WO2012176881A1 - Composition de cire pour une bougie et bougie - Google Patents
Composition de cire pour une bougie et bougie Download PDFInfo
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- WO2012176881A1 WO2012176881A1 PCT/JP2012/065998 JP2012065998W WO2012176881A1 WO 2012176881 A1 WO2012176881 A1 WO 2012176881A1 JP 2012065998 W JP2012065998 W JP 2012065998W WO 2012176881 A1 WO2012176881 A1 WO 2012176881A1
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- WO
- WIPO (PCT)
- Prior art keywords
- component
- group
- wax
- candle
- wax composition
- Prior art date
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- 239000000203 mixture Substances 0.000 title claims abstract description 77
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- 125000000217 alkyl group Chemical group 0.000 description 10
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- 150000001336 alkenes Chemical class 0.000 description 5
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- UMJSCPRVCHMLSP-UHFFFAOYSA-N pyridine Natural products COC1=CC=CN=C1 UMJSCPRVCHMLSP-UHFFFAOYSA-N 0.000 description 1
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- 230000002040 relaxant effect Effects 0.000 description 1
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- 239000008165 rice bran oil Substances 0.000 description 1
- 238000005096 rolling process Methods 0.000 description 1
- 239000010666 rose oil Substances 0.000 description 1
- 235000019719 rose oil Nutrition 0.000 description 1
- 229930007790 rose oxide Natural products 0.000 description 1
- 239000010668 rosemary oil Substances 0.000 description 1
- 229940058206 rosemary oil Drugs 0.000 description 1
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- 229930195734 saturated hydrocarbon Natural products 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000012176 shellac wax Substances 0.000 description 1
- 229910010271 silicon carbide Inorganic materials 0.000 description 1
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 1
- 229920002050 silicone resin Polymers 0.000 description 1
- 229910001494 silver tetrafluoroborate Inorganic materials 0.000 description 1
- KZJPVUDYAMEDRM-UHFFFAOYSA-M silver;2,2,2-trifluoroacetate Chemical compound [Ag+].[O-]C(=O)C(F)(F)F KZJPVUDYAMEDRM-UHFFFAOYSA-M 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 229910021647 smectite Inorganic materials 0.000 description 1
- 239000011949 solid catalyst Substances 0.000 description 1
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- 230000002194 synthesizing effect Effects 0.000 description 1
- FKHIFSZMMVMEQY-UHFFFAOYSA-N talc Chemical compound [Mg+2].[O-][Si]([O-])=O FKHIFSZMMVMEQY-UHFFFAOYSA-N 0.000 description 1
- 239000000454 talc Substances 0.000 description 1
- 229910052623 talc Inorganic materials 0.000 description 1
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- 125000000999 tert-butyl group Chemical group [H]C([H])([H])C(*)(C([H])([H])[H])C([H])([H])[H] 0.000 description 1
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- ZNEOHLHCKGUAEB-UHFFFAOYSA-N trimethylphenylammonium Chemical compound C[N+](C)(C)C1=CC=CC=C1 ZNEOHLHCKGUAEB-UHFFFAOYSA-N 0.000 description 1
- RIOQSEWOXXDEQQ-UHFFFAOYSA-O triphenylphosphanium Chemical compound C1=CC=CC=C1[PH+](C=1C=CC=CC=1)C1=CC=CC=C1 RIOQSEWOXXDEQQ-UHFFFAOYSA-O 0.000 description 1
- UJMBCXLDXJUMFB-UHFFFAOYSA-K trisodium;5-oxo-1-(4-sulfonatophenyl)-4-[(4-sulfonatophenyl)diazenyl]-4h-pyrazole-3-carboxylate Chemical compound [Na+].[Na+].[Na+].[O-]C(=O)C1=NN(C=2C=CC(=CC=2)S([O-])(=O)=O)C(=O)C1N=NC1=CC=C(S([O-])(=O)=O)C=C1 UJMBCXLDXJUMFB-UHFFFAOYSA-K 0.000 description 1
- 229910052720 vanadium Inorganic materials 0.000 description 1
- GPPXJZIENCGNKB-UHFFFAOYSA-N vanadium Chemical compound [V]#[V] GPPXJZIENCGNKB-UHFFFAOYSA-N 0.000 description 1
- 235000015112 vegetable and seed oil Nutrition 0.000 description 1
- PXXNTAGJWPJAGM-UHFFFAOYSA-N vertaline Natural products C1C2C=3C=C(OC)C(OC)=CC=3OC(C=C3)=CC=C3CCC(=O)OC1CC1N2CCCC1 PXXNTAGJWPJAGM-UHFFFAOYSA-N 0.000 description 1
- 229940088594 vitamin Drugs 0.000 description 1
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- 229930003231 vitamin Natural products 0.000 description 1
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- 238000005406 washing Methods 0.000 description 1
- 229940045860 white wax Drugs 0.000 description 1
- 239000002023 wood Substances 0.000 description 1
- ZFNVDHOSLNRHNN-UHFFFAOYSA-N xi-3-(4-Isopropylphenyl)-2-methylpropanal Chemical compound O=CC(C)CC1=CC=C(C(C)C)C=C1 ZFNVDHOSLNRHNN-UHFFFAOYSA-N 0.000 description 1
- 239000008096 xylene Substances 0.000 description 1
- 229910052727 yttrium Inorganic materials 0.000 description 1
- VWQVUPCCIRVNHF-UHFFFAOYSA-N yttrium atom Chemical compound [Y] VWQVUPCCIRVNHF-UHFFFAOYSA-N 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
- XOOUIPVCVHRTMJ-UHFFFAOYSA-L zinc stearate Chemical compound [Zn+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O XOOUIPVCVHRTMJ-UHFFFAOYSA-L 0.000 description 1
- UHVMMEOXYDMDKI-JKYCWFKZSA-L zinc;1-(5-cyanopyridin-2-yl)-3-[(1s,2s)-2-(6-fluoro-2-hydroxy-3-propanoylphenyl)cyclopropyl]urea;diacetate Chemical compound [Zn+2].CC([O-])=O.CC([O-])=O.CCC(=O)C1=CC=C(F)C([C@H]2[C@H](C2)NC(=O)NC=2N=CC(=CC=2)C#N)=C1O UHVMMEOXYDMDKI-JKYCWFKZSA-L 0.000 description 1
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- 235000004835 α-tocopherol Nutrition 0.000 description 1
- 239000002076 α-tocopherol Substances 0.000 description 1
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11C—FATTY ACIDS FROM FATS, OILS OR WAXES; CANDLES; FATS, OILS OR FATTY ACIDS BY CHEMICAL MODIFICATION OF FATS, OILS, OR FATTY ACIDS OBTAINED THEREFROM
- C11C5/00—Candles
- C11C5/002—Ingredients
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L91/00—Compositions of oils, fats or waxes; Compositions of derivatives thereof
- C08L91/06—Waxes
Definitions
- the present invention relates to a wax composition for candles, and a candle having the wax composition and a combustion wick.
- the aroma candle is characterized by expressing an effect such as a relaxing effect by aroma while burning.
- Most waxes contain a fragrance so that the fragrance is diffused together with the wax during combustion (see Patent Documents 1 to 3).
- vegetable wax has the characteristics that it has less oil smoke compared to synthetic wax system, can diffuse the original fragrance sufficiently, and has less odor when extinguishing the flame. Recently, it has been favored and used. Furthermore, the appearance has been improved by adding liquid oil at normal temperature to wax (see Patent Documents 4 to 6).
- JP 7-48591 A Japanese Patent Laid-Open No. 9-188893 JP 2000-239694 A U.S. Pat. No. 4,224,204 US Pat. No. 6,776,808 US Patent Application Publication No. 2008/0092434
- the fragrance of the fragrance does not last long, and as soon as it is used (ignited), the fragrance fades away, making it impossible to increase the feeling of use, or the fragrance gradually fades during combustion due to the influence of additives.
- vegetable wax when vegetable wax is used, there is a problem that cracking is likely to occur and it is difficult to mold alone, and a method of improving by mixing with petroleum wax is known. There exists a problem that the said characteristic of itself reduces.
- the method of improving the appearance by adding liquid oil at normal temperature to wax generates oil bleed, so that it is difficult to apply the method to pillar candles and the like.
- an object of the present invention is to provide a wax composition for candles which is less likely to crack even when any wax is used, has high moldability, and has excellent burning sustainability, fragrance diffusibility and surface glossiness, and the wax composition.
- An object of the present invention is to provide a candle having a good appearance and having a small number of oil bleed.
- the present inventors have mixed wax with a specific higher ⁇ -olefin-based (co) polymer at a specific ratio, so that cracking hardly occurs and moldability is high.
- the present invention has been completed by finding that it has excellent burning sustainability, perfume diffusibility and surface glossiness, and that there is little oil bleed when it is made into a candle. Furthermore, by using a wax composition for candles in which a dye or pigment is added to a wax and a specific higher ⁇ -olefin-based (co) polymer, a stable pattern can be obtained even if the candle production conditions differ. The present inventors have found that the candle has a good appearance and completed the present invention.
- the content ratio of the component (A) to the component (B) [component (A): component (B)] is 81:19 to 99.99: 0.01 by mass ratio.
- Wax composition for candles. [2] The wax composition for candles according to the above [1], wherein the component (B) has the following characteristics (1) to (3). (1) The viscosity at 100 ° C.
- the wax composition for candles of the present invention is highly resistant to cracking and has high moldability. Moreover, since the wax composition for candles of the present invention is excellent in burning sustainability and perfume diffusibility, it is useful for aroma candles by containing perfume. In particular, when a vegetable wax is contained, the flammability is also excellent. Furthermore, the candle using the wax composition for candles of the present invention is excellent in the gloss of the candle surface on the side where the flame is lit, and does not impair the mood created by the candle. In addition, since the candle is provided with a pattern such as a floral pattern, snowflakes, snowflakes, stars, etc., the appearance is good, and the effect is that the melting point of the component (B) is 10 ° C. or lower than the component (A). Sometimes even more pronounced. Moreover, since there is little oil bleeding and a fragrance
- Example 8 It is a photograph which shows the state (however, the state put into the 15 ml glass tube) of the candle obtained in Example 8.
- FIG. It is a photograph which shows the state of the candle obtained in Example 9.
- FIG. It is a photograph which shows the state of the candle obtained in Example 10.
- FIG. It is a photograph which shows the state (however, the state put into a 15 ml glass tube) of the candle obtained in Reference Example 1.
- the candle wax composition of the present invention comprises: A wax composition for candles comprising (A) a wax and (B) a homopolymer or copolymer obtained using a higher ⁇ -olefin having 10 or more carbon atoms and having side chain crystallinity, A wax composition in which the content ratio of the component A) to the component (B) [component (A): component (B)] is 81:19 to 99.99: 0.01 by mass ratio.
- a wax composition for candles comprising (A) a wax and (B) a homopolymer or copolymer obtained using a higher ⁇ -olefin having 10 or more carbon atoms and having side chain crystallinity
- a wax composition in which the content ratio of the component A) to the component (B) [component (A): component (B)] is 81:19 to 99.99: 0.01 by mass ratio.
- As the wax of the component (A) a known wax used for coating the burning core of the candle can be used, and a solid at 25
- wax examples include animal waxes, vegetable waxes, mineral waxes, petroleum waxes, and synthetic waxes.
- animal waxes include beeswax, spermaceti, china wax (insect white wax), shellac wax, and lanolin (wool wax).
- vegetable wax examples include carnauba palm oil wax, cucumber palm oil wax, jojoba seed oil, candelilla wax, esparto wax, wood wax, soybean oil, white yam, jasmine plant oil, rice wax and rice bran oil.
- mineral wax examples include ozokerite, montan, and peat.
- petroleum waxes include paraffin wax and microcrystalline wax.
- Synthetic waxes include, for example, polyethylene wax, polypropylene wax, copolymer waxes such as ethylene / propylene / hexene / vinyl acetate, acrylic acid, hydrocarbon waxes such as Fischer-Tropsch wax and polymethylene wax, and synthetic amide waxes.
- the wax vegetable wax is preferable from the viewpoints of less oily smoke, sufficient diffusion of the original fragrance, less odor when extinguishing the flame, and sustainability of combustion. From the viewpoint of excellent moldability and low cost, petroleum wax is preferable.
- the component (B) preferably has side chain crystallinity and the following characteristics (1) to (3).
- the viscosity at 100 ° C. by a B-type viscometer is 10 to 10,000 mPa ⁇ s.
- the melting point obtained by a differential scanning calorimeter (DSC) is one, the melting point is in the range of 20 to 100 ° C., and the half-value width of the endothermic peak obtained when measuring the melting point is 10 ° C. or less. .
- Stereoregularity index value M2 is 75 mol% or less.
- “having crystallinity” means that a melting point as defined above is observed.
- side chain crystallinity means that the polymer has crystallinity at a site that becomes a side chain of a polymer other than a carbon-carbon double bond site that becomes a main chain. It has high crystallinity and is hard and has characteristics such as causing a solid-liquid phase change instantly and absorbing heat from the surroundings when it melts, and also has good thermal stability.
- the measurement method using a B-type viscometer is as follows.
- Measuring instrument Brookfield, LVDV-I (DV One Plus) for low viscosity
- Spindle Dedicated spindle No. 18 (SC4-18)
- Measuring method Set the sample at a predetermined temperature, and after the temperature is stable (within ⁇ 0.2 ° C.), heat for 10 minutes, immerse the spindle for 6 minutes, and measure the viscosity. With respect to the characteristic (1), the viscosity at 100 ° C.
- measured by a B-type viscometer is preferably 10 to 1,000 mPa ⁇ s, more preferably 10 to 500 mPa ⁇ s, and more preferably, from the viewpoint of fluidity and thus moldability. Is 30 to 500 mPa ⁇ s, more preferably 30 to 500 mPa ⁇ s, still more preferably 30 to 270 mPa ⁇ s, and particularly preferably 30 to 230 mPa ⁇ s.
- a differential scanning calorimeter (DSC) is used, and 10 mg of a sample is held at 190 ° C. for 5 minutes in a nitrogen atmosphere and then lowered to ⁇ 10 ° C. at 5 ° C./min.
- the melting point (Tm-B) is defined as the peak top temperature of the melting endotherm curve obtained by maintaining the temperature at ⁇ 10 ° C. for 5 minutes and then increasing the temperature to 190 ° C. at 10 ° C./min.
- the melting point (Tm-B) of the component (B) is preferably 20 to 80 ° C., more preferably 25 to 80 ° C., further preferably 30 to 80 ° C., and particularly preferably 30 to 65 ° C.
- the melting point (Tm-B) of the component (B) is preferably 20 to 55 ° C. from the viewpoint of the appearance of the candle. More preferably, it is 20 to 50 ° C., more preferably 25 to 50 ° C., further preferably 25 to 45 ° C., and particularly preferably 25 to 40 ° C. Further, in this case, the melting point (Tm ⁇ A) obtained by the differential scanning calorimeter (DSC) of the component (A) and the differential scanning calorific value of the component (B) in the same manner as the melting point (Tm ⁇ B) described above. It is preferable that the melting point (Tm-B) determined by the total (DSC) satisfies the relationship of the following formula (i). (Tm ⁇ A) ⁇ (Tm ⁇ B) +10 (i)
- the half-value width of the endothermic peak obtained upon measurement of the melting point of the component (B) is preferably 1 to 9 ° C., more preferably 1 to 7 ° C. from the viewpoint of crystal uniformity of the component (B).
- the temperature is preferably 2 to 7 ° C.
- a small half-value width indicates that the endothermic peak is sharp, that is, the melting behavior is rapid. In this case, problems such as storage stability and stickiness are suppressed by the low-temperature melting component.
- the half width is preferably 10 ° C. or less from the viewpoint of the appearance of the candle.
- the half-value width is 10 ° C. or less, so that the overlapping of the solidification temperatures of the component (A) and the component (B) is reduced, resulting in a uniform pattern. It is done.
- the full width at half maximum in this specification is an index representing the extent of the chevron shape of the endothermic peak obtained when measuring the melting point of the component (B), and the full width at half maximum (FWHM, Full Width at Half Maximum). ) Means.
- the stereoregularity index value M2 is a 13 C-NMR spectrum performed under the following apparatus and conditions, and is a methylene group (—CH 2 —
- the stereoregularity index value M2 is obtained by utilizing the fact that the carbon in the structure is split and observed reflecting the difference in stereoregularity.
- Apparatus “EX-400” (manufactured by JEOL Ltd.) Measurement temperature: 130 ° C Pulse width: 45 ° Integration frequency: 1,000 times Solvent: Mixed solvent of 1,2,4-trichlorobenzene and heavy benzene [90:10 (volume ratio)] Six large absorption peaks based on the mixed solvent are observed at 127 to 135 ppm. Among these peaks, the fourth peak value from the low magnetic field side is set to 131.1 ppm, which is used as a reference for chemical shift. At this time, an absorption peak based on carbon in the side chain ⁇ -position methylene group (—CH 2 —) is observed in the vicinity of 34 to 37 ppm.
- the stereoregularity index value M2 (mol%) is obtained using the following equation.
- M2 [(integral intensity of 36.2 to 35.3 ppm) / (integral intensity of 36.2 to 34.5 ppm)] ⁇ 100
- Apparatus “JNM-EX400 type 13 C-NMR” (manufactured by JEOL Ltd.)
- Method Proton complete decoupling method Concentration: 220 mg / ml
- Solvent Mixed solvent of 1,2,4-trichlorobenzene and heavy benzene [90:10 (volume ratio)] Temperature: 130 ° C.
- Pulse width 45 ° Pulse repetition time: 4 seconds Integration: 10,000 times This stereoregularity index value M2 Asakura, M .; Demura, Y .; This is obtained in accordance with the method proposed in “Macromolecules, 24, 2334 (1991)” reported by Nishiyama.
- the stereoregularity index value M2 is preferably 5 to 70 mol%, more preferably 10 to 70 mol%, more preferably 20 to 70 mol%, still more preferably 30 to 70 mol%, Particularly preferred is 40 to 70 mol%.
- the component (B) preferably satisfies the following property (4) from the viewpoint of influence on combustibility (flame size).
- the acid value measured according to the total acid value measuring method described in JIS K2501 (1980) is 5 mgKOH / g or less.
- the acid value is more preferably 3 mgKOH / g or less, further preferably 1 mgKOH / g or less, and particularly preferably substantially 0 mgKOH / g.
- the “higher ⁇ -olefin having 10 or more carbon atoms” is preferably a higher ⁇ -olefin having 10 to 40 carbon atoms, more preferably a higher ⁇ -olefin having 10 to 30 carbon atoms, and a higher ⁇ -olefin having 15 to 30 carbon atoms.
- -More preferred are olefins, and higher ⁇ -olefins having 18 to 25 carbon atoms are particularly preferred.
- Examples of higher ⁇ -olefins having 10 or more carbon atoms include 1-decene, 1-undecene, 1-dodecene, 1-tridecene, 1-tetradecene, 1-pentadecene, 1-hexadecene, 1-heptadecene, 1-octadecene, Examples thereof include 1-nonadecene, 1-eicosene, 1-docosene, 1-tetracocene, hexacocene, octacocene and triacontene.
- the component (B) used in the present invention is not particularly limited as long as it is obtained using such a higher ⁇ -olefin having 10 or more carbon atoms, and one or more higher ⁇ -olefins having 10 or more carbon atoms are used. May be obtained by polymerization or copolymerization, or may be obtained by copolymerization of one or more higher ⁇ -olefins having 10 or more carbon atoms and one or more other olefins. .
- the other olefin is, for example, ethylene or an ⁇ -olefin having less than 10 carbon atoms.
- the use ratio of the higher ⁇ -olefin having 10 or more carbon atoms and the other olefin is preferably such that the use amount of the higher ⁇ -olefin having 10 or more carbon atoms is 80 mol% or more with respect to the total amount thereof. More preferably, it is 90 mol% or more, More preferably, it is 95 mol% or more, It is especially preferable that it is substantially 100 mol%.
- a homopolymer or copolymer obtained using a higher ⁇ -olefin having 10 or more carbon atoms and having side chain crystallinity [hereinafter sometimes referred to as a crystalline higher ⁇ -olefin (co) polymer. ]
- a crystalline higher ⁇ -olefin (co) polymer can be produced using the metallocene catalyst shown below, and among them, it is particularly preferable to use a C 2 symmetric and C 1 symmetric transition metal compound capable of synthesizing an isotactic polymer.
- a transition metal compound represented by the following general formula (I) (a) a transition metal compound represented by the following general formula (I), and (b) a compound that can react with the transition metal compound of the component (a) or a derivative thereof to form an ionic complex [ (B-1)] and aluminoxane [(b-2)] are polymerized in the presence of a polymerization catalyst containing at least one component selected from one or more higher ⁇ -olefins having 10 or more carbon atoms.
- a copolymerization method, or a method of copolymerizing one or more higher ⁇ -olefins having 10 or more carbon atoms with one or more other olefins (a) a transition metal compound represented by the following general formula (I), and (b) a compound that can react with the transition metal compound of the component (a) or a derivative thereof to form an ionic complex [ (B-1)] and aluminoxane [(b-2)] are polymerized in
- M represents a metal element of Groups 3 to 10 or a lanthanoid series of the periodic table.
- E 1 and E 2 respectively represent a substituted cyclopentadienyl group, an indenyl group, a substituted indenyl group, a heterocyclopentadienyl group, a substituted heterocyclopentadienyl group, an amide group (—N ⁇ ), a phosphine group (— P ⁇ ), hydrocarbon group [>CR-,> C ⁇ ] and silicon-containing group [>SiR-,> Si ⁇ ] (where R is hydrogen, a hydrocarbon group having 1 to 20 carbon atoms, or a heteroatom-containing group) And a cross-linked structure is formed via A 1 and A 2 , and they may be the same as or different from each other.
- X represents a ⁇ -bonding ligand, and when there are a plurality of Xs, the plurality of Xs may be the same or different, and may be cross-linked with other X, E 1 , E 2 or Y.
- substitution refers to, for example, a hydrogen atom, a hydrocarbon group having 1 to 20 carbon atoms (preferably 1 to 10 carbon atoms, more preferably 1 to 5 carbon atoms), a silicon-containing group, or a heteroatom-containing group.
- Y represents a Lewis base
- the plurality of Y may be the same or different, and may be cross-linked with other Y, E 1 , E 2 or X.
- a 1 and A 2 are divalent bridging groups for linking two ligands, and are a hydrocarbon group having 1 to 20 carbon atoms, a halogen-containing hydrocarbon group having 1 to 20 carbon atoms, a silicon-containing group, Germanium-containing group, tin-containing group, —O—, —CO—, —S—, —SO 2 —, —Se—, —NR 1 —, —PR 1 —, —P (O) R 1 —, —BR 1 -or -AlR 1 -is shown.
- R 1 represents a hydrogen atom, a halogen atom, a hydrocarbon group having 1 to 20 carbon atoms, or a halogen-containing hydrocarbon group having 1 to 20 carbon atoms, which may be the same or different from each other.
- q represents an integer of 1 to 5 and represents [(valence of M) ⁇ 2], and r represents an integer of 0 to 3.
- Examples of M include titanium, zirconium, hafnium, yttrium, vanadium, chromium, manganese, nickel, cobalt, palladium, and lanthanoid metals.
- a metal element belonging to Group 4 of the periodic table is preferable, and among these, titanium, zirconium, and hafnium are more preferable.
- E 1 and E 2 substituted cyclopentadienyl group, indenyl group, substituted indenyl group.
- X include a halogen atom, a hydrocarbon group having 1 to 20 carbon atoms, an alkoxy group having 1 to 20 carbon atoms, an aryloxy group having 6 to 20 carbon atoms, an amide group having 1 to 20 carbon atoms, carbon Examples thereof include a silicon-containing group having 1 to 20 carbon atoms, a phosphide group having 1 to 20 carbon atoms, a sulfide group having 1 to 20 carbon atoms, and an acyl group having 1 to 20 carbon atoms. Among these, a halogen atom is preferable.
- Specific examples of the Lewis base represented by Y include amines, ethers, phosphines, thioethers, and the like.
- a 1 and A 2 are divalent bridging groups that bind two ligands.
- bridging groups include those represented by the general formula: (D is carbon, silicon or tin, R 2 and R 3 are each a hydrogen atom or a hydrocarbon group having 1 to 20 carbon atoms, which may be the same as or different from each other, and are bonded to each other to form a ring structure.
- E represents an integer of 1 to 4) The thing represented by is mentioned.
- an ethylene group, an isopropylidene group, and a dimethylsilylene group are preferable.
- the transition metal compound which makes the ligand the double bridge type biscyclopentadienyl derivative represented by these is preferable.
- M, A 1 , A 2 , q and r are the same as those in the general formula (I).
- X 1 represents a ⁇ -bonding ligand, and when plural X 1, a plurality of X 1 may be the same or different, may be crosslinked with other X 1 or Y 1.
- Specific examples of X 1 include the same ones as exemplified in the description of X in the general formula (I), and preferred ones are also the same.
- Y 1 represents a Lewis base, if Y 1 is plural, Y 1 may be the same or different, may be crosslinked with other Y 1 or X 1.
- R 4 to R 9 each independently represents a hydrogen atom, a halogen atom, a hydrocarbon group having 1 to 20 carbon atoms, a halogen-containing hydrocarbon group having 1 to 20 carbon atoms, a silicon-containing group or a heteroatom-containing group. , At least one of them must not be a hydrogen atom.
- R 4 to R 9 may be the same or different from each other, and adjacent groups may be bonded to each other to form a ring. Among these, it is preferable that R 6 and R 7 form a ring and R 8 and R 9 form a ring.
- R 4 and R 5 are preferably a group containing a heteroatom such as oxygen, halogen or silicon from the viewpoint of increasing the polymerization activity.
- the transition metal compound having the double-bridged biscyclopentadienyl derivative as a ligand preferably contains silicon in the bridging group between the ligands.
- Specific examples of the transition metal compound represented by the general formula (I) include (1,2′-ethylene) (2,1′-ethylene) -bis (indenyl) zirconium dichloride, (1,2′-methylene).
- (1,1 '-) (2,2'-) may be (1,2'-) (2,1'-) or (1,2 '-) (2 , 1'-) may be (1, 1'-) (2, 2'-).
- any compound that can react with the transition metal compound of the component (a) to form an ionic complex can be used.
- those represented by the following general formulas (III) and (IV) can be preferably used.
- L 1 is a Lewis base
- [Z] ⁇ is a non-coordinating anion [Z 1 ] ⁇ and [Z 2 ] ⁇
- [Z 1 ] ⁇ is a plurality of An anion in which a group is bonded to an element, that is, [M 1 G 1 G 2 ... G f ] ⁇ (where M 1 is an element of Group 5 to 15 of the periodic table, preferably 13 to 15 of the periodic table.
- G 1 to G f each independently represent a hydrogen atom, a halogen atom, an alkyl group having 1 to 20 carbon atoms, a dialkylamino group having 2 to 40 carbon atoms, an alkoxy group having 1 to 20 carbon atoms, An aryl group having 6 to 20 carbon atoms, an aryloxy group having 6 to 20 carbon atoms, an alkylaryl group having 7 to 40 carbon atoms, an arylalkyl group having 7 to 40 carbon atoms, and a halogen-substituted hydrocarbon group having 1 to 20 carbon atoms , An acyloxy group having 1 to 20 carbon atoms, an organic metalloid group, or a heteroatom having 2 to 20 carbon atoms Represents a hydrocarbon group, and two or more of G 1 to G f may form a ring, and f represents an integer of ((valence of central metal M 1 ) +1).
- [Z 2 ] ⁇ is a Bronsted acid alone or a conjugate base of a combination of Bronsted acid and Lewis acid having a logarithm (pKa) of the reciprocal of the acid dissociation constant of ⁇ 10 or less, or an acid generally defined as a super strong acid
- pKa logarithm
- a Lewis base may be coordinated.
- R 10 represents a hydrogen atom, an alkyl group having 1 to 20 carbon atoms, an aryl group having 6 to 20 carbon atoms, an alkylaryl group or an arylalkyl group, and R 11 and R 12 are each independently a cyclopenta A dienyl group, a substituted cyclopentadienyl group, an indenyl group or a fluorenyl group; R 13 represents an alkyl group having 1 to 20 carbon atoms, an aryl group, an alkylaryl group or an arylalkyl group.
- R 14 represents a macrocyclic ligand such as tetraphenylporphyrin or phthalocyanine.
- k is an integer of 1 to 3 in terms of ionic valences of [L 1 -R 10 ] and [L 2 ], a is an integer of 1 or more, and b is (k ⁇ a).
- M 2 includes elements in groups 1 to 3, 11 to 13, and 17 of the periodic table, and M 3 represents elements in groups 7 to 12 of the periodic table.
- L 1 examples include ammonia, methylamine, aniline, dimethylamine, diethylamine, N-methylaniline, diphenylamine, N, N-dimethylaniline, trimethylamine, triethylamine, tri-n-butylamine, methyldiphenylamine, amines such as p-bromo-N, N-dimethylaniline and p-nitro-N, N-dimethylaniline; nitrogen-containing heterocyclic compounds such as pyridine; phosphines such as triethylphosphine, triphenylphosphine and diphenylphosphine; Examples include thioethers such as tetrahydrothiophene; esters such as ethyl benzoate; nitriles such as acetonitrile and benzonitrile.
- R 10 include hydrogen, methyl group, ethyl group, benzyl group, trityl group and the like.
- R 11 and R 12 include a cyclopentadienyl group, a methylcyclopentadienyl group, an ethylcyclopentadienyl group, and a pentamethylcyclopentadienyl group.
- R 13 include a phenyl group, a p-tolyl group, and a p-methoxyphenyl group.
- R 14 include tetraphenylporphyrin, phthalocyanine, allyl, methallyl and the like.
- M 2 include Li, Na, K, Ag, Cu, Br, I, I 3 and the like.
- M 3 include Mn, Fe, Co, Ni, Zn and the like.
- M 1 include B, Al, Si, P, As, Sb, etc. B and Al.
- G 1 and G 2 to G f include a dialkylamino group substituted with an alkyl group having 1 to 5 carbon atoms such as a dimethylamino group and a diethylamino group; a methoxy group, an ethoxy group, an n-butoxy group, An alkoxy group having 1 to 6 carbon atoms such as a phenoxy group or an aryloxy group having 6 to 10 carbon atoms; methyl group, ethyl group, n-propyl group, isopropyl group, n-butyl group, isobutyl group, n-octyl group, an alkyl group having 1 to 20 carbon atoms such as n-eicosyl group; an aryl group having 6 to 20 carbon
- non-coordinating anions that is, Bronsted acids having a pKa of ⁇ 10 or less or a conjugate base [Z 2 ] ⁇ of a combination of Bronsted acids and Lewis acids
- trifluoromethanesulfonic acid anions CF 3 SO 3 ) ⁇
- bis (trifluoromethanesulfonyl) methyl anion bis (trifluoromethanesulfonyl) benzyl anion, bis (trifluoromethanesulfonyl) amide
- perchlorate anion (ClO 4 ) ⁇ trifluoroacetate anion (CF 3 CO 2 ) ⁇ , hexafluoroantimony anion (SbF 6 ) ⁇
- fluorosulfonate anion (FSO 3 ) ⁇ chlorosulfonate anion (ClSO 3 ) ⁇
- fluorosulfonate anion / 5-antimony fluoride F
- ionic compound that reacts with the transition metal compound of the component (a) to form an ionic complex include triethylammonium tetraphenylborate, tetraphenylboric acid.
- Tri-n-butylammonium trimethylammonium tetraphenylborate, tetraethylammonium tetraphenylborate, methyl (tri-n-butyl) ammonium tetraphenylborate, benzyl (tri-n-butyl) ammonium tetraphenylborate, dimethyldiphenyl tetraphenylborate Ammonium, triphenyl (methyl) ammonium tetraphenylborate, trimethylanilinium tetraphenylborate, methylpyridinium tetraphenylborate, benzylpyridinium tetraphenylborate, tetraphenylboron Methyl (2-cyanopyridinium), tetrakis (pentafluorophenyl) triethylammonium borate, tetrakis (pentafluorophenyl) tri-n
- R 15 represents a hydrocarbon group such as an alkyl group, alkenyl group, aryl group or arylalkyl group having 1 to 20 carbon atoms, preferably 1 to 12 carbon atoms or a halogen atom, and w represents an average degree of polymerization. Usually, it is an integer of 2 to 50, preferably 2 to 40. Note that each R 15 may be the same or different.
- R 15 and w are the same as those in the general formula (V).
- the cyclic aluminoxane shown by these is mentioned.
- Examples of the method for producing the aluminoxane include a method in which an alkylaluminum is brought into contact with a condensing agent such as water, but the means thereof is not particularly limited and may be reacted according to a known method.
- a method in which an organoaluminum compound is dissolved in an organic solvent and brought into contact with water a method in which an organoaluminum compound is initially added during polymerization, and water is added later, a metal
- a method of reacting water adsorbed on salt or the like with water adsorbed on inorganic or organic materials with an organoaluminum compound a method of reacting a tetraalkyldialuminoxane with a trialkylaluminum and further reacting with water.
- the aluminoxane may be insoluble in toluene. These aluminoxanes may be used alone or in combination of two or more.
- the use ratio of the component (a) to the component (b) is preferably 10: 1 to 1: 100, more preferably 2 when the compound (b-1) is used as the component (b).
- the range of: 1 to 1:10 is desirable, and if it is within the above range, the catalyst cost per unit mass polymer does not become so high and is practical.
- the compound (b-2) is used, the molar ratio is preferably in the range of 1: 1 to 1: 1,000,000, more preferably 1:10 to 1: 10,000. If it exists in this range, the catalyst cost per unit mass polymer will not become so high, and it is practical.
- one type of compound (b-1) and compound (b-2) may be used alone, or two or more types may be used in combination.
- the polymerization catalyst for producing the crystalline higher ⁇ -olefin (co) polymer can use an organoaluminum compound as the component (c).
- an organoaluminum compound of component (c) the general formula (VII) R 16 v AlJ 3-v (VII) (Wherein R 16 represents an alkyl group having 1 to 10 carbon atoms, and J represents a hydrogen atom, an alkoxy group having 1 to 20 carbon atoms, an aryl group having 6 to 20 carbon atoms, or a halogen atom. v is an integer of 1 to 3.) The compound shown by these is used.
- Examples of the alkyl group having 1 to 10 carbon atoms represented by R 16 include those having 1 to 5 carbon atoms such as methyl group, ethyl group, n-propyl group, isopropyl group, n-butyl group, isobutyl group and t-butyl group.
- An alkyl group is preferred.
- Examples of the alkoxy group having 1 to 20 carbon atoms represented by J include a methoxy group, an ethoxy group, an n-propoxy group, an isopropoxy group, and an n-butoxy group, and an alkoxy group having 1 to 10 carbon atoms is preferable.
- An alkoxy group of 1 to 5 is more preferable.
- Examples of the aryl group having 6 to 20 carbon atoms represented by J include a phenyl group, a naphthyl group, and an anthryl group, and an aryl group having 6 to 10 carbon atoms is preferable.
- Examples of the halogen atom represented by J include a fluorine atom, a chlorine atom, a bromine atom, and an iodine atom.
- v is preferably 3.
- the compound represented by the general formula (VII) include trimethylaluminum, triethylaluminum, triisopropylaluminum, triisobutylaluminum, dimethylaluminum chloride, diethylaluminum chloride, methylaluminum dichloride, ethylaluminum dichloride, dimethylaluminum fluoride. , Diisobutylaluminum hydride, diethylaluminum hydride, ethylaluminum sesquichloride and the like. Among these, triisobutylaluminum is preferable. These organoaluminum compounds may be used individually by 1 type, and may use 2 or more types together.
- the use ratio of the component (a) to the component (c) is preferably 1: 1 to 1: 10,000, more preferably 1: 5 to 1: 2,000, and still more preferably 1:10 in molar ratio. A range of ⁇ 1: 1,000 is desirable.
- the component (c) the polymerization activity per transition metal can be improved, but if it is too much, the organoaluminum compound is wasted and a large amount remains in the polymer, which is not preferable.
- at least one catalyst component can be supported on a suitable carrier and used.
- the type of the carrier is not particularly limited, and any of inorganic oxide carriers, other inorganic carriers, and organic carriers can be used. In particular, inorganic oxide carriers or other inorganic carriers are preferable.
- the polymerization method is not particularly limited, and any of slurry polymerization method, gas phase polymerization method, bulk polymerization method, solution polymerization method, suspension polymerization method, bulk polymerization method, etc. Although a method may be used, a solution polymerization method and a bulk polymerization method are particularly preferable.
- the polymerization temperature is usually ⁇ 100 to 250 ° C., preferably ⁇ 50 to 200 ° C., more preferably 0 to 150 ° C.
- the polymerization time is usually preferably 5 minutes to 10 hours, and the reaction pressure is usually preferably normal pressure to 20 MPa (gauge), more preferably normal pressure to 10 MPa (gauge).
- the pressure is usually from normal pressure to 5 MPa (gauge), preferably from normal pressure to 3 MPa (gauge), more preferably from normal pressure to 2 MPa (gauge).
- a polymerization solvent for example, aromatic hydrocarbons such as benzene, toluene, xylene, and ethylbenzene, alicyclic hydrocarbons such as cyclopentane, cyclohexane, and methylcyclohexane, and aliphatic hydrocarbons such as pentane, hexane, heptane, and octane , Halogenated hydrocarbons such as chloroform and dichloromethane can be used. These solvents may be used alone or in combination of two or more. A monomer such as ⁇ -olefin may be used as a solvent. Depending on the polymerization method, it can be carried out without solvent.
- aromatic hydrocarbons such as benzene, toluene, xylene, and ethylbenzene
- alicyclic hydrocarbons such as cyclopentane, cyclohexane, and methylcyclohexane
- prepolymerization can be performed using the polymerization catalyst.
- the prepolymerization can be performed, for example, by bringing a small amount of ⁇ -olefin into contact with the solid catalyst component, but the method is not particularly limited, and a known method can be used.
- the ⁇ -olefin used in the prepolymerization is not particularly limited, and examples thereof include those similar to those exemplified above, for example, ethylene, ⁇ -olefin having 3 to 20 carbon atoms, or a mixture thereof. It is advantageous to use the same ⁇ -olefin as the higher ⁇ -olefin or other ⁇ -olefin used in the reaction.
- the prepolymerization temperature is usually ⁇ 20 to 200 ° C., preferably ⁇ 10 to 130 ° C., more preferably 0 to 80 ° C.
- an aliphatic hydrocarbon, aromatic hydrocarbon, monomer or the like can be used as a solvent. Of these, aliphatic hydrocarbons are particularly preferred. Moreover, you may perform prepolymerization without a solvent.
- the intrinsic viscosity [ ⁇ ] (measured in 135 ° C.
- the method for adjusting the molecular weight of the polymer includes selection of the type of each catalyst component, the amount used, the polymerization temperature, and polymerization in the presence of hydrogen. An inert gas such as nitrogen may be present.
- the homopolymer or copolymer thus obtained has a comb structure rather than a hyperbranch structure, and therefore has side chain crystallinity.
- the content ratio of the component (A) and the component (B) in the candle wax composition of the present invention is from 81:19 to 99.99: 0.01 in terms of mass ratio from the viewpoint of combustion sustainability and moldability. There must be. From this viewpoint, the content ratio of the component (A) and the component (B) in the candle wax composition of the present invention is preferably a mass ratio of 85:15 to 99.9: 0.1, more preferably 87: 13-99.9: 0.1. From the viewpoint of combustibility, it is particularly preferably 90:10 to 99.9: 0.1, and most preferably 95: 5 to 99.9: 0.1.
- the candle composition for candles of the present invention may further contain a fragrance as the component (C), whereby a wax composition useful as an aroma candle can be obtained.
- a fragrance useful as an aroma candle can be obtained.
- the perfume ingredient is not particularly limited, but for example, limonene, lemon oil, orange oil, bitter orange oil, sweet orange oil, grapefruit oil, bergamot oil, mandarin oil, lime oil, citral, n-octanal (Aldehyde C-8), n-nonenal (aldehyde C-9), decanal (aldehyde C-10), undecanal (aldehyde C-11), ⁇ -damascon, ⁇ -damascon, ⁇ -damascon, ⁇ -damascon, Citrus flavors such as ⁇ -terpineol; cis-3-hexenol, galvanum oil, star anise oil, sage oil, violet leaf oil, rosemary oil, basil oil, lavandin oil, lavender oil, laurel oil, cassis base 345, Styraryl acetate, cis-3-hexenyl acetate, sali Green perfumes such as cis-3-hexenyl
- the content thereof is preferably 0.1 to 30 parts by mass with respect to 100 parts by mass of the total amount of the components (A) and (B).
- the amount is preferably 0.5 to 20 parts by mass, more preferably 1 to 15 parts by mass, and particularly preferably 3 to 10 parts by mass.
- the wax composition for candles of the present invention further contains a dye or pigment as the component (D). can do.
- a dye or pigment can be used to color the candle, and examples of the dye include oil-based dyes, aqueous dyes, and oil dyes.
- the pigment may be an inorganic pigment or an organic pigment, and crayon is preferably used.
- the wax composition for candles contains a dye or pigment, the content thereof is preferably 0.01 to 20 parts by mass, more preferably 100 parts by mass of the total amount of component (A) and component (B). Is 0.05 to 20 parts by mass, more preferably 0.05 to 10 parts by mass, and particularly preferably 0.1 to 10 parts by mass.
- the melting point (Tm-B) of the component (B) is 20 to 55 ° C. (more preferably 20 to 50 ° C., more preferably 25 to 50 ° C., further preferably 25 to 45 ° C., particularly preferably 25 to 40 ° C.), the candle has a pattern of flowers, snowflakes, snowflakes, stars, etc. Since it is imparted, the appearance is further improved. The effect becomes more prominent when the melting point of the component (B) is 10 ° C. or higher (preferably 13 ° C. or higher, more preferably 15 ° C. or higher, more preferably 20 ° C. or higher) lower than the component (A).
- the melting point (Tm-B) of the component (B) is significantly lower than the melting point of the component (A), so that when the candle is produced, the component (A) is solidified and the component (B) is in a liquid state Via. Since the component (B) condenses when solidified, a void is formed between the component (A) and the component (B), and the void looks like the pattern, so that the appearance is improved.
- oil is added to the composition for the purpose of improving the appearance, but in this case, an oil bleeding problem may occur. However, according to the present invention, the addition of the oil is not denied, but the appearance can be improved without adding the oil, so that the problem of oil bleeding can be avoided.
- oil is a liquid at normal temperature, and there is no restriction
- the wax composition for candles of the present invention comprises, in addition to the above-mentioned components (A) and (B), furthermore, in addition to the components (C) and (D), known components used for constituting candle wax.
- examples of such components include surfactants, oily components, powders, antioxidants, cosmetic components, preservatives, water-soluble polymers, ultraviolet absorbers, aqueous components, gelling agents, oil-soluble resins, chelating agents, Examples include medicinal ingredients, but are not limited thereto. By adding such components, it can be expected that effects such as an improvement in appearance (hue, pattern, shape), a relaxation effect, environmental compatibility, and the like are exhibited.
- surfactant examples include nonionic surfactants, anionic surfactants, and amphoteric surfactants.
- Nonionic surfactants include, for example, glycerin fatty acid esters and alkylene glycol adducts thereof, polyglycerin fatty acid ester alkylene glycol adducts, propylene glycol fatty acid esters and alkylene glycol adducts, sorbitan fatty acid esters and alkylene glycol adducts thereof.
- Fatty acid ester of sorbitol and its alkylene glycol adduct Fatty acid ester of sorbitol and its alkylene glycol adduct, polyalkylene glycol fatty acid ester, sucrose fatty acid ester, polyoxyalkylene alkyl ether, glycerin alkyl ether, polyoxyethylene alkyl phenyl ether, polyoxyethylene hydrogenated castor oil, alkylene glycol of lanolin Adduct, polyoxyalkylene-modified silicone, polyoxyalkylene alkyl co-modified silico Emissions, and the like.
- anionic surfactant examples include fatty acids such as stearic acid and lauric acid and their inorganic and organic salts, alkylbenzene sulfates, alkyl sulfonates, ⁇ -olefin sulfonates, dialkyl sulfosuccinates, ⁇ - Sulfonated fatty acid salt, acylmethyl taurate, N-methyl-N-alkyl taurate, polyoxyethylene alkyl ether sulfate, polyoxyethylene alkyl phenyl ether sulfate, alkyl phosphate, polyoxyethylene alkyl ether phosphate, poly Examples thereof include oxyethylene alkylphenyl ether phosphates, N-acyl amino acid salts, N-acyl-N-alkyl amino acid salts, o-alkyl substituted malates, and alkyl sulfosuccinates.
- fatty acids such as stearic acid and lauric acid and their inorgan
- amphoteric surfactants include amino acid type and betaine type carboxylic acid types, sulfate ester types, sulfonic acid types, and phosphate ester types, and those that are safe for the human body can be used.
- Oil component ⁇ examples include liquid saturated hydrocarbons such as liquid paraffin, fats and oils such as owl, olive oil, castor oil, mink oil and macadamian nut oil, waxes such as beeswax, carnauba wax, candelilla and gay wax, stearic acid , Fatty acids such as lauric acid, myristic acid, behenic acid, isostearic acid, oleic acid, higher alcohols such as stearyl alcohol, cetyl alcohol, lauryl alcohol, oleyl alcohol, isostearyl alcohol, behenyl alcohol, dimethylpolysiloxane, methylphenylpoly Siloxane, Decamethylcyclopentasiloxane, Octamethylcyclotetrasiloxane, Polyether-modified Organopolysiloxane, Polyoxyalkylene, Alkylmethyl Polysiloxane, Methyl Polysiro Sun copolymers, silicone
- the powder is not particularly limited by a spherical shape, a plate shape, a needle-like shape, a foggy shape, a fine particle, a particle size such as a pigment grade, a particle structure such as a porous or non-porous material, and the like.
- Examples include glitter powders, organic powders, pigment powders, metal powders, and composite powders.
- white inorganic pigments such as titanium oxide, zinc oxide, cerium oxide and barium sulfate, colored inorganic pigments such as iron oxide, carbon black, chromium oxide, chromium hydroxide, bitumen and ultramarine, talc, muscovite, gold Mica, red mica, biotite, synthetic mica, sericite (sericite), synthetic sericite, kaolin, silicon carbide, bentonite, smectite, aluminum oxide, magnesium oxide, zirconium oxide, antimony oxide, diatomaceous earth, aluminum silicate , Magnesium Metasilicate, Calcium Silicate, Barium Silicate, Magnesium Silicate, Calcium Carbonate, Magnesium Carbonate, Hydroxyapatite, Boron Nitride Powder, Titanium Dioxide Coated Mica, Titanium Dioxide Coated Bismuth Oxychloride, Iron Oxide Mica titanium, bitumen treated mica titanium, mosquito Bright powder such as min-treated mica titanium, bismuth
- Natural organic powder red 201, red 202, red 205, red 226, red 228, orange 203, orange 204, blue 404, yellow 401, etc., organic pigment powder, red 3 , Red 104, red 106, orange 205, yellow 4, yellow 5, green 3, blue 1, etc.
- Organic pigment powder such as barium or aluminum lake or metal powder such as aluminum powder, gold powder, silver powder, fine titanium oxide coated mica titanium, fine zinc oxide coated mica titanium, barium sulfate coated mica titanium, titanium dioxide containing silicon dioxide
- composite powders such as zinc oxide-containing silicon dioxide, polyethylene terephthalate / aluminum / epoxy laminated powder, polyethylene terephthalate / polyolefin laminated film powder, and lamellar agent of polyethylene terephthalate / polymethyl methacrylate laminated film powder.
- antioxidant examples include ⁇ -tocopherol and ascorbic acid.
- Beauty ingredients examples include vitamins, amino acids, anti-inflammatory agents and the like.
- Preservative examples include p-oxybenzoic acid ester and phenoxyethanol.
- Water-soluble polymer- Examples of water-soluble polymers include natural products such as guar gum, sodium chondroitin sulfate, hyaluronic acid, gum arabic, and carrageenan, semi-synthetic products such as methylcellulose, hydroxyethylcellulose, and carboxymethylcellulose, and synthetic systems such as carboxyvinyl polymer. Can be mentioned.
- the manufacturing method of a well-known candle can be utilized.
- the wax composition for candles of the present invention is melted at 50 to 100 ° C. and stirred and mixed, and then by a molding method, dipping method, rolling method, pressing method, etc., preferably at 40 ° C. or less, using a combustion core. More preferably, the candle can be produced by cooling to 0 to 40 ° C., more preferably 10 to 40 ° C.
- the present invention also provides a candle having the candle wax composition thus obtained and a combustion wick.
- the candle of the present invention preferably has a penetration (unit: 10 ⁇ 1 mm) of 1 to 9 measured according to the following method from the viewpoint of suppressing cracking and increasing moldability, and preferably 1 to 4. More preferably, it is more preferably 1 to 3, more preferably 1 to 2.5, and particularly preferably 1.5 to 2.5. (Measurement method of penetration) In accordance with JIS K2235, the length (mm) that the needle has entered when the needle is inserted for 5 seconds at a load of 100 g at 25 ° C. is measured, and the value 10 times that value is defined as the “needle penetration”.
- Synthesis Example 1 Synthesis of 2-chlorodimethylsilylindene Under a nitrogen stream, 50 ml of THF (tetrahydrofuran) and 2.5 g (41 mmol) of magnesium were added to a 1 L three-necked flask. 1 ml was added and stirred for 30 minutes to activate the magnesium. After stirring, the solvent was extracted and 50 ml of THF was newly added. A solution of 5.0 g (25.6 mmol) of 2-bromoindene in THF (200 ml) was added dropwise thereto over 2 hours.
- THF tetrahydrofuran
- lithium salt (6.97 mmol) of (1,2′-dimethylsilylene) (2,1′-dimethylsilylene) bis (indene) was dissolved in 50 ml of THF, and 2.1 ml of iodomethyltrimethylsilane at room temperature ( 14.2 mmol) was slowly added dropwise and stirred for 12 hours.
- the solvent was distilled off, and 50 ml of ether was added, followed by washing with a saturated ammonium chloride solution.
- TMS represents a trimethylsilyl group.
- ⁇ Production Example 2 Production of higher ⁇ -olefin copolymer 2 having side chain crystallinity An ⁇ -olefin mixture having a carbon number of 20, 22, and 24 [42:37:21 (molar ratio) was added to a heat-dried 1 L autoclave.
- ⁇ Production Example 4 Production of higher ⁇ -olefin homopolymer 4 having side chain crystallinity
- synthesis example (1,1′-SiMe 2 SiMe 2 ) (2,2′-SiMe 2 ) bis (indenyl) zirconium dichloride 1 ⁇ mol obtained in 4 and dimethylanilinium tetrakispentafluorophenylborate [component (b-1)] 4 ⁇ mol
- 0.05 MPa of hydrogen was further introduced, and polymerization was performed at a polymerization temperature of 90 ° C.
- the ber 103, the ber 260, and the ber 343 all have a hyper-branch structure.
- ⁇ After 10 minutes, the size of the flame is almost the same as the initial level of ignition, and even after 30 minutes, it is not likely to disappear at all. ⁇ : After 10 minutes, the size of the flame is similar to that at the beginning of ignition, and after 30 minutes, the flame is small, but the state of the flame is stable. X: The flame has already become small after 15 minutes, and it is in a state where it is likely to disappear.
- the smaller the value, the smaller the roughness and the surface gloss. (Appearance evaluation method) The candle was visually observed and evaluated according to the following evaluation criteria. The state of the candle obtained in each example is shown in FIGS. ⁇ : The candle has a pattern (mottled pattern). X: The candle has no pattern.
- the candles obtained by the present invention are less prone to cracking, have high moldability, are excellent in burning sustainability and perfume diffusibility, and are excellent in surface gloss.
- vegetable wax was utilized as (A) component, it was excellent also in combustibility.
- the candles obtained in Examples 7 to 10 to which a pigment has been added have an excellent appearance.
- the external appearance of a candle can be made favorable, without adding liquid oil at normal temperature.
- none of the comparative examples satisfies all of moldability, burning sustainability, perfume diffusivity, surface glossiness and appearance, and there remains a problem in using as a candle.
- Comparative Examples 7 and 8 have a high penetration, because (1) the ber 103 and the ber 206 also contain low molecular weight components because of the wide molecular weight distribution, and ( 2) Since the ber 103 and the ber 206 have a hyperbranch structure and a high acid value, it is considered that the compatibility with the paraffin wax is insufficient, and thus there is a poor dispersion and a soft part exists. I guess that.
- a degreased paper was laid on an aluminum pan (aluminum frying pan), and a cylindrical molded product was placed thereon and kept at 35 ° C. for 24 hours.
- the oil bleed amount (unit: g) was measured by subtracting the weight of the cylindrical molded product before heating from the weight of the subsequent degreased paper. The smaller the value, the less oil bleed, that is, the better the property of keeping the fragrance inside the candle.
- the state of the surface of the candle left at 35 ° C. for 2 days was visually observed and evaluated according to the following evaluation criteria. ⁇ : No change on the surface.
- X Oil droplets are observed on the surface. (appearance) The candle was visually observed and evaluated according to the following evaluation criteria.
- FIGS. ⁇ The state of the candle obtained in each example is shown in FIGS. ⁇ : The candle has a pattern (mottled pattern).
- X The candle has no pattern. (Pattern stability) When the temperature for solidification is changed to 35 ° C. and a candle is produced, “ ⁇ ” is used when a pattern is formed in the same manner as when it is cooled to 20 ° C. and solidified, and “X” is displayed when no pattern is formed. " When it is ⁇ , the pattern expression does not depend on the production conditions, and it can be said that the pattern expression is highly stable.
- the candle obtained by the present invention is excellent in fragrance diffusibility, has a small amount of oil bleed, has a high fragrance sustainability, and does not impair the appearance, and further exhibits a pattern, particularly manufactured. It can be seen that the pattern can be presented stably without depending on the conditions. Comparing Example 11 with Comparative Example 18 and Example 12 with Comparative Example 19, it can be seen that Comparative Examples 18 and 19 are inferior in fragrance diffusibility and at the same time have a large amount of oil bleed. Further, when Example 13 and Comparative Example 20 are compared, the amount of oil bleed in Comparative Example 20 is slightly inferior, but oil droplets are observed on the surface of the candle left at 35 ° C. for 2 days. It turns out that the appearance of is damaged.
- the wax composition of the present invention is highly resistant to cracking and has high moldability. Furthermore, since it is excellent in burning sustainability, perfume diffusibility, and surface glossiness, has an excellent appearance when made into a candle, and has a small amount of oil bleed, it is useful for candles. Furthermore, the wax composition of the present invention is useful for an aroma candle by containing a fragrance, and further a dye or a pigment.
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Abstract
L'invention propose : une composition de cire pour une bougie; et une bougie qui comprend la composition de cire et une mèche. Même lorsque n'importe quel composant de cire est utilisé, la composition de cire est moins susceptible à un craquage et présente une excellente aptitude au moulage, une excellente durée de combustion, une excellente diffusion d'arôme et une excellente brillance de surface. Lorsqu'elle est moulée en une bougie, la composition de cire assure un excellent aspect de surface et provoque peu d'exsudation d'huile. De manière spécifique, l'invention propose une composition de cire pour une bougie et une bougie qui comprend la composition de cire et une mèche, ladite composition de cire étant une composition qui comprend (A) une cire et (B) un polymère seul ou copolymère cristallin à chaîne latérale préparé à l'aide d'une α-oléfine supérieure ayant au moins 10 atomes de carbone et qui est caractérisée en ce que le rapport en teneur en masse de composant (A) : composant (B) est de 81:19 à 99:0,01.
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN113425880A (zh) * | 2021-04-29 | 2021-09-24 | 河北古城香业集团股份有限公司 | 一种环保型无烟燃香及制备方法 |
US20220178761A1 (en) * | 2020-12-08 | 2022-06-09 | Temptime Corporation | Time-temperature exposure indicator with delayed threshold response |
Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
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JP2002508436A (ja) * | 1997-12-17 | 2002-03-19 | エス.シー. ジョンソン アンド サン、インコーポレイテッド | エアフレッシュナ先細状蝋燭製品 |
JP2002527559A (ja) * | 1998-10-12 | 2002-08-27 | クラリアント・インターナシヨナル・リミテツド | 着色、成形された固形ワックス物品 |
-
2012
- 2012-06-22 WO PCT/JP2012/065998 patent/WO2012176881A1/fr active Application Filing
Patent Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
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JP2002508436A (ja) * | 1997-12-17 | 2002-03-19 | エス.シー. ジョンソン アンド サン、インコーポレイテッド | エアフレッシュナ先細状蝋燭製品 |
JP2002527559A (ja) * | 1998-10-12 | 2002-08-27 | クラリアント・インターナシヨナル・リミテツド | 着色、成形された固形ワックス物品 |
Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US20220178761A1 (en) * | 2020-12-08 | 2022-06-09 | Temptime Corporation | Time-temperature exposure indicator with delayed threshold response |
US12140480B2 (en) * | 2020-12-08 | 2024-11-12 | Temptime Corporation | Time-temperature exposure indicator with delayed threshold response |
CN113425880A (zh) * | 2021-04-29 | 2021-09-24 | 河北古城香业集团股份有限公司 | 一种环保型无烟燃香及制备方法 |
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