JPH04370188A - Thixotropy imparter - Google Patents
Thixotropy imparterInfo
- Publication number
- JPH04370188A JPH04370188A JP24289591A JP24289591A JPH04370188A JP H04370188 A JPH04370188 A JP H04370188A JP 24289591 A JP24289591 A JP 24289591A JP 24289591 A JP24289591 A JP 24289591A JP H04370188 A JPH04370188 A JP H04370188A
- Authority
- JP
- Japan
- Prior art keywords
- fibrous
- magnesium oxysulfate
- acicular
- acicular magnesium
- thixotropy
- 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
- 239000011777 magnesium Substances 0.000 claims abstract description 77
- 229910052749 magnesium Inorganic materials 0.000 claims abstract description 77
- CENHPXAQKISCGD-UHFFFAOYSA-N trioxathietane 4,4-dioxide Chemical compound O=S1(=O)OOO1 CENHPXAQKISCGD-UHFFFAOYSA-N 0.000 claims abstract description 77
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims abstract description 76
- 150000001875 compounds Chemical class 0.000 claims abstract description 20
- 125000002887 hydroxy group Chemical group [H]O* 0.000 claims abstract description 20
- 230000001476 alcoholic effect Effects 0.000 claims abstract description 18
- 230000009974 thixotropic effect Effects 0.000 claims abstract description 4
- 239000003795 chemical substances by application Substances 0.000 claims description 9
- 125000004432 carbon atom Chemical group C* 0.000 claims description 2
- 230000007547 defect Effects 0.000 abstract 1
- 239000000203 mixture Substances 0.000 description 50
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 40
- 229920000642 polymer Polymers 0.000 description 26
- 239000007788 liquid Substances 0.000 description 25
- CSNNHWWHGAXBCP-UHFFFAOYSA-L Magnesium sulfate Chemical compound [Mg+2].[O-][S+2]([O-])([O-])[O-] CSNNHWWHGAXBCP-UHFFFAOYSA-L 0.000 description 20
- 239000003822 epoxy resin Substances 0.000 description 14
- 229920000647 polyepoxide Polymers 0.000 description 14
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 12
- 239000006185 dispersion Substances 0.000 description 12
- 238000001027 hydrothermal synthesis Methods 0.000 description 12
- 238000010438 heat treatment Methods 0.000 description 11
- VTHJTEIRLNZDEV-UHFFFAOYSA-L magnesium dihydroxide Chemical compound [OH-].[OH-].[Mg+2] VTHJTEIRLNZDEV-UHFFFAOYSA-L 0.000 description 11
- 239000000347 magnesium hydroxide Substances 0.000 description 11
- 229910001862 magnesium hydroxide Inorganic materials 0.000 description 11
- 239000000463 material Substances 0.000 description 11
- 239000002798 polar solvent Substances 0.000 description 11
- 229910052943 magnesium sulfate Inorganic materials 0.000 description 10
- 235000019341 magnesium sulphate Nutrition 0.000 description 10
- 239000002002 slurry Substances 0.000 description 10
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 9
- 239000013078 crystal Substances 0.000 description 9
- 230000007423 decrease Effects 0.000 description 9
- 238000000034 method Methods 0.000 description 9
- 239000000243 solution Substances 0.000 description 9
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 8
- 238000001914 filtration Methods 0.000 description 8
- 238000002156 mixing Methods 0.000 description 8
- 239000002202 Polyethylene glycol Substances 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 6
- 229920001223 polyethylene glycol Polymers 0.000 description 6
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 description 5
- 239000007864 aqueous solution Substances 0.000 description 4
- 235000019441 ethanol Nutrition 0.000 description 4
- 235000011187 glycerol Nutrition 0.000 description 4
- 239000003960 organic solvent Substances 0.000 description 4
- ZWEHNKRNPOVVGH-UHFFFAOYSA-N 2-Butanone Chemical compound CCC(C)=O ZWEHNKRNPOVVGH-UHFFFAOYSA-N 0.000 description 3
- QPRQEDXDYOZYLA-UHFFFAOYSA-N 2-methylbutan-1-ol Chemical compound CCC(C)CO QPRQEDXDYOZYLA-UHFFFAOYSA-N 0.000 description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 3
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 description 3
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 3
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 3
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 3
- 230000002776 aggregation Effects 0.000 description 3
- MTHSVFCYNBDYFN-UHFFFAOYSA-N diethylene glycol Chemical compound OCCOCCO MTHSVFCYNBDYFN-UHFFFAOYSA-N 0.000 description 3
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 description 3
- 229920005989 resin Polymers 0.000 description 3
- 239000011347 resin Substances 0.000 description 3
- 239000011593 sulfur Substances 0.000 description 3
- 229910052717 sulfur Inorganic materials 0.000 description 3
- 230000008719 thickening Effects 0.000 description 3
- 238000005406 washing Methods 0.000 description 3
- KBPLFHHGFOOTCA-UHFFFAOYSA-N 1-Octanol Chemical compound CCCCCCCCO KBPLFHHGFOOTCA-UHFFFAOYSA-N 0.000 description 2
- FRDAATYAJDYRNW-UHFFFAOYSA-N 3-methyl-3-pentanol Chemical compound CCC(C)(O)CC FRDAATYAJDYRNW-UHFFFAOYSA-N 0.000 description 2
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 2
- JLVVSXFLKOJNIY-UHFFFAOYSA-N Magnesium ion Chemical compound [Mg+2] JLVVSXFLKOJNIY-UHFFFAOYSA-N 0.000 description 2
- AMQJEAYHLZJPGS-UHFFFAOYSA-N N-Pentanol Chemical compound CCCCCO AMQJEAYHLZJPGS-UHFFFAOYSA-N 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 238000005054 agglomeration Methods 0.000 description 2
- 239000010425 asbestos Substances 0.000 description 2
- WERYXYBDKMZEQL-UHFFFAOYSA-N butane-1,4-diol Chemical compound OCCCCO WERYXYBDKMZEQL-UHFFFAOYSA-N 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000000835 fiber Substances 0.000 description 2
- 230000005484 gravity Effects 0.000 description 2
- LNEPOXFFQSENCJ-UHFFFAOYSA-N haloperidol Chemical compound C1CC(O)(C=2C=CC(Cl)=CC=2)CCN1CCCC(=O)C1=CC=C(F)C=C1 LNEPOXFFQSENCJ-UHFFFAOYSA-N 0.000 description 2
- ZSIAUFGUXNUGDI-UHFFFAOYSA-N hexan-1-ol Chemical compound CCCCCCO ZSIAUFGUXNUGDI-UHFFFAOYSA-N 0.000 description 2
- ZXEKIIBDNHEJCQ-UHFFFAOYSA-N isobutanol Chemical compound CC(C)CO ZXEKIIBDNHEJCQ-UHFFFAOYSA-N 0.000 description 2
- 229910001425 magnesium ion Inorganic materials 0.000 description 2
- 239000000395 magnesium oxide Substances 0.000 description 2
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 2
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 description 2
- 239000011259 mixed solution Substances 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- AQIXEPGDORPWBJ-UHFFFAOYSA-N pentan-3-ol Chemical compound CCC(O)CC AQIXEPGDORPWBJ-UHFFFAOYSA-N 0.000 description 2
- 239000003208 petroleum Substances 0.000 description 2
- 229920005749 polyurethane resin Polymers 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 239000006254 rheological additive Substances 0.000 description 2
- 229910052895 riebeckite Inorganic materials 0.000 description 2
- 238000004381 surface treatment Methods 0.000 description 2
- VZGDMQKNWNREIO-UHFFFAOYSA-N tetrachloromethane Chemical compound ClC(Cl)(Cl)Cl VZGDMQKNWNREIO-UHFFFAOYSA-N 0.000 description 2
- 239000013008 thixotropic agent Substances 0.000 description 2
- DNIAPMSPPWPWGF-VKHMYHEASA-N (+)-propylene glycol Chemical compound C[C@H](O)CO DNIAPMSPPWPWGF-VKHMYHEASA-N 0.000 description 1
- DNIAPMSPPWPWGF-GSVOUGTGSA-N (R)-(-)-Propylene glycol Chemical compound C[C@@H](O)CO DNIAPMSPPWPWGF-GSVOUGTGSA-N 0.000 description 1
- YPFDHNVEDLHUCE-UHFFFAOYSA-N 1,3-propanediol Substances OCCCO YPFDHNVEDLHUCE-UHFFFAOYSA-N 0.000 description 1
- POAOYUHQDCAZBD-UHFFFAOYSA-N 2-butoxyethanol Chemical compound CCCCOCCO POAOYUHQDCAZBD-UHFFFAOYSA-N 0.000 description 1
- ZNQVEEAIQZEUHB-UHFFFAOYSA-N 2-ethoxyethanol Chemical compound CCOCCO ZNQVEEAIQZEUHB-UHFFFAOYSA-N 0.000 description 1
- 239000004925 Acrylic resin Substances 0.000 description 1
- 229920000178 Acrylic resin Polymers 0.000 description 1
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 1
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- 235000008733 Citrus aurantifolia Nutrition 0.000 description 1
- NTIZESTWPVYFNL-UHFFFAOYSA-N Methyl isobutyl ketone Chemical compound CC(C)CC(C)=O NTIZESTWPVYFNL-UHFFFAOYSA-N 0.000 description 1
- UIHCLUNTQKBZGK-UHFFFAOYSA-N Methyl isobutyl ketone Natural products CCC(C)C(C)=O UIHCLUNTQKBZGK-UHFFFAOYSA-N 0.000 description 1
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 description 1
- ALQSHHUCVQOPAS-UHFFFAOYSA-N Pentane-1,5-diol Chemical compound OCCCCCO ALQSHHUCVQOPAS-UHFFFAOYSA-N 0.000 description 1
- 235000011941 Tilia x europaea Nutrition 0.000 description 1
- XSTXAVWGXDQKEL-UHFFFAOYSA-N Trichloroethylene Chemical group ClC=C(Cl)Cl XSTXAVWGXDQKEL-UHFFFAOYSA-N 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- 229920000180 alkyd Polymers 0.000 description 1
- 150000001412 amines Chemical class 0.000 description 1
- 239000010426 asphalt Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000011575 calcium Substances 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 239000000378 calcium silicate Substances 0.000 description 1
- 229910052918 calcium silicate Inorganic materials 0.000 description 1
- OYACROKNLOSFPA-UHFFFAOYSA-N calcium;dioxido(oxo)silane Chemical compound [Ca+2].[O-][Si]([O-])=O OYACROKNLOSFPA-UHFFFAOYSA-N 0.000 description 1
- 150000003857 carboxamides Chemical class 0.000 description 1
- 239000004359 castor oil Substances 0.000 description 1
- 235000019438 castor oil Nutrition 0.000 description 1
- 239000004927 clay Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- -1 coatings Substances 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 239000000499 gel Substances 0.000 description 1
- ZEMPKEQAKRGZGQ-XOQCFJPHSA-N glycerol triricinoleate Natural products CCCCCC[C@@H](O)CC=CCCCCCCCC(=O)OC[C@@H](COC(=O)CCCCCCCC=CC[C@@H](O)CCCCCC)OC(=O)CCCCCCCC=CC[C@H](O)CCCCCC ZEMPKEQAKRGZGQ-XOQCFJPHSA-N 0.000 description 1
- 239000010440 gypsum Substances 0.000 description 1
- 229910052602 gypsum Inorganic materials 0.000 description 1
- 229940035429 isobutyl alcohol Drugs 0.000 description 1
- 239000003350 kerosene Substances 0.000 description 1
- 239000004571 lime Substances 0.000 description 1
- DNIAPMSPPWPWGF-UHFFFAOYSA-N monopropylene glycol Natural products CC(O)CO DNIAPMSPPWPWGF-UHFFFAOYSA-N 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
- XNGIFLGASWRNHJ-UHFFFAOYSA-L phthalate(2-) Chemical compound [O-]C(=O)C1=CC=CC=C1C([O-])=O XNGIFLGASWRNHJ-UHFFFAOYSA-L 0.000 description 1
- 229920005862 polyol Polymers 0.000 description 1
- 229920000098 polyolefin Polymers 0.000 description 1
- 150000003077 polyols Chemical class 0.000 description 1
- 229920000166 polytrimethylene carbonate Polymers 0.000 description 1
- 238000000634 powder X-ray diffraction Methods 0.000 description 1
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 description 1
- 235000013772 propylene glycol Nutrition 0.000 description 1
- 239000000565 sealant Substances 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- BDHFUVZGWQCTTF-UHFFFAOYSA-M sulfonate Chemical compound [O-]S(=O)=O BDHFUVZGWQCTTF-UHFFFAOYSA-M 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- 229920006337 unsaturated polyester resin Polymers 0.000 description 1
- 150000003672 ureas Chemical class 0.000 description 1
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 description 1
- 229920002554 vinyl polymer Polymers 0.000 description 1
- 239000001993 wax Substances 0.000 description 1
- 239000008096 xylene Substances 0.000 description 1
Landscapes
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
Description
【0001】0001
【産業上の利用分野】本発明は表面処理された繊維状も
しくは針状マグネシウムオキシサルフェートからなる揺
変性付与剤に関する。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a thixotropic agent comprising surface-treated fibrous or acicular magnesium oxysulfate.
【0002】0002
【従来の技術】増粘性や揺変性の流動特性を調整するレ
オロジー調整剤は、各種の塗料、コーティング剤、接着
剤やシーラント等の広い分野で使用されている。このよ
うなレオロジー調整剤としては、構造粘性を付与する変
成ひまし油誘導体、ポリオレフィンワックス、有機アミ
ド、尿素化合物、微粉シリカ、塩基性カルシウムスルホ
ネートゲル、有機ミクロゲル、非水ディスパージョン樹
脂粒子、アミン処理粘土質等がある。BACKGROUND OF THE INVENTION Rheology modifiers that adjust flow characteristics such as thickening and thixotropy are used in a wide range of fields such as various paints, coatings, adhesives, and sealants. Such rheology modifiers include modified castor oil derivatives that impart structural viscosity, polyolefin waxes, organic amides, urea compounds, finely divided silica, basic calcium sulfonate gels, organic microgels, nonaqueous dispersion resin particles, and amine-treated clay. etc.
【0003】アスベストは増粘性と揺変性を付与する優
れた性能を有しているが、健康に対して害があるといわ
れている。また、特開昭63−314250号公報には
、10〜150μmの粒度の針状珪酸カルシウム結晶よ
りなる揺変性付与剤が開示されている。[0003] Although asbestos has excellent properties of imparting thickening properties and thixotropy, it is said to be harmful to health. Further, JP-A-63-314250 discloses a thixotropy imparting agent comprising acicular calcium silicate crystals with a particle size of 10 to 150 μm.
【0004】繊維状もしくは針状マグネシウムオキシサ
ルフェートの増粘性については、石膏と石灰、No.2
16、337〜339(1988)に記載されているよ
うに、アスベストと同様、水、エポキシ樹脂、ポリウレ
タン樹脂の原料であるポリオールおよびアスファルトに
添加すると粘度が高くなることが示されている。しかし
、揺変性については述べられていない。Regarding the thickening properties of fibrous or acicular magnesium oxysulfate, gypsum and lime, No. 2
16, 337-339 (1988), it has been shown that, like asbestos, when added to water, epoxy resins, polyols that are raw materials for polyurethane resins, and asphalt, the viscosity increases. However, thixotropy is not mentioned.
【0005】繊維状もしくは針状マグネシウムオキシサ
ルフェートは特願平2−123076号に記載されてい
るように優れた揺変性を示す。Fibrous or acicular magnesium oxysulfate exhibits excellent thixotropy as described in Japanese Patent Application No. 2-123076.
【0006】特願平2−123076号には、繊維状も
しくは針状マグネシウムオキシサルフェートと液状ポリ
マーの混合物が揺変性を呈することが示されている。ま
た、繊維状もしくは針状マグネシウムオキシサルフェー
ト、液状ポリマーと有機溶剤の混合物において、有機溶
剤が分子内にアルコール性水酸基または硫黄を少なくと
も1個有する化合物である極性溶剤であると、揺変性が
著しく向上し、この場合の極性溶剤と繊維状もしくは針
状マグネシウムオキシサルフェートの混合割合は、極性
溶剤100重量部当たり繊維状もしくは針状マグネシウ
ムオキシサルフェート1〜100重量部、好ましくは5
〜50重量部であることが示されている。[0006] Japanese Patent Application No. 2-123076 discloses that a mixture of fibrous or acicular magnesium oxysulfate and a liquid polymer exhibits thixotropy. In addition, in a mixture of fibrous or acicular magnesium oxysulfate, liquid polymer, and organic solvent, when the organic solvent is a polar solvent that is a compound having at least one alcoholic hydroxyl group or sulfur in the molecule, the thixotropy is significantly improved. However, in this case, the mixing ratio of the polar solvent and the fibrous or acicular magnesium oxysulfate is 1 to 100 parts by weight, preferably 5 parts by weight of the fibrous or acicular magnesium oxysulfate per 100 parts by weight of the polar solvent.
~50 parts by weight.
【0007】[0007]
【発明が解決しようとする課題】特願平2−12307
6号には、繊維状もしくは針状マグネシウムオキシサル
フェートは、化学的に活性なマグネシウムイオン、アル
カリ性水酸基および硫酸イオンを持つため、液状ポリマ
ーと混合すると、あるいは液状ポリマーと分子内にアル
コール性水酸基または硫黄を少なくとも1個有する化合
物である極性溶剤の混合物と混合すると、混合により得
られた組成物に揺変性を付与することが示されている。
しかしながら、繊維状もしくは針状マグネシウムオキシ
サルフェートは凝集性が高く分散性が悪いので、特に上
記のような極性溶剤を使用せずに混合すると、液状ポリ
マーの中に繊維状もしくは針状マグネシウムオキシサル
フェートの凝集物を存在させるという課題があった。[Problem to be solved by the invention] Patent application No. 2-12307
No. 6 states that fibrous or acicular magnesium oxysulfate has chemically active magnesium ions, alkaline hydroxyl groups, and sulfate ions, so when mixed with a liquid polymer, or with a liquid polymer, alcoholic hydroxyl groups or sulfur in the molecule. It has been shown that when mixed with a mixture of polar solvents, which is a compound having at least one compound, it imparts thixotropy to the resulting composition. However, since fibrous or acicular magnesium oxysulfate has high agglomeration and poor dispersibility, especially when mixed without using the above-mentioned polar solvent, fibrous or acicular magnesium oxysulfate may not be present in the liquid polymer. There was a problem with the presence of aggregates.
【0008】また、液状ポリマーあるいはその極性溶剤
との混合物と繊維状もしくは針状マグネシウムオキシサ
ルフェートとの組成物の温度が変化して組成物の粘度が
低下すると、揺変性が低下するという課題があった。[0008] Another problem is that when the temperature of a composition of a liquid polymer or its mixture with a polar solvent and fibrous or acicular magnesium oxysulfate changes and the viscosity of the composition decreases, the thixotropy decreases. Ta.
【0009】本発明の目的は、繊維状もしくは針状マグ
ネシウムオキシサルフェートを液状ポリマーあるいは液
状ポリマーと極性溶剤に混合したときの分散性が良く、
組成物の温度が上昇し粘度が低下しても揺変性が低下し
ない揺変性付与剤を提供することにある。The object of the present invention is to provide good dispersibility when fibrous or acicular magnesium oxysulfate is mixed in a liquid polymer or a liquid polymer and a polar solvent;
It is an object of the present invention to provide a thixotropy-imparting agent whose thixotropy does not decrease even when the temperature of the composition increases and the viscosity decreases.
【0010】0010
【課題を解決するための手段】上記の本発明の目的は、
分子内にアルコール性水酸基を少なくとも1個有する化
合物で表面処理された長さ0.5〜50μm、直径0.
05〜1μm、アスペクト比(長さ/直径)10〜30
0の繊維状もしくは針状マグネシウムオキシサルフェー
トからなる揺変性付与剤、によって達成される。[Means for Solving the Problems] The above objects of the present invention are as follows:
Surface treated with a compound having at least one alcoholic hydroxyl group in the molecule, length 0.5 to 50 μm, diameter 0.5 μm.
05-1μm, aspect ratio (length/diameter) 10-30
This is achieved by using a thixotropic agent consisting of 0 fibrous or acicular magnesium oxysulfate.
【0011】更に、上記の本発明の目的は、分子内にア
ルコール性水酸基を少なくとも2個有し、且つ炭素数が
2以上の化合物で表面処理された長さ0.5〜50μm
、直径0.05〜1μm、アスペクト比(長さ/直径)
10〜300の繊維状もしくは針状マグネシウムオキシ
サルフェートからなる揺変性付与剤、によってより好適
に達成される。Furthermore, the above object of the present invention is to provide a molecule having a length of 0.5 to 50 μm that has at least two alcoholic hydroxyl groups in its molecule and has been surface-treated with a compound having 2 or more carbon atoms.
, diameter 0.05-1 μm, aspect ratio (length/diameter)
This is more preferably achieved by a thixotropy imparting agent consisting of 10 to 300 fibrous or acicular magnesium oxysulfate.
【0012】繊維状もしくは針状マグネシウムオキシサ
ルフェートは、特開平1−126218号公報に記載の
方法、すなわち硫酸マグネシウム水溶液にBET比表面
積が20m2/g以下の水酸化マグネシウムまたは酸化
マグネシウムをその濃度が25重量%以下になる様に分
散させた後、100〜300℃の温度で水熱反応させる
方法により好適に製造することが出来る。Fibrous or acicular magnesium oxysulfate can be prepared by the method described in JP-A-1-126218, that is, by adding magnesium hydroxide or magnesium oxide having a BET specific surface area of 20 m2/g or less to an aqueous magnesium sulfate solution at a concentration of 25 m2/g or less. It can be suitably produced by a method of dispersing to a weight percent or less and then subjecting it to a hydrothermal reaction at a temperature of 100 to 300°C.
【0013】また、特開平1−41544号公報に記載
の方法、すなわち硫酸マグネシウムと水酸化マグネシウ
ムまたは酸化マグネシウムをその濃度が25重量%以下
になる様に分散させた後、100〜300℃の温度で水
熱反応させて繊維状もしくは針状マグネシウムオキシサ
ルフェートを製造するに際し、水熱反応系に界面活性剤
を含有させる方法により上記の方法と同様に好適に製造
することが出来る。[0013] Furthermore, the method described in JP-A-1-41544 is used, that is, after dispersing magnesium sulfate and magnesium hydroxide or magnesium oxide so that the concentration thereof is 25% by weight or less, the dispersion is carried out at a temperature of 100 to 300°C. When producing fibrous or acicular magnesium oxysulfate by hydrothermal reaction, it can be suitably produced in the same manner as the above method by incorporating a surfactant into the hydrothermal reaction system.
【0014】得られた繊維状もしくは針状マグネシウム
オキシサルフェートは、その粉末X線回折スペクトルが
ASTMNo.7−415のそれと良く一致しており、
代表的には該ASTMNo.7−415に記載の示性式
であるMgSO4・5Mg(OH)2・3H2Oで表す
ことが出来ると考えられる。The obtained fibrous or acicular magnesium oxysulfate has a powder X-ray diffraction spectrum of ASTM No. It is in good agreement with that of 7-415,
Typically, the ASTM No. It is thought that it can be expressed by the specific formula MgSO4.5Mg(OH)2.3H2O described in No. 7-415.
【0015】繊維状もしくは針状マグネシウムオキシサ
ルフェートの一般的形態は、比重が2.0〜2.5、長
さ(繊維長)数ミクロン〜1000μm、見掛け比重0
.05〜0.3であり極めて嵩高い繊維状もしくは針状
の物質であり、商品名モスハイジ(宇部興産(株)製)
として市場に流通している。The general form of fibrous or acicular magnesium oxysulfate has a specific gravity of 2.0 to 2.5, a length (fiber length) of several microns to 1000 μm, and an apparent specific gravity of 0.
.. 05 to 0.3, it is an extremely bulky fibrous or needle-like substance, and its trade name is Moshyge (manufactured by Ube Industries, Ltd.).
It is distributed in the market as.
【0016】繊維状もしくは針状マグネシウムオキシサ
ルフェートは、化学的に活性なマグネシウムイオン、ア
ルカリ性水酸基および硫酸イオンを持つため、液状ポリ
マーと混合すると、あるいは液状ポリマーと分子内にア
ルコール性水酸基または硫黄を少なくとも1個有する化
合物である極性溶剤の混合物と混合すると、混合により
得られた組成物に揺変性を付与する。しかしながら、繊
維状もしくは針状マグネシウムオキシサルフェートは凝
集性が高く分散性が悪いので、特に上記のような極性溶
剤を使用せずに混合すると、液状ポリマーの中に繊維状
もしくは針状マグネシウムオキシサルフェートの凝集物
を存在させ、揺変性が低下するという課題があった。Fibrous or acicular magnesium oxysulfate has chemically active magnesium ions, alkaline hydroxyl groups, and sulfate ions, so when mixed with a liquid polymer, or with a liquid polymer, it has at least an alcoholic hydroxyl group or sulfur in the molecule. When mixed with a mixture of polar solvents, the compound imparts thixotropy to the resulting composition. However, since fibrous or acicular magnesium oxysulfate has high agglomeration and poor dispersibility, especially when mixed without using the above-mentioned polar solvent, fibrous or acicular magnesium oxysulfate may not be present in the liquid polymer. There was a problem in that the presence of aggregates led to a decrease in thixotropy.
【0017】また、液状ポリマーあるいはその極性溶剤
との混合物と繊維状もしくは針状マグネシウムオキシサ
ルフェートとの組成物の温度が変化して組成物の粘度が
低下すると、揺変性が低下するという課題があった。[0017] Another problem is that when the temperature of the composition of the liquid polymer or its mixture with a polar solvent and fibrous or acicular magnesium oxysulfate changes and the viscosity of the composition decreases, the thixotropy decreases. Ta.
【0018】そこで、繊維状もしくは針状マグネシウム
オキシサルフェートを液状ポリマーあるいはその極性溶
剤との混合物に混合しても揺変性は低下せず、且つ組成
物の温度が変化して組成物の揺変性が低下しない方法に
ついて種々検討した結果、繊維状もしくは針状マグネシ
ウムオキシサルフェートの表面をアルコール性水酸基を
有する化合物で処理することにより上記の課題が解決さ
れることを見出し本発明に到達した。Therefore, even if fibrous or acicular magnesium oxysulfate is mixed with a liquid polymer or a mixture thereof with a polar solvent, the thixotropy does not decrease, and the thixotropy of the composition changes as the temperature of the composition changes. As a result of various studies on methods that would not cause the decrease, it was discovered that the above problems could be solved by treating the surface of fibrous or acicular magnesium oxysulfate with a compound having an alcoholic hydroxyl group, and the present invention was achieved.
【0019】液状ポリマーと繊維状もしくは針状マグネ
シウムオキシサルフェートとを混合した場合の揺変作用
は、繊維状もしくは針状マグネシウムオキシサルフェー
トが液状ポリマーの中で網目構造を生成するために生ず
ると考えられる。アルコール性水酸基を有する化合物は
液状ポリマーに容易に溶解するので、繊維状もしくは針
状マグネシウムオキシサルフェートの表面をアルコール
性水酸基を有する化合物で処理すると、繊維状もしくは
針状マグネシウムオキシサルフェートの凝集を防ぎ、液
状ポリマーに混合した時の分散を良好にし、また、アル
コール性水酸基を有する化合物が液状ポリマーに溶解す
ると、繊維状もしくは針状マグネシウムオキシサルフェ
ートの表面は活性な状態に戻り、揺変性を示す網目構造
の生成が容易となり、揺変性が大きくなると考えられる
。[0019] The thixotropic effect when a liquid polymer and fibrous or acicular magnesium oxysulfate are mixed is thought to occur because the fibrous or acicular magnesium oxysulfate forms a network structure in the liquid polymer. . Compounds having alcoholic hydroxyl groups easily dissolve in liquid polymers, so treating the surface of fibrous or acicular magnesium oxysulfate with a compound having alcoholic hydroxyl groups prevents the aggregation of fibrous or acicular magnesium oxysulfate, It improves dispersion when mixed into a liquid polymer, and when a compound with an alcoholic hydroxyl group is dissolved in the liquid polymer, the surface of the fibrous or acicular magnesium oxysulfate returns to an active state, forming a network structure that exhibits thixotropy. It is thought that the formation of is facilitated and the thixotropy is increased.
【0020】繊維状もしくは針状マグネシウムオキシサ
ルフェートは、通常原料として水酸化マグネシウムと硫
酸を用いて水熱反応を行った後、濾過、洗浄および乾燥
を行って製造するので、繊維状もしくは針状マグネシウ
ムオキシサルフェートの表面をアルコール性水酸基を有
する化合物で処理する方法としては次の二つの方法が適
している。すなわち、Fibrous or acicular magnesium oxysulfate is usually produced by carrying out a hydrothermal reaction using magnesium hydroxide and sulfuric acid as raw materials, followed by filtration, washing and drying. The following two methods are suitable for treating the surface of oxysulfate with a compound having an alcoholic hydroxyl group. That is,
【0021】■ 洗浄後得られた繊維状もしくは針状
マグネシウムオキシサルフェートの脱水ケーキに水を加
えて再びスラリーとし、このスラリーにアルコール性水
酸基を有する化合物を添加する方法、および■ A method of adding water to the dehydrated cake of fibrous or acicular magnesium oxysulfate obtained after washing to form a slurry again, and adding a compound having an alcoholic hydroxyl group to this slurry;
【0022
】■ 洗浄後得られた繊維状もしくは針状マグネシウ
ムオキシサルフェートの脱水ケーキにアルコール性水酸
基を有する化合物を添加する方法、である。0022
]■ This is a method in which a compound having an alcoholic hydroxyl group is added to a dehydrated cake of fibrous or acicular magnesium oxysulfate obtained after washing.
【0023】このような方法で繊維状もしくは針状マグ
ネシウムオキシサルフェートの表面を処理し、その後必
要に応じて濾過を行い、乾燥して本発明の揺変性付与剤
を得る。[0023] The surface of the fibrous or acicular magnesium oxysulfate is treated by such a method, and then, if necessary, it is filtered and dried to obtain the thixotropy imparting agent of the present invention.
【0024】繊維状もしくは針状マグネシウムオキシサ
ルフェートに添加するアルコール性水酸基を有する化合
物の量は、繊維状もしくは針状マグネシウムオキシサル
フェート100重量部当たり0.1〜20重量部、好ま
しくは1〜5重量部である。The amount of the compound having an alcoholic hydroxyl group to be added to the fibrous or acicular magnesium oxysulfate is 0.1 to 20 parts by weight, preferably 1 to 5 parts by weight, per 100 parts by weight of the fibrous or acicular magnesium oxysulfate. Department.
【0025】本発明の揺変性付与剤が揺変性を付与する
液状ポリマーは、例えばエポキシ樹脂、フタル酸樹脂、
アミノアルキド樹脂、ビニル樹脂、ポリウレタン樹脂、
不飽和ポリエステル樹脂、アクリル樹脂である。これら
の液状ポリマーは市場において種々の有機溶剤、すなわ
ちメチルアルコール、エチルアルコール、イソプロピル
アルコール、ブチルアルコール、酢酸エチル、エチルセ
ロソルブ、ブチルセロソルブ、アセトン、メチルエチル
ケトン、メチルイソブチルケトン、トルエン、キシレン
、石油エーテル、石油ベンジン、ガソリン、ケロシン、
トリクロルエチレン、四塩化炭素等と併用して使用され
ることが多い。Liquid polymers to which the thixotropy imparting agent of the present invention imparts thixotropy include, for example, epoxy resins, phthalate resins,
Amino alkyd resin, vinyl resin, polyurethane resin,
Unsaturated polyester resin and acrylic resin. These liquid polymers are commercially available in various organic solvents, namely methyl alcohol, ethyl alcohol, isopropyl alcohol, butyl alcohol, ethyl acetate, ethyl cellosolve, butyl cellosolve, acetone, methyl ethyl ketone, methyl isobutyl ketone, toluene, xylene, petroleum ether, petroleum benzine. , gasoline, kerosene,
It is often used in combination with trichlorethylene, carbon tetrachloride, etc.
【0026】揺変性付与剤に適する繊維状もしくは針状
マグネシウムオキシサルフェートは、長さ0.5〜50
μm、直径0.05〜1μm、アスペクト比(長さ/直
径)10〜300の形状を有するものである。長さが5
0μmを超えたりアスペクト比が300を超えると、繊
維状もしくは針状マグネシウムオキシサルフェートが絡
み合い十分な効果を発揮しない。[0026] Fibrous or acicular magnesium oxysulfate suitable as a thixotropy imparting agent has a length of 0.5 to 50 mm.
μm, a diameter of 0.05 to 1 μm, and an aspect ratio (length/diameter) of 10 to 300. length is 5
If it exceeds 0 μm or the aspect ratio exceeds 300, the fibrous or acicular magnesium oxysulfate becomes entangled and does not exhibit sufficient effects.
【0027】本発明の揺変性付与剤である繊維状もしく
は針状マグネシウムオキシサルフェートと液状ポリマー
の混合割合は、対象となる液状ポリマーの種類、有機溶
剤の有無および種類、目的とする揺変性の程度により異
なるので一概に表し難いが、通常液状ポリマー100重
量部当たり0.5〜20重量部、好ましくは1〜10重
量部である。The mixing ratio of the fibrous or acicular magnesium oxysulfate, which is the thixotropy-imparting agent of the present invention, and the liquid polymer depends on the type of the target liquid polymer, the presence or absence of an organic solvent, the type, and the desired degree of thixotropy. Although it is difficult to make a general statement because it varies depending on the type of polymer, it is usually 0.5 to 20 parts by weight, preferably 1 to 10 parts by weight, per 100 parts by weight of the liquid polymer.
【0028】本発明で使用する分子内にアルコール性水
酸基を少なくとも1個有する化合物としては、エタノー
ル、1−プロパノール、1−ブタノール、イソブチルア
ルコール、1−ペンタノール、3−ペンタノール、2−
メチル−1−ブタノール、1−ヘキサノール、3−メチ
ル−3−ペンタノール、1−オクタノール、エチレング
リコール、ジエチレングリコール、1,2−プロパンジ
オール、1,3−プロパンジオール、1,4−ブタンジ
ール、1,5−ペンタンジオール、グリセリン、ポリエ
チレングリコール等が挙げられる。Compounds having at least one alcoholic hydroxyl group in the molecule used in the present invention include ethanol, 1-propanol, 1-butanol, isobutyl alcohol, 1-pentanol, 3-pentanol, 2-
Methyl-1-butanol, 1-hexanol, 3-methyl-3-pentanol, 1-octanol, ethylene glycol, diethylene glycol, 1,2-propanediol, 1,3-propanediol, 1,4-butanediol, 1, Examples include 5-pentanediol, glycerin, polyethylene glycol, and the like.
【0029】[0029]
【実施例】この明細書の実施例および比較例で用いる液
状ポリマーの主な性状は表1のとおりである。[Examples] Table 1 shows the main properties of the liquid polymers used in the Examples and Comparative Examples of this specification.
【0030】[0030]
【表1】[Table 1]
【0031】実施例1
硫酸マグネシウム水溶液に種晶の繊維状もしくは針状マ
グネシウムオキシサルフェートと水酸化マグネシウムス
ラリーを添加して良く分散させた後、分散液をオートク
レーブに入れて温度180℃、圧力10kg/cm2・
Gにて2時間水熱反応を行った。Example 1 After adding fibrous or acicular magnesium oxysulfate seed crystals and magnesium hydroxide slurry to an aqueous magnesium sulfate solution and thoroughly dispersing them, the dispersion was placed in an autoclave at a temperature of 180°C and a pressure of 10 kg/kg. cm2・
A hydrothermal reaction was carried out at G for 2 hours.
【0032】反応後、生成物を濾過し、水洗して水分が
77.6%の繊維状もしくは針状マグネシウムオキシサ
ルフェートの脱水ケーキを得た。この脱水ケーキ112
gと水1500gを3000mlのビーカーに入れ、ホ
モミキサー(特殊機化工業(株)製4C型、以下同じ)
で5分間分散処理をした。次に、500gの水にエチレ
ングリコールを12g加えて調製したエチレングリコー
ル水溶液を添加して、ホモミキサーにて5分間表面処理
をした。更に、濾過し、得られた水分77.7%の脱水
ケーキを温度125℃で5時間乾燥した。この乾燥物を
簡単にほぐし、1.5mmの篩で篩い分けを行い、1.
5mmの篩を通過したものを試験に使用した。このよう
にして得られた繊維状もしくは針状マグネシウムオキシ
サルフェートの形状は長さ5〜20μm、直径0.3〜
0.7μmであった。After the reaction, the product was filtered and washed with water to obtain a dehydrated cake of fibrous or acicular magnesium oxysulfate having a water content of 77.6%. This dehydrated cake 112
Put g and 1500 g of water into a 3000 ml beaker, and use a homomixer (4C type manufactured by Tokushu Kika Kogyo Co., Ltd., the same applies hereinafter).
Dispersion treatment was carried out for 5 minutes. Next, an ethylene glycol aqueous solution prepared by adding 12 g of ethylene glycol to 500 g of water was added, and the surface was treated with a homomixer for 5 minutes. Furthermore, the dehydrated cake obtained by filtration and having a water content of 77.7% was dried at a temperature of 125° C. for 5 hours. This dried material was easily loosened and sieved through a 1.5 mm sieve.1.
Those that passed through a 5 mm sieve were used for the test. The fibrous or acicular magnesium oxysulfate thus obtained has a length of 5 to 20 μm and a diameter of 0.3 to 20 μm.
It was 0.7 μm.
【0033】次に、このようにして得られた繊維状もし
くは針状マグネシウムオキシサルフェート15gとエポ
キシ樹脂■500gとを卓上型ニーダー(入江商会(株
)製PNV−1型、以下同じ)に入れ25℃に加熱して
減圧下で1時間混合して混合物を製造した。この混合物
を予め25℃に加熱しておいた500mlのビーカーに
取り出し、25℃に加熱した減圧装置に入れて減圧し気
泡を除去した後、25℃加熱下においてB型粘度計で粘
度を測定した。その結果を表2に示す。Next, 15 g of the fibrous or acicular magnesium oxysulfate obtained in this way and 500 g of epoxy resin were placed in a tabletop kneader (Model PNV-1 manufactured by Irie Shokai Co., Ltd., hereinafter the same) and heated for 25 minutes. A mixture was prepared by heating to 0.degree. C. and mixing under reduced pressure for 1 hour. This mixture was taken out into a 500 ml beaker that had been preheated to 25°C, and the mixture was placed in a vacuum device heated to 25°C to reduce the pressure and remove air bubbles, and then the viscosity was measured using a B-type viscometer while heating at 25°C. . The results are shown in Table 2.
【0034】実施例2〜4
エチレングリコールを1,5−ペンタンジオール(実施
例2)、グリセリン(実施例3)、平均分子量200の
ポリエチレングリコール(実施例4)に代えて表面処理
を行った繊維状もしくは針状マグネシウムオキシサルフ
ェートを使用した以外は、実施例1と同様に繊維状もし
くは針状マグネシウムオキシサルフェートとエポキシ樹
脂■との混合物を製造し、実施例1と同様に粘度を測定
した。その結果を表2に示す。Examples 2 to 4 Fibers subjected to surface treatment by replacing ethylene glycol with 1,5-pentanediol (Example 2), glycerin (Example 3), or polyethylene glycol with an average molecular weight of 200 (Example 4) A mixture of fibrous or acicular magnesium oxysulfate and epoxy resin (2) was prepared in the same manner as in Example 1, except that acicular or acicular magnesium oxysulfate was used, and the viscosity was measured in the same manner as in Example 1. The results are shown in Table 2.
【0035】比較例1
硫酸マグネシウム水溶液に種晶の繊維状もしくは針状マ
グネシウムオキシサルフェートと水酸化マグネシウムス
ラリーを添加して良く分散させた後、分散液をオートク
レーブに入れて温度180℃、圧力10kg/cm2・
Gにて2時間水熱反応を行った。Comparative Example 1 After adding fibrous or acicular magnesium oxysulfate seed crystals and magnesium hydroxide slurry to an aqueous magnesium sulfate solution and thoroughly dispersing them, the dispersion was placed in an autoclave at a temperature of 180°C and a pressure of 10 kg/kg. cm2・
A hydrothermal reaction was carried out at G for 2 hours.
【0036】反応後、生成物を濾過し、水洗して水分が
77.6%の繊維状もしくは針状マグネシウムオキシサ
ルフェートの脱水ケーキを得た。この脱水ケーキ112
gと水1500gを3000mlのビーカーに入れ、ホ
モミキサーで5分間分散処理をした。次に、500gの
水を加えてホモミキサーにて更に5分間分散処理をした
。更に、濾過し、得られた水分77.6%の脱水ケーキ
を温度125℃で5時間乾燥した。この乾燥物を簡単に
ほぐし、1.5mmの篩で篩い分けを行い、1.5mm
の篩を通過したものを試験に使用した。得られた繊維状
もしくは針状マグネシウムオキシサルフェートの形状は
長さ5〜20μm、直径0.3〜0.7μmであった。After the reaction, the product was filtered and washed with water to obtain a dehydrated cake of fibrous or acicular magnesium oxysulfate having a water content of 77.6%. This dehydrated cake 112
g and 1,500 g of water were placed in a 3,000 ml beaker, and dispersed for 5 minutes using a homomixer. Next, 500 g of water was added and the mixture was further dispersed for 5 minutes using a homomixer. Furthermore, the dehydrated cake obtained by filtration and having a water content of 77.6% was dried at a temperature of 125° C. for 5 hours. This dried material is easily loosened and sieved through a 1.5 mm sieve.
Those that passed through the sieve were used for the test. The shape of the obtained fibrous or acicular magnesium oxysulfate was 5 to 20 μm in length and 0.3 to 0.7 μm in diameter.
【0037】次に、このようにして得られた繊維状もし
くは針状マグネシウムオキシサルフェート15gとエポ
キシ樹脂■500gとを卓上型ニーダーに入れ25℃に
加熱して減圧下で1時間混合して混合物を製造した。こ
の混合物を予め25℃に加熱しておいた500mlのビ
ーカーに取り出し、25℃に加熱した減圧装置に入れて
減圧し気泡を除去した後、25℃加熱下においてB型粘
度計で粘度を測定した。その結果を表2に示す。Next, 15 g of the fibrous or acicular magnesium oxysulfate thus obtained and 500 g of epoxy resin were placed in a tabletop kneader, heated to 25° C., and mixed for 1 hour under reduced pressure to form a mixture. Manufactured. This mixture was taken out into a 500 ml beaker that had been preheated to 25°C, and the mixture was placed in a vacuum device heated to 25°C to reduce the pressure and remove air bubbles, and then the viscosity was measured using a B-type viscometer while heating at 25°C. . The results are shown in Table 2.
【0038】実施例5
硫酸マグネシウム水溶液に種晶の繊維状もしくは針状マ
グネシウムオキシサルフェートと水酸化マグネシウムス
ラリーを添加して良く分散させた後、分散液をオートク
レーブに入れて温度180℃、圧力10kg/cm2・
Gにて2時間水熱反応を行った。Example 5 After adding fibrous or acicular magnesium oxysulfate seed crystals and magnesium hydroxide slurry to an aqueous magnesium sulfate solution and thoroughly dispersing them, the dispersion was placed in an autoclave at a temperature of 180°C and a pressure of 10 kg/kg. cm2・
A hydrothermal reaction was carried out at G for 2 hours.
【0039】反応後、生成物を濾過し、水洗して水分が
77.6%の繊維状もしくは針状マグネシウムオキシサ
ルフェートの脱水ケーキを得た。この脱水ケーキ112
gと水1500gを3000mlのビーカーに入れ、ホ
モミキサーで5分間分散処理をした。次に、500gの
水に平均分子量200のポリエチレングリコールを12
g加えて調製したポリエチレングリコール水溶液を添加
して、ホモミキサーにて5分間表面処理をした。更に、
濾過し、得られた水分77.7%の脱水ケーキを温度1
25℃で5時間乾燥した。この乾燥物を簡単にほぐし、
1.5mmの篩で篩い分けを行い、1.5mmの篩を通
過したものを試験に使用した。このようにして得られた
繊維状もしくは針状マグネシウムオキシサルフェートの
形状は長さ5〜20μm、直径0.3〜0.7μmであ
った。After the reaction, the product was filtered and washed with water to obtain a dehydrated cake of fibrous or acicular magnesium oxysulfate having a water content of 77.6%. This dehydrated cake 112
g and 1,500 g of water were placed in a 3,000 ml beaker, and dispersed for 5 minutes using a homomixer. Next, add 12% of polyethylene glycol with an average molecular weight of 200 to 500g of water.
A polyethylene glycol aqueous solution prepared by adding g was added thereto, and the surface was treated with a homomixer for 5 minutes. Furthermore,
Filter the resulting dehydrated cake with a moisture content of 77.7% at a temperature of 1
It was dried at 25°C for 5 hours. Easily loosen this dried material,
The material was sieved using a 1.5 mm sieve, and the material that passed through the 1.5 mm sieve was used for the test. The fibrous or acicular magnesium oxysulfate thus obtained had a length of 5 to 20 μm and a diameter of 0.3 to 0.7 μm.
【0040】次に、このようにして得られた繊維状もし
くは針状マグネシウムオキシサルフェート15gを、エ
ポキシ樹脂■500gとエチルアルコール100gとを
混合して調製しておいた混合液と共に卓上型ニーダーに
入れ、25℃に加熱して減圧下で1時間混合して混合物
を製造した。この混合物を予め25℃に加熱しておいた
500mlのビーカーに取り出し、25℃に加熱した減
圧装置に入れて減圧し気泡を除去した後、25℃加熱下
においてB型粘度計で粘度を測定した。その結果を表2
に示す。Next, 15 g of the fibrous or acicular magnesium oxysulfate thus obtained was placed in a tabletop kneader together with a mixed solution prepared by mixing 500 g of epoxy resin (1) and 100 g of ethyl alcohol. , heated to 25° C. and mixed under reduced pressure for 1 hour to prepare a mixture. This mixture was taken out into a 500 ml beaker that had been preheated to 25°C, and the mixture was placed in a vacuum device heated to 25°C to reduce the pressure and remove air bubbles, and then the viscosity was measured using a B-type viscometer while heating at 25°C. . Table 2 shows the results.
Shown below.
【0041】比較例2
硫酸マグネシウム水溶液に種晶の繊維状もしくは針状マ
グネシウムオキシサルフェートと水酸化マグネシウムス
ラリーを添加して良く分散させた後、分散液をオートク
レーブに入れて温度180℃、圧力10kg/cm2・
Gにて2時間水熱反応を行った。Comparative Example 2 After adding fibrous or acicular magnesium oxysulfate seed crystals and magnesium hydroxide slurry to an aqueous magnesium sulfate solution and thoroughly dispersing them, the dispersion was placed in an autoclave at a temperature of 180°C and a pressure of 10 kg/kg. cm2・
A hydrothermal reaction was carried out at G for 2 hours.
【0042】反応後、生成物を濾過し、水洗して水分が
77.6%の繊維状もしくは針状マグネシウムオキシサ
ルフェートの脱水ケーキを得た。この脱水ケーキ112
gと水1500gを3000mlのビーカーに入れ、ホ
モミキサーで5分間分散処理をした。次に、500gの
水を加えてホモミキサーにて更に5分間分散処理をした
。更に、濾過し、得られた水分77.6%の脱水ケーキ
を温度125℃で5時間乾燥した。この乾燥物を簡単に
ほぐし、1.5mmの篩で篩い分けを行い、1.5mm
の篩を通過したものを試験に使用した。得られた繊維状
もしくは針状マグネシウムオキシサルフェートの形状は
長さ5〜20μm、直径0.3〜0.7μmであった。After the reaction, the product was filtered and washed with water to obtain a dehydrated cake of fibrous or acicular magnesium oxysulfate having a water content of 77.6%. This dehydrated cake 112
g and 1,500 g of water were placed in a 3,000 ml beaker, and dispersed for 5 minutes using a homomixer. Next, 500 g of water was added and the mixture was further dispersed for 5 minutes using a homomixer. Furthermore, the dehydrated cake obtained by filtration and having a water content of 77.6% was dried at a temperature of 125° C. for 5 hours. This dried material is easily loosened and sieved through a 1.5 mm sieve.
Those that passed through the sieve were used for the test. The shape of the obtained fibrous or acicular magnesium oxysulfate was 5 to 20 μm in length and 0.3 to 0.7 μm in diameter.
【0043】次に、このようにして得られた繊維状もし
くは針状マグネシウムオキシサルフェート15gを、エ
ポキシ樹脂■500gとエチルアルコール100gとを
混合して調製しておいた混合液と共に卓上型ニーダーに
入れ、25℃に加熱して減圧下で1時間混合して混合物
を製造した。この混合物を予め25℃に加熱しておいた
500mlのビーカーに取り出し、25℃に加熱した減
圧装置に入れて減圧し気泡を除去した後、25℃加熱下
においてB型粘度計で粘度を測定した。その結果を表2
に示す。Next, 15 g of the fibrous or acicular magnesium oxysulfate thus obtained was placed in a tabletop kneader together with a mixed solution prepared by mixing 500 g of epoxy resin (1) and 100 g of ethyl alcohol. , heated to 25° C. and mixed under reduced pressure for 1 hour to prepare a mixture. This mixture was taken out into a 500 ml beaker that had been preheated to 25°C, and the mixture was placed in a vacuum device heated to 25°C to reduce the pressure and remove air bubbles, and then the viscosity was measured using a B-type viscometer while heating at 25°C. . Table 2 shows the results.
Shown below.
【0044】[0044]
【表2】[Table 2]
【0045】実施例6、7
エポキシ樹脂■をエポキシ樹脂■(実施例6)、エポキ
シ樹脂■(実施例7)に代えた以外は実施例4と同様に
混合物を製造し、実施例4と同様に粘度を測定した。そ
の結果を表3に示す。Examples 6 and 7 A mixture was produced in the same manner as in Example 4, except that epoxy resin ■ was replaced with epoxy resin ■ (Example 6) and epoxy resin ■ (Example 7). The viscosity was measured. The results are shown in Table 3.
【0046】比較例3
硫酸マグネシウム水溶液に種晶の繊維状もしくは針状マ
グネシウムオキシサルフェートと水酸化マグネシウムス
ラリーを添加して良く分散させた後、分散液をオートク
レーブに入れて温度180℃、圧力10kg/cm2・
Gにて2時間水熱反応を行った。Comparative Example 3 After adding fibrous or acicular magnesium oxysulfate seed crystals and magnesium hydroxide slurry to an aqueous magnesium sulfate solution and thoroughly dispersing them, the dispersion was placed in an autoclave at a temperature of 180°C and a pressure of 10 kg/kg. cm2・
A hydrothermal reaction was carried out at G for 2 hours.
【0047】反応後、生成物を濾過し、水洗して水分が
77.6%の繊維状もしくは針状マグネシウムオキシサ
ルフェートの脱水ケーキを得た。この脱水ケーキ112
gと水1500gを3000mlのビーカーに入れ、ホ
モミキサーで5分間分散処理をした。次に、500gの
水を加えてホモミキサーにて更に5分間分散処理をした
。更に、濾過し、得られた水分77.6%の脱水ケーキ
を温度125℃で5時間乾燥した。この乾燥物を簡単に
ほぐし、1.5mmの篩で篩い分けを行い、1.5mm
の篩を通過したものを試験に使用した。得られた繊維状
もしくは針状マグネシウムオキシサルフェートの形状は
長さ5〜20μm、直径0.3〜0.7μmであった。After the reaction, the product was filtered and washed with water to obtain a dehydrated cake of fibrous or acicular magnesium oxysulfate having a water content of 77.6%. This dehydrated cake 112
g and 1,500 g of water were placed in a 3,000 ml beaker, and dispersed for 5 minutes using a homomixer. Next, 500 g of water was added and the mixture was further dispersed for 5 minutes using a homomixer. Furthermore, the dehydrated cake obtained by filtration and having a water content of 77.6% was dried at a temperature of 125° C. for 5 hours. This dried material is easily loosened and sieved through a 1.5 mm sieve.
Those that passed through the sieve were used for the test. The shape of the obtained fibrous or acicular magnesium oxysulfate was 5 to 20 μm in length and 0.3 to 0.7 μm in diameter.
【0048】次に、このようにして得られた繊維状もし
くは針状マグネシウムオキシサルフェート15gとエポ
キシ樹脂■500gとを卓上型ニーダーに入れ25℃に
加熱して減圧下で1時間混合して混合物を製造した。こ
の混合物を予め25℃に加熱しておいた500mlのビ
ーカーに取り出し、25℃に加熱した減圧装置に入れて
減圧し気泡を除去した後、25℃加熱下においてB型粘
度計で粘度を測定した。その結果を表3に示す。Next, 15 g of the fibrous or acicular magnesium oxysulfate thus obtained and 500 g of epoxy resin were placed in a tabletop kneader, heated to 25° C., and mixed for 1 hour under reduced pressure to form a mixture. Manufactured. This mixture was taken out into a 500 ml beaker that had been preheated to 25°C, and the mixture was placed in a vacuum device heated to 25°C to reduce the pressure and remove air bubbles, and then the viscosity was measured using a B-type viscometer while heating at 25°C. . The results are shown in Table 3.
【0049】比較例4
硫酸マグネシウム水溶液に種晶の繊維状もしくは針状マ
グネシウムオキシサルフェートと水酸化マグネシウムス
ラリーを添加して良く分散させた後、分散液をオートク
レーブに入れて温度180℃、圧力10kg/cm2・
Gにて2時間水熱反応を行った。Comparative Example 4 After adding fibrous or acicular magnesium oxysulfate seed crystals and magnesium hydroxide slurry to an aqueous magnesium sulfate solution and thoroughly dispersing them, the dispersion was placed in an autoclave at a temperature of 180°C and a pressure of 10 kg/kg. cm2・
A hydrothermal reaction was carried out at G for 2 hours.
【0050】反応後、生成物を濾過し、水洗して水分が
77.6%の繊維状もしくは針状マグネシウムオキシサ
ルフェートの脱水ケーキを得た。この脱水ケーキ112
gと水1500gを3000mlのビーカーに入れ、ホ
モミキサーで5分間分散処理をした。次に、500gの
水を加えてホモミキサーにて更に5分間分散処理をした
。更に、濾過し、得られた水分77.6%の脱水ケーキ
を温度125℃で5時間乾燥した。この乾燥物を簡単に
ほぐし、1.5mmの篩で篩い分けを行い、1.5mm
の篩を通過したものを試験に使用した。得られた繊維状
もしくは針状マグネシウムオキシサルフェートの形状は
長さ5〜20μm、直径0.3〜0.7μmであった。After the reaction, the product was filtered and washed with water to obtain a dehydrated cake of fibrous or acicular magnesium oxysulfate having a water content of 77.6%. This dehydrated cake 112
g and 1,500 g of water were placed in a 3,000 ml beaker, and dispersed for 5 minutes using a homomixer. Next, 500 g of water was added and the mixture was further dispersed for 5 minutes using a homomixer. Furthermore, the dehydrated cake obtained by filtration and having a water content of 77.6% was dried at a temperature of 125° C. for 5 hours. This dried material is easily loosened and sieved through a 1.5 mm sieve.
Those that passed through the sieve were used for the test. The shape of the obtained fibrous or acicular magnesium oxysulfate was 5 to 20 μm in length and 0.3 to 0.7 μm in diameter.
【0051】次に、このようにして得られた繊維状もし
くは針状マグネシウムオキシサルフェート15gとエポ
キシ樹脂■500gとを卓上型ニーダーに入れ25℃に
加熱して減圧下で1時間混合して混合物を製造した。こ
の混合物を予め25℃に加熱しておいた500mlのビ
ーカーに取り出し、25℃に加熱した減圧装置に入れて
減圧し気泡を除去した後、25℃加熱下においてB型粘
度計で粘度を測定した。その結果を表3に示す。Next, 15 g of the fibrous or acicular magnesium oxysulfate thus obtained and 500 g of epoxy resin were placed in a tabletop kneader, heated to 25° C., and mixed for 1 hour under reduced pressure to form a mixture. Manufactured. This mixture was taken out into a 500 ml beaker that had been preheated to 25°C, and the mixture was placed in a vacuum device heated to 25°C to reduce the pressure and remove air bubbles, and then the viscosity was measured using a B-type viscometer while heating at 25°C. . The results are shown in Table 3.
【0052】実施例8、9
硫酸マグネシウム水溶液に種晶の繊維状もしくは針状マ
グネシウムオキシサルフェートと水酸化マグネシウムス
ラリーを添加して良く分散させた後、分散液をオートク
レーブに入れて温度180℃、圧力10kg/cm2・
Gにて2時間水熱反応を行った。Examples 8 and 9 After adding fibrous or acicular magnesium oxysulfate seed crystals and magnesium hydroxide slurry to an aqueous magnesium sulfate solution and thoroughly dispersing them, the dispersion was placed in an autoclave and heated at a temperature of 180°C and a pressure. 10kg/cm2・
A hydrothermal reaction was carried out at G for 2 hours.
【0053】反応後、生成物を濾過し、水洗して水分が
77.6%の繊維状もしくは針状マグネシウムオキシサ
ルフェートの脱水ケーキを得た。この脱水ケーキ112
gと水1500gを3000mlのビーカーに入れ、ホ
モミキサーで5分間分散処理をした。次に、500gの
水にグリセリン12g(実施例8)あるいは平均分子量
200のポリエチレングリコール(実施例9)を加えて
調製したグリセリン水溶液(実施例8)あるいはポリエ
チレングリコール水溶液(実施例9)を添加して、ホモ
ミキサーにて5分間表面処理をした。更に、濾過し、得
られた水分77.7%の脱水ケーキを温度125℃で5
時間乾燥した。この乾燥物を簡単にほぐし、1.5mm
の篩で篩い分けを行い、1.5mmの篩を通過したもの
を試験に使用した。このようにして得られた繊維状もし
くは針状マグネシウムオキシサルフェートの形状は長さ
5〜20μm、直径0.3〜0.7μmであった。After the reaction, the product was filtered and washed with water to obtain a dehydrated cake of fibrous or acicular magnesium oxysulfate having a water content of 77.6%. This dehydrated cake 112
g and 1,500 g of water were placed in a 3,000 ml beaker, and dispersed for 5 minutes using a homomixer. Next, a glycerin aqueous solution (Example 8) or a polyethylene glycol aqueous solution (Example 9) prepared by adding 12 g of glycerin (Example 8) or polyethylene glycol with an average molecular weight of 200 (Example 9) to 500 g of water was added. Then, surface treatment was performed for 5 minutes using a homomixer. Furthermore, the dehydrated cake with a moisture content of 77.7% obtained by filtration was heated at a temperature of 125°C for 5 minutes.
Dry for an hour. Easily loosen this dried material into 1.5mm pieces.
The material that passed through the 1.5 mm sieve was used for the test. The fibrous or acicular magnesium oxysulfate thus obtained had a length of 5 to 20 μm and a diameter of 0.3 to 0.7 μm.
【0054】次に、このようにして得られた繊維状もし
くは針状マグネシウムオキシサルフェート15gとエポ
キシ樹脂■500gとを卓上型ニーダーに入れ25℃に
加熱して減圧下で1時間混合し、更に55℃に昇温して
30分間混合して混合物を製造した。この混合物を予め
55℃に加熱しておいた500mlのビーカーに取り出
し、55℃に加熱した減圧装置に入れて減圧し気泡を除
去した後、55℃加熱下においてB型粘度計で粘度を測
定した。その結果を表3に示す。Next, 15 g of the fibrous or acicular magnesium oxysulfate thus obtained and 500 g of epoxy resin were placed in a tabletop kneader, heated to 25° C., and mixed for 1 hour under reduced pressure. A mixture was prepared by heating the mixture to 0.degree. C. and mixing for 30 minutes. This mixture was taken out into a 500 ml beaker that had been previously heated to 55°C, and the mixture was placed in a vacuum device heated to 55°C to reduce the pressure and remove air bubbles, and then the viscosity was measured using a B-type viscometer while heating at 55°C. . The results are shown in Table 3.
【0055】比較例5
硫酸マグネシウム水溶液に種晶の繊維状もしくは針状マ
グネシウムオキシサルフェートと水酸化マグネシウムス
ラリーを添加して良く分散させた後、分散液をオートク
レーブに入れて温度180℃、圧力10kg/cm2・
Gにて2時間水熱反応を行った。Comparative Example 5 After adding fibrous or acicular magnesium oxysulfate seed crystals and magnesium hydroxide slurry to an aqueous magnesium sulfate solution and thoroughly dispersing them, the dispersion was placed in an autoclave at a temperature of 180°C and a pressure of 10 kg/kg. cm2・
A hydrothermal reaction was carried out at G for 2 hours.
【0056】反応後、生成物を濾過し、水洗して水分が
77.6%の繊維状もしくは針状マグネシウムオキシサ
ルフェートの脱水ケーキを得た。この脱水ケーキ112
gと水1500gを3000mlのビーカーに入れ、ホ
モミキサーで5分間分散処理をした。次に、500gの
水を加えてホモミキサーにて更に5分間分散処理をした
。更に、濾過し、得られた水分77.6%の脱水ケーキ
を温度125℃で5時間乾燥した。この乾燥物を簡単に
ほぐし、1.5mmの篩で篩い分けを行い、1.5mm
の篩を通過したものを試験に使用した。得られた繊維状
もしくは針状マグネシウムオキシサルフェートの形状は
長さ5〜20μm、直径0.3〜0.7μmであった。After the reaction, the product was filtered and washed with water to obtain a dehydrated cake of fibrous or acicular magnesium oxysulfate having a water content of 77.6%. This dehydrated cake 112
g and 1,500 g of water were placed in a 3,000 ml beaker, and dispersed for 5 minutes using a homomixer. Next, 500 g of water was added and the mixture was further dispersed for 5 minutes using a homomixer. Furthermore, the dehydrated cake obtained by filtration and having a water content of 77.6% was dried at a temperature of 125° C. for 5 hours. This dried material is easily loosened and sieved through a 1.5 mm sieve.
Those that passed through the sieve were used for the test. The shape of the obtained fibrous or acicular magnesium oxysulfate was 5 to 20 μm in length and 0.3 to 0.7 μm in diameter.
【0057】次に、このようにして得られた繊維状もし
くは針状マグネシウムオキシサルフェート15gとエポ
キシ樹脂■500gとを卓上型ニーダーに入れ25℃に
加熱して減圧下で1時間混合し、更に55℃に昇温して
30分間混合して混合物を製造した。この混合物を予め
55℃に加熱しておいた500mlのビーカーに取り出
し、55℃に加熱した減圧装置に入れて減圧し気泡を除
去した後、55℃加熱下においてB型粘度計で粘度を測
定した。その結果を表3に示す。Next, 15 g of the fibrous or acicular magnesium oxysulfate thus obtained and 500 g of epoxy resin were placed in a tabletop kneader, heated to 25° C., and mixed for 1 hour under reduced pressure. A mixture was prepared by heating the mixture to 0.degree. C. and mixing for 30 minutes. This mixture was taken out into a 500 ml beaker that had been previously heated to 55°C, and the mixture was placed in a vacuum device heated to 55°C to reduce the pressure and remove air bubbles, and then the viscosity was measured using a B-type viscometer while heating at 55°C. . The results are shown in Table 3.
【0058】[0058]
【表3】[Table 3]
【0059】[0059]
【発明の効果】本発明は、繊維状もしくは針状マグネシ
ウムオキシサルフェートを分子内にアルコール性水酸基
を少なくとも1個有する化合物で表面処理することによ
り、液状ポリマー等と混合して揺変性組成物として利用
する時の分散性が悪い、揺変性が不安定であるという課
題を解決することに成功している。Effects of the Invention The present invention utilizes fibrous or acicular magnesium oxysulfate as a thixotropic composition by surface-treating it with a compound having at least one alcoholic hydroxyl group in the molecule and mixing it with a liquid polymer or the like. We have succeeded in solving the problems of poor dispersibility and unstable thixotropy when dispersing.
Claims (2)
なくとも1個有する化合物で表面処理された長さ0.5
〜50μm、直径0.05〜1μm、アスペクト比(長
さ/直径)10〜300の繊維状もしくは針状マグネシ
ウムオキシサルフェートからなる揺変性付与剤。Claim 1: A molecule having a length of 0.5 and whose surface has been treated with a compound having at least one alcoholic hydroxyl group in the molecule.
A thixotropy imparting agent consisting of fibrous or acicular magnesium oxysulfate having a diameter of ~50 μm, a diameter of 0.05 to 1 μm, and an aspect ratio (length/diameter) of 10 to 300.
なくとも2個有し、且つ炭素数が2以上の化合物で表面
処理された請求項1に記載の繊維状もしくは針状マグネ
シウムオキシサルフェートからなる揺変性付与剤。2. A thixotropic compound comprising the fibrous or acicular magnesium oxysulfate according to claim 1, which has at least two alcoholic hydroxyl groups in its molecule and has been surface-treated with a compound having two or more carbon atoms. agent.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP3242895A JP2803073B2 (en) | 1991-06-18 | 1991-06-18 | Thixotropic agent |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP3242895A JP2803073B2 (en) | 1991-06-18 | 1991-06-18 | Thixotropic agent |
Publications (2)
Publication Number | Publication Date |
---|---|
JPH04370188A true JPH04370188A (en) | 1992-12-22 |
JP2803073B2 JP2803073B2 (en) | 1998-09-24 |
Family
ID=17095818
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
JP3242895A Expired - Fee Related JP2803073B2 (en) | 1991-06-18 | 1991-06-18 | Thixotropic agent |
Country Status (1)
Country | Link |
---|---|
JP (1) | JP2803073B2 (en) |
Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPS5996153A (en) * | 1982-11-25 | 1984-06-02 | Ube Ind Ltd | Vinyl chloride resin molding material |
JPS6291547A (en) * | 1985-10-18 | 1987-04-27 | Idemitsu Petrochem Co Ltd | Polypropylene resin composition |
JPS63314276A (en) * | 1987-04-01 | 1988-12-22 | ダブリユー・アール・グレイス・アンド・カンパニー−コネチカツト | Improvemant on rheology characteristics of organic liquid |
JPH01224041A (en) * | 1988-03-04 | 1989-09-07 | Mizusawa Ind Chem Ltd | Rheology modifier |
-
1991
- 1991-06-18 JP JP3242895A patent/JP2803073B2/en not_active Expired - Fee Related
Patent Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPS5996153A (en) * | 1982-11-25 | 1984-06-02 | Ube Ind Ltd | Vinyl chloride resin molding material |
JPS6291547A (en) * | 1985-10-18 | 1987-04-27 | Idemitsu Petrochem Co Ltd | Polypropylene resin composition |
JPS63314276A (en) * | 1987-04-01 | 1988-12-22 | ダブリユー・アール・グレイス・アンド・カンパニー−コネチカツト | Improvemant on rheology characteristics of organic liquid |
JPH01224041A (en) * | 1988-03-04 | 1989-09-07 | Mizusawa Ind Chem Ltd | Rheology modifier |
Also Published As
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JP2803073B2 (en) | 1998-09-24 |
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