JP6291732B2 - 複合粉体分散体の製造方法 - Google Patents
複合粉体分散体の製造方法 Download PDFInfo
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- JP6291732B2 JP6291732B2 JP2013133749A JP2013133749A JP6291732B2 JP 6291732 B2 JP6291732 B2 JP 6291732B2 JP 2013133749 A JP2013133749 A JP 2013133749A JP 2013133749 A JP2013133749 A JP 2013133749A JP 6291732 B2 JP6291732 B2 JP 6291732B2
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- GCLGEJMYGQKIIW-UHFFFAOYSA-H sodium hexametaphosphate Chemical compound [Na]OP1(=O)OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])O1 GCLGEJMYGQKIIW-UHFFFAOYSA-H 0.000 description 1
- 235000019982 sodium hexametaphosphate Nutrition 0.000 description 1
- 239000001540 sodium lactate Substances 0.000 description 1
- 229940005581 sodium lactate Drugs 0.000 description 1
- 235000011088 sodium lactate Nutrition 0.000 description 1
- NNMHYFLPFNGQFZ-UHFFFAOYSA-M sodium polyacrylate Chemical compound [Na+].[O-]C(=O)C=C NNMHYFLPFNGQFZ-UHFFFAOYSA-M 0.000 description 1
- 235000019830 sodium polyphosphate Nutrition 0.000 description 1
- 229940035044 sorbitan monolaurate Drugs 0.000 description 1
- 235000011071 sorbitan monopalmitate Nutrition 0.000 description 1
- 239000001570 sorbitan monopalmitate Substances 0.000 description 1
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- 229960002920 sorbitol Drugs 0.000 description 1
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- 229910052712 strontium Inorganic materials 0.000 description 1
- CIOAGBVUUVVLOB-UHFFFAOYSA-N strontium atom Chemical compound [Sr] CIOAGBVUUVVLOB-UHFFFAOYSA-N 0.000 description 1
- 229920005792 styrene-acrylic resin Polymers 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
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- 238000000967 suction filtration Methods 0.000 description 1
- 150000005846 sugar alcohols Polymers 0.000 description 1
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- 229920001059 synthetic polymer Polymers 0.000 description 1
- 239000003760 tallow Substances 0.000 description 1
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- LRBQNJMCXXYXIU-NRMVVENXSA-N tannic acid Chemical compound OC1=C(O)C(O)=CC(C(=O)OC=2C(=C(O)C=C(C=2)C(=O)OC[C@@H]2[C@H]([C@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)[C@@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)[C@@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)O2)OC(=O)C=2C=C(OC(=O)C=3C=C(O)C(O)=C(O)C=3)C(O)=C(O)C=2)O)=C1 LRBQNJMCXXYXIU-NRMVVENXSA-N 0.000 description 1
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- 239000001577 tetrasodium phosphonato phosphate Substances 0.000 description 1
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- OULAJFUGPPVRBK-UHFFFAOYSA-N tetratriacontyl alcohol Natural products CCCCCCCCCCCCCCCCCCCCCCCCCCCCCCCCCCO OULAJFUGPPVRBK-UHFFFAOYSA-N 0.000 description 1
- 238000005979 thermal decomposition reaction Methods 0.000 description 1
- 239000002562 thickening agent Substances 0.000 description 1
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- 239000004408 titanium dioxide Substances 0.000 description 1
- 229940042585 tocopherol acetate Drugs 0.000 description 1
- VZCYOOQTPOCHFL-UHFFFAOYSA-N trans-butenedioic acid Natural products OC(=O)C=CC(O)=O VZCYOOQTPOCHFL-UHFFFAOYSA-N 0.000 description 1
- LOIYMIARKYCTBW-OWOJBTEDSA-N trans-urocanic acid Chemical compound OC(=O)\C=C\C1=CNC=N1 LOIYMIARKYCTBW-OWOJBTEDSA-N 0.000 description 1
- PHYFQTYBJUILEZ-IUPFWZBJSA-N triolein Chemical class CCCCCCCC\C=C/CCCCCCCC(=O)OCC(OC(=O)CCCCCCC\C=C/CCCCCCCC)COC(=O)CCCCCCC\C=C/CCCCCCCC PHYFQTYBJUILEZ-IUPFWZBJSA-N 0.000 description 1
- SVETUDAIEHYIKZ-IUPFWZBJSA-N tris[(z)-octadec-9-enyl] phosphate Chemical compound CCCCCCCC\C=C/CCCCCCCCOP(=O)(OCCCCCCCC\C=C/CCCCCCCC)OCCCCCCCC\C=C/CCCCCCCC SVETUDAIEHYIKZ-IUPFWZBJSA-N 0.000 description 1
- 239000006097 ultraviolet radiation absorber Substances 0.000 description 1
- 235000015112 vegetable and seed oil Nutrition 0.000 description 1
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- 239000008158 vegetable oil Substances 0.000 description 1
- 229920002554 vinyl polymer Polymers 0.000 description 1
- 239000011653 vitamin D2 Substances 0.000 description 1
- MECHNRXZTMCUDQ-RKHKHRCZSA-N vitamin D2 Chemical compound C1(/[C@@H]2CC[C@@H]([C@]2(CCC1)C)[C@H](C)/C=C/[C@H](C)C(C)C)=C\C=C1\C[C@@H](O)CCC1=C MECHNRXZTMCUDQ-RKHKHRCZSA-N 0.000 description 1
- 235000001892 vitamin D2 Nutrition 0.000 description 1
- 239000001993 wax Substances 0.000 description 1
- 229920001285 xanthan gum Polymers 0.000 description 1
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- HEBKCHPVOIAQTA-SCDXWVJYSA-N xylitol Chemical compound OC[C@H](O)[C@@H](O)[C@H](O)CO HEBKCHPVOIAQTA-SCDXWVJYSA-N 0.000 description 1
- 229960002675 xylitol Drugs 0.000 description 1
- XSMMCTCMFDWXIX-UHFFFAOYSA-N zinc silicate Chemical compound [Zn+2].[O-][Si]([O-])=O XSMMCTCMFDWXIX-UHFFFAOYSA-N 0.000 description 1
- 235000019352 zinc silicate Nutrition 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
- 229910052726 zirconium Inorganic materials 0.000 description 1
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- Inks, Pencil-Leads, Or Crayons (AREA)
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Description
上記撥水性有機化合物は、シリコーンオイル、アルキルシラン、アルキルチタネート、アルキルアルミネート、金属石鹸、アミノ酸、及び、アミノ酸塩からなる群より選択される少なくとも一種であることが好ましい。
上記無機粉体は、紫外線遮蔽効果を有する無機粉体であることが好ましい。
上記無機粉体は、酸化亜鉛、酸化チタン、酸化鉄及び酸化セリウムからなる群より選択される少なくとも一種であることが好ましい。
本発明は、撥水性有機化合物からなる第一の被覆層を有する無機粉体上に、ケイ素酸化物、ケイ素酸化物の水和物、アルミニウムの酸化物及びアルミニウムの水酸化物からなる群から選択される少なくとも1種の化合物からなる第二の被覆層を湿式法で形成することによって複合粉体を得る工程(1)、前記第二の被覆層の形成後、粉体を乾燥させる工程を経ることなく、複合粉体と液体媒体が混和した含溶媒ケーキとする工程(2)、及び、前記工程(2)によって得られた含溶媒ケーキを湿潤状態のままで水と混合し水分散体とする工程(3)によって得られた水分散体を配合することによって得られたことを特徴とするインキ組成物でもある。
これに対して、本発明の分散体の製造方法によって得られた分散体では、第二の被覆層である含水無機酸化物層、例えばシリカの亀裂が起きないこと、また乾燥凝集をしていなことからネットワークを作る力も弱いために低粘度の分散体になったと推測される。また、乾燥工程を経ないために、使用エネルギー的にも優位である。
NHLB=(E+P)/5
(NHLB:HLB値、E:ポリオキシエチレン部の分散剤分子全体に対する重量%、P:多価アルコール部の分散剤分子全体に対する重量%)
純水500mLにポリエーテル変性シリコーン(KF−6043:信越化学工業製:HLB14.5)を20g入れ、更にハイドロゲンジメチコン4%で処理された酸化亜鉛(FINEX−30S−LPT、酸化亜鉛粒子径35nm)100gを加えて、混合分散させた。この分散液にケイ酸Na水溶液(SiO2:403.9g/L、Na2O:130.7g/L)を27.5ml(SiO2量として11.1g、処理後の粉体全体の10重量%)添加し、20分以上撹拌した。その後、液温を70℃にし、希硫酸を一定量滴下して中和を行なった。この中和の際にpH8.5以上での状態が90分以上であるように硫酸滴下量を調整し、pH6.5まで中和を行なった。中和終了後、液温70℃のまま、1時間熟成した。その後、濾過、水洗し、ウェットケーキを得た。このウェットケーキの固型分量を赤外線水分計(sartrius社製MA−35)で測定すると、74.7重量%であった。このウェットケーキ67g(固形分としては50g)と純水33gをマヨネーズ瓶に入れ、更にφ0.5mmジルコニアビーズ100gを投入し、ペイントシェーカーで60分間分散し、水分散体1を得た。
純水500mLにポリエーテル変性シリコーン(KF−6011:信越化学工業製:HLB14.5)を20g入れ、更にハイドロゲンジメチコン7%で処理された酸化亜鉛(FINEX−50−LPT、酸化亜鉛粒子径20nm)100gを加えて、混合分散させた。この分散液にケイ酸Na水溶液(SiO2:403.9g/L、Na2O:130.7g/L)を27.5ml(SiO2量として11.1g、処理後の粉体全体の10重量%)添加し、20分以上撹拌した。その後、液温を75℃にし、希硫酸を一定量滴下して中和を行なった。この中和の際にpH8.5以上での状態が90分以上であるように硫酸滴下量を調整し、pH6.5まで中和を行なった。中和終了後、液温75℃のまま、1時間熟成した。その後、濾過、水洗し、ウェットケーキを得た。このウェットケーキの固型分量を赤外線水分計(sartrius社製MA−35)で測定すると、55.7重量%であった。このウェットケーキ72g(固形分としては40g)と純水18g、1,3−ブチレングリコール10gをマヨネーズ瓶に入れ、更にφ0.5mmジルコニアビーズ100gを投入し、ペイントシェーカーで60分間分散し、水分散体2を得た
実施例1で得たウェットケーキを120℃で12時間乾燥することにより、乾燥粉体を得た。この乾燥粉体50gと純水50gをマヨネーズ瓶に入れ、更にφ0.5mmジルコニアビーズ100gを投入し、ペイントシェーカーで60分間分散し、水分散体3を得た。
得られた水分散体を確認した結果、水分散体3は粉体が水に馴染んではいるものの、クリーム状になっており、自然濾過ではジルコニアビーズの分離も不可能であった。水分散体1は粘度も低く、安定的な水分散体が得られた。25℃でB型粘度計によって測定したジルコニアビーズ分離後の分散体1の粘度は、30mPa・sで、同じくジルコニアビーズ分離後の分散体2の粘度は550mPa・sであった。吸引濾過でジルコニアビーズ分離して同様に測定した分散体3の粘度は、10000mPa・s以上であった。
Claims (15)
- 撥水性有機化合物からなる第一の被覆層を有する無機粉体上に、ケイ素酸化物、ケイ素酸化物の水和物、アルミニウムの酸化物及びアルミニウムの水酸化物からなる群から選択される少なくとも1種の化合物からなる第二の被覆層を湿式法で形成することによって複合粉体を得る工程(1)、
前記第二の被覆層の形成後、粉体を乾燥させる工程を経ることなく、複合粉体と液体媒体が混和した含溶媒ケーキとする工程(2)、
及び、前記工程(2)によって得られた含溶媒ケーキを湿潤状態のままで水と混合し水分散体とする工程(3)
によって得られた前記水分散体を配合することによって得られたことを特徴とする化粧料。 - 含溶媒ケーキは、水を30〜90重量%含有する含水ケーキである請求項1記載の化粧料。
- 撥水性有機化合物は、シリコーンオイル、アルキルシラン、アルキルチタネート、アルキルアルミネート、金属石鹸、アミノ酸、及び、アミノ酸塩からなる群より選択される少なくとも一種である請求項1又は2記載の化粧料。
- 無機粉体は、紫外線遮蔽効果を有する無機粉体である請求項1,2又は3記載の化粧料。
- 無機粉体は、酸化亜鉛、酸化チタン、酸化鉄及び酸化セリウムからなる群より選択される少なくとも一種である請求項1,2,3又は4記載の化粧料。
- 撥水性有機化合物からなる第一の被覆層を有する無機粉体上に、ケイ素酸化物、ケイ素酸化物の水和物、アルミニウムの酸化物及びアルミニウムの水酸化物からなる群から選択される少なくとも1種の化合物からなる第二の被覆層を湿式法で形成することによって複合粉体を得る工程(1)、
前記第二の被覆層の形成後、粉体を乾燥させる工程を経ることなく、複合粉体と液体媒体が混和した含溶媒ケーキとする工程(2)、
及び、前記工程(2)によって得られた含溶媒ケーキを湿潤状態のままで水と混合し水分散体とする工程(3)
によって得られた前記水分散体を配合することによって得られたことを特徴とする塗料組成物。 - 含溶媒ケーキは、水を30〜90重量%含有する含水ケーキである請求項6記載の塗料組成物。
- 撥水性有機化合物は、シリコーンオイル、アルキルシラン、アルキルチタネート、アルキルアルミネート、金属石鹸、アミノ酸、及び、アミノ酸塩からなる群より選択される少なくとも一種である請求項6又は7記載の塗料組成物。
- 無機粉体は、紫外線遮蔽効果を有する無機粉体である請求項6,7又は8記載の塗料組成物。
- 無機粉体は、酸化亜鉛、酸化チタン、酸化鉄及び酸化セリウムからなる群より選択される少なくとも一種である請求項6,7,8又は9記載の塗料組成物。
- 撥水性有機化合物からなる第一の被覆層を有する無機粉体上に、ケイ素酸化物、ケイ素酸化物の水和物、アルミニウムの酸化物及びアルミニウムの水酸化物からなる群から選択される少なくとも1種の化合物からなる第二の被覆層を湿式法で形成することによって複合粉体を得る工程(1)、
前記第二の被覆層の形成後、粉体を乾燥させる工程を経ることなく、複合粉体と液体媒体が混和した含溶媒ケーキとする工程(2)、
及び、前記工程(2)によって得られた含溶媒ケーキを湿潤状態のままで水と混合し水分散体とする工程(3)
によって得られた前記水分散体を配合することによって得られたことを特徴とするインキ組成物。 - 含溶媒ケーキは、水を30〜90重量%含有する含水ケーキである請求項11記載のインキ組成物。
- 撥水性有機化合物は、シリコーンオイル、アルキルシラン、アルキルチタネート、アルキルアルミネート、金属石鹸、アミノ酸、及び、アミノ酸塩からなる群より選択される少なくとも一種である請求項11又は12記載のインキ組成物。
- 無機粉体は、紫外線遮蔽効果を有する無機粉体である請求項11,12又は13記載のインキ組成物。
- 無機粉体は、酸化亜鉛、酸化チタン、酸化鉄及び酸化セリウムからなる群より選択される少なくとも一種である請求項11,12,13又は14記載のインキ組成物。
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