JPS6354485A - Fluidity improver for powder - Google Patents
Fluidity improver for powderInfo
- Publication number
- JPS6354485A JPS6354485A JP19838186A JP19838186A JPS6354485A JP S6354485 A JPS6354485 A JP S6354485A JP 19838186 A JP19838186 A JP 19838186A JP 19838186 A JP19838186 A JP 19838186A JP S6354485 A JPS6354485 A JP S6354485A
- Authority
- JP
- Japan
- Prior art keywords
- powder
- silica
- fluidity
- fluidity improver
- mixture
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- 239000000843 powder Substances 0.000 title claims abstract description 104
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 110
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 46
- 229910021485 fumed silica Inorganic materials 0.000 claims abstract description 15
- 239000000203 mixture Substances 0.000 claims abstract description 13
- SCPYDCQAZCOKTP-UHFFFAOYSA-N silanol Chemical compound [SiH3]O SCPYDCQAZCOKTP-UHFFFAOYSA-N 0.000 claims abstract description 13
- HEMHJVSKTPXQMS-UHFFFAOYSA-M sodium hydroxide Inorganic materials [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 12
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000006185 dispersion Substances 0.000 claims abstract description 7
- 125000005843 halogen group Chemical group 0.000 claims abstract description 4
- 125000002887 hydroxy group Chemical group [H]O* 0.000 claims abstract 2
- 238000004448 titration Methods 0.000 claims description 11
- 239000007864 aqueous solution Substances 0.000 claims description 8
- 125000001183 hydrocarbyl group Chemical group 0.000 claims description 3
- 239000000126 substance Substances 0.000 claims description 2
- 230000002209 hydrophobic effect Effects 0.000 abstract description 21
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 15
- 238000004438 BET method Methods 0.000 abstract description 11
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 abstract description 11
- 229910052799 carbon Inorganic materials 0.000 abstract description 11
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 abstract description 8
- 239000011780 sodium chloride Substances 0.000 abstract description 4
- 150000002430 hydrocarbons Chemical group 0.000 abstract description 3
- 239000004215 Carbon black (E152) Substances 0.000 abstract description 2
- 229930195733 hydrocarbon Natural products 0.000 abstract description 2
- 230000006835 compression Effects 0.000 abstract 1
- 238000007906 compression Methods 0.000 abstract 1
- 229910052736 halogen Inorganic materials 0.000 abstract 1
- 239000008240 homogeneous mixture Substances 0.000 abstract 1
- 239000007788 liquid Substances 0.000 abstract 1
- 230000000717 retained effect Effects 0.000 abstract 1
- 238000000034 method Methods 0.000 description 17
- KPUWHANPEXNPJT-UHFFFAOYSA-N disiloxane Chemical class [SiH3]O[SiH3] KPUWHANPEXNPJT-UHFFFAOYSA-N 0.000 description 11
- 239000011812 mixed powder Substances 0.000 description 8
- -1 dimethylsiloxane Chemical class 0.000 description 7
- 239000002245 particle Substances 0.000 description 7
- 229910052710 silicon Inorganic materials 0.000 description 7
- 239000010703 silicon Substances 0.000 description 7
- 238000003860 storage Methods 0.000 description 7
- 230000007423 decrease Effects 0.000 description 6
- LIKFHECYJZWXFJ-UHFFFAOYSA-N dimethyldichlorosilane Chemical compound C[Si](C)(Cl)Cl LIKFHECYJZWXFJ-UHFFFAOYSA-N 0.000 description 5
- 238000009835 boiling Methods 0.000 description 4
- 238000006243 chemical reaction Methods 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 4
- 238000010438 heat treatment Methods 0.000 description 4
- 239000000047 product Substances 0.000 description 4
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 3
- 229910001873 dinitrogen Inorganic materials 0.000 description 3
- 229920001903 high density polyethylene Polymers 0.000 description 3
- 239000004700 high-density polyethylene Substances 0.000 description 3
- 125000005372 silanol group Chemical group 0.000 description 3
- VXEGSRKPIUDPQT-UHFFFAOYSA-N 4-[4-(4-methoxyphenyl)piperazin-1-yl]aniline Chemical compound C1=CC(OC)=CC=C1N1CCN(C=2C=CC(N)=CC=2)CC1 VXEGSRKPIUDPQT-UHFFFAOYSA-N 0.000 description 2
- 239000006227 byproduct Substances 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 239000002537 cosmetic Substances 0.000 description 2
- 239000003814 drug Substances 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000003337 fertilizer Substances 0.000 description 2
- 235000013305 food Nutrition 0.000 description 2
- 125000000524 functional group Chemical group 0.000 description 2
- FFUAGWLWBBFQJT-UHFFFAOYSA-N hexamethyldisilazane Chemical compound C[Si](C)(C)N[Si](C)(C)C FFUAGWLWBBFQJT-UHFFFAOYSA-N 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 239000000049 pigment Substances 0.000 description 2
- 229910052573 porcelain Inorganic materials 0.000 description 2
- 239000010453 quartz Substances 0.000 description 2
- 229920005989 resin Polymers 0.000 description 2
- 239000011347 resin Substances 0.000 description 2
- 239000005049 silicon tetrachloride Substances 0.000 description 2
- 229920002050 silicone resin Polymers 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- 239000000725 suspension Substances 0.000 description 2
- 229910002012 Aerosil® Inorganic materials 0.000 description 1
- 239000004965 Silica aerogel Substances 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 125000000484 butyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 239000004568 cement Substances 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000003776 cleavage reaction Methods 0.000 description 1
- 238000009841 combustion method Methods 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000006482 condensation reaction Methods 0.000 description 1
- 125000004122 cyclic group Chemical group 0.000 description 1
- GSQKXUNYYCYYKT-UHFFFAOYSA-N cyclo-trialuminium Chemical compound [Al]1[Al]=[Al]1 GSQKXUNYYCYYKT-UHFFFAOYSA-N 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- MNFGEHQPOWJJBH-UHFFFAOYSA-N diethoxy-methyl-phenylsilane Chemical compound CCO[Si](C)(OCC)C1=CC=CC=C1 MNFGEHQPOWJJBH-UHFFFAOYSA-N 0.000 description 1
- 229920005645 diorganopolysiloxane polymer Polymers 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 229910001507 metal halide Inorganic materials 0.000 description 1
- 150000005309 metal halides Chemical class 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 1
- 244000005700 microbiome Species 0.000 description 1
- 238000004806 packaging method and process Methods 0.000 description 1
- 239000000575 pesticide Substances 0.000 description 1
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 1
- 229920001296 polysiloxane Polymers 0.000 description 1
- 239000011164 primary particle Substances 0.000 description 1
- 125000001436 propyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- 230000008707 rearrangement Effects 0.000 description 1
- 230000007017 scission Effects 0.000 description 1
- 238000007711 solidification Methods 0.000 description 1
- 230000008023 solidification Effects 0.000 description 1
- 238000004381 surface treatment Methods 0.000 description 1
- XJDNKRIXUMDJCW-UHFFFAOYSA-J titanium tetrachloride Chemical compound Cl[Ti](Cl)(Cl)Cl XJDNKRIXUMDJCW-UHFFFAOYSA-J 0.000 description 1
Classifications
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/72—Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds
- A61K8/84—Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds obtained by reactions otherwise than those involving only carbon-carbon unsaturated bonds
- A61K8/89—Polysiloxanes
- A61K8/891—Polysiloxanes saturated, e.g. dimethicone, phenyl trimethicone, C24-C28 methicone or stearyl dimethicone
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/19—Cosmetics or similar toiletry preparations characterised by the composition containing inorganic ingredients
- A61K8/25—Silicon; Compounds thereof
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
- A61Q1/00—Make-up preparations; Body powders; Preparations for removing make-up
- A61Q1/12—Face or body powders for grooming, adorning or absorbing
Landscapes
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Public Health (AREA)
- Veterinary Medicine (AREA)
- Animal Behavior & Ethology (AREA)
- General Health & Medical Sciences (AREA)
- Epidemiology (AREA)
- Birds (AREA)
- Chemical & Material Sciences (AREA)
- Inorganic Chemistry (AREA)
- Medicinal Preparation (AREA)
- Cosmetics (AREA)
- Processes Of Treating Macromolecular Substances (AREA)
- Silicon Compounds (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
Description
【発明の詳細な説明】
〔産業上の利用分野］
本発明は、粉体の流動性向上剤に関し、詳しくは疎水化
処理されたシリカ系微粉末からなる、粉体の流動性向上
剤に関する。DETAILED DESCRIPTION OF THE INVENTION [Industrial Field of Application] The present invention relates to a powder fluidity improver, and more particularly to a powder fluidity improver comprising a hydrophobized silica-based fine powder.
［従来の技術Ｊ
シリカ微粉末は、多くの工業分野で粉体の固化を防止し
、流動性を増大させるために、使用されてきた。例えば
、肥料、食品、医薬品、化粧品、粉末消火剤、セラミッ
クス微粉体、顔料、粉末塗料、有機樹脂粉末等の粉体に
添加され、流動性を改善するのに使用されている。[Prior Art J Silica fine powder has been used in many industrial fields to prevent powder solidification and increase fluidity. For example, it is added to powders such as fertilizers, foods, medicines, cosmetics, powder fire extinguishers, ceramic fine powders, pigments, powder coatings, and organic resin powders, and is used to improve fluidity.
粉体状製品は、その化学成分や使用方法に関係なく、凝
集しケーキ状になる傾向がある。Powdered products, regardless of their chemical composition or method of use, tend to clump and cake.
従って、このような製品の包装、貯蔵等の取扱いには困
難を伴う。従来、このような粉体状製品の流動性向上剤
としては、シリカ微粉末やケイＭ塩微粉末が知られてお
り、特に気相法で得られたフユームドシリ力が知られて
いる。Therefore, packaging, storage, and other handling of such products are difficult. Conventionally, fine silica powder and fine silica salt powder have been known as fluidity improvers for such powdered products, and in particular, fumed silica obtained by a gas phase method is known.
シリカ微粉末、特にフユームドシリ力は、粒子の径が非
常に小さく、粒度分布が狭く、かさ密度が非常に小さい
という、流動性向上剤として有利な特徴を有している。Fine silica powder, especially fumed silica powder, has advantageous characteristics as a fluidity improver, such as very small particle size, narrow particle size distribution, and very low bulk density.
しかしながら、親水性であるために、粉体に添加混合後
、長期間貯蔵すると、空気中の湿気を吸着して、互いに
付着し合い、粉体の流動性が低下するという欠点があっ
た。However, because they are hydrophilic, if they are stored for a long time after being added to the powder and mixed, they adsorb moisture in the air and adhere to each other, resulting in a decrease in the fluidity of the powder.
そこで、シリカ微粉末を表面処理して疎水化し、流動性
の向上及び貯蔵中の同化を防止する試みが行なわれでき
た。例えば、（１）シリカ微粉末をジメチルジクロルシ
ランにより、渦動懸垂状態で処理する方法（米国特許第
３９２４０２９号明ｉＩｌ書）、り′２Ｊシリカ微粉末
を環状ジオルガノポリシロキサンと塩基系の触媒により
、有機液体中でスラリー状にして処理する方法（米国特
許第３３３４０６２号明細１１）、（３シリカ微粉末を
少量の水とともにヘキサメチルジシラザンなどにより、
機械的外力を作用させながら処理する方法（特開昭５０
−５１４９４号公報）などが知られている。Therefore, attempts have been made to surface-treat silica fine powder to make it hydrophobic, thereby improving fluidity and preventing assimilation during storage. For example, (1) a method in which fine silica powder is treated with dimethyldichlorosilane in a vortex suspension state (US Pat. No. 3,924,029), a method in which fine silica powder is treated with cyclic diorganopolysiloxane and a basic catalyst (U.S. Pat. No. 3,334,062 specification 11), a method in which 3-silica fine powder is treated with a small amount of water using hexamethyldisilazane, etc.
Method of processing while applying mechanical external force (Japanese Patent Application Laid-open No. 1983
-51494) and the like are known.
［発明が解決しようとしている問題点］しかし、上記（
１）の方法は、処理剤の揮発性が高いために、高度に疎
水化処理することが困難であり、粉体の流動性向上剤と
して使用された場合、依然、高温高湿下で吸湿し、貯蔵
中に流動性が低下するという欠点があった。[Problem to be solved by the invention] However, the above (
In method 1), it is difficult to perform a highly hydrophobic treatment due to the high volatility of the treatment agent, and when used as a powder fluidity improver, it still absorbs moisture under high temperature and high humidity conditions. However, there was a drawback that the fluidity decreased during storage.
そこで、高度な処理を行なうために、連発したジメチル
ジクロルシランの蒸気を冷却器で凝縮し、還流させて処
理する方法が知られている。しかし、この方法や上記（
２や（３の方法によると高度に疎水化処理することが可
能であるが、シリカ微粉末の有する高い構造性が失われ
て、二次凝集が激しくなり、かさ密度が増大する傾向に
ある。従って、これを粉体の流動性向上剤として使用し
た場合には、粉体の貯蔵安定性は向上するが、流動性の
向上は十分でないという欠点があった。Therefore, in order to perform advanced treatment, a method is known in which the continuously emitted dimethyldichlorosilane vapor is condensed in a cooler and refluxed. However, this method and the above (
Although it is possible to perform highly hydrophobic treatment using methods 2 and 3, the high structural properties of fine silica powder tend to be lost, secondary aggregation becomes more intense, and the bulk density tends to increase. Therefore, when this is used as a fluidity improver for powder, the storage stability of the powder is improved, but there is a drawback that the improvement in fluidity is not sufficient.
そこで、本発明者らは、従来の粉体の流動性向上剤の持
つ欠点を解消すべく鋭意研究した結果、本発明に到達し
た。Therefore, the present inventors conducted intensive research to eliminate the drawbacks of conventional powder fluidity improvers, and as a result, they arrived at the present invention.
本発明の目的は、粉体に添加した際に、粉体の流動性を
大幅に向上させ、かつ長期間にわたって向上した流動性
を保つことのできる粉体の流動性向上剤を提供すること
にある。An object of the present invention is to provide a powder fluidity improver that, when added to powder, can significantly improve the fluidity of the powder and maintain the improved fluidity for a long period of time. be.
［問題点の解決手段およびその作用］
前記した本発明の目的は、
一般 式
（式中、Ｒは一価炭化水素基であり、ｎは１〜１５の整
数であり、Ｑはハロゲン原子、水酸基またＧ、ｔ −Ｏ
Ｒ１であり、Ｒ１は一価炭化水素基である）で表わされ
るジオルガノシロキサンオリゴマーにより疎水化処理さ
れ、ＢＥＴ法比表面積 １８０±１００ｍ”／９炭素
含有量 ５±３ 重量％見掛は密度
７５±３５ ９／、５１．５９の試料を３．４
Ｋｇ／ａ＋ｆ
の圧力下に４分周おいたときの
圧縮密度 ２００±３５ １（１／ａ＋ｆシ
ラノ一ル滴定量 １．０±１．０ｉｄ（ここでシラノ
ール滴定量は、２．０９の試料を２５ｍのエタノールと
７５ａｌｔの２０重量％Ｎａｃｌ水溶液との混合液に分
散させてなる分散液のＰＨを４．０から９．０に変える
のに必要な０．１Ｎ−水酸化ナトリウム水溶液の滴定伍
を意味している）を有するシリカ系微粉末の採用によっ
て達成される。[Means for Solving the Problems and Their Effects] The object of the present invention described above is to solve the following problems: Also G, t −O
Hydrophobized with a diorganosiloxane oligomer represented by R1, R1 is a monovalent hydrocarbon group), BET method specific surface area 180±100 m''/9 carbon content 5±3 wt% apparent density
75±35 9/, 51.59 sample to 3.4
Compressed density when placed under a pressure of Kg/a+f for 4 minutes 200±35 1(1/a+f Silanol titer 1.0±1.0id (Here, the silanol titer is the sample of 2.09 Titration step of 0.1N-sodium hydroxide aqueous solution required to change the pH of the dispersion in a mixture of 25m ethanol and 75alt 20% by weight NaCl aqueous solution from 4.0 to 9.0. This is achieved by employing a silica-based fine powder having a
本発明の流動性向上剤を製造するのに使用されるシリカ
系微粉末としては、フユームドシリ力、シリカアエロゲ
ル、沈澱シリカが例示される。Examples of the silica-based fine powder used to produce the fluidity improver of the present invention include fumed silica, silica aerogel, and precipitated silica.
粉体の流動性向上剤としての性能上、
１３０−４００ｍ２／９のＢＥＴ法比法面表面積するも
のが好ましい。In terms of performance as a powder fluidity improver, those having a BET specific surface area of 130 to 400 m2/9 are preferred.
シリカ微粉末は、通常０．１〜５重両％、場合によって
はそれ以上の吸着水を含有することが知れている。この
吸着水は、疎水化処理時にシリカの一次粒子から成る鎖
状体の解裂および再配列をひき起し、シリカ微粉末の有
する高度の構造性を幾分低下させる。そのためシリカ微
粉末の水分含有率は小さいことが好ましい。ましてや、
特開昭５０−
５１４９４で提案されている疎水化処理時の水の添加は
避けるべきである。It is known that fine silica powder usually contains 0.1 to 5% by weight of adsorbed water, and in some cases more than that. This adsorbed water causes cleavage and rearrangement of chain bodies made of silica primary particles during the hydrophobization treatment, and somewhat reduces the high degree of structure possessed by the fine silica powder. Therefore, it is preferable that the moisture content of the silica fine powder is small. Much less,
Addition of water during the hydrophobization treatment proposed in JP-A-50-51494 should be avoided.
したがって、水分含有率が小さく、大きなかさ容積を有
する点で、フユームドシリ力が好ましい。Therefore, fumed silicon is preferable because it has a low moisture content and a large bulk volume.
フユームドシリ力は、四塩化ケイ素のみから製造したも
のだけでなく、四塩化ケイ素と他の金属ハロゲン化物、
例えば三基アルミニウム、四塩化チタン等と併用して製
造したシリカ微粉末と他の金属酸化物微粉末と複合微粉
末であってもよく、それらも包含する。Fumed silicon is not only made from silicon tetrachloride, but also silicon tetrachloride and other metal halides,
For example, it may be a composite fine powder of silica fine powder produced in combination with tri-aluminum, titanium tetrachloride, etc., and other metal oxide fine powder, and these are also included.
このようなシリカ系微粉末としては、例えば、以下の商
品名で市販されているものがある。Examples of such fine silica powders include those commercially available under the following trade names.
日本アエロジル株式会社製の Ａｃｒｏｓｉ１１３０．
２００．３００．３８０、ＴＴ６００、ＭＯＸ６０、
ＭＯＸ １７０：米国のキャボット社製のＣａｂｏｓ
ｉｌ Ｍ−５、ＭＳ−７、ＭＳ−７５、ＨＳ −５、
ＥＨ−５：***のワラカーケミ−社製のＨＤＫＮ２０、
Ｖ１５、Ｔ２Ｏ，Ｔ２Ｏ、なトチアル。Acrosi1130 manufactured by Nippon Aerosil Co., Ltd.
200.300.380, TT600, MOX60,
MOX 170: Cabos manufactured by Cabot Corporation in the United States
il M-5, MS-7, MS-75, HS-5,
EH-5: HDKN20 manufactured by Walaker Chemie in West Germany,
V15, T2O, T2O, Totial.
これらシリカ系微粉末は、一般式
（式中、Ｒは一価炭化水素基であり、ｎは１〜１５の整
数であり、Ｑはハロゲン原子、水！！または式ＯＲ１で
あり、Ｒ１は一価炭化水素基である）で表わされるジオ
ルガノシロキサンオリゴマーによって表面処理される。These silica-based fine powders have a general formula (wherein R is a monovalent hydrocarbon group, n is an integer of 1 to 15, Q is a halogen atom, water!! or the formula OR1, and R1 is a The surface is treated with a diorganosiloxane oligomer represented by a valent hydrocarbon group.
Ｒとしてはメチル基、エチル基、プロピル基、ブチル基
、フェニル基が例示される。同一分子中のＲは、同じで
も異なっていてもよい。Examples of R include a methyl group, an ethyl group, a propyl group, a butyl group, and a phenyl group. R's in the same molecule may be the same or different.
Ｒ１としてはＲと同様なものが例示される。Examples of R1 include those similar to R.
ｎは１〜１５の整数であり、ｎがＯであると、疎水化率
が劣り、ｎが１６以上の場合には該シロキサンオリゴマ
ー中の官能基Ｑの含有率が減少して、シリカ系微粉末の
疎水化が困難となる。該シロキサンオリゴマーは、ハロ
ゲン原子、水Ｍ基、または式ＯＲ１である官能基Ｑが、
シリカ微粉末表面のシラノール基と縮合反応し、シリカ
系微粉末表面と結合して、シリカ系微粉末を疎水化させ
る。n is an integer from 1 to 15; when n is O, the hydrophobicity is poor; when n is 16 or more, the content of the functional group Q in the siloxane oligomer decreases, resulting in a silica-based microorganism. It becomes difficult to make the powder hydrophobic. The siloxane oligomer has a halogen atom, a water M group, or a functional group Q having the formula OR1,
It undergoes a condensation reaction with the silanol groups on the surface of the fine silica powder, bonds with the surface of the fine silica powder, and makes the fine silica powder hydrophobic.
シリカ系微粉末に対する該シロキサンオリゴマーの使用
昂は、シリカ系微粉末の有する単位表面積当りのシラノ
ール基数や、比表面積、Ｑの含有量などによって適宜か
わるため、特に限定されないが、通常、シリカ系微粉末
１００重量部に対し、１〜５０重ｊ部の範囲である。The degree of use of the siloxane oligomer for silica-based fine powder is not particularly limited, as it varies depending on the number of silanol groups per unit surface area, specific surface area, Q content, etc. of the silica-based fine powder, but it is usually used for silica-based fine powder. The amount is in the range of 1 to 50 parts by weight per 100 parts by weight of powder.
該シロキサンオリゴマーでシリカ系微粉末を表面処理す
るには、例えばシリカ系微粉末に、該シロキサンオリゴ
マーを加え、均一になるまで混合して、加熱するという
方法が採用される。あるいは、シリカ系微粉末を加熱下
で、混合しながら、該シロキサンオリゴマーを加えると
いう方法でも良い。In order to surface-treat the silica-based fine powder with the siloxane oligomer, for example, a method is employed in which the siloxane oligomer is added to the silica-based fine powder, mixed until uniform, and heated. Alternatively, the siloxane oligomer may be added while mixing the silica-based fine powder under heating.
この際に、全く混合状態に置かないで、加熱を行なった
場合には、該シロキサンオリゴマーの蒸気圧が低いため
に、疎水化処理が不均一となる。一方、激しい混合状態
にした場合、シリカ系微粉末の相互接触によって、構造
性が失われ、かさ密度が増大し、その結果、粉体の流動
性向上能が低下する。従って、穏和な混合条件が好まし
い。At this time, if heating is performed without being in a mixed state at all, the hydrophobization treatment will be non-uniform because the vapor pressure of the siloxane oligomer is low. On the other hand, when the mixture is vigorously mixed, the silica-based fine powders come into contact with each other, resulting in a loss of structure and an increase in bulk density, resulting in a decrease in the ability to improve the fluidity of the powder. Therefore, mild mixing conditions are preferred.
また、好ましい加熱温度範囲は、１００〜２００℃であ
る。１００℃未満では、シリカ系微粉末と該シロキサン
オリゴマーの反応が完結しにくくなり、２００℃を超え
る温度は不経済である。Moreover, a preferable heating temperature range is 100 to 200°C. If the temperature is lower than 100°C, the reaction between the silica-based fine powder and the siloxane oligomer will be difficult to complete, and if the temperature exceeds 200°C, it is uneconomical.
しかして、該シロキサンオリゴマーを用いて上記好まし
い条件でシリカ系微粉末を処理した場合には、該シロキ
サンオリゴマーの沸点が高く蒸気圧が小さいため、揮発
により損失がなく、また、該シロキサンオリゴマーの反
応性の高さによって、温和な条件下において、高度に表
面改質された疎水性シリカ系微粉末となり、加えて、シ
リカ系微粉末のかさ密度が増加することがない。Therefore, when silica-based fine powder is treated using the siloxane oligomer under the above-mentioned preferable conditions, since the siloxane oligomer has a high boiling point and a low vapor pressure, there is no loss due to volatilization, and the reaction of the siloxane oligomer is Due to its high properties, it becomes a highly surface-modified hydrophobic silica-based fine powder under mild conditions, and in addition, the bulk density of the silica-based fine powder does not increase.
本発明の粉体の流動性向上剤は、下記の特性を具備して
いる。The powder fluidity improver of the present invention has the following properties.
ＢＥＴ法比法面表面積１８０±１００ｍ’／９炭素含有
聞 ５±３ 重量％見掛は密度
７５±３５ ９／１１．５９の試料を３．４Ｋｔ１
０＃
の圧力下に４分間おいたときの
圧縮密度 ２００±３５ １Ｍ−シラノール
滴定ｆｆｉ １．０±１．Ｏｄ（ここでシラノール滴
定量は１．２．０９の試料を２５ＩＩｆｔのエタノール
と７５ａｄ！の２０重量％Ｎａｃｌ水溶液との混合液に
分散させてなる分散液のＰＨを４，０から９．０に変え
るのに必要な０．１Ｎ水酸化ナトリウム水溶液の滴定量
を意味している）
ＢＥＴ法比法面表面積０ｍ’／９未満の場合は、粒子径
が大きくなるために、流動性向上能が劣り、２８０１Ｔ
Ｉ２／９を超えるものは表面の疎水化処理が困難となり
、やはり流動性向上能が劣る。BET method slope surface area 180±100m'/9 Carbon content 5±3% by weight Apparent density
75±35 9/11.59 sample 3.4Kt1
Compressed density when placed under pressure of 0# for 4 minutes 200±35 1M-silanol titration ffi 1.0±1. Od (here, the silanol titer is 1.2.09 sample is dispersed in a mixture of 25IIft of ethanol and 75ad! of 20% NaCl aqueous solution, and the pH of the dispersion is changed from 4.0 to 9.0. (means the titration amount of 0.1N sodium hydroxide aqueous solution required to change the amount) If the BET ratio slope surface area is less than 0 m'/9, the particle size will become large and the ability to improve fluidity will be poor. , 2801T
If it exceeds I2/9, it becomes difficult to perform surface hydrophobization treatment, and the ability to improve fluidity is still inferior.
炭素含有量が２重囲％未満の場合は、疎水化処理が不十
分なため流動性向上能が劣り、一方、８重量％を超える
場合は、流動性向上能はそれ以上向上しないので不経済
である。If the carbon content is less than 2% by weight, the hydrophobization treatment is insufficient and the ability to improve fluidity is poor, while if it exceeds 8% by weight, the ability to improve fluidity will not improve any further, making it uneconomical. It is.
見掛は密度が４０９／を未満の場合は、疎水化処理が不
十分であり、１１０９／／：を超える場合は、シリカ系
微粉末の高い構造性が失われており、ともに流動性向上
能が劣る。If the apparent density is less than 409//, the hydrophobization treatment is insufficient, and if it exceeds 1109//:, the high structural properties of the silica-based fine powder have been lost, both of which impair the ability to improve fluidity. is inferior.
圧縮密度も見掛は密度と同様にシリカ系微粉末の構造性
を見るための有益な方法である。Similar to apparent density, compressed density is also a useful method for viewing the structural properties of silica-based fine powder.
見掛は密度は、シリカ系微粉末の輸送時の圧力履歴や、
測定誤差によって変動した値を与えるのに対し、圧縮密
度はそのような誤差が少なく、より正確な値を与える。The apparent density depends on the pressure history during transportation of the silica-based fine powder,
Whereas measurement errors give values that vary, compressed density has fewer such errors and gives more accurate values.
圧縮密度の上記範囲を超えるものは、見掛は密度と同様
な理由によって、流動性向上能が劣る。If the compressed density exceeds the above range, the ability to improve fluidity is apparently inferior for the same reason as the density.
シラノール適定量は、表面処理率の尺度であり、２ｄを
超える場合は、シリカ系微粉末の表面に残存するシラノ
ール基が多いため、粉体の流動性向上剤として使用され
た場合、高温高湿度の環境下で吸湿し、貯蔵中に流動性
が低下する。The appropriate amount of silanol is a measure of the surface treatment rate, and if it exceeds 2d, there are many silanol groups remaining on the surface of the silica-based fine powder, so when used as a powder fluidity improver, high temperature and high humidity It absorbs moisture in an environment where fluidity decreases during storage.
これら特性の測定法については、実施例中でさらに説明
する。Methods for measuring these properties are further described in the Examples.
本発明の粉体の流動性向上剤は、シリカ系微粉末が
一般 式
（式中のＲｌＱ、ｎは前述どおりである）で表わされる
ジオルガノシロキサンオリゴマーによりへ度に疎水化処
理されており、大きなかさ容積を保持しているので、粉
体に添加混合されたときに粉体の流動性を大きく向上さ
せ、その粉体を長期間貯蔵しても流動性がほとんど低下
することがない。In the powder fluidity improver of the present invention, a silica-based fine powder is subjected to a hydrophobic treatment using a diorganosiloxane oligomer represented by the general formula (wherein RlQ and n are as described above), Since it maintains a large bulk volume, it greatly improves the fluidity of the powder when it is added and mixed with the powder, and the fluidity hardly decreases even if the powder is stored for a long period of time.
本発明の粉体の流動性向上剤は、種々の粉体に適してい
る。The powder fluidity improver of the present invention is suitable for various powders.
粉体の具体例として肥料、農薬、食品、医薬品、化粧品
、粉末消火剤、顔料、充てん剤、粉体塗料、セメント、
有機樹脂粉末がある。Specific examples of powder include fertilizers, pesticides, foods, pharmaceuticals, cosmetics, powder fire extinguishers, pigments, fillers, powder coatings, cement,
There is organic resin powder.
これらの粉体への好ましい添加圏は、
０．２〜０．３重量％程度であり、通常０．５〜１重量
％である。The preferred amount of addition to these powders is about 0.2 to 0.3% by weight, usually 0.5 to 1% by weight.
また、粉体への添加方法は、粉体に流動性向上剤を添加
する方法でも、流動性向上剤に粉体を添加していく方法
でも良いが、より効果的な方法は、粉体の一部を前もっ
て流動性向上剤と混合し、これに残りの粉体を加えて混
合し、所定の割合にするという方法である。In addition, the method of adding the powder to the powder may be a method of adding the fluidity improver to the powder or a method of adding the powder to the fluidity improver, but a more effective method is to add the fluidity improver to the powder. A part of the powder is mixed with a fluidity improver in advance, and the remaining powder is added and mixed to achieve a predetermined ratio.
［実 施 例］ 以下に、本発明実施例と比較例を示す。[Example] Examples of the present invention and comparative examples are shown below.
実施例および比較例中、部とあるのは重量部を意味する
。In Examples and Comparative Examples, parts mean parts by weight.
炭素含有囚は試料に、１５０℃で窒素ガスを流して充分
に乾燥した後、燃焼法により求めた。Carbon-containing particles were determined by the combustion method after thoroughly drying the sample by flowing nitrogen gas at 150°C.
圧縮密度は１．５９の試料を５ａ１１のシリンダー状容
器に入れ、３．４Ｋｇ／ｌｉの圧力下に４分間おいたと
きの密度により求めた。The compressed density was determined from the density when a sample of 1.59 was placed in a 5a11 cylindrical container and placed under a pressure of 3.4 Kg/li for 4 minutes.
粉体および粉体に流動性向上剤を添加混合したものの流
動性および貯蔵後の流動性は、安息角の測定によって求
めた。The fluidity of the powder and the fluidity improver added to the powder and the fluidity after storage were determined by measuring the angle of repose.
実施例１
ジメチルジクロロシランに寮母の水を
添加して得た加水分解物から、低沸点成分を減圧下除去
して、一般式
（ｎは４〜１２である）で示されるジ
メチルシロキサンオリゴマーを得た。Example 1 A dimethylsiloxane oligomer represented by the general formula (n is 4 to 12) was obtained by removing low boiling point components under reduced pressure from a hydrolyzate obtained by adding dormer water to dimethyldichlorosilane. Ta.
ＢＥＴ法比表面積が２２０ｔｎ’／９であり、１重量％
の水含有率を有するフユームドシリカ１０ｏ９を５ｔセ
パラブルフラスコにとり、上記ジメチルシロキサンオリ
ゴマー２０９を滴下して、１時ｉ混合した。ついで、こ
れを１５０℃に昇温し３時間混合して、疎水性フユーム
ドシリ力を得た。BET method specific surface area is 220tn'/9, 1% by weight
Fumed silica 10o9 having a water content of 100% was placed in a 5t separable flask, and the above dimethylsiloxane oligomer 209 was added dropwise and mixed for 1 hour. Subsequently, this was heated to 150° C. and mixed for 3 hours to obtain hydrophobic fumed silica.
この疎水性フユームドシリ力の特性は、下記の通りであ
った。The characteristics of this hydrophobic fumed silicon were as follows.
ＢＥＴ法比表面積 １６０ ｍ２／９炭素含有量
４．１重量％見掛は密度 ６
０ ９／を圧縮密度 １９０ １Ｑ／ａ
１１シラノ一ル滴定Ｎ Ｏ，２ｍ
この疎水性フユームドシリカ０．７部
を、平均粒径１００μ園であり、安息角が２９°である
シリコーン樹脂粉末
１００部に加え、タービュラーミキサーで１０分間混合
した。BET method specific surface area 160 m2/9 Carbon content 4.1% by weight Apparent density 6
0 9/ compressed density 190 1Q/a
11 Silanol Titration N O, 2 m 0.7 part of this hydrophobic fumed silica was added to 100 parts of silicone resin powder having an average particle size of 100 μm and an angle of repose of 29°, and mixed for 10 minutes with a turbular mixer.
この混合粉末の安息角は、１５°であ った。The angle of repose of this mixed powder is 15°. It was.
また、この混合粉末を、温度２５℃、
湿度７０％ＲＨの雰囲気下で１ケ月放置した後の安息角
は、１５°であり、まったく変化していなかった。Further, after this mixed powder was left for one month in an atmosphere with a temperature of 25° C. and a humidity of 70% RH, the angle of repose was 15° and did not change at all.
比較例１
実施例１と同様に、シリコーン樹脂粉１末１００部に対
し、市販のジメチルジクロロシランで疎水化処理された
フユームドシリカ０．７部を添加′して混合した。Comparative Example 1 In the same manner as in Example 1, 0.7 parts of fumed silica hydrophobized with commercially available dimethyldichlorosilane was added to 100 parts of silicone resin powder 1 and mixed.
この混合粉末の安息角は１９°であっ
たゆまた、この混合粉末を温度２５℃、湿度７０％ＲＨ
の雰囲気下で１ケ月放置した後の安息角は２１°であっ
た。The angle of repose of this mixed powder was 19°.
The angle of repose after being left for one month in an atmosphere of was 21°.
なお、上記疎水化処理シリカの特性は、下記の通りであ
った。The properties of the hydrophobized silica were as follows.
ＢＥＴ法比表面積 １１０ が／９炭素含有ｆｆｉ
１．１重量％見掛は密度 ６
０ ９／を圧縮密度 ２２０ １（＋／
ａＩシラノール滴定ｍ １．Ｏｍ
実施例２
メチルフェニルジエトキシシランに、
少量の水を添加して得た加水分解物から、低沸点成分を
減圧下除去して、一般式
（式中ｎは３〜１０である）で示され
るメチルフェニルシロキサンオリゴマーを得た。BET method specific surface area 110 is /9 carbon content ffi
1.1% by weight apparent density 6
0 9/ to compressed density 220 1(+/
aI silanol titration m 1. Om Example 2 Low boiling point components were removed under reduced pressure from a hydrolyzate obtained by adding a small amount of water to methylphenyldiethoxysilane to obtain a compound represented by the general formula (in the formula, n is 3 to 10). A methylphenylsiloxane oligomer was obtained.
ＢＥＴ法比表面積が２００が７９であ
り、２重量％の水含有率を有するフユームドシリカ１０
０９を５ｔセパラブルフラスコにとり、上記メチルフェ
ニルシロキサンオリゴマー２５９を滴下して１時間混合
した。ついでこの混合物を１５０℃に昇温し、反応副生
物が除去されるまで、攪拌しながら窒素ガスを流して疎
水性フユームドシリ力を得た。Fumed silica 10 having a BET specific surface area of 200 to 79 and a water content of 2% by weight
09 was placed in a 5t separable flask, the above methylphenylsiloxane oligomer 259 was added dropwise, and the mixture was mixed for 1 hour. The mixture was then heated to 150° C. and nitrogen gas was passed through the mixture with stirring until reaction by-products were removed to obtain hydrophobic fumed silicon.
この疎水性フユームドシリ力の特性は、下記の通りであ
った。The characteristics of this hydrophobic fumed silicon were as follows.
ＢＥＴ法比表面積 １３０ ｔｎ’／９炭素含有
ｆｆｉ ８ 重器％見掛は密度
７０ ９／を圧縮密度 １９２
ｍ！ｌｌ１０＋１シラノール滴定母 ０．２ｍｌ
！この疎水性シリカ微粉末０．８部を、
平均粒径３５０μ−であり、安息角が
４８°である高密度ポリエチレン粉末
１０部に加えてタービュラーミキサーで混合し、さらに
同じ高密度ポリエチレン粉末９０部を５分割して添加し
、１０分間混合した。BET method specific surface area 130 tn'/9 Carbon content ffi 8 Heavy equipment% Apparent density
70 9/ compressed density 192
m! ll10+1 silanol titration mother 0.2ml
! 0.8 parts of this hydrophobic silica fine powder was added to 10 parts of high-density polyethylene powder with an average particle size of 350 μ- and an angle of repose of 48°, and mixed in a turbular mixer, followed by 90 parts of the same high-density polyethylene powder. was added in 5 portions and mixed for 10 minutes.
この混合粉末の安息角は、３０”であ った。The angle of repose of this mixed powder is 30”. It was.
また、この混合粉末を、温度２５℃、
湿度７０％ＲＨの雰囲気下で１ｔ月放置した後の安息角
は３１°であり、はとんど変化していなかった。The angle of repose of this mixed powder after being left for 1 ton in an atmosphere of 25° C. and 70% RH was 31°, which was almost unchanged.
比較例２
ＢＥＴ法比表面積が２２０が７９であ
り、１重間％の水含有率を有し、見掛は密度が６０９／
ｌであるフユームドシリカ２００９を、実施例１と同じ
一般式
（口は４〜１２である）で示されるジ
メチルシロキサンオリゴマー４０９および水２ｇと混合
し、容積５ｔを有し、その内の１．５ｔは直径１５〜４
０ｎｗａを有する磁器法が充填されている磁器製ボール
ミルに装入した。ボールミルを室温および７０ ｒｐｍ
で２時間運転した。ついで、ボールミルの内容物を１５
０℃で３時間加熱して乾燥することにより、疎水性フユ
ームドシリ力を得た。Comparative Example 2 The BET method specific surface area is 220/79, the water content is 1% by weight, and the apparent density is 609/
1 of fumed silica 2009 is mixed with dimethylsiloxane oligomer 409 having the same general formula as in Example 1 (the number is 4 to 12) and 2 g of water to have a volume of 5 t, of which 1.5 t is Diameter 15~4
A porcelain ball mill filled with a porcelain mill having 0 nwa was charged. Ball mill at room temperature and 70 rpm
I drove for 2 hours. Next, reduce the contents of the ball mill to 15
Hydrophobic fumed silicone was obtained by heating and drying at 0° C. for 3 hours.
この疎水性フユームドシリ力の特性は、下記の通りであ
った。The characteristics of this hydrophobic fumed silicon were as follows.
ＢＥＴ法比表面積 １６５ ｍ’／９炭素含有吊
４．０重量％見掛は密度 ２０
０ ９／を圧縮密度 ５００ ■！；１
１０１１シラノール滴定！Ｉ Ｏ，５ａｅ実施
例２と同様に、高密度ポリエチレ
ン粉末合計１００部に対し、上記疎水性フユームドシリ
カ０６８部を添加して混合した。BET method specific surface area 165 m'/9 Carbon content suspension 4.0% by weight Apparent density 20
0 9/ compressed density 500 ■! ;1
1011 silanol titration! IO, 5aeSimilarly to Example 2, 068 parts of the hydrophobic fumed silica was added to and mixed with a total of 100 parts of high-density polyethylene powder.
混合粉末の安息角は３９°であった。The angle of repose of the mixed powder was 39°.
また、この混合粉末を温度２５℃、湿度７０％ＲＨの雰
囲気下で、１ｔ月放置した後の安息角は４０°であり、
はとんど変化していなかった。In addition, the angle of repose of this mixed powder after being left for 1 ton in an atmosphere with a temperature of 25°C and a humidity of 70% RH is 40°,
had not changed much.
実施例３ ′
ジメチルジクロルシランに少量の水を
添加して得た加水分解物から、低沸点成分を減圧上除去
して、一般式、
（式中ｎは２〜６である）で示される
ジメチルシロキサンオリゴマーを得た。Example 3' Low-boiling components were removed under reduced pressure from a hydrolyzate obtained by adding a small amount of water to dimethyldichlorosilane to obtain a product represented by the general formula (wherein n is 2 to 6). A dimethylsiloxane oligomer was obtained.
ＢＥＴ法比表面積が３００ｍ２／９であり、１．５１１
％の水含有率を有するフユームドシリカ１００ｇを５ｔ
セパラブルフラスコにとり、上記ジメチルシロキサンオ
ゴマ−２０９を滴下して、１時間混合した。ついでこの
混合物を２００”Ｃに４温し、反応副生物が除去される
まで、攪拌しながら窒素ガスを流して疎水性フユームド
シリ力を得た。BET method specific surface area is 300 m2/9, 1.511
100g of fumed silica with a water content of 5t
The above dimethylsiloxane ogomer-209 was added dropwise to a separable flask and mixed for 1 hour. The mixture was then heated to 200''C and nitrogen gas was passed through it with stirring until the reaction by-products were removed to obtain a hydrophobic fumed silica.
この疎水性フユームドシリ力の特性は、下記の通りであ
った。The characteristics of this hydrophobic fumed silicon were as follows.
ＢＥＴ法比法面表面積２００ ｍ２／９炭素含有色
４．２重信％見掛は密度 ６
０ ９／ｆ圧縮密度 １９２ ｓｏ／
ｃｉシラノール滴定量 ０．２１ｄｌこの疎水性
フユームドシリカ０．８部
を、平均粒径４μ謬であり、安息角が
６９°である石英粉末１０部に加えてタービュラーミキ
サーで混合し、さらに同じ石英粉末９０部を５分割して
添加し、１０分間混合した。BET method ratio slope surface area 200 m2/9 Carbon content color 4.2 Shigenobu% Apparent density 6
0 9/f compressed density 192 so/
ci silanol titer: 0.21 dl 0.8 parts of this hydrophobic fumed silica was added to 10 parts of quartz powder with an average particle size of 4 μm and an angle of repose of 69°, and mixed in a turbular mixer, and then 90 parts of the same quartz powder was added. Added in 5 portions and mixed for 10 minutes.
この混合粉末の安息角は、６３°であ った。The angle of repose of this mixed powder is 63°. It was.
［発明の効果］
本発明の粉体の流動性向上剤は、一般式（式中、、Ｒ，
ＱＳｎは前述どおりである）で表わされるジオルガノシ
ロキサンオリゴマーによって疎水化処理されたシリカ系
微粉末であり、
ＢＥＴ法比法面表面８！ｉ１８０±１００１１２／９炭
素含有１ ５±３ 重量％見掛は密度
７５±３５ ９／１１．５９の試料を３．４
に宮／ｄ
の圧力下に４分間おいたときの
圧縮密度 ２００±３５１ｇ／ａ／シラ／
−／Ｌ／ ＦＲ定！ｌ １゜Ｏ＋１．０ｄ（ここで
シラノール滴定母は、２．０９の試料を２５ｍのエタノ
ールと７５ｄの２０重憬％Ｎａｃｌ水溶液との混合液に
分散させてなる分散液のＰＨを４．０から９．０に変え
るのに必要な０．ＩＮ水酸化ナトリウム水溶液の滴定ｍ
を意味している）
という特性を有しているので、種々の粉体の流動性を大
幅に向上させることができ、その流動性向上剤を添加し
た粉体を長期間貯蔵しても流動性がほとんど低下するこ
とがないという特徴を有している。[Effects of the Invention] The powder fluidity improver of the present invention has the general formula (wherein, R,
QSn is a silica-based fine powder that has been hydrophobized with a diorganosiloxane oligomer (as described above), and has a BET ratio slope surface of 8! i180±100112/9 Carbon content 1 5±3 Weight%Appearance is density
75±35 9/11.59 sample 3.4
Compressed density when placed under pressure of Ninomiya/d for 4 minutes: 200±351g/a/Sira/
-/L/ FR fixed! l 1゜O + 1.0d (here, the silanol titration mother is a dispersion obtained by dispersing a sample of 2.09 in a mixture of 25m of ethanol and a 20% NaCl aqueous solution of 75d), and the pH of the dispersion is from 4.0 to 1.0d. Titration of 0.IN sodium hydroxide aqueous solution required to change to 9.0 m
The fluidity improver can significantly improve the fluidity of various powders, and the fluidity of powders containing this fluidity improver remains unchanged even after long-term storage. It has the characteristic that it hardly decreases.
Claims (1)
数であり、Ｑはハロゲン原子、水酸基または−ＯＲ＾１
であり、Ｒ＾１は一価炭化水素基である）で表わされる
ジオルガノシロキサンオリゴマーにより疎水化処理され
、 ＢＥＴ法比表面積１８０±１００ｍ＾２／ｇ炭素含有量
５±３重量％ 見掛け密度７５±３５ｇ／ｌ １．５ｇの試料を３．４Ｋｇ／ｃｍ＾２ の圧力下に４分間おいたときの 圧縮密度２００±３５ｍｇ／ｃｍ＾３ シラノール滴定量１．０±１．０ｍｌ （ここでシラノール滴定量は、２．０ｇの 試料を２５ｍｌのエタノールと７５ｍｌの２０重量％Ｎ
ａｃｌ水溶液との混合液に分散させてなる分散液のＰＨ
を４．０から９．０に変えるのに必要な０．１Ｎ−水酸
化ナトリウム水溶液の滴定量を意味している）を有する
シリカ系微粉末であることを特徴とする、粉体の流動性
向上剤。 ２ シリカ系微粉末がフュームドシリカである特許請求
の範囲第１項記載の流動性向上剤。[Claims] 1 General formula▲ Numerical formula, chemical formula, table, etc.▼ (In the formula, R is a monovalent hydrocarbon group, n is an integer from 1 to 15, and Q is a halogen atom, a hydroxyl group, or -OR^1
Hydrophobized with a diorganosiloxane oligomer represented by ±35g/l Compressed density when a 1.5g sample is placed under a pressure of 3.4Kg/cm^2 for 4 minutes 200±35mg/cm^3 Silanol titration 1.0±1.0ml (here, silanol The titration amount is as follows: 2.0 g of sample is mixed with 25 ml of ethanol and 75 ml of 20% N by weight.
PH of the dispersion obtained by dispersing the mixture with the acl aqueous solution
The fluidity of the powder is characterized by being a silica-based fine powder having a titer of 0.1N-sodium hydroxide aqueous solution necessary to change from 4.0 to 9.0. improver. 2. The fluidity improver according to claim 1, wherein the silica-based fine powder is fumed silica.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP19838186A JPH078981B2 (en) | 1986-08-25 | 1986-08-25 | Powder fluidity improver |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP19838186A JPH078981B2 (en) | 1986-08-25 | 1986-08-25 | Powder fluidity improver |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS6354485A true JPS6354485A (en) | 1988-03-08 |
| JPH078981B2 JPH078981B2 (en) | 1995-02-01 |
Family
ID=16390175
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP19838186A Expired - Lifetime JPH078981B2 (en) | 1986-08-25 | 1986-08-25 | Powder fluidity improver |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH078981B2 (en) |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE19537292A1 (en) * | 1994-10-07 | 1996-04-11 | Toshiba Machine Co Ltd | Spindle rotation angle control machining method |
| JPH10237348A (en) * | 1997-02-26 | 1998-09-08 | Nippon Shokubai Co Ltd | Production of complex silica fine particle |
| JPH10338781A (en) * | 1997-06-11 | 1998-12-22 | Daicel Chem Ind Ltd | Styrene-based resin composition and formed material thereof |
| JPH11500440A (en) * | 1995-02-22 | 1999-01-12 | ヘキスト・アクチェンゲゼルシャフト | Use of aerogels in agriculture |
| JP2001139814A (en) * | 1999-11-11 | 2001-05-22 | Dow Corning Toray Silicone Co Ltd | Silicone rubber composition and its production method |
| GB2357497A (en) * | 1999-12-22 | 2001-06-27 | Degussa | Hydrophobic silica |
| JP2015537077A (en) * | 2012-10-31 | 2015-12-24 | ソルヴェイ（ソシエテ アノニム） | Method for producing fluoropolymer hybrid composite |
-
1986
- 1986-08-25 JP JP19838186A patent/JPH078981B2/en not_active Expired - Lifetime
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE19537292A1 (en) * | 1994-10-07 | 1996-04-11 | Toshiba Machine Co Ltd | Spindle rotation angle control machining method |
| US5713253A (en) * | 1994-10-07 | 1998-02-03 | Toshiba Kikai Kabushiki Kaisha | Rotational machining method |
| JPH11500440A (en) * | 1995-02-22 | 1999-01-12 | ヘキスト・アクチェンゲゼルシャフト | Use of aerogels in agriculture |
| JPH10237348A (en) * | 1997-02-26 | 1998-09-08 | Nippon Shokubai Co Ltd | Production of complex silica fine particle |
| JPH10338781A (en) * | 1997-06-11 | 1998-12-22 | Daicel Chem Ind Ltd | Styrene-based resin composition and formed material thereof |
| JP2001139814A (en) * | 1999-11-11 | 2001-05-22 | Dow Corning Toray Silicone Co Ltd | Silicone rubber composition and its production method |
| JP4528392B2 (en) * | 1999-11-11 | 2010-08-18 | 東レ・ダウコーニング株式会社 | Silicone rubber composition and method for producing the same |
| GB2357497A (en) * | 1999-12-22 | 2001-06-27 | Degussa | Hydrophobic silica |
| US7282236B2 (en) | 1999-12-22 | 2007-10-16 | Degussa Gmbh | Hydrophobic silica |
| JP2015537077A (en) * | 2012-10-31 | 2015-12-24 | ソルヴェイ（ソシエテ アノニム） | Method for producing fluoropolymer hybrid composite |
Also Published As
| Publication number | Publication date |
|---|---|
| JPH078981B2 (en) | 1995-02-01 |
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