JP5607873B2 - Heat ray shielding polyester fiber - Google Patents
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- JP5607873B2 JP5607873B2 JP2008251388A JP2008251388A JP5607873B2 JP 5607873 B2 JP5607873 B2 JP 5607873B2 JP 2008251388 A JP2008251388 A JP 2008251388A JP 2008251388 A JP2008251388 A JP 2008251388A JP 5607873 B2 JP5607873 B2 JP 5607873B2
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- 229920000728 polyester Polymers 0.000 title claims description 47
- 239000000835 fiber Substances 0.000 title claims description 42
- 239000000843 powder Substances 0.000 claims description 118
- -1 sulfonic acid compound Chemical class 0.000 claims description 36
- 238000002834 transmittance Methods 0.000 claims description 21
- 229920001225 polyester resin Polymers 0.000 claims description 7
- 239000004645 polyester resin Substances 0.000 claims description 7
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 claims description 6
- 239000003063 flame retardant Substances 0.000 claims description 6
- 230000005855 radiation Effects 0.000 claims description 6
- 239000006097 ultraviolet radiation absorber Substances 0.000 claims description 6
- 239000000758 substrate Substances 0.000 claims description 5
- 125000000217 alkyl group Chemical group 0.000 claims description 4
- PJXISJQVUVHSOJ-UHFFFAOYSA-N indium(iii) oxide Chemical compound [O-2].[O-2].[O-2].[In+3].[In+3] PJXISJQVUVHSOJ-UHFFFAOYSA-N 0.000 claims description 4
- IAYPIBMASNFSPL-UHFFFAOYSA-N Ethylene oxide Chemical compound C1CO1 IAYPIBMASNFSPL-UHFFFAOYSA-N 0.000 claims description 3
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 3
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 claims description 3
- 229910052739 hydrogen Inorganic materials 0.000 claims description 3
- 239000001257 hydrogen Substances 0.000 claims description 3
- 229910003437 indium oxide Inorganic materials 0.000 claims description 3
- 125000001449 isopropyl group Chemical group [H]C([H])([H])C([H])(*)C([H])([H])[H] 0.000 claims description 3
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 claims description 3
- 125000001436 propyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])[H] 0.000 claims description 3
- 238000004381 surface treatment Methods 0.000 claims description 3
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 claims description 3
- 229910001887 tin oxide Inorganic materials 0.000 claims description 3
- 230000000694 effects Effects 0.000 description 16
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 13
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 11
- 239000007788 liquid Substances 0.000 description 9
- 150000001875 compounds Chemical class 0.000 description 8
- 238000009987 spinning Methods 0.000 description 8
- 229920000139 polyethylene terephthalate Polymers 0.000 description 7
- 239000005020 polyethylene terephthalate Substances 0.000 description 7
- 229920003171 Poly (ethylene oxide) Polymers 0.000 description 6
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 6
- 239000000523 sample Substances 0.000 description 5
- 239000012756 surface treatment agent Substances 0.000 description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 4
- 238000010521 absorption reaction Methods 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 229910019142 PO4 Inorganic materials 0.000 description 3
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 3
- 239000006096 absorbing agent Substances 0.000 description 3
- 229910044991 metal oxide Inorganic materials 0.000 description 3
- 150000004706 metal oxides Chemical class 0.000 description 3
- 239000010452 phosphate Substances 0.000 description 3
- 150000003014 phosphoric acid esters Chemical class 0.000 description 3
- 238000000926 separation method Methods 0.000 description 3
- 229910052708 sodium Inorganic materials 0.000 description 3
- 239000011734 sodium Substances 0.000 description 3
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 3
- LSNNMFCWUKXFEE-UHFFFAOYSA-M Bisulfite Chemical compound OS([O-])=O LSNNMFCWUKXFEE-UHFFFAOYSA-M 0.000 description 2
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 2
- OFOBLEOULBTSOW-UHFFFAOYSA-N Malonic acid Chemical compound OC(=O)CC(O)=O OFOBLEOULBTSOW-UHFFFAOYSA-N 0.000 description 2
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 2
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 2
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 2
- 239000011248 coating agent Substances 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 239000004744 fabric Substances 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- VTHJTEIRLNZDEV-UHFFFAOYSA-L magnesium dihydroxide Chemical compound [OH-].[OH-].[Mg+2] VTHJTEIRLNZDEV-UHFFFAOYSA-L 0.000 description 2
- 239000000347 magnesium hydroxide Substances 0.000 description 2
- 229910001862 magnesium hydroxide Inorganic materials 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- FFJCNSLCJOQHKM-CLFAGFIQSA-N (z)-1-[(z)-octadec-9-enoxy]octadec-9-ene Chemical compound CCCCCCCC\C=C/CCCCCCCCOCCCCCCCC\C=C/CCCCCCCC FFJCNSLCJOQHKM-CLFAGFIQSA-N 0.000 description 1
- CMLFRMDBDNHMRA-UHFFFAOYSA-N 2h-1,2-benzoxazine Chemical compound C1=CC=C2C=CNOC2=C1 CMLFRMDBDNHMRA-UHFFFAOYSA-N 0.000 description 1
- 239000011358 absorbing material Substances 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 125000001931 aliphatic group Chemical group 0.000 description 1
- 229910052787 antimony Inorganic materials 0.000 description 1
- WATWJIUSRGPENY-UHFFFAOYSA-N antimony atom Chemical compound [Sb] WATWJIUSRGPENY-UHFFFAOYSA-N 0.000 description 1
- 125000003118 aryl group Chemical group 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000004737 colorimetric analysis Methods 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 230000008878 coupling Effects 0.000 description 1
- 238000010168 coupling process Methods 0.000 description 1
- 238000005859 coupling reaction Methods 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- 239000010419 fine particle Substances 0.000 description 1
- 238000010304 firing Methods 0.000 description 1
- 229910052738 indium Inorganic materials 0.000 description 1
- APFVFJFRJDLVQX-UHFFFAOYSA-N indium atom Chemical compound [In] APFVFJFRJDLVQX-UHFFFAOYSA-N 0.000 description 1
- 239000011777 magnesium Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 238000000034 method Methods 0.000 description 1
- 239000012046 mixed solvent Substances 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- RCMHUQGSSVZPDG-UHFFFAOYSA-N phenoxybenzene;phosphoric acid Chemical class OP(O)(O)=O.C=1C=CC=CC=1OC1=CC=CC=C1 RCMHUQGSSVZPDG-UHFFFAOYSA-N 0.000 description 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 1
- 229920001707 polybutylene terephthalate Polymers 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 239000011164 primary particle Substances 0.000 description 1
- 239000013074 reference sample Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 239000011342 resin composition Substances 0.000 description 1
- SLBXZQMMERXQAL-UHFFFAOYSA-M sodium;1-dodecoxy-4-hydroxy-1,4-dioxobutane-2-sulfonate Chemical compound [Na+].CCCCCCCCCCCCOC(=O)C(S(O)(=O)=O)CC([O-])=O SLBXZQMMERXQAL-UHFFFAOYSA-M 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 230000037072 sun protection Effects 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- 230000037303 wrinkles Effects 0.000 description 1
- 239000011787 zinc oxide Substances 0.000 description 1
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- Inorganic Compounds Of Heavy Metals (AREA)
- Artificial Filaments (AREA)
Description
本発明は、熱線遮蔽性を有するポリエステル繊維に関する。より詳しくは、ITO粉末やATO粉末を含有し、これらの含有量が多くても紡糸性が良く、熱線遮蔽性に優れたポリエステル繊維に関する。 The present invention relates to a polyester fiber having heat ray shielding properties. More specifically, the present invention relates to a polyester fiber containing ITO powder or ATO powder, having good spinnability even when the content of these is large, and excellent heat ray shielding properties.
ポリエステル繊維は強度、耐光性、耐水性、弾力性に優れており、皺になり難く、熱に強いため衣料品などは始めとして広く利用されている。このポリエステル繊維について、従来、酸化チタンなどを含有させて紫外線吸収性を持たせたものや(特許文献1)、金属酸化物からなる赤外線吸収材を含有させたものが知られている(特許文献2)。 Polyester fibers are excellent in strength, light resistance, water resistance, and elasticity, do not easily become wrinkles, and are resistant to heat, and are therefore widely used as clothing items. As for this polyester fiber, there are conventionally known ones containing titanium oxide or the like to impart ultraviolet absorption properties (Patent Document 1), and those containing an infrared absorbing material made of a metal oxide (Patent Documents). 2).
例えば、特許文献2には、ポリエステル重量に対して、金属酸化物系微粒子からなる赤外線吸収剤が0.1〜2.0重量%、有機系紫外線吸収剤が0.1〜5.0重量%おのおの含むことによって、赤外線吸収性と保温性を有するポリエステル繊維が記載されている。
特許文献2のポリエステル繊維は、赤外線吸収剤としてITO粉末やATO粉末が例示されているが、これらの含有量は0.1〜2.0重量%に制限されており、この含有量が2.0重量%を超えると、ポリエステル繊維を紡糸する際に糸切れなどの生じやすくなるので好ましくないとされている。しかし、赤外線吸収効果はITO粉末やATO粉末に依存しているので、これらの含有量が少ないと赤外線吸収効果も低下すると云う問題がある。 As for the polyester fiber of patent document 2, ITO powder and ATO powder are illustrated as an infrared absorber, However, These content is restrict | limited to 0.1 to 2.0 weight%, This content is 2. If it exceeds 0% by weight, it is considered undesirable because yarn breakage or the like is likely to occur when spinning polyester fibers. However, since the infrared absorption effect depends on the ITO powder and the ATO powder, there is a problem that the infrared absorption effect is lowered when the content of these is small.
本発明は、特定の処理剤によって表面処理したITO粉末およびATO粉末を用いることによって、ITO粉末やATO粉末の含有量が多くても紡糸性が良く、熱線遮蔽性に優れたポリエステル繊維を提供する。 The present invention provides a polyester fiber that has good spinnability and excellent heat ray shielding properties by using ITO powder and ATO powder surface-treated with a specific treatment agent, even if the content of ITO powder or ATO powder is large. .
本発明は、以下に示す構成によって上記課題を解決した熱線遮蔽性ポリエステル繊維に関する。
〔1〕スズドープ酸化インジウム(ITO)粉末および/またはアンチモンドープ酸化スズ(ATO)粉末を含有し、熱線遮蔽性を有するポリエステル繊維であって、ITO粉末ないしATO粉末の一種の含有量または二種の合計含有量が2.0重量%より多く10重量%以下であり、ITO粉末ないしATO粉末が、次式[1]〔R:アルキル基またはアルキルアリル基、R1:水素またはR(CH 2 CH 2 O)基、n:エチレンオキサイド付加モル数〕によって示されるリン酸ポリエステルによって表面処理されており、または次式[2]〔Rは上記と同じ〕によって示されるスルホン酸化合物によって表面処理されており、または次式[3]〔Rは上記と同じ、R2:メチル基、エチル基、イソプロピル基、プロピル基〕によって示されるスルホン酸化合物によって表面処理されていることを特徴とするポリエステル繊維。
〔3〕ITO粉末ないしATO粉末と共に紫外線吸収剤を含有する請求項1または請求項2に記載するポリエステル繊維。
〔4〕ITO粉末ないしATO粉末と共に難燃剤を含有する請求項1〜請求項3の何れかに記載するポリエステル繊維。
The present invention relates to a heat ray-shielding polyester fiber that has solved the above-described problems with the following configuration.
[1] Polyester fiber containing tin-doped indium oxide (ITO) powder and / or antimony-doped tin oxide (ATO) powder and having a heat ray shielding property, the content of one kind or two kinds of ITO powder or ATO powder The total content is more than 2.0% by weight and not more than 10% by weight, and the ITO powder or ATO powder has the following formula [1] [R: alkyl group or alkylallyl group, R1: hydrogen or R (CH 2 CH 2 O) group, n: surface treated with a phosphoric acid polyester represented by ethylene oxide addition mole number], or surface treated with a sulfonic acid compound represented by the following formula [2] [R is the same as above] Or a sulfonic acid represented by the following formula [3] [R is the same as above, R2: methyl group, ethyl group, isopropyl group, propyl group] Polyester fiber characterized in that it is surface-treated with compound.
[3] The polyester fiber according to claim 1 or 2, which contains an ultraviolet absorber together with ITO powder or ATO powder.
[4] The polyester fiber according to any one of claims 1 to 3, which contains a flame retardant together with ITO powder or ATO powder.
本発明のポリエステル繊維は、上記式[1]〜上記式[2]に示す化合物によって表面処理したITO粉末もしくはATO粉末を用いることによって、これらの一種の含有量または二種の合計含有量を2.0重量%より多く高めたものである。従来のポリエステル繊維において、これらの金属酸化物粉末の含有量は2.0重量%が限界であった。本発明のポリエステル繊維では、ITO粉末ないしATO粉末の含有量が2.0重量%より多く10重量%以下であり、従来のポリエステル繊維に含まれる含有量より格段に多いので、熱線遮蔽効果に優れる。 The polyester fiber of the present invention uses the ITO powder or ATO powder surface-treated with the compound represented by the above formula [1] to the above formula [2], so that one kind of content or two kinds of total content is 2 It is higher than 0.0% by weight. In conventional polyester fibers, the limit of the content of these metal oxide powders is 2.0% by weight. In the polyester fiber of the present invention, the content of ITO powder or ATO powder is more than 2.0% by weight and 10% by weight or less, which is much higher than the content contained in the conventional polyester fiber, so that the heat ray shielding effect is excellent. .
特に、ITO粉末に関しては、含有量が2.0重量%より多いと、図1および表1に示すように、可視光線透過率を損なわずに、大幅に日射透過率を下げることができ、赤外線カット効果を高めることが分かった。具体的には、本発明によれば、例えば、1mm厚さのPET基材において、可視光線透過率[%Tv]が10%以上、日射透過率が[%Ts]30%以下であって、熱線遮蔽比([%Tv]/[%Ts])が0.85以上のポリエステル繊維を得ることができる。 In particular, regarding the ITO powder, when the content is more than 2.0% by weight, as shown in FIG. 1 and Table 1, the solar radiation transmittance can be significantly lowered without impairing the visible light transmittance, It was found that the cutting effect was enhanced. Specifically, according to the present invention, for example, in a PET substrate having a thickness of 1 mm, the visible light transmittance [% Tv] is 10% or more, and the solar transmittance is [% Ts] 30% or less, A polyester fiber having a heat ray shielding ratio ([% Tv] / [% Ts]) of 0.85 or more can be obtained.
本発明のポリエステル繊維において、リン酸化合物またはスルホン酸化合物によって表面処理されたITO粉末ないしATO粉末を含有することによって、これらの一種の含有量または二種の合計含有量を2.0重量%〜10重量%に高めても、紡糸の際に糸切れの少ないポリエステル繊維を得ることができる。 In the polyester fiber of the present invention, by containing the ITO powder or ATO powder surface-treated with a phosphoric acid compound or a sulfonic acid compound, the content of these one kind or the total content of the two kinds is from 2.0% by weight to Even when the content is increased to 10% by weight, a polyester fiber with little yarn breakage can be obtained during spinning.
具体的には、例えば、上記式[1]によって示されるリン酸ポリエステル、または、上記式[2]ないし、チタネート系カップリング材によって示されるスルホン酸化合物によって表面処理されたITO粉末ないしATO粉末を含有することによって、上記含有量でも糸切れの少ないポリエステル繊維を得ることができる。 Specifically, for example, an ITO powder or ATO powder surface-treated with a phosphoric acid polyester represented by the above formula [1], or the above formula [2] or a sulfonic acid compound represented by a titanate coupling material. By containing, a polyester fiber with little yarn breakage can be obtained even with the above content.
以下、本発明を実施形態に基づいて具体的に説明する。
本発明のポリエステル繊維は、スズドープ酸化インジウム(ITO)粉末および/またはアンチモンドープ酸化スズ(ATO)粉末を含有し、熱線遮蔽性を有するポリエステル繊維であって、ITO粉末ないしATO粉末の一種の含有量または二種の合計含有量が2.0重量%より多く10重量%以下であることを特徴とし、好ましくは、ITO粉末ないしATO粉末がリン酸化合物またはスルホン酸化合物によって表面処理されているポリエステル繊維である。
Hereinafter, the present invention will be specifically described based on embodiments.
The polyester fiber of the present invention contains a tin-doped indium oxide (ITO) powder and / or an antimony-doped tin oxide (ATO) powder and has a heat ray shielding property, and is a kind of content of ITO powder or ATO powder. Alternatively, the total content of the two kinds is more than 2.0% by weight and not more than 10% by weight, and preferably the polyester fiber in which ITO powder or ATO powder is surface-treated with a phosphoric acid compound or a sulfonic acid compound It is.
本発明のポリエステル繊維は、ポリエステルの種類は限定されない。例えば、ポリエチレンテレフタレート、ポリブチレンテレフタレートなど、またはこれらのポリマーを基本骨格として芳香族ジカルボン酸脂肪族ジカルボン酸を共重合したものなどを広く用いることができる。 As for the polyester fiber of this invention, the kind of polyester is not limited. For example, polyethylene terephthalate, polybutylene terephthalate, or the like, or those obtained by copolymerizing aromatic dicarboxylic acid or aliphatic dicarboxylic acid using these polymers as a basic skeleton can be widely used.
本発明に用いるITO粉末ないしATO粉末は平均一次粒子径が0.5μm以下であるものが好ましい。粉末の粒子径がこれより大きいと、ポリエステル繊維を紡糸する工程で糸切れを生じやすくなり、添加量を多くすることができず、熱線遮蔽効果を得難くなる。 The ITO powder or ATO powder used in the present invention preferably has an average primary particle size of 0.5 μm or less. When the particle diameter of the powder is larger than this, yarn breakage is likely to occur in the process of spinning the polyester fiber, the amount added cannot be increased, and the heat ray shielding effect is difficult to obtain.
本発明のポリエステル繊維は、ITO粉末またはATO粉末の一種または二種を2.0重量%より多く10重量%以下含有する。この含有量が2.0重量%以下では熱線遮蔽効果が低く、10重量%を上回ると紡糸し難くなるので好ましくない。 The polyester fiber of this invention contains more than 2.0 weight% and 10 weight% or less of 1 type or 2 types of ITO powder or ATO powder. If the content is 2.0% by weight or less, the heat ray shielding effect is low, and if it exceeds 10% by weight, spinning becomes difficult.
リン酸化合物またはスルホン酸化合物によって表面処理したITO粉末およびATO粉末を用いることによって、2.0重量%〜10重量%の含有量でも、紡糸の際に糸切れの極めて少ないポリエステル繊維を得ることができる。 By using ITO powder and ATO powder surface-treated with a phosphoric acid compound or a sulfonic acid compound, it is possible to obtain polyester fibers with very little yarn breakage during spinning even with a content of 2.0 wt% to 10 wt%. it can.
表面処理剤として用いるリン酸化合物は次式[1]によって示される化合物が好ましい。次式[1]のリン酸化合物は酸価40以上であって、分子量3000以下が良く、1600以下がさらに好ましい。 The phosphate compound used as the surface treatment agent is preferably a compound represented by the following formula [1]. The phosphoric acid compound of the following formula [1] has an acid value of 40 or more, preferably a molecular weight of 3000 or less, and more preferably 1600 or less.
上記式[1]のリン酸化合物としては、具体的には、ポリオキシエチレンステアリルエーテルリン酸エステル、ポリオキシエチレンオレイルエーテルリン酸エステル、ポリオキシエチレンアルキルエーテルリン酸エステル、ポリオキシエチレンアルキルアリルエーテルリン酸エステル、ポリオキシエチレントリデシルエーテルリン酸エステル、ポリオキシエチレンスチレン化フェニルエーテルリン酸エステル、ポリオキシエチレンアルキルエーテルリン酸エステル、ポリオキシエチレンラウリルエーテルリン酸エステルなどが挙げられる。 Specific examples of the phosphoric acid compound of the above formula [1] include polyoxyethylene stearyl ether phosphate, polyoxyethylene oleyl ether phosphate, polyoxyethylene alkyl ether phosphate, polyoxyethylene alkyl allyl ether Examples thereof include phosphate esters, polyoxyethylene tridecyl ether phosphate esters, polyoxyethylene styrenated phenyl ether phosphate esters, polyoxyethylene alkyl ether phosphate esters, and polyoxyethylene lauryl ether phosphate esters.
表面処理剤として用いるスルホン酸化合物は次式[2]または次式[3]によって示される化合物が好ましい。これらの化合物は分子量3000以下が好ましい。 The sulfonic acid compound used as the surface treatment agent is preferably a compound represented by the following formula [2] or the following formula [3]. These compounds preferably have a molecular weight of 3000 or less.
上記式[2]のスルホン酸化合物としては、具体的には、ジアルキルスルホコハク酸エステルナトリウム、ポリオキシエチレンアルキルスルホコハク酸ナトリウム、ポリオキシエチレンスルホコハク酸ラウリルナトリウム、スルホコハク酸ラウリルナトリウムなどが挙げられる。 Specific examples of the sulfonic acid compound of the formula [2] include sodium dialkylsulfosuccinate ester, sodium polyoxyethylene alkylsulfosuccinate, sodium lauryl polyoxyethylenesulfosuccinate, sodium lauryl sulfosuccinate and the like.
上記式[3]のアルキルもしくはアルキルアリルスルホン酸型チタネートとしては、例えば、味の素社製KR−9SA等が挙げられる。 Examples of the alkyl or alkylallyl sulfonic acid type titanate of the above formula [3] include KR-9SA manufactured by Ajinomoto Co., Inc.
上記リン酸化合物またはスルホン酸化合物を用いて、ITO粉末ないしATO粉末を表面処理するには、上記化合物を溶解した溶液にITO粉末ないしATO粉末を投入して分散させた後にITO粉末ないしATO粉末を固液分離して回収すればよい。 In order to surface-treat ITO powder or ATO powder using the phosphoric acid compound or sulfonic acid compound, the ITO powder or ATO powder is dispersed in the solution in which the compound is dissolved, and then the ITO powder or ATO powder is dispersed. What is necessary is just to collect by solid-liquid separation.
具体的には、例えば、上記化合物をトルエン、エタノール、もしくはこれらの混合溶媒等に溶解した処理液を用い、この処理液100重量部に対して1〜250重量部のITO粉末ないしATO粉末を加えて攪拌混合し、必要に応じてさらにメディアを用いて分散させ、これらの粉末表面に上記リン酸化合物または上記スルホン酸化合物を付着させた後に固液分離し、乾燥工程を経て、上記化合物を付着させたITO粉末ないしATO粉末を回収する。もしくは、上記リン酸化合物とITO粉末ないしATO粉末を混合した液を固液分離せず、直接、乾燥工程を経ても構わない。 Specifically, for example, using a treatment liquid in which the above compound is dissolved in toluene, ethanol, or a mixed solvent thereof, 1 to 250 parts by weight of ITO powder or ATO powder is added to 100 parts by weight of this treatment liquid. Mix with stirring, and if necessary, disperse with media, attach the phosphoric acid compound or sulfonic acid compound to the surface of these powders, solid-liquid separate, and attach the compound through a drying process Collected ITO powder or ATO powder. Or the liquid which mixed the said phosphoric acid compound, ITO powder thru | or ATO powder may be directly passed through a drying process, without carrying out solid-liquid separation.
処理液中の表面処理剤の濃度は、例えば0.01〜15wt%が好ましい、なお、この処理液に投入する粉末重量が高濃度であればあるほど、有機溶媒の使用量が少なくてすむため、工業的に有利である。ただし、高濃度過ぎると、分散が出来ず、粉末の表面処理が出来なくなるので、粉末量は上記範囲が適当である。 The concentration of the surface treatment agent in the treatment liquid is preferably, for example, 0.01 to 15 wt%. Note that the higher the weight of the powder charged into the treatment liquid, the smaller the amount of organic solvent used. Industrially advantageous. However, if the concentration is too high, dispersion cannot be performed, and the surface treatment of the powder cannot be performed, so the above range is appropriate for the amount of powder.
上記表面処理されたITO粉末ないしATO粉末において、これらの粉末表面付着している表面処理剤の量は、粉末重量に対して、0.01〜20重量%が好ましい。 In the surface-treated ITO powder or ATO powder, the amount of the surface treatment agent adhering to the powder surface is preferably 0.01 to 20% by weight with respect to the weight of the powder.
上記リン酸化合物またはスルホン酸化合物によって表面処理したITO粉末ないしATO粉末をポリエステル樹脂に混合し、含有量を2.0重量%より多く10重量%以下に調整し、混錬して上記粉末を樹脂中に分散させた後に紡糸して本発明のポリエステル繊維を得ることができる。 ITO powder or ATO powder surface-treated with the above phosphoric acid compound or sulfonic acid compound is mixed with a polyester resin, the content is adjusted to more than 2.0% by weight and not more than 10% by weight, and kneaded to mix the above powder with resin. The polyester fiber of the present invention can be obtained by spinning after being dispersed therein.
本発明において用いるITO粉末ないしATO粉末は、Lab表色系において、色度(a・b/L、a<0、b<0)0.3以上のものが好ましい。これら粉末の色度(a・b/L)が0.3より小さいと、熱線遮蔽比([%Tv]/[%Ts])が低下する。ITO粉のインジウムとスズの比率は特に限定されないが、モル比にて、In:Sn=97:3からIn:Sn=80:20が好ましい。ATO粉のアンチモンとスズの比率は特に限定されないが、モル比にて、Sb:Sn=1:99からSb:Sn=20:80が好ましい。 The ITO powder or ATO powder used in the present invention preferably has a chromaticity (a · b / L, a <0, b <0) of 0.3 or more in the Lab color system. When the chromaticity (a · b / L) of these powders is smaller than 0.3, the heat ray shielding ratio ([% Tv] / [% Ts]) is lowered. Although the ratio of indium and tin in the ITO powder is not particularly limited, In: Sn = 97: 3 to In: Sn = 80: 20 are preferable in terms of molar ratio. The ratio of antimony and tin in the ATO powder is not particularly limited, but is preferably from Sb: Sn = 1: 99 to Sb: Sn = 20: 80 in terms of molar ratio.
本発明のポリエステル繊維は、ITO粉末ないしATO粉末と共に、紫外線吸収剤を含有することができる。紫外線吸収剤としては酸化チタンや酸化亜鉛などの無機粉末、酸化チタンにATOを被覆した無機粉末(具体例として、三菱マテリアル製S−1粉)あるいはベンゾオキサジンなどの有機粉末を用いることができる。紫外線吸収剤を併用することによって、赤外線に対する吸収効果(熱線遮蔽効果)と共に紫外線遮蔽効果を有することができ、熱線遮蔽効果と共に日焼け防止効果を有するポリエステル繊維を得ることができる。 The polyester fiber of this invention can contain a ultraviolet absorber with ITO powder thru | or ATO powder. As the ultraviolet absorber, inorganic powder such as titanium oxide and zinc oxide, inorganic powder obtained by coating titanium oxide with ATO (specifically, S-1 powder manufactured by Mitsubishi Materials), or organic powder such as benzoxazine can be used. By using an ultraviolet absorber in combination, it is possible to have an ultraviolet ray shielding effect as well as an infrared ray absorption effect (heat ray shielding effect), and a polyester fiber having a heat ray shielding effect and a sun protection effect can be obtained.
本発明のポリエステル繊維は、ITO粉末ないしATO粉末と共に、難燃剤を含有することができる。難燃剤としては水酸化マグネシウムMg(OH)2などを用いることができる。ITO粉末は赤外線を吸収して熱を持つので、難燃剤を併用することによって、ポリエステル繊維の発火を防止することができる。また、水酸化マグネシウムは白色粉末なので、これを含有することによってポリエステル繊維の白色性がより向上する。 The polyester fiber of the present invention can contain a flame retardant together with ITO powder or ATO powder. As the flame retardant, magnesium hydroxide Mg (OH) 2 or the like can be used. Since the ITO powder absorbs infrared rays and has heat, it is possible to prevent the firing of the polyester fiber by using a flame retardant together. Moreover, since magnesium hydroxide is a white powder, the whiteness of the polyester fiber is further improved by containing it.
紫外線吸収剤および難燃剤の含有量は、ITO粉末ないしATO粉末との合計量で10重量%以下が適当である。 The content of the UV absorber and the flame retardant is suitably 10% by weight or less in total with the ITO powder or ATO powder.
以下、本発明の実施例を比較試料と共に示す。
〔粉末の表面処理〕ATO粉およびITO粉を、表面処理剤を溶解したトルエン・エタノール液に混合して分散させ、固液分離して回収した。
〔透過率の測定〕表面処理したATO粉およびITO粉をポリエステル樹脂に、3本ロールにて混練し、樹脂組成物を厚さ1mmのPET基材に成形した。この塗膜について、可視光線透過率[%Tv]、日射透過率[%Ts]を測定した。[%Tv]および[%Ts]の測定は分光光度計(日立社製品U-4000)を用いた。
〔粉末の色度〕ATO粉およびITO粉の色度を色差計(日本電色社の測色色差計SE 2000)によって色度(L,a,b)測定し、a・b/Lを求めた。
Examples of the present invention are shown below together with comparative samples.
[Surface Treatment of Powder] ATO powder and ITO powder were mixed and dispersed in a toluene / ethanol solution in which a surface treatment agent was dissolved, and were collected by solid-liquid separation.
[Measurement of Transmittance] Surface-treated ATO powder and ITO powder were kneaded with a polyester resin with three rolls, and the resin composition was molded into a PET substrate having a thickness of 1 mm. About this coating film, visible light transmittance [% Tv] and solar radiation transmittance [% Ts] were measured. [% Tv] and [% Ts] were measured using a spectrophotometer (Hitachi U-4000).
[Chromaticity of the powder] The chromaticity of the ATO powder and the ITO powder is measured with a color difference meter (colorimetry color difference meter SE 2000 of Nippon Denshoku) to determine a · b / L. It was.
〔実施例1〕
リン酸ポリエステルによって表面処理したATO粉〔色度L:34.4、a:-2.0、b:-6.9〕およびITO粉〔色度L:50.3、a:-4.9、b:-14.4〕を表1に示す量に従ってポリエステル樹脂に混合した。このポリエステル樹脂組成物を用いて厚さ1mmのPET基材に形成し、可視光線透過率[%Tv]、日射透過率[%Ts]を測定した。この結果を表1に示した。さらに、粉末含有量と波長域の透過率を図1に示した。また、比較基準として粉末が混合されていないPET基材について、[%Tv]および[%Ts]を表1に示した。
[Example 1]
Table 1 shows ATO powder [chromaticity L: 34.4, a: -2.0, b: -6.9] and ITO powder [chromaticity L: 50.3, a: -4.9, b: -14.4] surface-treated with phosphoric polyester. The polyester resin was mixed according to the indicated amount. This polyester resin composition was used to form a PET substrate having a thickness of 1 mm, and the visible light transmittance [% Tv] and solar transmittance [% Ts] were measured. The results are shown in Table 1. Further, the powder content and the transmittance in the wavelength region are shown in FIG. Moreover, [% Tv] and [% Ts] are shown in Table 1 for the PET base material with no powder mixed as a reference for comparison.
表1に示すように、1mm厚さにて、ITO粉末2.5wt%を含むPET基材の試料No.A2の[%Tv]は27.7であり、10%以上の可視光線透過率[%Tv]を有する。同様に、ITO粉末10wt%を含むPET基材の試料No.A3の[%Tv]20.1であり、10%以上の可視光線透過率[%Tv]を有している。 As shown in Table 1, [% Tv] of PET base sample No. A2 containing 2.5 wt% of ITO powder at a thickness of 1 mm is 27.7, and a visible light transmittance of 10% or more [ % Tv]. Similarly, it is [% Tv] 20.1 of the sample No. A3 of the PET base material containing 10 wt% of the ITO powder, and has a visible light transmittance [% Tv] of 10% or more.
また、表1に示すように、No.A2およびNo.A3の試料は基準試料に対して、日射透過率[%Ts]は30%以下である。
また、これらの熱線遮蔽比〔[%Tv]/[%Ts]〕は何れも0.85以上である。
Further, as shown in Table 1, the solar radiation transmittance [% Ts] of the samples No. A2 and No. A3 is 30% or less with respect to the reference sample.
Further, these heat ray shielding ratios [[% Tv] / [% Ts]] are all 0.85 or more.
さらに、試料No.A1と試料No.A2を比較すると、No.A2のITO粉末含有量はNo.A1の5倍であるが、可視光線透過率の差は小さく、No.A2の試料は多量のITO粉末を含有しても可視光線の透過率が優れている。一方、No.A2の日射透過率は大幅に低下しており、熱線遮蔽性に優れている。No.A3についても同様である。これは図1のグラフにも示されている。 Further, comparing sample No. A1 and sample No. A2, the ITO powder content of No. A2 is five times that of No. A1, but the difference in visible light transmittance is small, and the sample of No. A2 is abundant. Even if the ITO powder is contained, the visible light transmittance is excellent. On the other hand, the solar radiation transmittance of No. A2 is greatly reduced, and is excellent in heat ray shielding properties. The same applies to No. A3. This is also shown in the graph of FIG.
〔実施例2〕
ポリエステル樹脂にATO粉〔色度L:34.4、a:-2.0、b:-6.9〕およびITO粉〔色度L:50.3、a:-4.9、b:-14.4〕を練り込み、溶融紡糸してポリエステル繊維を形成した。このポリエステル繊維によって布を形成し、熱線遮蔽効果を調べた。この試験は、上面に透明ガラスを設けた箱を用い、透明ガラスの上に試験用の布を被せ、10cm上方から赤外線ランプ(IR 100/110V 250W RH)を1時間照射して箱の内部温度を測定した。この結果を表2および図2に示した。
[Example 2]
ATO powder [chromaticity L: 34.4, a: -2.0, b: -6.9] and ITO powder [chromaticity L: 50.3, a: -4.9, b: -14.4] are kneaded into a polyester resin and melt-spun. Polyester fibers were formed. A cloth was formed from this polyester fiber, and the heat ray shielding effect was examined. This test uses a box with a transparent glass on the top, covers the transparent glass with a test cloth, and irradiates an infrared lamp (
表2に示すように、表面処理しないITO粉を用いたものは、粉末の含有量が2.5重量%で紡糸不能である(No.B2)。一方、表面処理したITO粉を用いたものは、その含有量が2重量%〜10重量%で紡糸可能であり、高い熱線遮蔽効果を有する(No.B3〜B5)。ただし、表面処理したITO粉でもその含有量が15重量%では、糸切れが多発し、紡糸困難になる(No.B6)。同様に表面処理したATO粉を用いたものは、その含有量が2.5重量%〜5.0重量%で紡糸可能であり、高い熱線遮蔽効果を有する(No.B7〜B8)。また、ATOとITOを混合した系も、2種類の合計2.5重量%にて、紡糸可能であることを確認し、また熱線遮蔽効果があることも確認できた。 As shown in Table 2, in the case of using ITO powder that was not surface-treated, the content of the powder was 2.5% by weight and spinning was not possible (No. B2). On the other hand, the one using the surface-treated ITO powder can be spun at a content of 2 to 10% by weight and has a high heat ray shielding effect (No. B3 to B5). However, even if the surface-treated ITO powder has a content of 15% by weight, yarn breakage frequently occurs and spinning becomes difficult (No. B6). Similarly, the one using the surface-treated ATO powder can be spun at a content of 2.5% to 5.0% by weight and has a high heat ray shielding effect (No. B7 to B8). In addition, it was confirmed that the mixed system of ATO and ITO can be spun at a total of 2.5% by weight of the two types, and that it has a heat ray shielding effect.
また、図2に示すように、ITO含有量が2重量%より多い範囲で試験箱の内部温度は急激に低下する。この結果から、十分な熱線遮蔽効果を得るにはITO粉末などの含有量は2重量%以上が適当である。 In addition, as shown in FIG. 2, the internal temperature of the test box rapidly decreases in the range where the ITO content is more than 2% by weight. From this result, in order to obtain a sufficient heat ray shielding effect, the content of ITO powder or the like is appropriately 2% by weight or more.
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