TWI429717B - 碳黑、彼之製法及用於實施此方法之裝置 - Google Patents
碳黑、彼之製法及用於實施此方法之裝置 Download PDFInfo
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- TWI429717B TWI429717B TW096128438A TW96128438A TWI429717B TW I429717 B TWI429717 B TW I429717B TW 096128438 A TW096128438 A TW 096128438A TW 96128438 A TW96128438 A TW 96128438A TW I429717 B TWI429717 B TW I429717B
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- carbon black
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- 239000006229 carbon black Substances 0.000 title claims description 56
- 238000000034 method Methods 0.000 title claims description 14
- 238000001816 cooling Methods 0.000 claims description 28
- 239000007789 gas Substances 0.000 claims description 16
- 239000000203 mixture Substances 0.000 claims description 14
- 238000009826 distribution Methods 0.000 claims description 11
- 238000000576 coating method Methods 0.000 claims description 10
- 239000011248 coating agent Substances 0.000 claims description 9
- 239000012159 carrier gas Substances 0.000 claims description 8
- 239000000463 material Substances 0.000 claims description 4
- 239000002994 raw material Substances 0.000 claims description 4
- 239000012763 reinforcing filler Substances 0.000 claims description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical group [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 3
- 239000007788 liquid Substances 0.000 claims description 3
- 238000004519 manufacturing process Methods 0.000 claims description 3
- 239000000049 pigment Substances 0.000 claims description 3
- 239000010426 asphalt Substances 0.000 claims description 2
- 239000004566 building material Substances 0.000 claims description 2
- 239000004567 concrete Substances 0.000 claims description 2
- 239000000123 paper Substances 0.000 claims description 2
- 239000004033 plastic Substances 0.000 claims description 2
- 229920003023 plastic Polymers 0.000 claims description 2
- 239000000326 ultraviolet stabilizing agent Substances 0.000 claims description 2
- 239000003795 chemical substances by application Substances 0.000 claims 1
- 239000003973 paint Substances 0.000 claims 1
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 18
- 238000005259 measurement Methods 0.000 description 10
- 239000003570 air Substances 0.000 description 8
- 239000000243 solution Substances 0.000 description 8
- 239000003921 oil Substances 0.000 description 7
- 239000000523 sample Substances 0.000 description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 5
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 3
- 239000000654 additive Substances 0.000 description 3
- 239000006185 dispersion Substances 0.000 description 3
- 239000012530 fluid Substances 0.000 description 3
- 239000011521 glass Substances 0.000 description 3
- 239000001257 hydrogen Substances 0.000 description 3
- 229910052739 hydrogen Inorganic materials 0.000 description 3
- 239000000976 ink Substances 0.000 description 3
- OFBQJSOFQDEBGM-UHFFFAOYSA-N n-pentane Natural products CCCCC OFBQJSOFQDEBGM-UHFFFAOYSA-N 0.000 description 3
- 238000002360 preparation method Methods 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- 210000003523 substantia nigra Anatomy 0.000 description 3
- 238000012546 transfer Methods 0.000 description 3
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonium chloride Substances [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 description 2
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- ATUOYWHBWRKTHZ-UHFFFAOYSA-N Propane Chemical compound CCC ATUOYWHBWRKTHZ-UHFFFAOYSA-N 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 229920004890 Triton X-100 Polymers 0.000 description 2
- 239000013504 Triton X-100 Substances 0.000 description 2
- 235000011114 ammonium hydroxide Nutrition 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- -1 coatings Substances 0.000 description 2
- SNRUBQQJIBEYMU-UHFFFAOYSA-N dodecane Chemical compound CCCCCCCCCCCC SNRUBQQJIBEYMU-UHFFFAOYSA-N 0.000 description 2
- 239000012632 extractable Substances 0.000 description 2
- 239000003517 fume Substances 0.000 description 2
- 229930195733 hydrocarbon Natural products 0.000 description 2
- 150000002430 hydrocarbons Chemical class 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Chemical compound [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 description 2
- 150000003839 salts Chemical class 0.000 description 2
- 238000004448 titration Methods 0.000 description 2
- 239000003039 volatile agent Substances 0.000 description 2
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 description 1
- OTMSDBZUPAUEDD-UHFFFAOYSA-N Ethane Chemical compound CC OTMSDBZUPAUEDD-UHFFFAOYSA-N 0.000 description 1
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 description 1
- 239000005977 Ethylene Substances 0.000 description 1
- VCUFZILGIRCDQQ-KRWDZBQOSA-N N-[[(5S)-2-oxo-3-(2-oxo-3H-1,3-benzoxazol-6-yl)-1,3-oxazolidin-5-yl]methyl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C1O[C@H](CN1C1=CC2=C(NC(O2)=O)C=C1)CNC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F VCUFZILGIRCDQQ-KRWDZBQOSA-N 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 238000011481 absorbance measurement Methods 0.000 description 1
- 238000009825 accumulation Methods 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 239000000443 aerosol Substances 0.000 description 1
- HSFWRNGVRCDJHI-UHFFFAOYSA-N alpha-acetylene Natural products C#C HSFWRNGVRCDJHI-UHFFFAOYSA-N 0.000 description 1
- 239000012080 ambient air Substances 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 239000012496 blank sample Substances 0.000 description 1
- 239000001273 butane Substances 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 1
- 239000003638 chemical reducing agent Substances 0.000 description 1
- 239000000567 combustion gas Substances 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 230000003750 conditioning effect Effects 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 239000002826 coolant Substances 0.000 description 1
- 230000001186 cumulative effect Effects 0.000 description 1
- 125000002534 ethynyl group Chemical group [H]C#C* 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- IJDNQMDRQITEOD-UHFFFAOYSA-N n-butane Chemical compound CCCC IJDNQMDRQITEOD-UHFFFAOYSA-N 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000003348 petrochemical agent Substances 0.000 description 1
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N phenol group Chemical group C1(=CC=CC=C1)O ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 1
- 239000004810 polytetrafluoroethylene Substances 0.000 description 1
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 1
- 229910000027 potassium carbonate Inorganic materials 0.000 description 1
- 239000001294 propane Substances 0.000 description 1
- 238000011002 quantification Methods 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 239000011541 reaction mixture Substances 0.000 description 1
- 239000012488 sample solution Substances 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000002893 slag Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000006228 supernatant Substances 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 238000011144 upstream manufacturing Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
- C09C1/44—Carbon
- C09C1/48—Carbon black
- C09C1/52—Channel black ; Preparation thereof
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
- C09C1/44—Carbon
- C09C1/46—Graphite
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K3/04—Carbon
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
- C09C1/44—Carbon
- C09C1/48—Carbon black
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/50—Agglomerated particles
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/51—Particles with a specific particle size distribution
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/12—Surface area
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/60—Optical properties, e.g. expressed in CIELAB-values
- C01P2006/66—Hue (H*)
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
- Y10T428/00—Stock material or miscellaneous articles
- Y10T428/29—Coated or structually defined flake, particle, cell, strand, strand portion, rod, filament, macroscopic fiber or mass thereof
- Y10T428/2982—Particulate matter [e.g., sphere, flake, etc.]
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- Chemical Kinetics & Catalysis (AREA)
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- Polymers & Plastics (AREA)
- Pigments, Carbon Blacks, Or Wood Stains (AREA)
- Inks, Pencil-Leads, Or Crayons (AREA)
- Ink Jet (AREA)
- Paints Or Removers (AREA)
Description
本發明係關於一種碳黑、碳黑之製法及用於實施此方法之裝置。
DE 2404536揭示一種製造具有低的可萃取物含量的氣黑(gas blacks)的方法,其中使用富含氫之混合物以作為碳黑油蒸氣之載體氣體,且收集沉積於冷卻輥上之碳黑。這些氣黑具有少於0.100重量%之可萃取物含量。
另外,WO 2005/033217揭示未篩選、未處理之碳黑,其具有小於或等於6.0之酸鹼值,在點然後有小於或等於0.1%之殘留物及小於或等於200 ppm之5微米之篩分殘留物。這些黑質是藉以下方法步驟予以產製:藉熱傳導或輻射將火焰所生之熱除去,形成薄的氣體邊界層,及加速或擴張藉火焰及邊界層所形成之流動。
已知黑質之缺點是塗覆應用時差的色相貢獻。
本發明之目的是要提供一種特徵為塗覆應用時具有高度正面色相貢獻的碳黑。本發明之其他目的是要提供一種盡可能地除去火焰所生之熱,且不使所得之黑質累積在冷的表面上之方法。
本發明提供一種碳黑,其特徵在於聚集體尺寸分布之(d90
-d10
)/d50
比例為小於或等於1.1,較佳是小於0.8,更佳是小於0.65。
本發明之碳黑可以具有大於50毫莫耳/公斤,較佳是大於100毫莫耳/公斤,更佳是大於120毫莫耳/公斤之表面氧化物含量。
本發明之碳黑的聚集體尺寸分布之半高全寬值(FWHM)對Dmode
之比例可以是小於或等於0.6,較佳為小於0.58,更佳為小於0.56。
本發明之碳黑可以是氣黑。
本發明之碳黑的酸鹼值可以是小於7.0,較佳是小於6.0,更佳是小於5.0。
本發明之碳黑可以具有20-300平方米/克,較佳具有50-220平方米/克,更佳具有70-200平方米/克之STSA值。
本發明之碳黑可以具有2.0-20.0%,較佳具有3.0-12%,更佳具有4.0-9.0%之揮發物含量。
本發明之碳黑可以具有90-180%,較佳具有105-106%,更佳具有120-150%之色調。
本發明另外提供一種產製本發明之碳黑之方法,其特徵在於視需要摻合一包含載體氣體及碳黑原料的氣體混合物與熱空氣,使該氣體混合物通入燃燒器管中,在燃燒器管開口處燃燒氣體混合物,連同從外部被自由抽吸拉引之周圍空氣將火焰抽吸經過一冷卻之變窄的間隙,且進行冷卻,該冷卻之變窄的間隙具有1-100,較佳具有5-50,更佳具有10-40之高度(h)對寬度(b)之比例,寬度是基於間隙之頂邊,寬度(b)是0.5至10毫米,較佳是1至5毫米,且在間隙之最窄點的流速是10-200米/秒,較佳是15-150米/秒,更佳是20-100米/秒。
可以由操作之氣體體積對間隙面積的比例計算流速。操作之氣體體積是藉由風扇抽吸取出之氣體體積。間隙面積是由間隙寬度b及冷卻之變窄間隙的頂邊A1
A2
的乘積所給定的。
用於變窄之間隙的冷卻劑可以是水、空氣、蒸氣及熱傳油。
在商業上慣用之薄膜型蒸發器中,碳黑原料可以被加熱及蒸發。碳黑原料蒸氣藉載體氣流供應至燃燒器管。接近燃燒氣管上游時(例如DE-C 671739中所述的),氣體混合物可以與高達400℃的溫度之熱空氣摻合,且供應至火焰。所產製之碳黑可以在商業上慣用之濾器系統中分離。
所用之碳黑原料可以包含含碳氣體或可蒸發之含碳液體。所用之碳黑原料可以包含烴類,例如乙炔、甲烷、乙烯、乙烷、丙烷、丁烷或戊烷,或碳黑油。碳黑油可以源自石油化學品或碳化學品。所用之碳黑原料可以是烴類及/或碳黑油類之混合物。
氣態或蒸氣化之碳黑原料可以具有高達400℃,較佳具有250-400℃,更佳具有250-350℃之溫度。
可能使用可燃燒氣體,較佳是具有大於50體積%,更佳為大於60體積%之氫分率的氣體混合物以作為載體氣體。
為要防止冷凝,載體氣體溫度及熱空氣溫度可以至少與氣態或蒸氣化之碳黑原料溫度相當。
圖1顯示裝置之概略構造,其中參考符號具有以下意義:A1
A2
,A1’
,A2’
:冷卻之變窄間隙的頂邊,B1
,B2
,B1’
,B2’
:冷卻之變窄間隙的底邊,A1’
,A1
,A2’
,A2
:冷卻之變窄間隙的最窄點,b:冷卻間隙之寬度=A1’
,A1
或A2’
,A2
,B1’
,B1
,B2’
,B2
:冷卻之變窄間隙的最寬點,h:在上區中冷卻之變窄間隙的高度,h’:未冷卻或冷卻之傾斜會合側壁之高度,C1
B1
B2
C2
:未冷卻或冷卻之傾斜會合側壁,C1’
B1’
B2’
C2’
:未冷卻或冷卻之傾斜會合側壁,D1’
,D1
:垂直安置之裝置的寬度,E:高度可調節之燃燒器管,E,A1
A1’
:燃燒器空間
α角可以是70°至89°,較佳是80°至89°,更佳是83°至88°。
高度h’可以是0至250毫米,較佳是100至250毫米,更佳是140至180毫米。
垂直安置之裝置的寬度(C1’
C1
=D1’
D1
)可達100至500毫米,較佳是150至210毫米。
排氣通風櫥可以直接在間隙之後且可以連接至抽吸拉引扇。
裝置可以是不鏽鋼製以抑制典型的雜質(硬渣)。在本發明方法之情況中,無需轉動之冷卻輥。燃燒器管之火焰可被抽吸經過一冷卻之變窄間隙並冷卻。
如本發明之裝置的剖面圖式所示(圖1),間隙可延伸過裝置之全部長度,且可以平行於燃燒器管,亦即彼可以較佳集中安置於燃燒器管之上。垂直安置之裝置的側壁起初可以彼此平行行進(C1
D1
D2
C2
或C1’
D1’
D2’
C2’
),而後彼此傾斜會合(C1
B1
B2
C2
或C1’
B1’
B2’
C2’
),且結束於冷卻之變窄間隙(A1
B1
B2
A2
或A1’
B1’
B2’
A2’
)。
與冷卻之變窄間隙相關之燃燒器空間是可變的。可以提供此調節設備以使得以實現最佳之燃燒器高度。
在裝置之圓錐形會合區(h’)中,側壁可能是水冷卻的。然而在此區(h’)中,此僅可保護材料免於遭受火焰之溫度,因為彼僅處於上區(h),對應地稱為冷卻間隙,是欲冷卻反應混合物之處。
可以設計冷卻間隙之構造以使在產生冷卻間隙處之層狀邊界層後可以抑制碳黑之累積。
可以添加添加劑至碳黑油。添加劑可以是鹽於水、醇、油或其混合物中所成之溶液。添加劑可以轉變成氣溶膠。所用之鹽較佳是碳酸鉀。
本發明另外提供一種用於實施本發明方法的裝置,其具有一燃燒器及一正對著火焰被導引的方向之冷卻用表面,其特徵在於該冷卻之變窄的間隙具有1-100,較佳具有5-50,更佳具有10-40之高度(h)對寬度(b)之比例,寬度是基於間隙之頂邊,寬度(b)是0.5至10毫米,較佳是1至5毫米且在間隙之最窄之點的流速是10-200米/秒,較佳是15-150米/秒,更佳是20-100米/秒。
可以使用本發明之碳黑以作為非強化用填料、強化用填料、紫外線安定劑、導電黑或顏料。本發明之碳黑可用於橡膠、塑膠、印刷用墨水、液態墨水、噴墨墨水、調色劑、塗覆材料、塗料、紙、瀝青、混凝土及其他建築材料中。本發明之碳黑可用來作為冶金之還原劑。
本發明之碳黑具有可產製具有窄的聚集體尺寸分布之黑質及塗覆應用中絕對色相貢獻(dM)極高之優點。
本發明之方法具有黑質不沉積於冷卻之表面及因此可沉積於裝置外部之優點。
另一優點是:在本發明裝置中,不再有任何轉動之部分,以致能降低資金成本及維護成本,以及不再有輥之黑質與濾器之黑質間之分離,且因此所產生之產物被均質化。再者由於省略機械傳送,可能降低產物中之雜質。
依圖1之實例中所用之本發明之裝置具有177毫米之側壁距離(D1’
D1
)及600毫米之高度(D1
C1
)。在600毫米高度之上,側壁彼此傾斜會合且結束於冷卻之變窄間隙。在以下實例中,此冷卻間隙之長度A1
A2
達2000毫米且高度(h)達50毫米。以下實例中之間隙高度(h’)達159毫米。α角是87°。
酸鹼值依照DIN EN ISO 787-9 20測定酸鹼值。
揮發物依照DIN 53552在950℃下測定揮發物。
BET表面積依照ASTM D-6556-00測定BET表面積。
STSA表面積依照ASTM規格之D-6556-00測定STSA表面積。
色調依照ASTM規格之D-3265測定色調強度。
使用具有紅光二極體之Brookhaven BI-DCP碟式離心機測量聚集體尺寸分布曲線。此裝置是特別發展以用於經由吸收率測量以測定細分固體之聚集體尺寸分布曲線,且配備有自動測量及評估程式以測定聚集體尺寸分布。
為進行測量,首先從200毫升乙醇、5滴氨溶液及0.5克Triton X-100,且以去礦質之水補充成1000毫升以製備分散溶液。另外,從0.5克Triton X-100及5滴氨溶液,且以去礦質之水補充成1000毫升以製備旋轉流體。
隨後20毫升分散溶液添加至20毫克碳黑,於100瓦之超音波(80%脈衝)的冷卻浴中,該碳黑懸浮於該溶液中歷時4.5分鐘。
在開始實際測量前,以每分鐘11 000轉之速度進行離心30分鐘。隨著碟旋轉,注入1毫升之乙醇,而後15毫升之旋轉流體之底層小心地留下。在約1分鐘後,注入250微升之黑色懸浮液,且開始裝置之測量程式,且於離心機中之旋轉流體中加入50微升之十二烷。對每一測量樣品進行二次測定。
而後使用裝置之數學程式以評估原始數據曲線,且對散射光進行校正,並進行自動基線調整。
△D50
值(FWHM)是聚集體尺寸分布曲線在半峰高之寬度。Dmode
值(模態值)是出現率最高之聚集體尺寸(聚集體尺寸分布曲線之最大峰)。d10
、d50
及d90
之值分別是由具有10%、50%及90%之體積分率之累積曲線所決定之聚集體尺寸。
關於碳黑表面上之表面氧化物之鑑定及定量,在此亦即含氧之官能基,例如羧基、乳醇及酚基團:碳黑之起初質量mi
受所預期之表面氧化物之數目所支配。關於起初質量之開始點,可以利用碳黑之揮發物含量(表1)。
表1中所說明之在105℃下乾燥之定量的碳黑精確秤重至0.1毫克且置入玻璃離心管中,且添加25毫升(體積V1
)之0.05 M氫氧化鈉水溶液。離心管中樣品上之空氣被氮氣所代替,且該管嚴格地密封,置入支撐架中,且在轉動機中混合過夜。
在混合程序結束時,內容物傳遞至另一離心管中,且離心至少1分鐘。
10毫升(體積V2
)之上清液藉吸量管吸取出且傳遞至玻璃燒杯,添加20毫升之0.025 m硫酸,且簡單地煮沸該混合物以排除碳酸鹽。
樣品隨後用0.05m氫氧化鈉水溶液後滴定成酸鹼值6.5(酸鹼電極)。所消耗之氫氧化鈉溶液之量是V3
。
對應地製備空白樣品。為測定空白值,同樣地獲得所消耗之NaOH之量(Bl3
)。
以碳黑之起初質量mi
、體積V1-3
及Bl3
為基準,表面氧化物的量G(毫莫耳/公斤)按照以下等式來計算:
在此式中,各符號具有以下意義:mi
:碳黑之起初質量(克),V1
:添加至碳黑之試劑溶液之體積毫升(=25毫升),V2
:藉吸量管所吸取之樣品溶液之體積毫升(=10毫升),V3
:滴定所消耗之氫氧化鈉溶液之量(毫升),Bl3
:空白值滴定所消耗之氫氧化鈉的量(毫升)。
1.試劑之製備
此四種配方之構成成分被混合且保持於適合容器中。
2.黑色塗覆物之製備用以測定黑值My之黑色塗覆物之配方:
首先,塗覆物成分A及B被秤入PTFE燒杯中,而後在105℃下乾燥之碳黑顏料被秤入,且275克鋼珠(直徑=3毫米)被添加以作為研磨介質。最後,樣品在Skandex混合機中分散30分鐘。
在分散程序後,約1-2毫升之黑色塗覆物被取出以供拉伸且施加至載體板使成5公分長及約1公分寬之條狀物。必須小心以確保在塗覆條狀物中無氣泡。膜拉伸棒置於該塗覆條狀物上且均勻地拉伸過該板。產生一個約10公分長及6公分寬之拉伸物。該拉伸物必須被空氣乾燥(在通風櫥中)至少10分鐘。
隨後樣品在乾燥器中130℃下燒烤30分鐘。樣品可以在冷卻之後立即或稍後進行測量。可以使用具有WinQC+軟體之Pausch Q-Color 35裝置進行測量。經由玻璃進行測量。
3.計算3.1.各式及常數3.1.1.與色相無關之黑值My及與色相相關之黑值Mc首先從測量之三刺激值Y(光源D65/10)計算與色相無關之黑值My(等式1):
隨後計算與色相相關之黑值(等式2):
Xn
/Zn
/Yn
(DIN 6174)=以光源及觀察者為基準之座標源之三刺激值(DIN 5033/第7部分,光源D65/10°)Xn
=94.81 Zn
=107.34 Yn
=100.0 X/Y/Z=從樣品之測量所計算之三刺激值。
3.1.2.絕對色相貢獻dM從Mc及My計算絕對色相貢獻dM(等式3):(3)dM=Mc-My
用以產製本發明之碳黑之實例及比較性實例6之各項設定值列於表2中。使用如圖1之裝置。
對於本發明之實例及比較性實例6而言,熱空氣溫度是310℃,且載體氣體之氫含量是92-99體積%。
在表2中所報告之燃燒器空間是燃燒器管之頂邊(換言之,油蒸氣-載體氣體混合物出現之點)與該冷卻之變窄的冷卻間隙之頂邊間的距離。
在隨後之表(表3)中,顯示本發明碳黑及比較性黑質之分析數據。所用之比較性黑質(實例7)是WO 2005/033217之實例3之黑質。
結果顯示:本發明之碳黑(實例1-5)具有(d90
-d10
)/d50
比例為小於或等於1.1之聚集體尺寸分布。本發明之碳黑顯現出大於0.5之dM值及所得之較高之藍色相的優點。
圖1顯示裝置之概略構造。
Claims (6)
- 一種碳黑,其特徵在於聚集體尺寸分布之(d90 -d10 )/d50 比例為小於或等於1.1且半高全寬值(FWHM)對Dmode 之比例為小於或等於0.6,其中該碳黑是氣黑(gas black)。
- 如申請專利範圍第1項之碳黑,其中表面氧化物含量大於50毫莫耳/公斤。
- 一種製造如申請專利範圍第1項之碳黑的方法,其特徵在於視需要摻合一包含載體氣體及碳黑原料的氣體混合物與熱空氣,使該氣體混合物通入燃燒器管中,在燃燒器管開口處燃燒該氣體混合物,將火焰連同從外部被自由抽吸拉引之周圍空氣一起抽吸經過一冷卻之變窄的間隙,且進行冷卻,該冷卻之變窄的間隙具有1-100之高度(h)對寬度(b)之比例,寬度是基於間隙之頂邊,寬度(b)是0.5至10毫米,且在間隙之最窄點的流速是10-200米/秒。
- 一種用於實施如申請專利範圍第3項之方法的裝置,其具有一燃燒器及一正對著火焰被導引的方向之冷卻用表面,其特徵在於該冷卻之變窄的間隙具有1-100之高度(h)對寬度(b)之比例,寬度是基於間隙之頂邊,寬度(b)是0.5至10毫米,且在間隙之最窄之點的流速是10-200米/秒。
- 一種使用如申請專利範圍第1項之碳黑作為非強化用填料、強化用填料、紫外線安定劑、導電黑、顏料或還 原劑之用途。
- 一種使用如申請專利範圍第1項之碳黑於橡膠、塑膠、印刷用墨水、液態墨水、噴墨墨水、調色劑、塗覆材料、塗料、紙、瀝青、混凝土及其他建築材料中之用途。
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-
2006
- 2006-08-07 DE DE102006037079A patent/DE102006037079A1/de not_active Withdrawn
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2007
- 2007-07-10 ES ES07112149T patent/ES2397373T3/es active Active
- 2007-07-10 EP EP07112149A patent/EP1887051B1/de active Active
- 2007-08-02 TW TW096128438A patent/TWI429717B/zh active
- 2007-08-02 CL CL200702254A patent/CL2007002254A1/es unknown
- 2007-08-03 AR ARP070103429A patent/AR062201A1/es unknown
- 2007-08-03 CA CA2596164A patent/CA2596164C/en active Active
- 2007-08-03 AU AU2007203646A patent/AU2007203646A1/en not_active Abandoned
- 2007-08-03 MX MX2007009408A patent/MX2007009408A/es active IP Right Grant
- 2007-08-03 US US11/882,702 patent/US8236274B2/en active Active
- 2007-08-06 ZA ZA200706535A patent/ZA200706535B/xx unknown
- 2007-08-06 JP JP2007204559A patent/JP5988532B2/ja active Active
- 2007-08-06 CO CO07080106A patent/CO5950115A1/es not_active Application Discontinuation
- 2007-08-06 RU RU2007129923/05A patent/RU2441893C2/ru not_active IP Right Cessation
- 2007-08-06 SG SG200705719-3A patent/SG139719A1/en unknown
- 2007-08-06 IL IL185053A patent/IL185053A0/en unknown
- 2007-08-06 KR KR1020070078539A patent/KR101424256B1/ko active IP Right Grant
- 2007-08-07 BR BRPI0703408-3A patent/BRPI0703408A/pt not_active IP Right Cessation
- 2007-08-07 UA UAA200709098A patent/UA96410C2/ru unknown
- 2007-08-07 CN CN2007101400158A patent/CN101121829B/zh active Active
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2012
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Also Published As
Publication number | Publication date |
---|---|
US8236274B2 (en) | 2012-08-07 |
CA2596164C (en) | 2015-06-16 |
RU2441893C2 (ru) | 2012-02-10 |
JP2008038153A (ja) | 2008-02-21 |
KR20080013758A (ko) | 2008-02-13 |
JP5988532B2 (ja) | 2016-09-07 |
CO5950115A1 (es) | 2008-08-29 |
EP1887051A3 (de) | 2008-03-19 |
CL2007002254A1 (es) | 2008-02-08 |
ZA200706535B (en) | 2008-09-25 |
US20120328881A1 (en) | 2012-12-27 |
EP1887051A2 (de) | 2008-02-13 |
CN101121829A (zh) | 2008-02-13 |
KR101424256B1 (ko) | 2014-07-31 |
CN101121829B (zh) | 2012-05-30 |
RU2007129923A (ru) | 2009-02-20 |
ES2397373T3 (es) | 2013-03-06 |
TW200815538A (en) | 2008-04-01 |
UA96410C2 (ru) | 2011-11-10 |
AR062201A1 (es) | 2008-10-22 |
BRPI0703408A (pt) | 2008-04-01 |
EP1887051B1 (de) | 2012-10-24 |
DE102006037079A1 (de) | 2008-02-14 |
AU2007203646A1 (en) | 2008-02-21 |
US20080219915A1 (en) | 2008-09-11 |
SG139719A1 (en) | 2008-02-29 |
IL185053A0 (en) | 2008-12-29 |
MX2007009408A (es) | 2008-10-28 |
CA2596164A1 (en) | 2008-02-07 |
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