photoelectric functional glass obtained has outstanding illumination effect, fluorescent lifetime long, bright uniform.

Description

Advertisement light emitting word photoelectric functional method for glass preparation and its product
Technical field
The present invention relates to organic glass technical field more particularly to advertisement light emitting word photoelectric functional method for glass preparation and Its product.
Background technology
Organic glass is widely used, and is not only used in business, light industry, building, chemical industry etc., and advertising decoration, Using very extensive on sand table model, such as label, billboard, the panel etc. of lamp box.Organic glass is by methyl methacrylate (MMA)The high-molecular compound being polymerized is a kind of exploitation important thermoplastic earlier, and organic glass has preferable The advantages that transparency, chemical stability, mechanical property, weatherability, easy dyeing, easy processing and attractive appearance.
Long-persistence luminous phenomenon refers to the energy that certain material can absorb extraneous light radiation, and then this material is slow again The phenomenon that these storage energies are discharged in the form of visible light, long-persistence luminous phenomenon, which can be applicable to, forms advertisement in organic glass Luminescent characters.But long-persistence luminous raw material is difficult to be uniformly distributed in organic glass and long-term is easy precipitation agglomerate, after causing Phase molding organic glass there are non-uniform light, illumination effect is undesirable the problems such as.
Invention content
The present invention in view of the deficienciess of the prior art, provide advertisement light emitting word photoelectric functional method for glass preparation and Its product, specific technical solution are as follows:
Advertisement light emitting word photoelectric functional method for glass preparation, includes the following steps:
(1)Pre-polymerization material:Methyl methacrylate and azodiisobutyronitrile are added in a stirring kettle, stirs, has fed in charging Stirred tank be warming up to 75 DEG C and keep the temperature 45min after finishing, backward stirred tank in addition n-butanol, hexahydrophthalic anhydride, Modified luminescent powder, odium stearate, two contracting omega-diol diacrylates, triaryl hexafluorophosphoric acid sulfosalt are heated to 93 DEG C and keep the temperature 1 ~ 2h, system viscosity reaches 2000cP in kettle to be mixed, and cooling is spare;
(2)Moulding:Moulding, the moulding concrete operations are carried out in organic glass particular manufacturing craft after above-mentioned reaction system is filtered To pad upper one between the silica glass tablet of two pieces of cleaning, dryings by specific thickness and enclosing the rubber filler strip for being surrounded by glassine paper, with folder Tool clips, cast, exhaust bubble, sealing;
(3)Polymerization:The mold of casting complete is hung in constant temperature water tank and is totally submerged, control temperature at 55 ~ 75 DEG C and keep 2 ~ 4h;Then it hangs out mold and is put into high temperature drying chamber, control temperature is at 95 ~ 115 DEG C and keeps 1 ~ 3h, and simultaneously at ultraviolet light Reason;
(4)Post-processing:The mold that polymerization is completed is placed under light protected environment and is cooled to room temperature die sinking;It takes out among after molding Methacrylate sheet, trimming are cut, packaging.
Further, the preparation method of the modified luminescent powder is that methacrylic acid and silane crosslinker are added to dress Have in the stirred tank of ethylene glycol, stir and is warming up to 85 ~ 95 DEG C of 30 ~ 90min of holding;Then reaction system is transferred to sonic oscillation In device, luminescent powder, oxidized polyethylene wax, stearic acid sodium, 30 ~ 45min of ultrasonic disperse is added;It is filtered by vacuum and dries, with high speed Ball mill grinding is sieved up to the modified luminescent powder.
Further, advertisement light emitting word photoelectric functional glassware, including following component according to the mass fraction: 105 ~ 140 parts of methyl methacrylate, 3 ~ 7 parts of azodiisobutyronitrile, 1 ~ 3 part of n-butanol, hexahydrophthalic anhydride 15 ~ 25 Part, modified 8 ~ 18 parts of luminescent powder, 3 ~ 8 parts of stearic acid sodium, 0.1 ~ 1 part of two contracting omega-diol diacrylate, triaryl hexafluorophosphoric acid sulphur 0.5 ~ 1.5 part of salt.
Further, the modified luminescent powder includes following component according to the mass fraction:30 ~ 40 parts of methacrylic acid, 5 ~ 10 parts of silane crosslinker, 60 ~ 80 parts of ethylene glycol, 55 ~ 75 parts of luminescent powder, 3 ~ 10 parts of oxidized polyethylene wax, stearic acid sodium 4 ~ 12 Part.
Beneficial effects of the present invention:Photoelectric functional method for glass preparation of the present invention is simple and practical, solves luminous The problem of powder is difficult to be uniformly distributed in methyl methacrylate and long-term is easy precipitation agglomerate, and photoelectric functional glass obtained Glass has outstanding illumination effect, fluorescent lifetime long, bright uniform.
Specific implementation mode
In order to make the purpose , technical scheme and advantage of the present invention be clearer, with reference to embodiments, to the present invention It is further elaborated.It should be appreciated that the specific embodiments described herein are merely illustrative of the present invention, it is not used to Limit the present invention.
Embodiment 1
Advertisement light emitting word photoelectric functional method for glass preparation, includes the following steps:
(1)Pre-polymerization material:Methyl methacrylate and azodiisobutyronitrile are added in a stirring kettle, stirs, has fed in charging Stirred tank be warming up to 75 DEG C and keep the temperature 45min after finishing, backward stirred tank in addition n-butanol, hexahydrophthalic anhydride, Modified luminescent powder, odium stearate, two contracting omega-diol diacrylates, triaryl hexafluorophosphoric acid sulfosalt, are heated to 93 DEG C and keep the temperature 1h, system viscosity reaches 2000cP in kettle to be mixed, and cooling is spare;
(2)Moulding:Moulding, the moulding concrete operations are carried out in organic glass particular manufacturing craft after above-mentioned reaction system is filtered To pad upper one between the silica glass tablet of two pieces of cleaning, dryings by specific thickness and enclosing the rubber filler strip for being surrounded by glassine paper, with folder Tool clips, cast, exhaust bubble, sealing;
(3)Polymerization:The mold of casting complete is hung in constant temperature water tank and is totally submerged, control temperature at 55 DEG C and keeps 2h;So After hang out mold and be put into high temperature drying chamber, control temperature at 95 DEG C and keeps 1h, and is handled simultaneously with ultraviolet light;
(4)Post-processing:The mold that polymerization is completed is placed under light protected environment and is cooled to room temperature die sinking;It takes out among after molding Methacrylate sheet, trimming are cut, packaging.
In the present embodiment, the preparation method of the modified luminescent powder is to be added to methacrylic acid and silane crosslinker In stirred tank equipped with ethylene glycol, stirs and be warming up to 85 DEG C of holding 30min;Then reaction system is transferred to ultrasonator In, luminescent powder, oxidized polyethylene wax, stearic acid sodium, ultrasonic disperse 30min is added;It is filtered by vacuum and dries, use high speed ball mill It is ground up, sieved up to the modified luminescent powder.
In the present embodiment, advertisement light emitting word photoelectric functional glassware, including according to the mass fraction such as the following group Point:105 parts of methyl methacrylate, 3 parts of azodiisobutyronitrile, 1 part of n-butanol, 15 parts of hexahydrophthalic anhydride, modified hair 8 parts of light powder, 3 parts of stearic acid sodium, 0.1 part of two contracting omega-diol diacrylate, 0.5 part of triaryl hexafluorophosphoric acid sulfosalt.
In the present embodiment, the modified luminescent powder includes following component according to the mass fraction:30 parts of methacrylic acid, silicon 5 parts of alkane crosslinking agent, 60 parts of ethylene glycol, 55 parts of luminescent powder, 3 parts of oxidized polyethylene wax, 4 parts of stearic acid sodium.
Embodiment 2
Advertisement light emitting word photoelectric functional method for glass preparation, includes the following steps:
(1)Pre-polymerization material:Methyl methacrylate and azodiisobutyronitrile are added in a stirring kettle, stirs, has fed in charging Stirred tank be warming up to 75 DEG C and keep the temperature 45min after finishing, backward stirred tank in addition n-butanol, hexahydrophthalic anhydride, Modified luminescent powder, odium stearate, two contracting omega-diol diacrylates, triaryl hexafluorophosphoric acid sulfosalt, are heated to 93 DEG C and keep the temperature 1.5h, system viscosity reaches 2000cP in kettle to be mixed, and cooling is spare;
(2)Moulding:Moulding, the moulding concrete operations are carried out in organic glass particular manufacturing craft after above-mentioned reaction system is filtered To pad upper one between the silica glass tablet of two pieces of cleaning, dryings by specific thickness and enclosing the rubber filler strip for being surrounded by glassine paper, with folder Tool clips, cast, exhaust bubble, sealing;
(3)Polymerization:The mold of casting complete is hung in constant temperature water tank and is totally submerged, control temperature at 65 DEG C and keeps 3h;So After hang out mold and be put into high temperature drying chamber, control temperature is at 105 DEG C and keeps 1 ~ 3h, and is handled simultaneously with ultraviolet light;
(4)Post-processing:The mold that polymerization is completed is placed under light protected environment and is cooled to room temperature die sinking;It takes out among after molding Methacrylate sheet, trimming are cut, packaging.
In the present embodiment, the preparation method of the modified luminescent powder is to be added to methacrylic acid and silane crosslinker In stirred tank equipped with ethylene glycol, stirs and be warming up to 90 DEG C of holding 60min;Then reaction system is transferred to ultrasonator In, luminescent powder, oxidized polyethylene wax, stearic acid sodium, ultrasonic disperse 40min is added;It is filtered by vacuum and dries, use high speed ball mill It is ground up, sieved up to the modified luminescent powder.
In the present embodiment, advertisement light emitting word photoelectric functional glassware, including according to the mass fraction such as the following group Point:120 parts of methyl methacrylate, 5 parts of azodiisobutyronitrile, 2 parts of n-butanol, 20 parts of hexahydrophthalic anhydride, modified hair 13 parts of light powder, 5 parts of stearic acid sodium, 0.5 part of two contracting omega-diol diacrylate, 1 part of triaryl hexafluorophosphoric acid sulfosalt.
In the present embodiment, the modified luminescent powder includes following component according to the mass fraction:35 parts of methacrylic acid, silicon 8 parts of alkane crosslinking agent, 70 parts of ethylene glycol, 65 parts of luminescent powder, 7 parts of oxidized polyethylene wax, 8 parts of stearic acid sodium.
Embodiment 3
Advertisement light emitting word photoelectric functional method for glass preparation, includes the following steps:
(1)Pre-polymerization material:Methyl methacrylate and azodiisobutyronitrile are added in a stirring kettle, stirs, has fed in charging Stirred tank be warming up to 75 DEG C and keep the temperature 45min after finishing, backward stirred tank in addition n-butanol, hexahydrophthalic anhydride, Modified luminescent powder, odium stearate, two contracting omega-diol diacrylates, triaryl hexafluorophosphoric acid sulfosalt, are heated to 93 DEG C and keep the temperature 2h, system viscosity reaches 2000cP in kettle to be mixed, and cooling is spare;
(2)Moulding:Moulding, the moulding concrete operations are carried out in organic glass particular manufacturing craft after above-mentioned reaction system is filtered To pad upper one between the silica glass tablet of two pieces of cleaning, dryings by specific thickness and enclosing the rubber filler strip for being surrounded by glassine paper, with folder Tool clips, cast, exhaust bubble, sealing;
(3)Polymerization:The mold of casting complete is hung in constant temperature water tank and is totally submerged, control temperature at 75 DEG C and keeps 4h;So After hang out mold and be put into high temperature drying chamber, control temperature at 115 DEG C and keeps 3h, and is handled simultaneously with ultraviolet light;
(4)Post-processing:The mold that polymerization is completed is placed under light protected environment and is cooled to room temperature die sinking;It takes out among after molding Methacrylate sheet, trimming are cut, packaging.
In the present embodiment, the preparation method of the modified luminescent powder is to be added to methacrylic acid and silane crosslinker In stirred tank equipped with ethylene glycol, stirs and be warming up to 95 DEG C of holding 90min;Then reaction system is transferred to ultrasonator In, luminescent powder, oxidized polyethylene wax, stearic acid sodium, ultrasonic disperse 45min is added;It is filtered by vacuum and dries, use high speed ball mill It is ground up, sieved up to the modified luminescent powder.
In the present embodiment, advertisement light emitting word photoelectric functional glassware, including according to the mass fraction such as the following group Point:140 parts of methyl methacrylate, 7 parts of azodiisobutyronitrile, 3 parts of n-butanol, 25 parts of hexahydrophthalic anhydride, modified hair 18 parts of light powder, 8 parts of stearic acid sodium, 1 part of two contracting omega-diol diacrylate, 1.5 parts of triaryl hexafluorophosphoric acid sulfosalt.
In the present embodiment, the modified luminescent powder includes following component according to the mass fraction:40 parts of methacrylic acid, silicon 10 parts of alkane crosslinking agent, 80 parts of ethylene glycol, 75 parts of luminescent powder, 10 parts of oxidized polyethylene wax, 12 parts of stearic acid sodium.
The poor compatibility of traditional luminescent powder and polymethyl methacrylate, although stirring can not also make it when pre-polymerization material Even distribution, and polymerization procedure is easy precipitation agglomerate, is modified luminescent powder in the present invention, methacrylic acid is to carry with ethylene glycol Body lytic agent, oxidized polyethylene wax has good wetability, dispersibility and coupled, with silane crosslinker, stearic acid sodium Synergy can build space network, improve the degree of scatter of luminescent powder;And in the preparation process of the present invention, it is added to Ultra-violet curing agent triaryl hexafluorophosphoric acid sulfosalt, is used in combination with hexahydrophthalic anhydride, two contracting omega-diol diacrylates Accelerate solidification progress, the luminescent powder of hardening time long initiation is avoided to precipitate agglomerate.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all essences in the present invention All any modification, equivalent and improvement etc., should all be included in the protection scope of the present invention made by within refreshing and principle.

Claims (4)

1. advertisement light emitting word photoelectric functional method for glass preparation, which is characterized in that include the following steps:
(1)Pre-polymerization material:Methyl methacrylate and azodiisobutyronitrile are added in a stirring kettle, stirs, has fed in charging Stirred tank be warming up to 75 DEG C and keep the temperature 45min after finishing, backward stirred tank in addition n-butanol, hexahydrophthalic anhydride, Modified luminescent powder, odium stearate, tripropylene glycol diacrylate, triaryl hexafluorophosphoric acid sulfosalt are heated to 93 DEG C and keep the temperature 1 ~ 2h, system viscosity reaches 2000cP in kettle to be mixed, and cooling is spare;
(2)Moulding:Moulding, the moulding concrete operations are carried out in organic glass particular manufacturing craft after above-mentioned reaction system is filtered To pad upper one between the silica glass tablet of two pieces of cleaning, dryings by specific thickness and enclosing the rubber filler strip for being surrounded by glassine paper, with folder Tool clips, cast, exhaust bubble, sealing;
(3)Polymerization:The mold of casting complete is hung in constant temperature water tank and is totally submerged, control temperature at 55 ~ 75 DEG C and keep 2 ~ 4h;Then it hangs out mold and is put into high temperature drying chamber, control temperature is at 95 ~ 115 DEG C and keeps 1 ~ 3h, and simultaneously at ultraviolet light Reason;
(4)Post-processing:The mold that polymerization is completed is placed under light protected environment and is cooled to room temperature die sinking;It takes out among after molding Methacrylate sheet, trimming are cut, packaging.
2. advertisement light emitting word as described in claim 1 photoelectric functional method for glass preparation, which is characterized in that the modified hair The preparation method of light powder is that methacrylic acid and silane crosslinker are added in the stirred tank equipped with ethylene glycol, stirs and rises Temperature to 85 ~ 95 DEG C holding 30 ~ 90min;Then reaction system is transferred in ultrasonator, luminescent powder, oxidic polyethylene is added Wax, stearic acid sodium, 30 ~ 45min of ultrasonic disperse;It is filtered by vacuum and dries, be ground up, sieved up to the modification with high speed ball mill Luminescent powder.
3. advertisement light emitting word photoelectric functional glassware, which is characterized in that include following component according to the mass fraction:Methyl 105 ~ 140 parts of methyl acrylate, 1 ~ 3 part of n-butanol, 15 ~ 25 parts of hexahydrophthalic anhydride, changes 3 ~ 7 parts of azodiisobutyronitrile 8 ~ 18 parts of luminescent powder of property, 3 ~ 8 parts of stearic acid sodium, 0.1 ~ 1 part of two contracting omega-diol diacrylate, triaryl hexafluorophosphoric acid sulfosalt 0.5 ~ 1.5 part.
4. advertisement light emitting word as claimed in claim 3 photoelectric functional glassware, which is characterized in that the modified luminescent powder Including following component according to the mass fraction:30 ~ 40 parts of methacrylic acid, 5 ~ 10 parts of silane crosslinker, 60 ~ 80 parts of ethylene glycol, 55 ~ 75 parts of luminescent powder, 3 ~ 10 parts of oxidized polyethylene wax, 4 ~ 12 parts of stearic acid sodium.
CN201810505209.1A 2018-05-24 2018-05-24 Advertisement light emitting word photoelectric functional method for glass preparation and its product Pending CN108727531A (en)

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Application Number Priority Date Filing Date Title
CN201810505209.1A CN108727531A (en) 2018-05-24 2018-05-24 Advertisement light emitting word photoelectric functional method for glass preparation and its product

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Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4839125A (en) * 1986-05-16 1989-06-13 Mitsubishi Rayon Co., Ltd. Process for preparation of light-diffusing methacrylic resin plates
CN1352206A (en) * 2001-12-03 2002-06-05 万发荣 Method for producing luminous organic glass and luminous organic glass made therein
CN1727371A (en) * 2005-05-25 2006-02-01 北京阿格蕾雅科技发展有限公司 method for preparing illuminant organic glass in long persistence, and organic glass prepared by the method
CN102161719A (en) * 2011-01-24 2011-08-24 陕西理工学院 Method for producing luminous organic glass embedded handicraft
CN103755864A (en) * 2014-01-20 2014-04-30 扬州大学 Preparation method of fluorescent organic glass

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4839125A (en) * 1986-05-16 1989-06-13 Mitsubishi Rayon Co., Ltd. Process for preparation of light-diffusing methacrylic resin plates
CN1352206A (en) * 2001-12-03 2002-06-05 万发荣 Method for producing luminous organic glass and luminous organic glass made therein
CN1727371A (en) * 2005-05-25 2006-02-01 北京阿格蕾雅科技发展有限公司 method for preparing illuminant organic glass in long persistence, and organic glass prepared by the method
CN102161719A (en) * 2011-01-24 2011-08-24 陕西理工学院 Method for producing luminous organic glass embedded handicraft
CN103755864A (en) * 2014-01-20 2014-04-30 扬州大学 Preparation method of fluorescent organic glass

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