CN1488784A - Long-persistence luminous composite fiber and preparing method thereof - Google Patents
Long-persistence luminous composite fiber and preparing method thereof Download PDFInfo
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- CN1488784A CN1488784A CNA031422276A CN03142227A CN1488784A CN 1488784 A CN1488784 A CN 1488784A CN A031422276 A CNA031422276 A CN A031422276A CN 03142227 A CN03142227 A CN 03142227A CN 1488784 A CN1488784 A CN 1488784A
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Abstract
The present invention discloses a long-afterglow luminous composite fibre and its preparation method. Said method includes the following steps: using luminous polyamide as core layer, and using fibre-formed polymer polyamide, polyester and polyolefin as skin layer, and making constituent spinning so as to obtain the invented product. The long-afterglow polymer polyamide fibre is formed from polyamide and alkaline earth metal aluminate which has luminous effective quantity and is activated by Eu(2+). The fluorescent powder is the alkaline earth metal aluminate series, and is non-toxic, has no radioactivity, high luminous intensity, long afterglow time and stable chemical property, so that it has extensive application range.
Description
Technical field
The present invention relates to a kind of luminous composite fibre, particularly long-afterglow luminous composite fibre and preparation method thereof.
Background technology
Long-persistence luminous fiber can be used as easy suit, full dress, caution clothes, ornament, safety sign etc.The International Maritime conference is clearly stipulated: the relevant positions such as passage, fire-fighting equipment and safe life-saving facility on the passenger-cargo vessel more than staffing 25 people that produced later in 1998 must be provided with luminous safety sign, to ensure safety.The irradiation luminescent fibre can be used as the evening dress in anti-false sign, the dance hall etc.
The development technique of luminescent fibre and the performance of phosphor are closely related, and the conventional fluorescent powder is because of poor stability, have shortcoming such as radioactivity and are difficult to use in exploitation luminescent fibre with practical value.Chemical stability is good, the Eu nontoxic, "dead", that brightness is high, persistence is long
2+The exploitation of the alkali earth metal aluminate fluorescent material that activates, a series of luminescent plastics that market prospects are arranged, rubber, coating, printing ink, fiber etc. are succeeded in developing in succession.
Japan Patent JP-A-49-47644.JP-B-3-70020 and JP-A-2-112414 have disclosed long-persistence luminous fabric or fiber preparation method, patent adopts conventional fluorescent powder sulfide as luminescent material, poor stability, the fiber luminosity is low. and persistence is short, if improve the luminosity and the fluorescent lifetime of fiber, certain radioactive element must be added, the needs of relevant department can not be satisfied.
Compare with other luminous high polymer material, the technology of preparing of luminescent fibre is had relatively high expectations to fluorescent material, so the difficulty of preparation technology of luminescent fibre is also bigger.Generally speaking, can be divided into three kinds of methods: (1) coating; (2) co-blended spinning method; (3) light emitting polymer direct spinning.
Patent CN1346857 discloses a kind of luminous coating composition, but by the coating composition that adhesive and luminescent fibre are formed, is used for the mark of object.Coating or method for printing are simple relatively, and applicable to multiple fiber and fabric, its shortcoming is to be easy to peel off, and service life is shorter.
The co-blended spinning method is the method for preparing luminescent fibre commonly used.Patent CN1081210 discloses a kind of manufacture method of luminous fibre at night, is to add 5～20% luminous agent to carry out spinning and prepare the luminous artificial fiber in the spinning viscose.Patent CN1374415 discloses a kind of manufacture method of RE luminous fiber, be in stated polyesters section, add luminous agent and nano assistant make the noctilucence master batch after with big bright PET chips co-blended spinning, but fibre strength is on the low side.Equally, patent US6162539 discloses a kind of method for preparing the high brightness fluorescent fiber, be with fluorescent RE powder and polyolefin blend as sandwich layer, polyolefin carries out composite spinning as cortex and prepares industrial luminous polyamide fiber.Japan Patent JP-A-7-300722 is that the method by composite spinning prepares luminescent fibre equally, and cortex is polyester polycaprolactam or polyhexamethylene adipamide, but the fluorescent material moisture-sensitive of being added and influence its luminosity.
Summary of the invention
The technical issues that need to address of the present invention are to disclose a kind of long-afterglow luminous composite fibre, to overcome the above-mentioned defective that prior art exists.
Another technical problem that the present invention need solve provides the preparation method of above-mentioned long-afterglow luminous composite fibre, so that industrializing implementation.
Long-afterglow luminous composite fibre of the present invention is to be sandwich layer with the luminous polyamide, and fibre-forming polymer polyamide, polyester, polyolefin are cortex, carries out composite spinning and makes, and the mass ratio of sandwich layer and cortex is 2: 3～3: 1, wherein:
Said luminous polyamide is by the Eu of polyamide and luminous effective dose
2+The alkali earth metal aluminate that activates is formed, and preferred ingredients and weight percent content comprise: polyamide 70%～98%, Eu
2+The alkali earth metal aluminate 2%～30% that activates.
Said polyamide comprises a kind of in polyamide 6, polyamide 66, polyamide 46, polyamide 1010, polyamide 6 10. polyamide, 11. polyamide 12 or the polyamide 6 12;
Said Eu
2+The alkali earth metal aluminate that activates is the compound with following general structure:
M
XAl
YO
Z:Eu
2+，N
3+
Wherein: M represents a kind of among Sr, Ca, Mg or the Ba;
N represents a kind of among Dy, Nd or the Pr;
The integer of X=1～4;
The integer of Y=2～14;
The integer of Z=4～25;
Preferred Eu
2+The alkali earth metal aluminate that activates comprises SrAl
2O
4: Eu
2+, Dy
3+, Sr
4Al
14O
25: Eu
2+, Dy
3+, CaAl
2O
4: Eu
2+, Nd
3+, BaAl
2O
4: Eu
2+, Pr
3+, MgAl
2O
4: Eu
2+, Nd
3+In a kind of;
The Eu that is addressed
2+The alkali earth metal aluminate that activates can adopt CN1212988 and CN1403533 patent or document (Chen Zhonglin. Wan Tizhi. Zhang Yuqi. Yan Dezhong, the illuminating engineering journal, 1999,10 (2), 35) disclosed method is prepared, also can adopt the commercially available prod, the trade mark of producing as Shanghai Yuelong New Material Co., Ltd. is the fluorescent material of YLAG.
Said luminous polyamide can preferably adopt the situ aggregation method preparation, and its architectural feature and preparation method thereof is at inventor's Chinese patent formerly, and application number is existing detailed description in 03142085.0, is summarized as follows:
Monomer of polyamide, auxiliary agent and water and the fluorescent material addressed are mixed, in inert atmosphere, under the pressure of normal pressure～2.0Mpa,, vacuumize then and continue reaction 0.2～1hr, promptly obtain long persistence luminous polyamide in 200～300 ℃ of reaction 2～8hr.
Said monomer of polyamide comprises caprolactam, adipic acid, hexamethylene diamine, decanedioic acid, decamethylene diamine, butanediamine, 11-aminoundecanoic acid, ten dicaprolactams, 12 diacid. one or more in polyamide fibre 66 salt, polyamide fibre 1010 salt or polyamide fibre 46 salt;
Said auxiliary agent comprises catalyst or/and stabilizing agent;
A kind of in preferred aminocaproic acid of said catalyst or the caprolactam;
A kind of in preferred adipic acid of said stabilizing agent or the decanedioic acid;
In the weight of monomer of polyamide, the addition of catalyst is 1～3%;
The addition of stabilizing agent is 0.1～0.6%;
The addition of water is 1～35%.
The luminous polyamide number-average molecular weight is 10000～15000.
The preparation method of long-afterglow luminous composite fibre of the present invention comprises the steps:
The sandwich layer component luminous polyamide of being addressed is carried out extracting in boiling water, remove unreacted monomer and oligomer, then at 90～100 ℃ of vacuumize 12～18hr;
The cortex component of being addressed is carried out vacuumize to moisture content＜50ppm;
Dried cortex, sandwich layer component are sent into composite spinning machine carry out melt spinning, the sandwich layer spinning temperature is 260～295 ℃, the spinning temperature of cortex is adjusted according to the cortex composition, be generally 250～290 ℃, spinning speed is 1000～3200m/min, stretch at last or add bullet, draw ratio is 1.6～3.5 times, promptly obtains long-afterglow luminous composite fibre of the present invention.
Advantage of the present invention is very significant, and the fluorescent material that is adopted is Eu
2+The alkali earth metal aluminate series that activates, nontoxic, "dead", luminosity is high, persistence is long, and chemical property is stablized.And can develop the fiber of different emission wavelengths as required; The luminous polyamide that in-situ polymerization is prepared has the chemical bonding effect between fluorescent material and the polyamide, fluorescent material is uniformly dispersed, incrust, good spinnability, the luminous polyamide of in-situ polymerization, molecular weight can be adjusted as required, the luminescent fibre of spinning different size, fibre strength height; Luminous composite fibre of the present invention, with conventional fibre-forming polymer is cortex, good spinnability, the post-stretching of as-spun fibre or to add elastic energy good, finished fiber intensity height, luminous composite fibre is a cortex with different conventional fibre-forming polymers, can spin the luminescent fibre of different cultivars, and not influence process conditions such as the dyeing of fiber, back arrangement; Luminous composite fibre, fluorescent material are covered by fibrous inside fully, and prolong service life greatly, can be widely used in fields such as decoration, clothes, fishery, industry, have application promise in clinical practice.
The specific embodiment
Embodiment 1
The preparation of PA6/PA6 long-afterglow luminous composite fibre
Raw material: caprolactam 190.4g
Aminocaproic acid 4.00g
Adipic acid 0.5g
Distilled water 6.00ml
Fluorescent material: CaAl
2O
4: Eu
2+, Nd
3+10.36g, average grain diameter:
Polyamide 6 (PA6): 300g, number-average molecular weight 11500
The preparation method:
(1) caprolactam, aminocaproic acid, adipic acid, distilled water are added in the reactor according to the above ratio, mix, logical nitrogen protection; slowly be heated to 140 ℃, stir, slowly be warming up to 250 ℃; behind the isothermal reaction 5hr, vacuumize and continue 0.5hr, obtain luminous polyamide 6.
(2) luminous polyamide 6 in the step (1) is carried out extracting 0.5hr in boiling water, dries after the taking-up, in vacuum drying chamber in 95 ℃ of dry 18hr down, as the sandwich layer component.
(3) get polyamide 6 300g, in vacuum drying chamber in 95 ℃ of following dry 18hr, as the cortex component.
(4) dried cortex, sandwich layer component are sent into composite spinning machine and carry out melt spinning, the sandwich layer spinning temperature is 280 ℃, and 285 ℃ of the spinning temperatures of cortex, spinning speed are 1000m/min, and draw ratio is 3.0 times.
The result: a luminous composite fibre stretching silk specification, 100dtex/20f, intensity 3.92cN/dtex, emission wavelength 420～440nm behind the illumination 10min, in the dark places 2hr, and after-glow brightness is 1.15mcd/m
2
Embodiment 2
The preparation of PA6/PET long afterglow composite fibre
Raw material: caprolactam 190.4g
Aminocaproic acid 4.00g
Adipic acid 0.5g
Distilled water 6.00ml
Fluorescent material: SrAl
2O
4: Eu
2+, Dy
3+31.08g, average grain diameter:
Polyethylene terephthalate (PET): 200g, intrinsic viscosity, 0.67
The preparation method:
(1) add caprolactam, aminocaproic acid, adipic acid, distilled water in the reactor according to the above ratio; mix, logical nitrogen protection slowly is heated to 140 ℃; stir; slowly be warming up to 210 ℃, behind the reaction 1hr, add fluorescent material; continue to be warming up to 250 ℃; behind the isothermal reaction 4.5hr, vacuumize and continue 0.5hr, obtain luminous polyamide 6.
(2) luminous polyamide 6 in the step (1) is carried out extracting 0.5hr in boiling water, dries after the taking-up, in vacuum drying chamber in 95 ℃ of dry 18hr down, as the sandwich layer component.
(3) get PET 200g, in vacuum drying chamber in 140 ℃ of following dry 24hr, as the cortex component.
(4) dried cortex, sandwich layer component are sent into composite spinning machine and carry out melt spinning, the sandwich layer spinning temperature is 285 ℃, and 290 ℃ of the spinning temperatures of cortex, spinning speed are 2500m/min, and draw ratio is 2.5 times.
The result: a luminous composite fibre stretching silk specification, 72dtex/24f, intensity 3.82cN/dtex, emission wavelength 510～525nm behind the illumination 10min, in the dark places 2hr, and after-glow brightness is 1.15mcd/m
2
Embodiment 3
The preparation of PA66/PA66 long-afterglow luminous composite fibre
Raw material: PA66 salt 200g
Adipic acid 1.80g
Caprolactam 4.00g
Distilled water 60g
Fluorescent material: SrAl
14O
25: Eu
2+, Dy
3+20g, average grain diameter:
Polyamide 66 100g, number-average molecular weight, 12000
The preparation method:
(1) PA66 salt, adipic acid, caprolactam, distilled water, fluorescent material in the above-mentioned raw materials are added in the autoclave, mix, logical N
2Drive away air, airtight, slowly be heated to 210 ℃, reaction 2hr, stirring continues slowly to be warming up to 270 ℃, and controlled pressure 1.47～1.96Mpa behind the continuation reaction 2hr, is released into normal pressure, after continuing to react 3hr, vacuumizes and continues to react 0.5hr, obtains polyamide 66.
(2) luminous polyamide 66 in the step (2) is carried out extracting 15min in boiling water, dry after the taking-up, in vacuum drying chamber, descend dry 16hr in 90 ℃.
(3) get polyamide 66 100g, in vacuum drying chamber in 90 ℃ of following dry 18hr, as the cortex component.
(4) dried cortex, sandwich layer component are sent into composite spinning machine and carry out melt spinning, the sandwich layer spinning temperature is 275 ℃, and 285 ℃ of the spinning temperatures of cortex, spinning speed are 1200m/min, and draw ratio is 3.5 times.
The result: the compound drawn yarn specification of luminous PA66/PA66 100dtex/20f, intensity 4.12cN/dtex, emission wavelength 485～495nm behind the illumination 10min, in the dark places 2hr, and after-glow brightness is 1.52mcd/m
2
Embodiment 4
The preparation of PA66/PP long-afterglow luminous composite fibre
Raw material: PA66 salt 200g
Adipic acid 1.80g
Caprolactam 4.00g
Distilled water 60g
Fluorescent material: SrAl
14O
25: Eu
2+, Dy
3+30g, average grain diameter:
Polypropylene (PP) 70g, melt index 20
The preparation method:
(1) PA66 salt, adipic acid, caprolactam, distilled water, fluorescent material in the above-mentioned raw materials are added in the autoclave, mix, logical N
2Drive away air, airtight, slowly be heated to 210 ℃, reaction 2hr, stirring continues slowly to be warming up to 270 ℃, and controlled pressure 1.47～1.96Mpa behind the continuation reaction 2hr, is released into normal pressure, after continuing to react 3hr, vacuumizes and continues to react 0.5hr, obtains polyamide 66.
(2) luminous polyamide 66 in the step (2) is carried out extracting 15min in boiling water, dry after the taking-up, in vacuum drying chamber, descend dry 16hr in 90 ℃.
(3) get polypropylene 70g, in vacuum drying chamber in 105 ℃ of following dry 5hr, as the cortex component.
(4) dried cortex, sandwich layer component are sent into composite spinning machine and carry out melt spinning, the sandwich layer spinning temperature is 275 ℃, and 260 ℃ of the spinning temperatures of cortex, spinning speed are 1000m/min, and draw ratio is 3.5 times.
The result: the compound drawn yarn specification of luminous PA66/PP 200dtex/20f, intensity 3.85cN/dtex, emission wavelength 485～495nm behind the illumination 10min, in the dark places 2hr, and after-glow brightness is 1.98mcd/m
2
Embodiment 5
The preparation of PA6/PE long afterglow composite fibre
Raw material: caprolactam 190.4g
Aminocaproic acid 4.00g
Adipic acid 0.5g
Distilled water 6.00ml
Fluorescent material: SrAl
2O
4: Eu
2+, Dy
3+22g, average grain diameter:
Polyethylene (PE): 80g, melt index 26
The preparation method:
(1) add caprolactam, aminocaproic acid, adipic acid, distilled water in the reactor according to the above ratio; mix, logical nitrogen protection slowly is heated to 140 ℃; stir; slowly be warming up to 210 ℃, behind the reaction 1hr, add fluorescent material; continue to be warming up to 250 ℃; behind the isothermal reaction 4.5hr, vacuumize and continue 0.5hr, obtain luminous polyamide 6.
(2) luminous polyamide 6 in the step (1) is carried out extracting 0.5hr in boiling water, dries after the taking-up, in vacuum drying chamber in 95 ℃ of dry 18hr down, as the sandwich layer component.
(3) get PE 80g, in vacuum drying chamber in 105 ℃ of following dry 4hr, as the cortex component.
(4) dried cortex, sandwich layer component are sent into composite spinning machine and carry out melt spinning, the sandwich layer spinning temperature is 265 ℃, and 250 ℃ of the spinning temperatures of cortex, spinning speed are 1000m/min, and draw ratio is 3.3 times.
The result: a luminous composite fibre stretching silk specification, 72dtex/24f, intensity 3.79cN/dtex, emission wavelength 510～525nm behind the illumination 10min, in the dark places 2hr, and after-glow brightness is 1.24mcd/m
2
Claims (9)
1. long-afterglow luminous composite fibre, it is characterized in that being is sandwich layer with the luminous polyamide, fibre-forming polymer polyamide, polyester, polyolefin are cortex, carrying out composite spinning makes, the mass ratio of sandwich layer and cortex is 2: 3～3: 1, and wherein: said luminous polyamide is by the Eu of polyamide and luminous effective dose
2+The alkali earth metal aluminate that activates is formed.
2. long-afterglow luminous composite fibre according to claim 1 is characterized in that, the component and the weight percent content of luminous polyamide comprise: polyamide 70%～98%, Eu
2+The alkali earth metal aluminate 2%～30% that activates.
3. long-afterglow luminous composite fibre according to claim 1 is characterized in that, said polyamide comprises a kind of in polyamide 6, polyamide 66, polyamide 46, polyamide 1010, polyamide 6 10. polyamide, 11. polyamide 12 or the polyamide 6 12.
4. long-afterglow luminous composite fibre according to claim 1 is characterized in that, said Eu
2+The alkali earth metal aluminate that activates is the compound with following general structure:
M
XAl
YO
Z:Eu
2+，N
3+
Wherein: M represents a kind of among Sr, Ca, Mg or the Ba;
N represents a kind of among Dy, Nd or the Pr;
The integer of X=1～4;
The integer of Y=2～14;
The integer of Z=4～25.
5. according to each described long-afterglow luminous composite fibre of claim 1～4, it is characterized in that Eu
2+The alkali earth metal aluminate that activates comprises SrAl
2O
4: Eu
2+, Dy
3+, Sr
4Al
14O
25: Eu
2+, Dy
3+, CaAl
2O
4: Eu
2+, Nd
3+, BaAl
2O
4: Eu
2+, Pr
3+, MgAl
2O
4: Eu
2+, Nd
3+In a kind of.
6. according to the preparation method of each described long-afterglow luminous composite fibre of claim 1～5, it is characterized in that, comprise the steps:
The sandwich layer component luminous polyamide of being addressed is carried out extracting, vacuumize then in boiling water;
The cortex component of being addressed is carried out vacuumize;
Dried cortex, sandwich layer component are sent into composite spinning machine carry out melt spinning.
7. method according to claim 6 is characterized in that, cortex and sandwich layer component are at 90～100 ℃ of vacuumize 12～18hr.
8. method according to claim 6 is characterized in that, with cortex and the vacuumize of sandwich layer component to moisture content＜50ppm.
9. method according to claim 6 is characterized in that, the sandwich layer spinning temperature is 260～295 ℃, and the spinning temperature of cortex is 250～290 ℃, and spinning speed is 1000～3200m/min, stretches at last or adds bullet, and draw ratio is 1.6～3.5 times.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA031422276A CN1488784A (en) | 2003-08-13 | 2003-08-13 | Long-persistence luminous composite fiber and preparing method thereof |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA031422276A CN1488784A (en) | 2003-08-13 | 2003-08-13 | Long-persistence luminous composite fiber and preparing method thereof |
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| Publication Number | Publication Date |
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| CN1488784A true CN1488784A (en) | 2004-04-14 |
Family
ID=34155666
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| CN103334176A (en) * | 2013-07-12 | 2013-10-02 | 乐美加特种纤维（连云港）有限公司 | Energy-storage long-persistence luminescent fiber |
| CN103924345A (en) * | 2014-05-04 | 2014-07-16 | 苏州市叶绣工艺厂 | Noctilucent fiber yarn for embroidery |
| CN104531145A (en) * | 2014-12-29 | 2015-04-22 | 福建农林大学 | Method for preparing bamboo strip/strontium aluminate fluorescent powder composite material |
| CN104674377A (en) * | 2014-12-05 | 2015-06-03 | 江苏旷达汽车织物集团股份有限公司 | Preparation method of luminescent low-stretch yarn for inner decorating materials for automobile |
| CN104805517A (en) * | 2015-02-15 | 2015-07-29 | 东华大学 | Two-component composite modified imitated fluff flash fiber and preparation method thereof |
| CN106758151A (en) * | 2016-12-01 | 2017-05-31 | 西南大学 | The preparation method of long afterglow green emitting dacron |
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| CN109338500A (en) * | 2018-10-08 | 2019-02-15 | 烟台泰和新材料股份有限公司 | A kind of noctilucence meta-aramid fibers and preparation method thereof |
| CN110345393A (en) * | 2019-07-26 | 2019-10-18 | 深圳大学 | A kind of motoricity excitation fluorescent apparatus and method |
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2003
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|---|---|---|---|---|
| CN103334176A (en) * | 2013-07-12 | 2013-10-02 | 乐美加特种纤维（连云港）有限公司 | Energy-storage long-persistence luminescent fiber |
| CN103924345A (en) * | 2014-05-04 | 2014-07-16 | 苏州市叶绣工艺厂 | Noctilucent fiber yarn for embroidery |
| CN104674377A (en) * | 2014-12-05 | 2015-06-03 | 江苏旷达汽车织物集团股份有限公司 | Preparation method of luminescent low-stretch yarn for inner decorating materials for automobile |
| CN104531145A (en) * | 2014-12-29 | 2015-04-22 | 福建农林大学 | Method for preparing bamboo strip/strontium aluminate fluorescent powder composite material |
| CN104805517A (en) * | 2015-02-15 | 2015-07-29 | 东华大学 | Two-component composite modified imitated fluff flash fiber and preparation method thereof |
| CN104805517B (en) * | 2015-02-15 | 2017-02-01 | 东华大学 | Two-component composite modified imitated fluff flash fiber and preparation method thereof |
| CN106758151A (en) * | 2016-12-01 | 2017-05-31 | 西南大学 | The preparation method of long afterglow green emitting dacron |
| CN107607528A (en) * | 2017-08-17 | 2018-01-19 | 天津科技大学 | The preparation method of the optical-fibre needle of recognizable poisonous and harmful substance |
| CN107604471A (en) * | 2017-08-29 | 2018-01-19 | 常熟市何市星晨纱厂（普通合伙） | A kind of high intensity core-sheath silk |
| CN107620131A (en) * | 2017-09-06 | 2018-01-23 | 广东大红马纺织新材料有限公司 | A kind of spot fluorescent fiber preparation method and fluorescent fabric |
| CN107620131B (en) * | 2017-09-06 | 2020-08-07 | 广东大红马纺织新材料有限公司 | Preparation method of spot fluorescent fiber and fluorescent fabric |
| CN109338500A (en) * | 2018-10-08 | 2019-02-15 | 烟台泰和新材料股份有限公司 | A kind of noctilucence meta-aramid fibers and preparation method thereof |
| CN111850718A (en) * | 2019-04-30 | 2020-10-30 | 东华大学 | Composite color fiber, spinning pack and preparation method thereof |
| CN110344150A (en) * | 2019-07-22 | 2019-10-18 | 南通汉卓纺织科技有限公司 | A kind of production method of high tensile flexible luminous yarn |
| CN110345393A (en) * | 2019-07-26 | 2019-10-18 | 深圳大学 | A kind of motoricity excitation fluorescent apparatus and method |
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