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1. 发明专利

JPH05178794A BIFUNCTIONAL (METH)ACRYLATE 失效
公开(公告)号：JPH05178794A
公开(公告)日：1993-07-20
申请号：JP34486091
申请日：1991-12-26
申请人： TOKUYAMA SODA KK
发明人： AIZAWA MASAYUKI , SATO TAKESHI
IPC分类号： C07C69/92 , C07C269/02 , C07C271/16 , C08F20/10 , C08F20/30 , C08F290/00 , C08F299/06
摘要： PURPOSE:To obtain the subject new compound useful as a material for providing a polymer having excellent physical strength and durability, especially by blending the compound with an inorganic filler and a radical polymerization initiator to provide a dental filler having excellent strength. CONSTITUTION:A bifunctional (meth)acrylate of formula I (R1 is H or CH3; (1) is 0 or 1; (m) is 2-4; (n) is 2-12) such as a compound of formula II. This compound is obtained by reacting a 4-hydroxybenzoic acid of formula III with a reactant such as KOH in a solvent such as alcohol to convert into a salt, etherifying the salt with a halogenated alcohol of the formula X-(CH2)n-OH (X is halogen) and reacting a prepared compound of formula IV with an isocyanatoalkyl (meth)acrylate of formula V (R2 is H or CH3) in a solvent in the presence of a basic catalyst such as pyridine.

2. 发明专利

JPH05170705A RADICALLY POLYMERIZABLE BIFUNCTIONAL (METH)ACRYLATE 失效
公开(公告)号：JPH05170705A
公开(公告)日：1993-07-09
申请号：JP34150991
申请日：1991-12-24
申请人： TOKUYAMA SODA KK
发明人： AIZAWA MASAYUKI , SATO TAKESHI , KAWAGUCHI TOSHIO
IPC分类号： C07C69/76 , C07C269/02 , C07C271/16 , C08F20/10 , C08F20/30
摘要： PURPOSE:To provide a new radically polymerizable (meth)acrylate useful as a monomer for the production of a polymer or copolymer having excellent physical strength and durability. CONSTITUTION:The radically polymerizable bifunctional (meth)acrylate of formula I (R is H or CH3; (1) is 0 or 1; (m) is 2-4; (n) is 2-12). The compound of formula I can be produced e.g. by reacting an alkyl diol of formula II with (meth) acryloyl chloride or an isocyanatoalkyl (meth)acrylate of formula III (R2 is R1) and reacting the resultant compound of formula IV with the compound of formula V.

3. 发明专利

JPH05170704A (METH)ACRYLATE 失效
公开(公告)号：JPH05170704A
公开(公告)日：1993-07-09
申请号：JP34150891
申请日：1991-12-24
申请人： TOKUYAMA SODA KK
发明人： KAWAGUCHI TOSHIO , SATO TAKESHI , AIZAWA MASAYUKI
IPC分类号： C07C69/76 , C08F20/10 , C08F20/30
摘要： PURPOSE:To provide a new (meth)acrylate useful as a monomer for the production of a polymer or copolymer having excellent physical strength and durability. CONSTITUTION:The (meth)acrylate of formula I (R is H or CH3; (h) is 2 or 3; (1) is 0 or 1), e.g. the compound of formula II. The compound of formula I can be produced e.g. by reacting a polyfunctional (meth)acrylate of formula III (R1 is CH3; (h) is 2; (i) is 0 or 1) with the compound of formula IV in the presence of a proper basic catalyst.

4. 发明专利

JPH06345614A DENTAL FILLING AND RESTORING MATERIAL AND RESIN COMPOSITION FOR DENTURE BASE 失效
公开(公告)号：JPH06345614A
公开(公告)日：1994-12-20
申请号：JP20917693
申请日：1993-08-24
申请人： TOKUYAMA SODA KK
发明人： AIZAWA MASAYUKI , KAWAGUCHI TOSHIO
IPC分类号： A61K6/00 , A61K6/083
摘要： PURPOSE:To obtain a dental hardenable material not only excellent in mechanical strength but also effective in preventing discoloration due to the adsorption of colored components by using an alpha-aminoacetophenone-based photopolymerization initiator as a photopolymerization initiator. CONSTITUTION:The dental filling and restoring material contains (A) 100 pts.wt. polyfunctional acrylate-based monomer, e.g. a mixture of 60 pts.wt. 2,2-bis[4-(3- methacryloxy-2-hydroxypropoxy)phenyl]propane with 40 pts.wt. triethylene glycol dimethacrylate, (B) 100-900 pts.wt. inorganic filler, e.g. a silica-zirconia- based spherical particle and (C) 0.01-10 pts.wt. alpha-aminoacetophenone-based photopolymerization initiator, e.g. 2-benzyl-2-dimethylamino-1-(4-morpholinophenyl)- butanone-1. Furthermore, the resin composition for a denture base contains 50-500 pts.wt. organic filler as the component (B). This material is polymerized and cured by irradiation of light having 250-600nm wavelength region. When a higher curing depth is required, an alpha-diketone, especially camphorquinone is preferably used in combination.

5. 发明专利

JPH03197311A PRODUCTION OF METALLIC OXIDE PARTICLE 失效
公开(公告)号：JPH03197311A
公开(公告)日：1991-08-28
申请号：JP33286189
申请日：1989-12-25
申请人： TOKUYAMA SODA KK
发明人： AIZAWA MASAYUKI , YUASA SHIGEKI
IPC分类号： B02C19/06 , C01B13/32 , C01B33/158 , C01B33/18 , C01B33/20 , C07F7/00 , C07F7/02 , C09C1/00
摘要： PURPOSE:To improve production efficiency by hydrolyzing hydrolyzable organosilicon compound or a mixture of organosilicon compound and organometallic compound of group IV of the periodic table in a specific alcohol to give a gelatinized substance, grinding and burning. CONSTITUTION:A hydrolyzable organosilicon compound shown by formula I (OR1 is 1-5C alkoxy) such as tetraethyl silicate or a low condensed organosilicon compound which is partially hydrolyzed to give a molar ratio of the total amount of dimer, trimer and oligomers to monomer of 0.1 to 9.9 is blended with an organometallic compound of group IV of the periodic table shown by formula II (M is Ti, Zr, etc., R1-5 are 1-5C alkoxyl or halogen) such as tetrabutyl zirconate in the molar ratio of (1:3). Then the mixture is dissolved in 4-10C alcohol such as n-butyl alcohol, blended with water in an amount to give a molar ratio of water to the whole hydrolyzable substance of 1.3 to 3.0 and treated at 100-150 deg.C into a gelatinized substance. The gelatinized substance is dried, ground by jet into =2mum average particle diameter.

6. 发明专利

JPH05229990A BIFUNCTIONAL (METH)ACRYLATE 失效
公开(公告)号：JPH05229990A
公开(公告)日：1993-09-07
申请号：JP3209492
申请日：1992-02-19
申请人： TOKUYAMA SODA KK
发明人： AIZAWA MASAYUKI , SATO TAKESHI , KAWAGUCHI TOSHIO
IPC分类号： C07C69/54 , C07C271/16
摘要： PURPOSE:To provide a new bifunctional (meth)acrylate containing naphthalene group and plural methacryl groups and urethane bonds in the molecule, exhibiting radical polymerizability and giving a polymer having excellent physical strength and durability. CONSTITUTION:The objective new bifunctional (meth)acrylate radially polymerizable to give a polymer having excellent physical strength and durability and expressed by formula V (R is H or methyl; (h) is 0 or 1) can be produced by heating and refluxing 2,6-dihydroxynaphthalene of formula I and a halogenated alcohol of formula II (X is Cl or Br; (n) is 2-12) (e.g. 4-bromo-1- butanol) in acetone in the presence of potassium carbonate for 30hr, reacting with a glycol of formula III and reacting the reaction product with an isocyanatoalkyl (meth)acrylate of formula IV (R is H or methyl; (m) is 2-4) or (meth)acrylic chloride, etc.

7. 发明专利

JPH02132102A CURABLE COMPOSITION 失效
公开(公告)号：JPH02132102A
公开(公告)日：1990-05-21
申请号：JP16783888
申请日：1988-07-07
申请人： TOKUYAMA SODA KK
发明人： YUASA SHIGEKI , KUSUMOTO KOJI , AIZAWA MASAYUKI
IPC分类号： A61K6/083 , A61K6/884 , A61K6/891 , C08F2/44 , C09D4/00
摘要： PURPOSE:To provide the title composition which is used as a repairing material for dental purpose, because it has high mechanical strength, especially very high bending strength by adding amorphous inorganic particles having specific particle size and properties and spherical inorganic particles of a specific particle size to polymerizable monomers. CONSTITUTION:The subject composition is obtained by using (A) polymerizable monomers. (B) amorphous inorganic particles which is at least partially amorphous, has 1-9mum average particle size, is occupied with more than 95wt.% of particles of 1 to 10mum. (C) spherical inorganic particles of 0.08 to 1mum average particle size, and (D) a polymerization initiator so that the total amount of components B and C becomes 300 to 900 pts.wt. per 100 pts.wt. of component A, and the weight ratio of B/C becomes 1 to 4. The component B is preferably an inorganic oxide such as silica and inorganic oxide conjugate. Component C is preferably a inorganic oxide, its conjugate, quartz or silicon nitride.

8. 发明专利

JPH0651735B2 失效
公开(公告)号：JPH0651735B2
公开(公告)日：1994-07-06
申请号：JP16783888
申请日：1988-07-07
申请人： TOKUYAMA SODA KK
发明人： YUASA SHIGEKI , KUSUMOTO KOJI , AIZAWA MASAYUKI
IPC分类号： A61K6/083 , A61K6/884 , A61K6/891 , C08F2/44 , C09D4/00

9. 发明专利

JPH0365506A HYDROPHOBIC INORGANIC PARTICLE 失效
公开(公告)号：JPH0365506A
公开(公告)日：1991-03-20
申请号：JP19927489
申请日：1989-08-02
申请人： TOKUYAMA SODA KK
发明人： AIZAWA MASAYUKI , YUASA SHIGEKI
IPC分类号： C01B33/18 , A61K6/884 , C01B13/14 , C01B21/06 , C09C3/12
摘要： PURPOSE:To improve the coloring resistance, hydrophobic properly and discoloration resistance of an inorganic filler by bonding a specific long chain silane coupling agent and a specified short chain silane coupling agent to the surface of the inorganic filler. CONSTITUTION:Inorganic filler particles are brought into contact with the primary amine or secondary amine in an inert solvent, subjected to the removal of the inert solvent and subsequently dried. 100 pts.wt. of the treated inorganic filler particles are brought into contact with (a) a long chain silane coupling agent of formula I (A is vinyl or isopropyl; B is a functional group linearly combined with at least two atoms; X1 is alkoxy or halogen) and (b) a short chain silane coupling agent in the presence of 200-2000 pts.wt. of an inert solvent (e.g. methanol) to bond the component (a) in an amount of 0.31X10 -2.5X10 mol/m and the component (b) in an amount of 5-50mol% based on the bonding amount of the component (a) to the surface of the inorganic filler particles.

10. 发明专利

JPH06157230A PRODUCTION OF INORGANIC FILLER AND DENTAL FILLING/ REPAIRING MATERIAL 失效
公开(公告)号：JPH06157230A
公开(公告)日：1994-06-03
申请号：JP31022892
申请日：1992-11-19
申请人： TOKUYAMA SODA KK
发明人： AIZAWA MASAYUKI , KAWAGUCHI TOSHIO
IPC分类号： A61K6/884 , A61K6/08
摘要： PURPOSE:To obtain an inorganic filler for dental filling/repairing materials of high mechanical strength and having gloss comparable to that of human teeth by mixing silica-based metallic oxides having at least two kinds of mean particle diameter followed by baking at a specified temperature. CONSTITUTION:Unbaked silica-based multiple oxides having at least two kinds of mean diameter with the mean particle diameter ratio of 4 to 20 are mixed and the resulting mixture is baked at a temperature below the sintering temperature (pref. 700-1100 deg.C) to obtain the objective filler. For this filler, respective particles are homogeneously dispersed and mixed; therefore, being fillable in high density. Furthermore, this filler can be used for dental filling/repairing materials not only excellent in surface smoothness and gloss but also having excellent physical properties. It is preferable that the range of the mean particle diameter for the filler fall between 0.01 and 100mum. The mixing operation can be made using a dispersion medium such as methanol, acetonitrile or water, with e.g. a ball mill, vibratory ball mill, attrition mill, grinder, hybridizer with high-speed jet stream method.

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