JP2016030753A5 - - Google Patents

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JP2016030753A5
JP2016030753A5 JP2015051943A JP2015051943A JP2016030753A5 JP 2016030753 A5 JP2016030753 A5 JP 2016030753A5 JP 2015051943 A JP2015051943 A JP 2015051943A JP 2015051943 A JP2015051943 A JP 2015051943A JP 2016030753 A5 JP2016030753 A5 JP 2016030753A5
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composite material
filler
polymerizable monomer
silane
silane treatment
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JP2015051943A
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JP2016030753A (en
JP6274582B2 (en
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フィラー、重合性単量体、重合開始剤を含む複合材料の製造方法であって、
下記に示される混合重合性単量体作製工程、シラン処理工程、シラン処理フィラー保存工程、複合材料製造工程を経ることを特徴とする複合材料の製造方法。
・混合重合性単量体作製工程とは、重合性単量体と重合開始剤を混合し混合重合性単量体を作製する工程、
・シラン処理工程とは、シランカップリング剤1〜40%と有機溶媒及び/または水99〜60%を混合したシラン処理液を作製し、混合容器中にフィラーを投入し1〜60℃の範囲で、混合時間は1分〜24時間であり、フィラーの量に対してシランカップリング剤を1〜15%に相当するシラン処理液を混合中に滴下することでシラン処理フィラーを製造する工程、
・シラン処理フィラー保存工程とは、シラン処理されたシラン処理フィラーを30〜600日保存する工程、
・複合材料製造工程とは、混合重合性単量体とシラン処理フィラーを混合し複合材料を製造する工程。
A method for producing a composite material including a filler, a polymerizable monomer, and a polymerization initiator,
The manufacturing method of the composite material characterized by passing through the mixed polymerizable monomer preparation process shown below, a silane processing process, a silane processing filler preservation | save process, and a composite material manufacturing process.
The mixed polymerizable monomer preparation step is a step of mixing a polymerizable monomer and a polymerization initiator to prepare a mixed polymerizable monomer,
The silane treatment step is to produce a silane treatment liquid in which 1 to 40% of a silane coupling agent and 99 to 60% of an organic solvent and / or water are mixed, and a filler is put into a mixing container to be in a range of 1 to 60 ° C. The mixing time is 1 minute to 24 hours, and the step of producing a silane-treated filler by dropping a silane treatment agent corresponding to 1 to 15% of the silane coupling agent with respect to the amount of the filler during mixing,
-The silane treatment filler storage step is a step of storing the silane treated silane treatment filler for 30 to 600 days,
-The composite material manufacturing process is a process of manufacturing a composite material by mixing a mixed polymerizable monomer and a silane-treated filler.
前記複合材料製造工程において、混合重合性単量体1重量部中にシラン処理フィラー0.1〜9重量部の投入後、5〜60℃にて混合時間は5〜40分間の条件でシラン処理フィラー混練工程を行い、その後に5〜200Torrにて脱泡時間は5〜30分の条件で、混合重合性単量体とシラン処理フィラーを混練しながら脱泡を行うことを特徴とする請求項1に記載の複合材料の製造方法。   In the composite material manufacturing process, after adding 0.1 to 9 parts by weight of the silane treatment filler in 1 part by weight of the mixed polymerizable monomer, the silane treatment is performed at 5 to 60 ° C. for 5 to 40 minutes. The filler kneading step is performed, and then defoaming is performed while kneading the mixed polymerizable monomer and the silane-treated filler at 5 to 200 Torr and a defoaming time of 5 to 30 minutes. 2. A method for producing a composite material according to 1. 前記複合材料製造工程において、混合重合性単量体1重量部中に微粒子フィラー0.01〜0.2重量部の投入後、5〜60℃にて混合時間は5〜30分間の条件で混合重合性単量体と微粒子フィラーの混練を行い、その後に5〜200Torrにて脱泡時間は5〜30分の条件で混合重合性単量体と微粒子フィラーの脱泡を行い、更にシラン処理フィラー0.1〜9重量部の投入後、5〜60℃にて混合時間は5〜40分間の条件で混合重合性単量体と微粒子フィラー、シラン処理フィラーの混練を行い、その後に5〜200Torrにて脱泡時間は5〜30分の条件で混合重合性単量体と微粒子フィラー、シラン処理フィラーを混練しながら脱泡を行うことを特徴とする請求項1に記載の複合材料の製造方法。   In the composite material manufacturing step, after adding 0.01 to 0.2 part by weight of the fine particle filler in 1 part by weight of the mixed polymerizable monomer, mixing is performed at 5 to 60 ° C. for 5 to 30 minutes. The polymerizable monomer and the fine particle filler are kneaded, and then the mixed polymerizable monomer and the fine particle filler are defoamed at 5 to 200 Torr and the defoaming time is 5 to 30 minutes. After the addition of 0.1 to 9 parts by weight, the mixed polymerizable monomer, the fine particle filler, and the silane-treated filler are kneaded at 5 to 60 ° C. for 5 to 40 minutes, and thereafter 5 to 200 Torr. The method for producing a composite material according to claim 1, wherein the defoaming time is 5 to 30 minutes while the mixed polymerizable monomer, the fine particle filler, and the silane-treated filler are kneaded. . 前記混合重合性単量体作製工程において、混合温度は1〜60℃、混合時間は1分〜24時間であることを特徴とする請求項1〜3のいずれか一項に記載の複合材料の製造方法。   In the said mixed polymerizable monomer preparation process, mixing temperature is 1-60 degreeC and mixing time is 1 minute-24 hours, The composite material as described in any one of Claims 1-3 characterized by the above-mentioned. Production method. 前記複合材料製造工程終了後、さらに下記に示される複合材料保存工程を経ることを特徴とする請求項1〜4のいずれか一項に記載の複合材料の製造方法。
・複合材料保存工程とは、複合材料製造工程で製造された1〜8リットルの複合材料を、保存温度は1〜25℃、保存期間は10日〜1.5年以内にて保存する工程。
5. The method for producing a composite material according to claim 1, further comprising a composite material storage step shown below after the completion of the composite material production step. 6.
The composite material storage step is a step of storing 1 to 8 liters of composite material manufactured in the composite material manufacturing step within a storage temperature of 1 to 25 ° C. and a storage period of 10 days to 1.5 years.
前記複合材料保存工程中に、複合材料評価工程を有することを特徴とする請求項5に記載の複合材料の製造方法。   6. The method for producing a composite material according to claim 5, further comprising a composite material evaluation step in the composite material storage step. 前記複合材料保存工程終了後、さらに下記に示される複合材料充填工程を経ることを特徴とする請求項5または6に記載の複合材料の製造方法。
・複合材料充填工程とは、充填機を用いてノズルから押し出された複合材料を、容量1〜50ccである少量保存容器に充填する工程。
The composite material manufacturing method according to claim 5 or 6, further comprising a composite material filling step described below after the composite material storage step.
A composite material filling step is a step of filling a small amount storage container having a capacity of 1 to 50 cc with a composite material extruded from a nozzle using a filling machine.
前記混合重合性単量体保存工程中に、混合重合性単量体評価工程を有することを特徴とする請求項1〜7のいずれか一項に記載の複合材料の製造方法。   The method for producing a composite material according to any one of claims 1 to 7, further comprising a mixed polymerizable monomer evaluation step in the mixed polymerizable monomer storage step. 請求項1〜8のいずれか一項に記載の複合材料の製造方法により製造される複合材料であって、前記複合材料は、製造終了120日後のフロー値をaとし、製造終了3年後のフロー値をbとして、フロー値の減少率(a-b)/aは10%以下であることを特徴とする複合材料。   It is a composite material manufactured by the manufacturing method of the composite material as described in any one of Claims 1-8, Comprising: The said composite material sets a flow value 120 days after manufacture completion as a, 3 years after completion of manufacture A composite material, wherein a flow value is b, and a flow rate reduction rate (ab) / a is 10% or less. フィラー、重合性単量体、重合開始剤を含む複合材料において、
重合性単量体と重合開始剤を混合し混合重合性単量体を作製する混合重合性単量体作製工程、
混合重合性単量体を保存容器内で保存する混合重合性単量体保存工程、
フィラーにシラン処理をして、シラン処理フィラーを作製するシラン処理工程、
シラン処理フィラーを保存容器にて保存するシラン処理フィラー保存工程、
混合重合性単量体とシラン処理フィラーを混合し複合材料を製造する複合材料製造工程、
複合材料を保存容器内で保存する複合材料保存工程、
複合材料を少量保存容器に充填する複合材料充填工程、
充填された少量保存容器で保存する少量保存容器保存工程を経て得られる複合材料であって、
前記複合材料は、製造終了120日後のフロー値をaとし、製造終了3年後のフロー値をbとして、フロー値の減少率(a-b)/aは10%以下であることを特徴とする複合材料。
In a composite material containing a filler, a polymerizable monomer, and a polymerization initiator,
A mixed polymerizable monomer preparation step of preparing a mixed polymerizable monomer by mixing a polymerizable monomer and a polymerization initiator;
A mixed polymerizable monomer storage step for storing the mixed polymerizable monomer in a storage container;
A silane treatment process for producing a silane treatment filler by silane treatment on the filler,
Silane treatment filler storage step of storing the silane treatment filler in a storage container,
A composite material manufacturing process for manufacturing a composite material by mixing a mixed polymerizable monomer and a silane treatment filler,
A composite material storage process for storing the composite material in a storage container;
Composite material filling process for filling a small amount of composite material into a storage container,
A composite material obtained through a small-volume storage container storage process for storing in a filled small-volume storage container,
The composite material is characterized in that a flow value after 120 days from the end of production is a, a flow value after 3 years from the end of production is b, and the rate of decrease in flow value (ab) / a is 10% or less. material.
フィラー、重合性単量体、重合開始剤を含む複合材料において、
重合性単量体と重合開始剤を混合し混合重合性単量体を作製する混合重合性単量体作製工程、
フィラーにシラン処理をして、シラン処理フィラーを作製するシラン処理工程、
シラン処理フィラーを保存容器にて保存するシラン処理フィラー保存工程、
混合重合性単量体とシラン処理フィラーを混合し複合材料を製造する複合材料製造工程、
複合材料を少量保存容器に充填する複合材料充填工程、
充填された少量保存容器で保存する少量保存容器保存工程を経て得られる複合材料であって、
複合材料製造工程に、微粒子フィラー混練工程及び微粒子フィラー混練後脱泡工程、シラン処理フィラー混練工程およびシラン処理フィラー混練後脱泡工程を行う工程を経り、
前記複合材料は、製造終了120日後のフロー値をaとし、製造終了3年後のフロー値をbとして、フロー値の減少率(a-b)/aは10%以下であることを特徴とする複合材料。
In a composite material containing a filler, a polymerizable monomer, and a polymerization initiator,
A mixed polymerizable monomer preparation step of preparing a mixed polymerizable monomer by mixing a polymerizable monomer and a polymerization initiator;
A silane treatment process for producing a silane treatment filler by silane treatment on the filler,
Silane treatment filler storage step of storing the silane treatment filler in a storage container,
A composite material manufacturing process for manufacturing a composite material by mixing a mixed polymerizable monomer and a silane treatment filler,
Composite material filling process for filling a small amount of composite material into a storage container,
A composite material obtained through a small-volume storage container storage process for storing in a filled small-volume storage container,
Through the composite material manufacturing process, the fine particle filler kneading step and the fine particle filler kneading defoaming step, the silane treatment filler kneading step and the silane treatment filler kneading defoaming step,
The composite material is characterized in that a flow value after 120 days from the end of production is a, a flow value after 3 years from the end of production is b, and the rate of decrease in flow value (ab) / a is 10% or less. material.
請求項9〜11のいずれか一項に記載の複合材料を歯科に用いる応用。
The application which uses the composite material as described in any one of Claims 9-11 for dentistry.
JP2015051943A 2015-03-16 2015-03-16 Dental material with stable paste properties Active JP6274582B2 (en)

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Family Cites Families (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH08143747A (en) * 1994-11-24 1996-06-04 San Medical Kk Composite filler, its production, and dental resin composition produced by using the same
JP3495171B2 (en) * 1996-01-25 2004-02-09 サンメディカル株式会社 Dental filling composition
WO2007088628A1 (en) * 2006-02-03 2007-08-09 Kabushiki Kaisha Shofu Composite resin cement for dental use, primer for dental use and adhesive kit for dental use containing the same
JP2009067746A (en) * 2007-09-14 2009-04-02 Shiyoufuu:Kk One-pack type dental adhesive composition
JP5276916B2 (en) * 2008-07-08 2013-08-28 株式会社松風 Dental two-paste self-adhesive resin cement
JP4447048B2 (en) * 2009-02-23 2010-04-07 株式会社松風 Dental adhesives using tin compounds
JP5769429B2 (en) * 2011-01-26 2015-08-26 株式会社トクヤマデンタル Dental composite restoration material

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