CN101950044A - Method for preparing halogen-free smoke-suppressant and flame-retardant plastic optical fiber sheath - Google Patents
Method for preparing halogen-free smoke-suppressant and flame-retardant plastic optical fiber sheath Download PDFInfo
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- CN101950044A CN101950044A CN2010102936145A CN201010293614A CN101950044A CN 101950044 A CN101950044 A CN 101950044A CN 2010102936145 A CN2010102936145 A CN 2010102936145A CN 201010293614 A CN201010293614 A CN 201010293614A CN 101950044 A CN101950044 A CN 101950044A
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Abstract
The invention discloses a method for preparing a halogen-free smoke-suppressant and flame-retardant plastic optical fiber sheath, which is characterized by comprising the following steps of: (1) modifying magnesium hydroxide; and (2) preparing a flame-retardant plastic optical fiber. The method has the advantages that: by modifying a magnesium hydroxide flame retardant by two steps, the affinity of the magnesium hydroxide flame retardant with a polyethylene matrix is greatly improved, a flame-retardant accelerant and a synergist are added, the reduction of the mechanical properties of the prepared flame-retardant plastic optical fiber sheath is a little under the condition of ensuring the flame retardance, and the mechanical demand of the product can be met.
Description
Technical field
The present invention relates to a kind of preparation method of plastic optical fiber sheath, relate in particular to a kind of Halogen, press down cigarette, the preparation method of flame retardant type plastic optical fiber sheath.
Background technology
Plastic optical fiber is to be a kind of novel optical fiber of light-conductive media with plastics, is considered to solve the optimal selection of optical fiber connection " last 100 meters " problem when Fiber to the home.The basis that Fiber to the home is " integration of three networks ", and " integration of three networks " is the important directions that present national industrial policies are greatly developed, and in the file of State Council and the issue of a plurality of ministries and commissions clear and definite elaboration carried out in the developing goal and the strategic planning of this industry.
The plastic optical fiber cost is low, bandwidth is high (comparing with the copper category-5 cable), core diameter is big, pliability good, connection is easy, the installation and maintenance expense is low, be routed to net fast.Because these conspicuous advantages, the existing and potential application market in aspects such as plastic optical fiber is interconnected in communication, automobile, aircraft, Industry Control, consumer electronics product, information, home network, medicine equipment, national defence is huge.
In order to protect plastic optical fiber to avoid the injury of extraneous mechanical force etc., coat the certain thickness plastic sheath of one deck in optical fiber (naked fibre) outside usually.The material of main part of naked fibre is polymethylmethacrylate (PMMA), and the sheath common used material is tygon (PE), and both are inflammable material, and its oxygen index is lower than 17%, has in use caused certain potential safety hazard.And flame retardant type plastic optical fiber product yet there are no sale in the market, does not also see relevant report.
Magnesium hydroxide is that a kind of addition type efficiently presses down cigarette, halogen-free flame retardants, in use can not discharge objectionable impurities, and can in and the sour corrosion gas that produces in the combustion process, be a kind of environment-friendly fire retardant.It has had certain application in electric wire.But its flame retarding efficiency is low, and in order to reach higher oxygen index, its addition must be bigger.Especially because usually the magnesium hydroxide of preparation has stronger polarity and water wettability, crystal grain trends towards secondary aggregation, and compatibility is poor between the nonpolar macromolecular material, disperses inhomogeneously, is difficult to form good binding and adhesion between its interface.Along with the increase of magnesium hydroxide content in the macromolecular material, its mechanical property and mechanical property sharply descend, so that can't process, lose use value especially.Flame retardant of magnesium hydroxide is carried out surface modification, is the important method that overcomes its above-mentioned defective, also is the necessary condition that this kind fire retardant is applied to product.And in plastic optical fiber; because can not add any fire retardant among the PMMA as the naked fibre of preparation; so in order to reach certain flame retardant effect; as adopt existing method; must strengthen the consumption of fire retardant in sheath; cause the sheath physical strength very low, so that do not have due protective effect, do not reach the plastic optical fiber product standard.This may also be one of reason of not seeing in the market flame retardant type plastic optical fiber product.
The present invention adopts the method for commercially available flame retardant of magnesium hydroxide being carried out two step surface modifications, improve itself and the compatibility of plastic substrate and the dispersiveness in matrix thereof, add a certain amount of promoter and synergist simultaneously, under the prerequisite that guarantees the sheath mechanical strength, improve the oxygen index of plastic optical fiber product, reached fire-retardant purpose.
Summary of the invention
The object of the present invention is to provide a kind of Halogen, press down cigarette, the preparation method of flame retardant type plastic optical fiber sheath, this plastic optical fiber sheath solves the problem that existing plastic optical fiber product is inflammable, have potential safety hazard.Products obtained therefrom is not roasted for a long time through naked light can discharge toxic and harmful, and from putting out, smog seldom from fire.Promote product specification, enlarged product applications.
The present invention is achieved like this, and it is characterized in that method step is:
(1) modification of magnesium hydroxide: selecting commercially available flame retardant of magnesium hydroxide for use is body material, joining and making concentration in the inertia spreading agent is 5% ~ 20% dispersion, stir evenly, add 3% ~ 10% the surfactant account for the magnesium hydroxide parts by weight, 40 ~ 90 ℃ of following modifications 20 ~ 120 minutes, with magnesium hydroxide filtration, oven dry, ball milling, obtain magnesium hydroxide powder through first step modification; This powder is added once more in the inertia spreading agent of 5 ~ 20 times of magnesium hydroxide parts by weight then, stir evenly, add the coupling agent of magnesium hydroxide parts by weight 2% ~ 8%, 40 ~ 90 ℃ of following modifications 20 ~ 120 minutes; Filtration, oven dry, ball milling obtain the magnesium hydroxide powder through the second step modification;
(2) preparation of flame retardant type plastic optical fiber: above-mentioned magnesium hydroxide powder through twice modification is joined in the Banbury mixer, add 9% ~ 12% fire-retardant promoter that accounts for magnesium hydroxide weight and 5% ~ 8% fire retarding synergist that accounts for magnesium hydroxide weight in proportion, 125 ~ 155 ℃ were descended mixing 20 ~ 50 minutes in Banbury mixer, product is made plastic optical fiber by extrusion equipment with naked fibre with product as the sheath of preparation plastic optical fiber.
Described inertia spreading agent is dimethylbenzene, diesel oil, kerosene, fusing point at the potpourri of a kind of of the whiteruss below 25 ℃, low viscosity methyl-silicone oil or some kinds.
Described surfactant is a lauryl sodium sulfate, neopelex, Tween-81 85, Tween-81 83, Tween-81 80, Tween-81 65, Tween-81 60, Tween-81 40, Tween-81 20, polyoxyethylene nonylphenol ether 10, sodium sulfate of polyethenoxy ether of fatty alcohol, peregal, turkey red oil, the potpourri of alginate propylene glycol a kind of or some kinds.
Described coupling agent is a silester, aminopropyl trimethoxysilane, glycidyl ether oxygen base propyl trimethoxy silicane methacryloxypropyl trimethoxy silane, methacryloxypropyl methyl dimethoxysilane vinyltriethoxysilane, the aminopropyl methyldiethoxysilane, urinate basic propyl-triethoxysilicane, isopropyl two oleic acid acyloxy (dioctyl phosphoric acid acyloxy) titanate esters, isopropyl three oleic acid acyloxy titanate esters, isopropyl three (dioctylphyrophosphoric acid acyloxy) titanate esters, two (dioctylphyrophosphoric acid ester group) ethylene titanate esters, tetra isopropyl two (dioctyl phosphorous acid acyloxy) titanate esters, stearic acid, palmitic acid, oleic acid, linoleic acid, olein, palmitin, glycerol tristearate, methyl stearate, ethyl stearte, soft-methyl ester, soft-ethyl ester, hexadecanol, 18 alcohol, the potpourri of tetradecyl alchohol a kind of or some kinds.
Described fire-retardant promoter is the potpourri of a kind of of aluminium hydroxide, antimony oxide, Firebrake ZB, molybdenum trioxide, zinc molybdate, titania, talcum, mica, pyrophyllite, porcelain earth, bentonitic clay, vermiculite, serpentine or some kinds; Above material is Powdered when using, particle diameter is below 300 microns.
Described fire retarding synergist is the potpourri of a kind of of red phosphorus, phosphorus pentoxide, sodium pyrophosphate, ammonium pyrophosphate, ammonium polyphosphate (per molecule phosphorous 500 ~ 1500), expanded graphite and some kinds.
Advantage of the present invention is: by micron-sized flame retardant of magnesium hydroxide being carried out the method for two step modifications, improved the affinity of itself and tygon matrix greatly, be aided with fire-retardant promoter and synergist again, final prepared flame retardant type plastic optical fiber mechanical property under the prerequisite that guarantees flame retardant effect descends few, can satisfy product requirement.
Embodiment
Embodiment 1
In 500 liters carbon steel still, add double centner dimethylbenzene, 20 kilograms of commercially available flame retardant of magnesium hydroxide powder and 1 kilogram of lauryl sodium sulfate, start stirring, stir evenly; Be warmed up to 70 ℃, insulation reaction 70 minutes; Stop to stir and heating,, obtain magnesium hydroxide powder through first step modification with reaction mass filtration, oven dry, ball milling.In 500 liters carbon steel still, add double centner dimethylbenzene, 20 kilograms of flame retardant of magnesium hydroxide powder and 0.6 kilogram of aminopropyl trimethoxysilane once more, start stirring, stir evenly through a step modification; Be warmed up to 85 ℃, insulation reaction 50 minutes; Stop to stir and heating,, obtain magnesium hydroxide powder through the second step modification with reaction mass filtration, oven dry, ball milling.
In Banbury mixer, add 60 kilograms of tygon, 0.9 kilogram of fire-retardant promoter aluminium hydroxide, 0.48 kilogram of fire retarding synergist ammonium polyphosphate, 9 kilograms of above-mentioned flame retardant of magnesium hydroxide through two step modifications, in 135 ℃ mixing 20 minutes down.Product is through the extrusion mould-outlet of the particular design sheath as plastic optical fiber.The oxygen index of final gained plastic optical fiber is 19.5%, and breaking elongation is 84.6%, and pulling strengrth is at 13.5MPa.
Embodiment 2
In 500 liters carbon steel still, add 350 kilograms of low viscosity methyl-silicone oils, 20 kilograms of commercially available flame retardant of magnesium hydroxide powder and 1.2 kilograms of Tween-81 85(Tween85), start stirring, stir evenly; Be warmed up to 75 ℃, insulation reaction 50 minutes; Stop to stir and heating,, obtain magnesium hydroxide powder through first step modification with reaction mass filtration, oven dry, ball milling.In 500 liters carbon steel still, add 350 kilograms of low viscosity methyl-silicone oils, 20 kilograms of flame retardant of magnesium hydroxide powder and 0.8 kilogram of basic propyl-triethoxysilicane of urine once more, start stirring, stir evenly through a step modification; Be warmed up to 8, ℃, insulation reaction 50 minutes; Stop to stir and heating,, obtain magnesium hydroxide powder through the second step modification with reaction mass filtration, oven dry, ball milling.
In Banbury mixer, add 60 kilograms of tygon, 1.2 kilograms of antimony oxides, 0.75 kilogram in red phosphorus, 12 kilograms of above-mentioned flame retardant of magnesium hydroxide through two step modifications, in 130 ℃ mixing 30 minutes down.Product is through the extrusion mould-outlet of the particular design sheath as plastic optical fiber.The oxygen index of final gained plastic optical fiber is 25.5%, and breaking elongation is 79.2%, and pulling strengrth is at 13.2MPa.
Embodiment 3
In 500 liters carbon steel still, add 150 kilograms of whiterusss, 20 kilograms of commercially available flame retardant of magnesium hydroxide powder and 1 kilogram of neopelex, start stirring, stir evenly; Be warmed up to 45 ℃, insulation reaction 100 minutes; Stop to stir and heating,, obtain magnesium hydroxide powder through first step modification with reaction mass filtration, oven dry, ball milling.In 500 liters carbon steel still, add 150 kilograms of whiterusss, 20 kilograms of flame retardant of magnesium hydroxide powder and 1 kilogram of stearic acid once more, start stirring, stir evenly through a step modification; Be warmed up to 75 ℃, insulation reaction 70 minutes; Stop to stir and heating,, obtain magnesium hydroxide powder through the second step modification with reaction mass filtration, oven dry, ball milling.
In Banbury mixer, add 60 kilograms of tygon, 1.5 kilograms of molybdenum trioxides, 1 kilogram of ammonium pyrophosphate, 15 kilograms of above-mentioned flame retardant of magnesium hydroxide through two step modifications, in 140 ℃ mixing 20 minutes down.Product is through the extrusion mould-outlet of the particular design sheath as plastic optical fiber.The oxygen index of final gained plastic optical fiber is 29.2%, and breaking elongation is 72.1%, and pulling strengrth is at 12.8MPa.
Embodiment 4
In 500 liters carbon steel still, add 180 kilograms of kerosene, 20 kilograms of commercially available flame retardant of magnesium hydroxide powder and 1.5 kilograms of Tween-81 80(Tween80), start stirring, stir evenly; Be warmed up to 80 ℃, insulation reaction 30 minutes; Stop to stir and heating,, obtain magnesium hydroxide powder through first step modification with reaction mass filtration, oven dry, ball milling.In 500 liters carbon steel still, add 180 kilograms of kerosene, 20 kilograms of flame retardant of magnesium hydroxide powder and 1.2 kilograms of soft-methyl esters once more, start stirring, stir evenly through a step modification; Be warmed up to 85 ℃, insulation reaction 50 minutes; Stop to stir and heating,, obtain magnesium hydroxide powder through the second step modification with reaction mass filtration, oven dry, ball milling.
In Banbury mixer, add 60 kilograms of tygon, 2 kilograms of bentonitic clays, 1.4 kilograms of expanded graphites, 18 kilograms of above-mentioned flame retardant of magnesium hydroxide through two step modifications, in 150 ℃ mixing 20 minutes down.Product is through the extrusion mould-outlet of the particular design sheath as plastic optical fiber.The oxygen index of final gained plastic optical fiber is 31.8%, and breaking elongation is 62.1%, and pulling strengrth is at 12.3MPa.
Claims (6)
- A Halogen, press down the preparation method of cigarette, flame retardant type plastic optical fiber sheath, it is characterized in that method step is:(1) modification of magnesium hydroxide: selecting commercially available flame retardant of magnesium hydroxide for use is body material, joining and making concentration in the inertia spreading agent is 5% ~ 20% dispersion, stir evenly, add 3% ~ 10% the surfactant account for the magnesium hydroxide parts by weight, 40 ~ 90 ℃ of following modifications 20 ~ 120 minutes, with magnesium hydroxide filtration, oven dry, ball milling, obtain magnesium hydroxide powder through first step modification; This powder is added once more in the inertia spreading agent of 5 ~ 20 times of magnesium hydroxide parts by weight then, stir evenly, add the coupling agent of magnesium hydroxide parts by weight 2% ~ 8%, 40 ~ 90 ℃ of following modifications 20 ~ 120 minutes; Filtration, oven dry, ball milling obtain the magnesium hydroxide powder through the second step modification;(2) preparation of flame retardant type plastic optical fiber: above-mentioned magnesium hydroxide powder through twice modification is joined in the Banbury mixer, add 9% ~ 12% fire-retardant promoter that accounts for magnesium hydroxide weight and 5% ~ 8% fire retarding synergist that accounts for magnesium hydroxide weight in proportion, 125 ~ 155 ℃ were descended mixing 20 ~ 50 minutes in Banbury mixer, product is made plastic optical fiber by extrusion equipment with naked fibre with product as the sheath of preparation plastic optical fiber.
- 2. a kind of Halogen according to claim 1, press down the preparation method of cigarette, flame retardant type plastic optical fiber sheath, it is characterized in that described inertia spreading agent is dimethylbenzene, diesel oil, kerosene, fusing point at the potpourri of a kind of of the whiteruss below 25 ℃, low viscosity methyl-silicone oil or some kinds.
- 3. a kind of Halogen according to claim 1, press down cigarette, the preparation method of flame retardant type plastic optical fiber sheath is characterized in that described surfactant is a lauryl sodium sulfate, neopelex, Tween-81 85, Tween-81 83, Tween-81 80, Tween-81 65, Tween-81 60, Tween-81 40, Tween-81 20, polyoxyethylene nonylphenol ether 10, sodium sulfate of polyethenoxy ether of fatty alcohol, peregal, turkey red oil, the potpourri of alginate propylene glycol a kind of or some kinds.
- 4. a kind of Halogen according to claim 1, press down cigarette, the preparation method of flame retardant type plastic optical fiber sheath is characterized in that described coupling agent is a silester, aminopropyl trimethoxysilane, glycidyl ether oxygen base propyl trimethoxy silicane methacryloxypropyl trimethoxy silane, methacryloxypropyl methyl dimethoxysilane vinyltriethoxysilane, the aminopropyl methyldiethoxysilane, urinate basic propyl-triethoxysilicane, isopropyl two oleic acid acyloxy (dioctyl phosphoric acid acyloxy) titanate esters, isopropyl three oleic acid acyloxy titanate esters, isopropyl three (dioctylphyrophosphoric acid acyloxy) titanate esters, two (dioctylphyrophosphoric acid ester group) ethylene titanate esters, tetra isopropyl two (dioctyl phosphorous acid acyloxy) titanate esters, stearic acid, palmitic acid, oleic acid, linoleic acid, olein, palmitin, glycerol tristearate, methyl stearate, ethyl stearte, soft-methyl ester, soft-ethyl ester, hexadecanol, 18 alcohol, the potpourri of tetradecyl alchohol a kind of or some kinds.
- 5. a kind of Halogen according to claim 1, press down the preparation method of cigarette, flame retardant type plastic optical fiber sheath, it is characterized in that described fire-retardant promoter is the potpourri of a kind of of aluminium hydroxide, antimony oxide, Firebrake ZB, molybdenum trioxide, zinc molybdate, titania, talcum, mica, pyrophyllite, porcelain earth, bentonitic clay, vermiculite, serpentine or some kinds; Above material is Powdered when using, particle diameter is below 300 microns.
- 6. a kind of Halogen according to claim 1, press down the preparation method of cigarette, flame retardant type plastic optical fiber sheath, it is characterized in that described fire retarding synergist is the potpourri of a kind of of red phosphorus, phosphorus pentoxide, sodium pyrophosphate, ammonium pyrophosphate, ammonium polyphosphate (per molecule phosphorous 500 ~ 1500), expanded graphite and some kinds.
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| CN201010293614.5A CN101950044B (en) | 2010-09-28 | 2010-09-28 | Method for preparing halogen-free smoke-suppressant and flame-retardant plastic optical fiber sheath |
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| CN201010293614.5A CN101950044B (en) | 2010-09-28 | 2010-09-28 | Method for preparing halogen-free smoke-suppressant and flame-retardant plastic optical fiber sheath |
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| CN102432732A (en) * | 2011-03-14 | 2012-05-02 | 新疆石河子中发化工有限责任公司 | Preparation method for polyvinyl chloride resin used for flame-retardant cable |
| CN103114433A (en) * | 2013-03-05 | 2013-05-22 | 南通大学 | Preparation method of open-fire resistance thermal insulation textile |
| CN104409178A (en) * | 2014-12-05 | 2015-03-11 | 江苏戴普科技有限公司 | Method for preparing corrosion-resisting cable |
| CN105061857A (en) * | 2015-08-06 | 2015-11-18 | 安徽电信器材贸易工业有限责任公司 | Heatproof aging-resistance sheath material |
| CN105086062A (en) * | 2015-08-06 | 2015-11-25 | 安徽电信器材贸易工业有限责任公司 | Optical fiber sheath material with resistance to environmental stress cracking |
| CN105652366A (en) * | 2014-07-09 | 2016-06-08 | 方亚琴 | Anti-bending optical fiber |
| CN106373666A (en) * | 2016-08-30 | 2017-02-01 | 江苏戴普科技有限公司 | Production method of flexible cable |
| CN107722506A (en) * | 2017-11-09 | 2018-02-23 | 陕西理工大学 | A kind of optical fiber of flame-retardant high-strength and preparation method thereof |
| CN110903544A (en) * | 2019-10-30 | 2020-03-24 | 许继集团有限公司 | Lithium ion battery flame-retardant material for energy storage and preparation method and application thereof |
| CN114031825A (en) * | 2021-11-30 | 2022-02-11 | 神州节能科技集团有限公司 | Non-combustible rubber and plastic foaming product with combustion performance reaching A level and preparation method thereof |
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102432732A (en) * | 2011-03-14 | 2012-05-02 | 新疆石河子中发化工有限责任公司 | Preparation method for polyvinyl chloride resin used for flame-retardant cable |
| CN102432732B (en) * | 2011-03-14 | 2014-06-18 | 新疆石河子中发化工有限责任公司 | Preparation method for polyvinyl chloride resin used for flame-retardant cable |
| CN103114433A (en) * | 2013-03-05 | 2013-05-22 | 南通大学 | Preparation method of open-fire resistance thermal insulation textile |
| CN105652366A (en) * | 2014-07-09 | 2016-06-08 | 方亚琴 | Anti-bending optical fiber |
| CN105652366B (en) * | 2014-07-09 | 2019-01-08 | 杭州金星通光纤科技有限公司 | A kind of bend resistant optical fibers |
| CN104409178A (en) * | 2014-12-05 | 2015-03-11 | 江苏戴普科技有限公司 | Method for preparing corrosion-resisting cable |
| CN105061857A (en) * | 2015-08-06 | 2015-11-18 | 安徽电信器材贸易工业有限责任公司 | Heatproof aging-resistance sheath material |
| CN105086062A (en) * | 2015-08-06 | 2015-11-25 | 安徽电信器材贸易工业有限责任公司 | Optical fiber sheath material with resistance to environmental stress cracking |
| CN106373666A (en) * | 2016-08-30 | 2017-02-01 | 江苏戴普科技有限公司 | Production method of flexible cable |
| CN107722506A (en) * | 2017-11-09 | 2018-02-23 | 陕西理工大学 | A kind of optical fiber of flame-retardant high-strength and preparation method thereof |
| CN110903544A (en) * | 2019-10-30 | 2020-03-24 | 许继集团有限公司 | Lithium ion battery flame-retardant material for energy storage and preparation method and application thereof |
| CN114031825A (en) * | 2021-11-30 | 2022-02-11 | 神州节能科技集团有限公司 | Non-combustible rubber and plastic foaming product with combustion performance reaching A level and preparation method thereof |
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Application publication date: 20110119 Assignee: Jiangxi well plastic optical fiber technology co Innovation Co., Ltd. Assignor: Jiangxi Daishing POF Co., Ltd. Contract record no.: 2019360000001 Denomination of invention: Method for preparing halogen-free smoke-suppressant and flame-retardant plastic optical fiber sheath Granted publication date: 20150722 License type: Exclusive License Record date: 20190411 |
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