CN101899144A - Method for preparing flame-retardant luminous polyethylene glycol terephthalate - Google Patents
Method for preparing flame-retardant luminous polyethylene glycol terephthalate Download PDFInfo
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- CN101899144A CN101899144A CN2009100857517A CN200910085751A CN101899144A CN 101899144 A CN101899144 A CN 101899144A CN 2009100857517 A CN2009100857517 A CN 2009100857517A CN 200910085751 A CN200910085751 A CN 200910085751A CN 101899144 A CN101899144 A CN 101899144A
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Abstract
The invention relates to a method for preparing flame-retardant luminous polyethylene glycol terephthalate. The flame-retardant luminous polyethylene glycol terephthalate is prepared from 0.1 to 20 weight percent of radiant agent, 0.1 to 20 weight percent of fire retardant and the balance of the polyethylene glycol terephthalate, wherein in an esterification reaction, the temperature is between 200 and 290 DEG C and the pressure is between 0.1 and 0.5 MPa; in a low-vacuum polycondensation reaction, the temperature is between 200 and 290 DEG C and the pressure is between 500 and 100,000 Pa; in a high-vacuum polycondensation reaction, the temperature is between 250 and 300 DEG C and the pressure is between 50 and 500Pa; the radiant agent accounts for 5 to 30 percent of the weight of slurry; the grain diameter of the radiant agent is between 1 nm and 1 micron; and the radiant agent with the grain diameter more than 760 nm accounts for 5 percent of the total weight of the radiant agent. The fiber fabric of the flame-retardant luminous polyethylene glycol terephthalate prepared from the composite materials has fire-retardant and luminous effects and is used for fire-fighting working clothes, marine working clothes and camping tents.
Description
Technical field:
The present invention relates to the matrix material of a kind of polyethylene terephthalate (PET), particularly a kind of compound by PET and luminous agent and fire retardant, have PET matrix material and preparation method fire-retardant, illumination effect.
Background technology:
Pet fiber is since the early 1950s industrialization, just with its modulus height, premium propertiess such as rebound resilience is good, photostabilization is good, wear resistance is good, good heat resistance be subjected to weaving people in the industry's favor and human consumer's welcome, Application Areas constantly enlarges, and demand increases gradually.Being extensive use of of synthon development and national economy is played an important role, but its inflammableness brought serious harm to human society again.Therefore, producing flame retardant textiles for the generation that prevents fire has become very important serious social concern, more and more is subjected to the extensive concern of society.At present, many in the world countries are according to the different purposes of textiles, the combustionproperty of fiber and goods thereof has all been proposed concrete requirement or restriction, and formulated corresponding laws and regulations.The scene of fire is all played inhibition because light is darker to rescue and escape, and the fabric with fiber production becomes to have the luminous performance can clearly indicate trapped personnel position and direction.
In the building-up process of polyethylene terephthalate, add fire retardant and luminous agent and other auxiliary agent, make polyethylene terephthalate section and fiber have fire-retardant and luminescent properties, be widely used in fields such as bunker clothing, offshore operation clothes, tents.
Summary of the invention:
The purpose of this invention is to provide a kind of flame-retardant luminous polyethylene terephthalate matrix material and preparation method thereof.
Luminous agent and ethylene glycol slurry, terephthalic acid and fire retardant be added to carry out esterification in the reactor,, obtain flame-retardant luminous polyethylene terephthalate matrix material again through rough vacuum polycondensation and high vacuum polycondensation;
By weight percentage, luminous agent accounts for 0.1～20% of matrix material; The luminous agent slurry is formulated by ethylene glycol and luminous agent, and fire retardant accounts for 0.1～20% of matrix material, and all the other are polyethylene terephthalate;
The temperature of reaction in esterification stage is 200～290 ℃, and reaction pressure is 0.1～0.5MPa, and the reaction times is 1～3 hour; Rough vacuum stage polycondensation temperature is 200～290 ℃, and reaction pressure is 100000～500Pa, and the reaction times is 10～90 minutes; High vacuum stage of Fig polycondensation temperature is 250～300 ℃, and reaction pressure is 500～50Pa, and the reaction times is 80～150 minutes;
Described luminous agent slurry is made up of luminous agent and ethylene glycol, and wherein luminous agent accounts for 5～30% of luminous agent slurry gross weight, and the particle diameter of luminous agent is 1nm～1um; Wherein particle diameter accounts for 5% of luminous agent gross weight greater than the luminous agent of 760nm.
Described luminous agent be zinc phosphate, strontium aluminate, the europkium-activated yttrium aluminum garnet of trivalent, divalent europium activated chlorine strontium phosphate, cerium activated yttrium aluminum garnet, bivalent manganese activate and the coactivated yttrium oxysulfide of divalent europium, divalent europium activated calcium chlorate magnesium in one or more mixture.
Described fire retardant is selected from one or more the mixture in decabromodiphynly oxide, poly-Dowspray 9, different hydrocinnamyl phenyl phosphate ester, antimonous oxide, triaryl phosphate, the 2-carboxyethyl phenyl phosphoric acid.
In the building-up process of the matrix material of flame-retardant luminous polyethylene terephthalate, luminous agent slurry and fire retardant are joined in the polymerization system of PET, obtain the matrix material be made up of PET and luminous agent and fire retardant, the fabric that is made into the fiber of this matrix material spinning has luminous and flame retardant properties.
The invention effect:
The fabric of the flame-retardant luminous pet fiber that is made by this matrix material has fire-retardant, illumination effect, can be widely used in fields such as fire-fighting operation clothes, offshore operation clothes, tents.
Embodiment:
Embodiment 1
Adding the weight percent that accounts for reaction mixture in the esterification technique stage of producing PET is 20% zinc phosphate slurry, and wherein, the weight percent that zinc phosphate accounts for slurry is 5%, and particle diameter is similar normal state and distributes between 1nm～50nm, and solvent is an ethylene glycol.Add the weight percent account for reaction mixture simultaneously and be 5% decabromodiphynly oxide.Esterification reaction temperature is 200～220 ℃, and reaction pressure is 0.1～0.25MPa, and the reaction times is 1～2 hour.The product of above-mentioned esterification technique obtains fire-retardant, luminous PET matrix material again through polycondensating process.Wherein, rough vacuum stage polycondensation temperature is 200～240 ℃, and reaction pressure is 100000～500Pa, reaction times is 10～30 minutes, high vacuum stage of Fig polycondensation temperature is 250～275 ℃, and reaction pressure is 500～50Pa, and the reaction times is 1～1.5 hour.
Embodiment 2
Adding the weight percent that accounts for reaction mixture in the esterification technique stage of producing PET is the slurry of the europkium-activated yttrium aluminum garnet of 30% trivalent, the weight percent that the europkium-activated yttrium aluminum garnet of trivalent in the slurry accounts for slurry is 30%, grain diameter is similar normal state and distributes between 5nm～10um, solvent is an ethylene glycol.Simultaneously, adding the weight percent account for reaction mixture is 7% fire retardant 2-carboxyethyl phenyl phosphoric acid.Wherein esterification reaction temperature is 220～240 ℃, and reaction pressure is 0.2～0.6MPa, and the reaction times is 1.5～2 hours.The product of above-mentioned esterification technique obtains fire-retardant, luminous PET matrix material again through polycondensating process.Wherein, rough vacuum stage polycondensation temperature is 230～250 ℃, and reaction pressure is 100000～500Pa, reaction times is 20～30 minutes, high vacuum stage of Fig polycondensation temperature is 250～275 ℃, and reaction pressure is 500～50Pa, and the reaction times is 2～2.5 hours.
Embodiment 3
Adding the weight percent that accounts for reaction mixture in the esterification technique stage of producing PET is 10% divalent europium activated chlorine strontium phosphate slurry, wherein, divalent europium activated chlorine strontium phosphate accounts for the 90wt% of additive total amount, grain diameter is similar normal state and distributes between 5nm～10um, solvent is an ethylene glycol.Simultaneously, adding the weight percent that accounts for reaction mixture is 10% antimonous oxide.Wherein esterification reaction temperature is 220～240 ℃, and reaction pressure is 0.2～0.25MPa, and the reaction times is 1.5～2 hours.The product of above-mentioned esterification technique obtains fire-retardant, luminous PET matrix material again through polycondensating process.Wherein, rough vacuum stage polycondensation temperature is 230～250 ℃, and reaction pressure is 100000～500Pa, reaction times is 20～30 minutes, high vacuum stage of Fig polycondensation temperature is 250～275 ℃, and reaction pressure is 500～50Pa, and the reaction times is 2～2.5 hours.
Embodiment 4
Adding the weight percent that does not account for reaction mixture in the esterification technique stage of producing PET is that 1% bivalent manganese activates and the coactivated yttrium oxysulfide slurry of divalent europium, wherein, bivalent manganese activates and the weight percent of the coactivated yttrium oxysulfide of divalent europium in slurry is 10%, grain diameter is similar normal state and distributes between 5nm～10um, solvent is an ethylene glycol.Simultaneously, adding the weight percent account for reaction mixture is 3% different hydrocinnamyl phenyl phosphate ester.Esterification reaction temperature is 230～250 ℃, and reaction pressure is 0.25～0.35MPa, and the reaction times is 1.5～2.5 hours.The product of above-mentioned esterification technique obtains fire-retardant, luminous PET matrix material again through polycondensating process.Wherein, rough vacuum stage polycondensation temperature is 240～260 ℃, and reaction pressure is 100000～500Pa, reaction times is 30～40 minutes, high vacuum stage of Fig polycondensation temperature is 275～285 ℃, and reaction pressure is 500～50Pa, and the reaction times is 2～2.5 hours minutes.
Embodiment 5
Adding the weight percent that accounts for reaction mixture in the esterification technique stage of producing PET is that 15% divalent europium activated calcium chlorate magnesium slurry, grain diameter are similar normal state and distribute between 5nm～10um, and solvent is an ethylene glycol.Add the weight percent account for reaction mixture simultaneously and be 7% different hydrocinnamyl phenyl phosphate ester.Esterification reaction temperature is 250～260 ℃, and reaction pressure is 0.25～0.35MPa, and the reaction times is 2.5～3 hours.The product of above-mentioned esterification technique obtains luminous fire-retardant PET matrix material again through polycondensating process.Wherein, rough vacuum stage polycondensation temperature is 250～260 ℃, and reaction pressure is 100000～500Pa, reaction times is 20～30 minutes, high vacuum stage of Fig polycondensation temperature is 275～280 ℃, and reaction pressure is 500～50Pa, and the reaction times is 3～3.5 hours.
Embodiment 6
Adding the weight percent that accounts for reaction mixture in the esterification technique stage of producing PET is that 20% bivalent manganese activates and the mixture of the coactivated yttrium oxysulfide slurry of divalent europium, wherein, the weight percent of yttrium oxysulfide in slurry is 25, grain diameter is similar normal state and distributes between 1nm～10um, solvent is an ethylene glycol.Simultaneously, adding the weight percent account for reaction mixture is 8% triaryl phosphate.Esterification reaction temperature is 250～290 ℃, and reaction pressure is 0.25～0.5MPa, and the reaction times is 3～4 hours.The product of above-mentioned esterification technique obtains fire-retardant, uvioresistant PET matrix material again through polycondensating process.Wherein, rough vacuum stage polycondensation temperature is 250～290 ℃, and reaction pressure is 100000～500Pa, reaction times is 40～70 minutes, high vacuum stage of Fig polycondensation temperature is 275～300 ℃, and reaction pressure is 500～50Pa, and the reaction times is 3～3.5 hours.
Claims (3)
1. flame-retardant luminous polyethylene terephthalate preparation method is characterized in that:
Luminous agent and ethylene glycol slurry, terephthalic acid and fire retardant be added to carry out esterification in the reactor,, obtain flame-retardant luminous polyethylene terephthalate matrix material again through rough vacuum polycondensation and high vacuum polycondensation;
By weight percentage, luminous agent accounts for 0.1～20% of matrix material; Fire retardant accounts for 0.1～20% of matrix material, and all the other are polyethylene terephthalate;
The temperature of reaction in esterification stage is 200～290 ℃, and reaction pressure is 0.1～0.5MPa, and the reaction times is 1～3 hour; Rough vacuum stage polycondensation temperature is 200～290 ℃, and reaction pressure is 100000～500Pa, and the reaction times is 10～90 minutes; High vacuum stage of Fig polycondensation temperature is 250～300 ℃, and reaction pressure is 500～50Pa, and the reaction times is 80～150 minutes;
Described luminous agent and ethylene glycol slurry: luminous agent accounts for 5～30% of luminous agent slurry gross weight, and the particle diameter of luminous agent is 1nm～1um; Wherein particle diameter accounts for 5% of luminous agent gross weight greater than the luminous agent of 760nm.
2. flame-retardant luminous polyethylene terephthalate preparation method according to claim 1 is characterized in that: described luminous agent be zinc phosphate, strontium aluminate, the europkium-activated yttrium aluminum garnet of trivalent, divalent europium activated chlorine strontium phosphate, cerium activated yttrium aluminum garnet, bivalent manganese activate and the coactivated yttrium oxysulfide of divalent europium, divalent europium activated calcium chlorate magnesium in one or more mixture.
3. flame-retardant luminous polyethylene terephthalate preparation method according to claim 1 is characterized in that: described fire retardant is one or more the mixture in decabromodiphynly oxide, poly-Dowspray 9, different hydrocinnamyl phenyl phosphate ester, antimonous oxide, triaryl phosphate, the 2-carboxyethyl phenyl phosphoric acid.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102408556A (en) * | 2011-09-26 | 2012-04-11 | 四川东材科技集团股份有限公司 | Preparation method of reactive flame retardant capable of resisting polyester melt drip |
| CN103374119A (en) * | 2012-04-13 | 2013-10-30 | 中国石油天然气股份有限公司 | Preparation method of luminous poly(1,3-trimethylene terephthalate) |
| CN103374121A (en) * | 2012-04-13 | 2013-10-30 | 中国石油天然气股份有限公司 | Luminous polyethylene terephthalate composite material |
| CN103374120A (en) * | 2012-04-13 | 2013-10-30 | 中国石油天然气股份有限公司 | Preparation method of luminous polyethylene terephthalate |
| CN103374209A (en) * | 2012-04-13 | 2013-10-30 | 中国石油天然气股份有限公司 | Luminous poly(1,3-trimethylene terephthalate) composite material |
| CN109972232A (en) * | 2019-03-26 | 2019-07-05 | 南通楠桥纹织有限公司 | A kind of production technology of light storage towel |
| CN111826738A (en) * | 2019-04-23 | 2020-10-27 | 苏州龙杰特种纤维股份有限公司 | Luminous terylene, braided layer with same and fire hose with same |
-
2009
- 2009-05-27 CN CN2009100857517A patent/CN101899144A/en active Pending
Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102408556A (en) * | 2011-09-26 | 2012-04-11 | 四川东材科技集团股份有限公司 | Preparation method of reactive flame retardant capable of resisting polyester melt drip |
| CN103374119A (en) * | 2012-04-13 | 2013-10-30 | 中国石油天然气股份有限公司 | Preparation method of luminous poly(1,3-trimethylene terephthalate) |
| CN103374121A (en) * | 2012-04-13 | 2013-10-30 | 中国石油天然气股份有限公司 | Luminous polyethylene terephthalate composite material |
| CN103374120A (en) * | 2012-04-13 | 2013-10-30 | 中国石油天然气股份有限公司 | Preparation method of luminous polyethylene terephthalate |
| CN103374209A (en) * | 2012-04-13 | 2013-10-30 | 中国石油天然气股份有限公司 | Luminous poly(1,3-trimethylene terephthalate) composite material |
| CN103374121B (en) * | 2012-04-13 | 2016-02-10 | 中国石油天然气股份有限公司 | A kind of luminous polyethylene terephthalate matrix material |
| CN103374120B (en) * | 2012-04-13 | 2016-03-09 | 中国石油天然气股份有限公司 | A kind of preparation method of luminous polyethylene terephthalate |
| CN103374119B (en) * | 2012-04-13 | 2016-03-09 | 中国石油天然气股份有限公司 | A kind of preparation method of luminous poly terephthalic acid 1,3 propylene glycol ester |
| CN103374209B (en) * | 2012-04-13 | 2016-08-03 | 中国石油天然气股份有限公司 | A kind of luminous poly terephthalic acid 1,3 propylene glycol ester composite |
| CN109972232A (en) * | 2019-03-26 | 2019-07-05 | 南通楠桥纹织有限公司 | A kind of production technology of light storage towel |
| CN111826738A (en) * | 2019-04-23 | 2020-10-27 | 苏州龙杰特种纤维股份有限公司 | Luminous terylene, braided layer with same and fire hose with same |
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Application publication date: 20101201 |