JP6779935B2 - Dental pretreatment agent and its manufacturing method - Google Patents
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- 238000004519 manufacturing process Methods 0.000 title claims description 6
- 239000003795 chemical substances by application Substances 0.000 claims description 68
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 64
- 239000002245 particle Substances 0.000 claims description 52
- 239000011163 secondary particle Substances 0.000 claims description 34
- 239000011260 aqueous acid Substances 0.000 claims description 33
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 31
- 238000004898 kneading Methods 0.000 claims description 29
- 239000003085 diluting agent Substances 0.000 claims description 10
- 239000000243 solution Substances 0.000 description 39
- 239000002253 acid Substances 0.000 description 15
- 239000007788 liquid Substances 0.000 description 15
- 238000000926 separation method Methods 0.000 description 15
- 239000000203 mixture Substances 0.000 description 14
- 230000000052 comparative effect Effects 0.000 description 12
- 239000007864 aqueous solution Substances 0.000 description 11
- 229910002013 Aerosil® 90 Inorganic materials 0.000 description 10
- 229910002014 Aerosil® 130 Inorganic materials 0.000 description 9
- 238000009826 distribution Methods 0.000 description 7
- 239000000945 filler Substances 0.000 description 7
- 239000011164 primary particle Substances 0.000 description 7
- OFOBLEOULBTSOW-UHFFFAOYSA-N Malonic acid Chemical compound OC(=O)CC(O)=O OFOBLEOULBTSOW-UHFFFAOYSA-N 0.000 description 5
- 208000002925 dental caries Diseases 0.000 description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 5
- 229910002012 Aerosil® Inorganic materials 0.000 description 4
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 4
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 3
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 description 3
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 3
- 239000012153 distilled water Substances 0.000 description 3
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 description 2
- 208000002599 Smear Layer Diseases 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- DTQVDTLACAAQTR-UHFFFAOYSA-N Trifluoroacetic acid Chemical compound OC(=O)C(F)(F)F DTQVDTLACAAQTR-UHFFFAOYSA-N 0.000 description 2
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 2
- 239000001055 blue pigment Substances 0.000 description 2
- 150000001732 carboxylic acid derivatives Chemical class 0.000 description 2
- JXTHNDFMNIQAHM-UHFFFAOYSA-N dichloroacetic acid Chemical compound OC(=O)C(Cl)Cl JXTHNDFMNIQAHM-UHFFFAOYSA-N 0.000 description 2
- 229910021485 fumed silica Inorganic materials 0.000 description 2
- 229910002011 hydrophilic fumed silica Inorganic materials 0.000 description 2
- JVTAAEKCZFNVCJ-UHFFFAOYSA-N lactic acid Chemical compound CC(O)C(O)=O JVTAAEKCZFNVCJ-UHFFFAOYSA-N 0.000 description 2
- 238000007561 laser diffraction method Methods 0.000 description 2
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 description 2
- 238000000790 scattering method Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 description 1
- FEWJPZIEWOKRBE-JCYAYHJZSA-N Dextrotartaric acid Chemical compound OC(=O)[C@H](O)[C@@H](O)C(O)=O FEWJPZIEWOKRBE-JCYAYHJZSA-N 0.000 description 1
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
- FOCAUTSVDIKZOP-UHFFFAOYSA-N chloroacetic acid Chemical compound OC(=O)CCl FOCAUTSVDIKZOP-UHFFFAOYSA-N 0.000 description 1
- 239000000805 composite resin Substances 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 210000004268 dentin Anatomy 0.000 description 1
- 229910003460 diamond Inorganic materials 0.000 description 1
- 239000010432 diamond Substances 0.000 description 1
- 229960005215 dichloroacetic acid Drugs 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 235000019253 formic acid Nutrition 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- 239000003178 glass ionomer cement Substances 0.000 description 1
- 239000004310 lactic acid Substances 0.000 description 1
- 235000014655 lactic acid Nutrition 0.000 description 1
- VZCYOOQTPOCHFL-UPHRSURJSA-N maleic acid Chemical compound OC(=O)\C=C/C(O)=O VZCYOOQTPOCHFL-UPHRSURJSA-N 0.000 description 1
- 239000011976 maleic acid Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 150000007522 mineralic acids Chemical class 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 150000007524 organic acids Chemical class 0.000 description 1
- 235000006408 oxalic acid Nutrition 0.000 description 1
- 239000000049 pigment Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 210000003296 saliva Anatomy 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000000527 sonication Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 229940095064 tartrate Drugs 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- VZCYOOQTPOCHFL-UHFFFAOYSA-N trans-butenedioic acid Natural products OC(=O)C=CC(O)=O VZCYOOQTPOCHFL-UHFFFAOYSA-N 0.000 description 1
- YNJBWRMUSHSURL-UHFFFAOYSA-N trichloroacetic acid Chemical compound OC(=O)C(Cl)(Cl)Cl YNJBWRMUSHSURL-UHFFFAOYSA-N 0.000 description 1
- 229920003169 water-soluble polymer Polymers 0.000 description 1
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- Dental Preparations (AREA)
Description
本発明は、歯科用前処理剤及び歯科用前処理剤の製造方法に関する。 The present invention relates to a dental pretreatment agent and a method for producing a dental pretreatment agent.
歯科治療において、ダイヤモンドポイント等を用いて、歯牙のう蝕部を切削して窩洞を形成した後、グラスアイオノマーセメント、コンポジットレジン等の充填材を用いて、窩洞に充填する保存修復治療が日常的に実施されている。ここで、充填材が窩洞内の歯質と強固に接着していないと、充填材が脱離する。また、充填材が脱離しなくても、窩洞と充填材の間に間隙が存在すると、二次う蝕が発症する可能性が高い。このため、充填材と窩洞内の歯質との間の接着性は、保存修復治療を成功させる上で、重要な要因の一つである。 In dental treatment, it is common practice to use diamond points to cut the carious part of the tooth to form a cavity, and then to fill the cavity with a filler such as glass ionomer cement or composite resin. It is carried out in. Here, if the filler is not firmly adhered to the tooth substance in the tooth cavity, the filler is detached. In addition, even if the filler is not detached, if there is a gap between the cavity and the filler, secondary caries is likely to occur. Therefore, the adhesion between the filler and the tooth substance in the tooth cavity is one of the important factors for the success of the conservative restoration treatment.
しかしながら、歯牙のう蝕部を切削して窩洞を形成する際に、切削屑、唾液等が歯面に擦り付けられ、厚さ１〜５μｍのスメアー層が形成される。このため、充填材と窩洞内の歯質との間の接着性を向上させるためには、スメアー層を除去する必要がある。 However, when the carious portion of the tooth is cut to form a tooth cavity, cutting chips, saliva, etc. are rubbed against the tooth surface to form a smear layer having a thickness of 1 to 5 μm. Therefore, it is necessary to remove the smear layer in order to improve the adhesion between the filler and the dentin in the tooth cavity.
特許文献１には、ヒュームドシリカが酸水溶液に分散されてなる歯科用前処理剤が開示されている。ここで、ヒュームドシリカは、平均一次粒子径が５〜１００ｎｍである。また、歯科用前処理剤を蒸留水に分散させたものをレーザー回折散乱法で測定した際に、ｉ）〜ｉｉｉ）の凝集二次粒子性状を満足して分散する。 Patent Document 1 discloses a dental pretreatment agent in which fumed silica is dispersed in an aqueous acid solution. Here, fumed silica has an average primary particle size of 5 to 100 nm. Further, when the dental pretreatment agent dispersed in distilled water is measured by a laser diffraction / scattering method, the aggregated secondary particle properties of i) to iii) are satisfied and dispersed.
ｉ）凝集二次粒子の体積平均粒子径が５〜５０μｍである。 i) The volume average particle diameter of the aggregated secondary particles is 5 to 50 μm.
ｉｉ）体積粒子径が１μｍ以下の凝集二次粒子の体積％が２０％以下である。 ii) The volume% of the aggregated secondary particles having a volume particle diameter of 1 μm or less is 20% or less.
ｉｉｉ）体積粒子径が１００μｍ以上の凝集二次粒子の体積％が５％以下である。 iii) The volume% of the aggregated secondary particles having a volume particle diameter of 100 μm or more is 5% or less.
しかしながら、シリンジに装着した吐出用チップの目詰まり及び液分離が発生するという問題がある。 However, there is a problem that the ejection tip attached to the syringe is clogged and liquid separation occurs.
本発明の一態様は、シリンジに装着した吐出用チップの目詰まり及び液分離の発生を抑制することが可能な歯科用前処理剤を提供することを目的とする。 One aspect of the present invention is to provide a dental pretreatment agent capable of suppressing clogging of a discharge tip attached to a syringe and occurrence of liquid separation.
本発明の一態様は、シリカ粒子及び／又はアルミナ粒子が凝集している凝集二次粒子が酸水溶液中に分散している歯科用前処理剤であって、前記凝集二次粒子は、シリカ粒子及びアルミナ粒子が凝集している凝集二次粒子を含み、当該歯科用前処理剤の水希釈液に含まれる凝集二次粒子は、体積平均粒径が０．１〜２０μｍであり、粒径が５０μｍ以上である凝集二次粒子の含有量が２０体積％以下である。 One aspect of the present invention is a dental pretreatment agent in which silica particles and / or agglomerated secondary particles in which alumina particles are agglomerated are dispersed in an acid aqueous solution, and the agglomerated secondary particles are silica particles. The agglomerated secondary particles containing the agglomerated secondary particles in which the alumina particles are agglomerated and contained in the aqueous diluent of the dental pretreatment agent have a volume average particle size of 0.1 to 20 μm and a particle size of 0.1 to 20 μm. The content of aggregated secondary particles having a size of 50 μm or more is 20% by volume or less.
本発明の一態様によれば、シリンジに装着した吐出用チップの目詰まり及び液分離の発生を抑制することが可能な歯科用前処理剤を提供することができる。 According to one aspect of the present invention, it is possible to provide a dental pretreatment agent capable of suppressing clogging of a discharge tip attached to a syringe and occurrence of liquid separation.
以下、本発明を実施するための形態について説明する。本発明は、下記の実施形態に限定されることはなく、特許請求の範囲に記載された範囲を逸脱することなく、下記の実施形態に種々の変形及び置換を加えることができる。 Hereinafter, modes for carrying out the present invention will be described. The present invention is not limited to the following embodiments, and various modifications and substitutions can be made to the following embodiments without departing from the scope of claims.
＜歯科用前処理剤＞
本実施形態の歯科用前処理剤は、シリカ粒子及び／又はアルミナ粒子が凝集している凝集二次粒子が酸水溶液中に分散している。ここで、シリカ粒子及び／又はアルミナ粒子が凝集している凝集二次粒子は、シリカ粒子及びアルミナ粒子が凝集している凝集二次粒子を含む。
<Dental pretreatment agent>
In the dental pretreatment agent of the present embodiment, aggregated secondary particles in which silica particles and / or alumina particles are aggregated are dispersed in an aqueous acid solution. Here, the aggregated secondary particles in which the silica particles and / or the alumina particles are aggregated include the aggregated secondary particles in which the silica particles and the alumina particles are aggregated.
本実施形態の歯科用前処理剤は、シリカ粒子、アルミナ粒子及び酸水溶液を混練することにより製造することができるが、その際に、シリカ粒子及びアルミナ粒子が凝集する。このため、歯科用前処理剤中には、シリカ粒子が凝集している凝集二次粒子と、アルミナ粒子が凝集している凝集二次粒子と、シリカ粒子及びアルミナ粒子が凝集している凝集二次粒子が存在する。 The dental pretreatment agent of the present embodiment can be produced by kneading silica particles, alumina particles and an aqueous acid solution, and at that time, the silica particles and the alumina particles agglomerate. Therefore, in the dental pretreatment agent, aggregated secondary particles in which silica particles are aggregated, aggregated secondary particles in which alumina particles are aggregated, and aggregated secondary particles in which silica particles and alumina particles are aggregated. There are subatomic particles.
歯科用前処理剤の水希釈液に含まれる凝集二次粒子の体積平均粒径は、０．１〜２０μｍであり、０．１５〜１０μｍであることが好ましい。歯科用前処理剤の水希釈液に含まれる凝集二次粒子の体積平均粒径が０．１μｍ未満であると、液分離が発生しやすくなり、２０μｍを超えると、シリンジに装着した吐出用チップの目詰まりが発生しやすくなる。 The volume average particle diameter of the aggregated secondary particles contained in the aqueous diluent of the dental pretreatment agent is 0.1 to 20 μm, preferably 0.15 to 10 μm. If the volume average particle size of the aggregated secondary particles contained in the water-diluted solution of the dental pretreatment agent is less than 0.1 μm, liquid separation is likely to occur, and if it exceeds 20 μm, the discharge tip attached to the syringe. Clogs are likely to occur.
歯科用前処理剤の水希釈液に含まれる凝集二次粒子中の粒径が５０μｍ以上である凝集二次粒子の含有量は、２０体積％以下であり、５体積％以下であることが好ましい。歯科用前処理剤の水希釈液に含まれる凝集二次粒子中の粒径が５０μｍ以上である凝集二次粒子の含有量が２０体積％を超えると、シリンジに装着した吐出用チップの目詰まりが発生しやすくなる。 The content of the aggregated secondary particles having a particle size of 50 μm or more in the water-diluted solution of the dental pretreatment agent is 20% by volume or less, preferably 5% by volume or less. .. When the content of the aggregated secondary particles having a particle size of 50 μm or more in the aqueous diluent of the dental pretreatment agent exceeds 20% by volume, the ejection tip attached to the syringe is clogged. Is likely to occur.
歯科用前処理剤の水希釈液に含まれる凝集二次粒子中の粒径が２０μｍ以下である凝集二次粒子の含有量は、６５体積％以上であることが好ましく、８０体積％以上であることがさらに好ましい。歯科用前処理剤の水希釈液に含まれる凝集二次粒子中の粒径が２０μｍ以下である凝集二次粒子の含有量が６５体積％以上であると、液分離が発生しにくくなる。 The content of the aggregated secondary particles having a particle size of 20 μm or less contained in the aqueous diluent of the dental pretreatment agent is preferably 65% by volume or more, preferably 80% by volume or more. Is even more preferable. When the content of the aggregated secondary particles having a particle size of 20 μm or less in the water-diluted solution of the dental pretreatment agent is 65% by volume or more, liquid separation is less likely to occur.
なお、歯科用前処理剤の水希釈液に含まれる凝集二次粒子の粒度分布は、レーザー回折散乱法により、歯科用前処理剤の水希釈液を測定することにより、求められる。 The particle size distribution of the aggregated secondary particles contained in the water-diluted solution of the dental pretreatment agent can be obtained by measuring the water-diluted solution of the dental pretreatment agent by a laser diffraction / scattering method.
ここで、歯科用前処理剤の水希釈液を作製する際、又は、歯科用前処理剤の水希釈液に含まれる凝集二次粒子の粒度分布を測定する際には、超音波処理しない。 Here, sonication is not performed when preparing the aqueous diluent of the dental pretreatment agent or when measuring the particle size distribution of the aggregated secondary particles contained in the aqueous diluent of the dental pretreatment agent.
酸水溶液に含まれる酸としては、例えば、カルボン酸等の有機酸、リン酸、硝酸、硫酸、フッ酸等の無機酸を使用することができる。 As the acid contained in the acid aqueous solution, for example, an organic acid such as a carboxylic acid or an inorganic acid such as phosphoric acid, nitric acid, sulfuric acid or hydrofluoric acid can be used.
カルボン酸の具体例としては、クエン酸、乳酸、リンゴ酸、マロン酸、マレイン酸、シュウ酸、酒石酸、酢酸、モノクロロ酢酸、ジクロロ酢酸、トリクロロ酢酸、トリフルオロ酢酸、ギ酸等が挙げられる。 Specific examples of the carboxylic acid include citric acid, lactic acid, malonic acid, malonic acid, maleic acid, oxalic acid, tartrate acid, acetic acid, monochloroacetic acid, dichloroacetic acid, trichloroacetic acid, trifluoroacetic acid, and formic acid.
なお、酸水溶液に含まれる酸は、単独で使用してもよいし、２種以上を併用してもよい。 The acid contained in the aqueous acid solution may be used alone or in combination of two or more.
歯科用前処理剤中の酸水溶液の含有量は、６０〜９５質量％であることが好ましく、７０〜９０質量％であることがさらに好ましい。 The content of the aqueous acid solution in the dental pretreatment agent is preferably 60 to 95% by mass, more preferably 70 to 90% by mass.
酸水溶液中の酸の含有量は、１〜９０質量％であることが好ましく、３０〜５０質量％であることがさらに好ましい。 The content of the acid in the aqueous acid solution is preferably 1 to 90% by mass, more preferably 30 to 50% by mass.
シリカ粒子の平均一次粒径は、７〜４０ｎｍであることが好ましい。 The average primary particle size of the silica particles is preferably 7 to 40 nm.
シリカ粒子のＢＥＴ比表面積は、５０〜３８０ｍ２／ｇであることが好ましい。 The BET specific surface area of the silica particles is preferably 50 to 380 m 2 / g.
シリカ粒子の市販品としては、親水性ヒュームドシリカ（日本アエロジル製）等が挙げられる。 Examples of commercially available silica particles include hydrophilic fumed silica (manufactured by Nippon Aerosil).
歯科用前処理剤中のシリカ粒子の含有量は、５〜２５質量％であることが好ましく、１０〜２０質量％であることがさらに好ましい。 The content of silica particles in the dental pretreatment agent is preferably 5 to 25% by mass, more preferably 10 to 20% by mass.
アルミナ粒子の平均一次粒径は、１０〜１７ｎｍであることが好ましい。 The average primary particle size of the alumina particles is preferably 10 to 17 nm.
アルミナ粒子のＢＥＴ比表面積は、６５〜１３０ｍ２／ｇであることが好ましい。 The BET specific surface area of the alumina particles is preferably 65 to 130 m 2 / g.
アルミナ粒子の市販品としては、親水性ヒュームドアルミナ（日本アエロジル製）等が挙げられる。 Examples of commercially available products of alumina particles include hydrophilic fumed alumina (manufactured by Nippon Aerosil).
歯科用前処理剤中のアルミナ粒子の含有量は、１〜１５質量％であることが好ましく、５〜１０質量％であることがさらに好ましい。 The content of alumina particles in the dental pretreatment agent is preferably 1 to 15% by mass, and more preferably 5 to 10% by mass.
歯科用前処理剤中のシリカ粒子に対するアルミナ粒子の質量比は、０．２５〜０．５５であることが好ましく、０．３〜０．５であることがさらに好ましい。 The mass ratio of the alumina particles to the silica particles in the dental pretreatment agent is preferably 0.25 to 0.55, more preferably 0.3 to 0.5.
本実施形態の歯科用前処理剤は、必要に応じて、顔料等をさらに含んでいてもよい。 The dental pretreatment agent of the present embodiment may further contain pigments and the like, if necessary.
なお、本実施形態の歯科用前処理剤は、水溶性高分子を実質的に含まない。 The dental pretreatment agent of the present embodiment does not substantially contain a water-soluble polymer.
＜歯科用前処理剤の製造方法＞
本実施形態の歯科用前処理剤の製造方法は、シリカ粒子、アルミナ粒子及び酸水溶液を混練する工程を含むが、シリカ粒子、アルミナ粒子及び酸水溶液を硬練りする工程を含むことが好ましい。これにより、歯科用前処理剤の吐出性が向上する。
<Manufacturing method of dental pretreatment agent>
The method for producing the dental pretreatment agent of the present embodiment includes a step of kneading the silica particles, the alumina particles and the acid aqueous solution, and preferably includes a step of kneading the silica particles, the alumina particles and the acid aqueous solution. This improves the discharge property of the dental pretreatment agent.
シリカ粒子、アルミナ粒子及び酸水溶液を硬練りする際には、シリカ粒子、アルミナ粒子及び全量の６５〜８５質量％の酸水溶液を混練することが好ましい。 When the silica particles, the alumina particles and the acid aqueous solution are hard-kneaded, it is preferable to knead the silica particles, the alumina particles and the acid aqueous solution having a total amount of 65 to 85% by mass.
シリカ粒子、アルミナ粒子及び酸水溶液を硬練りする際に用いる混練機としては、例えば、プラネタリミキサー（井上製作所製）等を用いることができる。 As the kneading machine used for kneading the silica particles, the alumina particles and the acid aqueous solution, for example, a planetary mixer (manufactured by Inoue Seisakusho) or the like can be used.
本実施形態においては、シリカ粒子、アルミナ粒子及び酸水溶液を硬練りした後、全量の１５〜３５質量％の酸水溶液を加え、混練することが好ましい。 In the present embodiment, it is preferable that the silica particles, the alumina particles and the acid aqueous solution are hard-kneaded, and then the total amount of the acid aqueous solution of 15 to 35% by mass is added and kneaded.
なお、酸水溶液を２回以上に分けて加えてもよい。 The acid aqueous solution may be added in two or more portions.
また、シリカ粒子、アルミナ粒子及び酸水溶液を２回以上硬練りしてもよい。 Further, the silica particles, the alumina particles and the acid aqueous solution may be kneaded twice or more.
以下、本発明の実施例を説明するが、本発明は実施例に限定されない。なお、部は、質量部を意味する。 Hereinafter, examples of the present invention will be described, but the present invention is not limited to the examples. In addition, a part means a mass part.
［シリカ粒子］
シリカ粒子として、親水性ヒュームドシリカＡＥＲＯＳＩＬ ５０、ＡＥＲＯＳＩＬ ９０、ＡＥＲＯＳＩＬ １３０（以上、日本アエロジル製）を用いた。
[Silica particles]
As the silica particles, hydrophilic fumed silica AEROSIL 50, AEROSIL 90, and AEROSIL 130 (all manufactured by Nippon Aerosil) were used.
ここで、ＡＥＲＯＳＩＬ ５０は、平均一次粒径が３０ｎｍ、ＢＥＴ比表面積が５０ｍ２／ｇである。ＡＥＲＯＳＩＬ ９０は、平均一次粒径が２０ｎｍ、ＢＥＴ比表面積が９０ｍ２／ｇである。ＡＥＲＯＳＩＬ １３０は、平均一次粒径が１６ｎｍ、ＢＥＴ比表面積が１３０ｍ２／ｇである。 Here, AEROSIL 50 has an average primary particle size of 30 nm and a BET specific surface area of 50 m 2 / g. AEROSIL 90 has an average primary particle size of 20 nm and a BET specific surface area of 90 m 2 / g. AEROSIL 130 has an average primary particle size of 16 nm and a BET specific surface area of 130 m 2 / g.
［アルミナ粒子］
アルミナ粒子として、親水性ヒュームドアルミナＡＥＲＯＸＩＤＥ Ａｌｕ Ｃ（日本アエロジル製）を用いた。
[Alumina particles]
As the alumina particles, hydrophilic fumed alumina AEROXIDE Alu C (manufactured by Nippon Aerosil) was used.
ここで、ＡＥＲＯＸＩＤＥ Ａｌｕ Ｃは、平均一次粒径が１３ｎｍ、ＢＥＴ比表面積が１００ｍ２／ｇである。 Here, AEROXIDE Alu C has an average primary particle size of 13 nm and a BET specific surface area of 100 m 2 / g.
［酸水溶液の作製］
８５質量％リン酸（日本化学工業製）４３．５質量部及び水５６．５質量部の混合物に青色顔料０．５質量部を加え、酸水溶液を作製した。
[Preparation of aqueous acid solution]
An aqueous acid solution was prepared by adding 0.5 parts by mass of a blue pigment to a mixture of 43.5 parts by mass of 85% by mass phosphoric acid (manufactured by Nippon Kagaku Kogyo) and 56.5 parts by mass of water.
なお、青色顔料は、後述する前処理剤の液分離を観察しやすくすることを目的に配合されている。 The blue pigment is blended for the purpose of facilitating the observation of liquid separation of the pretreatment agent described later.
［実施例１］
以下、自転公転式ミキサーのあわとり練太郎ＡＲＥ−３１０（ＴＨＩＮＫＹ製）を用いて、混練した。
[Example 1]
Hereinafter, kneading was performed using a rotating and revolving mixer, Awatori Rentaro ARE-310 (manufactured by THINKY).
まず、容器に６１．０ｇの酸水溶液を入れた後、５．０ｇのＡＥＲＯＸＩＤＥ Ａｌｕ Ｃ、７．０ｇのＡＥＲＯＳＩＬ ５０を加え、２０００ｒｐｍで１分間混練した。次に、７．０ｇのＡＥＲＯＳＩＬ ５０をさらに加え、２０００ｒｐｍで１分間混練した。次に、容器内に飛散したＡＥＲＯＳＩＬ ５０が残らないように留意しながら、２０００ｒｐｍで１分間混練する操作を３回繰り返した（硬練り）。 First, 61.0 g of an aqueous acid solution was placed in a container, 5.0 g of AEROXIDE Alu C and 7.0 g of AEROSIL 50 were added, and the mixture was kneaded at 2000 rpm for 1 minute. Next, 7.0 g of AEROSIL 50 was further added and kneaded at 2000 rpm for 1 minute. Next, the operation of kneading at 2000 rpm for 1 minute was repeated 3 times, taking care not to leave the scattered AEROSIL 50 in the container (hard kneading).
次に、７．０ｇの酸水溶液を加え、２０００ｒｐｍで１分間混練した後、１３．０ｇの酸水溶液をさらに加え、２０００ｒｐｍで１分間混練し、前処理剤を得た。 Next, 7.0 g of an aqueous acid solution was added and kneaded at 2000 rpm for 1 minute, then 13.0 g of an aqueous acid solution was further added and kneaded at 2000 rpm for 1 minute to obtain a pretreatment agent.
［実施例２］
以下、自転公転式ミキサーのあわとり練太郎ＡＲＥ−３１０（ＴＨＩＮＫＹ製）を用いて、混練した。
[Example 2]
Hereinafter, kneading was performed using a rotating and revolving mixer, Awatori Rentaro ARE-310 (manufactured by THINKY).
まず、容器に６２．４ｇの酸水溶液を入れた後、５．５ｇのＡＥＲＯＸＩＤＥ Ａｌｕ Ｃ、６．１ｇのＡＥＲＯＳＩＬ ９０を加え、２０００ｒｐｍで１分間混練した。次に、６．０ｇのＡＥＲＯＳＩＬ ９０をさらに加え、２０００ｒｐｍで１分間混練した。次に、容器内に飛散したＡＥＲＯＳＩＬ ９０が残らないように留意しながら、２０００ｒｐｍで１分間混練する操作を３回繰り返した（硬練り）。 First, 62.4 g of an aqueous acid solution was placed in a container, 5.5 g of AEROXIDE Alu C and 6.1 g of AEROSIL 90 were added, and the mixture was kneaded at 2000 rpm for 1 minute. Next, 6.0 g of AEROSIL 90 was further added and kneaded at 2000 rpm for 1 minute. Next, the operation of kneading at 2000 rpm for 1 minute was repeated 3 times, taking care not to leave the scattered AEROSIL 90 in the container (hard kneading).
次に、７．０ｇの酸水溶液を加え、２０００ｒｐｍで１分間混練した後、１３．０ｇの酸水溶液をさらに加え、２０００ｒｐｍで１分間混練し、前処理剤を得た。 Next, 7.0 g of an aqueous acid solution was added and kneaded at 2000 rpm for 1 minute, then 13.0 g of an aqueous acid solution was further added and kneaded at 2000 rpm for 1 minute to obtain a pretreatment agent.
［実施例３］
以下、自転公転式ミキサーのあわとり練太郎ＡＲＥ−３１０（ＴＨＩＮＫＹ製）を用いて、混練した。
[Example 3]
Hereinafter, kneading was performed using a rotating and revolving mixer, Awatori Rentaro ARE-310 (manufactured by THINKY).
まず、容器に６１．３ｇの酸水溶液を入れた後、５．０ｇのＡＥＲＯＸＩＤＥ Ａｌｕ Ｃ、６．９ｇのＡＥＲＯＳＩＬ １３０を加え、２０００ｒｐｍで１分間混練した。次に、６．８ｇのＡＥＲＯＳＩＬ １３０をさらに加え、２０００ｒｐｍで１分間混練した。次に、容器内に飛散したＡＥＲＯＳＩＬ １３０が残らないように留意しながら、２０００ｒｐｍで１分間混練する操作を３回繰り返した（硬練り）。 First, 61.3 g of an aqueous acid solution was placed in a container, 5.0 g of AEROXIDE Alu C and 6.9 g of AEROSIL 130 were added, and the mixture was kneaded at 2000 rpm for 1 minute. Next, 6.8 g of AEROSIL 130 was further added and kneaded at 2000 rpm for 1 minute. Next, the operation of kneading at 2000 rpm for 1 minute was repeated 3 times, taking care not to leave the scattered AEOSIL 130 in the container (hard kneading).
次に、７．０ｇの酸水溶液を加え、２０００ｒｐｍで１分間混練した後、１３．０ｇの酸水溶液をさらに加え、２０００ｒｐｍで１分間混練し、前処理剤を得た。 Next, 7.0 g of an aqueous acid solution was added and kneaded at 2000 rpm for 1 minute, then 13.0 g of an aqueous acid solution was further added and kneaded at 2000 rpm for 1 minute to obtain a pretreatment agent.
［実施例４］
以下、自転公転式ミキサーのあわとり練太郎ＡＲＥ−３１０（ＴＨＩＮＫＹ製）を用いて、混練した。
[Example 4]
Hereinafter, kneading was performed using a rotating and revolving mixer, Awatori Rentaro ARE-310 (manufactured by THINKY).
まず、容器に８５．７ｇの酸水溶液を入れた後、３．８ｇのＡＥＲＯＸＩＤＥ Ａｌｕ Ｃ、５．３ｇのＡＥＲＯＳＩＬ ５０を加え、２０００ｒｐｍで１分間混練した。次に、５．２ｇのＡＥＲＯＳＩＬ ５０をさらに加え、２０００ｒｐｍで１分間混練した。次に、２０００ｒｐｍで１分間混練し、前処理剤を得た。 First, 85.7 g of an aqueous acid solution was placed in a container, 3.8 g of AEROXIDE Alu C, 5.3 g of AEROSIL 50 was added, and the mixture was kneaded at 2000 rpm for 1 minute. Next, 5.2 g of AEROSIL 50 was further added and kneaded at 2000 rpm for 1 minute. Next, it was kneaded at 2000 rpm for 1 minute to obtain a pretreatment agent.
［比較例１］
以下、自転公転式ミキサーのあわとり練太郎ＡＲＥ−３１０（ＴＨＩＮＫＹ製）を用いて、混練した。
[Comparative Example 1]
Hereinafter, kneading was performed using a rotating and revolving mixer, Awatori Rentaro ARE-310 (manufactured by THINKY).
まず、容器に８８．２ｇの酸水溶液を入れた後、５．９ｇのＡＥＲＯＳＩＬ ５０を加え、２０００ｒｐｍで１分間混練した。次に、５．９ｇのＡＥＲＯＳＩＬ ５０をさらに加え２０００ｒｐｍで１分間混練した。次に、２０００ｒｐｍで１分間混練し、前処理剤を得た。 First, 88.2 g of an aqueous acid solution was placed in a container, 5.9 g of AEROSIL 50 was added, and the mixture was kneaded at 2000 rpm for 1 minute. Next, 5.9 g of AEROSIL 50 was further added and kneaded at 2000 rpm for 1 minute. Next, it was kneaded at 2000 rpm for 1 minute to obtain a pretreatment agent.
［比較例２］
以下、自転公転式ミキサーのあわとり練太郎ＡＲＥ−３１０（ＴＨＩＮＫＹ製）を用いて、混練した。
[Comparative Example 2]
Hereinafter, kneading was performed using a rotating and revolving mixer, Awatori Rentaro ARE-310 (manufactured by THINKY).
まず、容器に６０．８ｇの酸水溶液を入れた後、９．５ｇのＡＥＲＯＳＩＬ ５０を加え、２０００ｒｐｍで１分間混練した。次に、９．４ｇのＡＥＲＯＳＩＬ ５０をさらに加え、２０００ｒｐｍで１分間混練した。次に、容器内に飛散したＡＥＲＯＳＩＬ ５０が残らないように留意しながら、２０００ｒｐｍで１分間混練する操作を３回繰り返した（硬練り）。 First, 60.8 g of an aqueous acid solution was placed in a container, 9.5 g of AEROSIL 50 was added, and the mixture was kneaded at 2000 rpm for 1 minute. Next, 9.4 g of AEROSIL 50 was further added and kneaded at 2000 rpm for 1 minute. Next, the operation of kneading at 2000 rpm for 1 minute was repeated 3 times, taking care not to leave the scattered AEROSIL 50 in the container (hard kneading).
次に、６．８ｇの酸水溶液を加え、２０００ｒｐｍで１分間混練した後、１３．５ｇの酸水溶液をさらに加え、２０００ｒｐｍで１分間混練し、前処理剤を得た。 Next, 6.8 g of an aqueous acid solution was added and kneaded at 2000 rpm for 1 minute, then 13.5 g of an aqueous acid solution was further added and kneaded at 2000 rpm for 1 minute to obtain a pretreatment agent.
［比較例３］
以下、自転公転式ミキサーのあわとり練太郎ＡＲＥ−３１０（ＴＨＩＮＫＹ製）を用いて、混練した。
[Comparative Example 3]
Hereinafter, kneading was performed using a rotating and revolving mixer, Awatori Rentaro ARE-310 (manufactured by THINKY).
まず、容器に９０．９ｇの酸水溶液を入れた後、４．６ｇのＡＥＲＯＳＩＬ ９０を加え、２０００ｒｐｍで１分間混練した。次に、４．５ｇのＡＥＲＯＳＩＬ ９０をさらに加え、２０００ｒｐｍで１分間混練した。次に、２０００ｒｐｍで１分間混練し、前処理剤を得た。 First, 90.9 g of an aqueous acid solution was placed in a container, 4.6 g of AEROSIL 90 was added, and the mixture was kneaded at 2000 rpm for 1 minute. Next, 4.5 g of AEROSIL 90 was further added and kneaded at 2000 rpm for 1 minute. Next, it was kneaded at 2000 rpm for 1 minute to obtain a pretreatment agent.
［比較例４］
以下、自転公転式ミキサーのあわとり練太郎ＡＲＥ−３１０（ＴＨＩＮＫＹ製）を用いて、混練した。
[Comparative Example 4]
Hereinafter, kneading was performed using a rotating and revolving mixer, Awatori Rentaro ARE-310 (manufactured by THINKY).
まず、容器に６４．９ｇの酸水溶液を入れた後、６．８ｇのＡＥＲＯＳＩＬ ９０を加え、２０００ｒｐｍで１分間混練した。次に、６．７ｇのＡＥＲＯＳＩＬ ９０をさらに加え、２０００ｒｐｍで１分間混練した。次に、容器内に飛散したＡＥＲＯＳＩＬ ９０が残らないように留意しながら、２０００ｒｐｍで１分間混練する操作を３回繰り返した（硬練り）。 First, 64.9 g of an aqueous acid solution was placed in a container, 6.8 g of AEROSIL 90 was added, and the mixture was kneaded at 2000 rpm for 1 minute. Next, 6.7 g of AEROSIL 90 was further added and kneaded at 2000 rpm for 1 minute. Next, the operation of kneading at 2000 rpm for 1 minute was repeated 3 times, taking care not to leave the scattered AEROSIL 90 in the container (hard kneading).
次に、７．２ｇの酸水溶液を加え、２０００ｒｐｍで１分間混練した後、１４．４ｇの酸水溶液をさらに加え、２０００ｒｐｍで１分間混練し、前処理剤を得た。 Next, 7.2 g of an aqueous acid solution was added and kneaded at 2000 rpm for 1 minute, then 14.4 g of an aqueous acid solution was further added and kneaded at 2000 rpm for 1 minute to obtain a pretreatment agent.
［比較例５］
以下、自転公転式ミキサーのあわとり練太郎ＡＲＥ−３１０（ＴＨＩＮＫＹ製）を用いて、混練した。
[Comparative Example 5]
Hereinafter, kneading was performed using a rotating and revolving mixer, Awatori Rentaro ARE-310 (manufactured by THINKY).
まず、容器に９０．０ｇの酸水溶液を入れた後、５．０ｇのＡＥＲＯＳＩＬ １３０を加え、２０００ｒｐｍで１分間混練した。次に、５．０ｇのＡＥＲＯＳＩＬ １３０をさらに加え、２０００ｒｐｍで１分間混練した。次に、２０００ｒｐｍで１分間混練し、前処理剤を得た。 First, 90.0 g of an aqueous acid solution was placed in a container, 5.0 g of AEROSIL 130 was added, and the mixture was kneaded at 2000 rpm for 1 minute. Next, 5.0 g of AEROSIL 130 was further added and kneaded at 2000 rpm for 1 minute. Next, it was kneaded at 2000 rpm for 1 minute to obtain a pretreatment agent.
［比較例６］
以下、自転公転式ミキサーのあわとり練太郎ＡＲＥ−３１０（ＴＨＩＮＫＹ製）を用いて、混練した。
[Comparative Example 6]
Hereinafter, kneading was performed using a rotating and revolving mixer, Awatori Rentaro ARE-310 (manufactured by THINKY).
まず、容器に６４．３ｇの酸水溶液を入れた後、７．２ｇのＡＥＲＯＳＩＬ １３０を加え、２０００ｒｐｍで１分間混練した。次に、７．１ｇのＡＥＲＯＳＩＬ １３０をさらに加え、２０００ｒｐｍで１分間混練した。次に、容器内に飛散したＡＥＲＯＳＩＬ １３０が残らないように留意しながら、２０００ｒｐｍで１分間混練する操作を３回繰り返した（硬練り）。 First, 64.3 g of an aqueous acid solution was placed in a container, 7.2 g of AEROSIL 130 was added, and the mixture was kneaded at 2000 rpm for 1 minute. Next, 7.1 g of AEROSIL 130 was further added and kneaded at 2000 rpm for 1 minute. Next, the operation of kneading at 2000 rpm for 1 minute was repeated 3 times, taking care not to leave the scattered AEROSIL 130 in the container (hard kneading).
次に、７．１ｇの酸水溶液を加え、２０００ｒｐｍで１分間混練した後、１４．３ｇの酸水溶液をさらに加え、２０００ｒｐｍで１分間混練し、前処理剤を得た。 Next, 7.1 g of an aqueous acid solution was added and kneaded at 2000 rpm for 1 minute, then 14.3 g of an aqueous acid solution was further added and kneaded at 2000 rpm for 1 minute to obtain a pretreatment agent.
［比較例７］
以下、自転公転式ミキサーのあわとり練太郎ＡＲＥ−３１０（ＴＨＩＮＫＹ製）を用いて、混練した。
[Comparative Example 7]
Hereinafter, kneading was performed using a rotating and revolving mixer, Awatori Rentaro ARE-310 (manufactured by THINKY).
まず、容器に８１．８ｇの酸水溶液を入れた後、１８．２ｇのＡＥＲＯＸＩＤＥ Ａｌｕ Ｃを加え、２０００ｒｐｍで１分間混練した。次に、２０００ｒｐｍで１分間混練し、前処理剤を得た。 First, 81.8 g of an aqueous acid solution was placed in a container, 18.2 g of AEROXIDE Alu C was added, and the mixture was kneaded at 2000 rpm for 1 minute. Next, it was kneaded at 2000 rpm for 1 minute to obtain a pretreatment agent.
表１に、前処理剤の配合を示す。 Table 1 shows the formulation of the pretreatment agent.
［前処理剤の水希釈液に含まれる凝集二次粒子の粒度分布］
前処理剤の０．５ｇと蒸留水の１０ｇを混合した後、内径３．１ｃｍ、高さ５．５ｃｍの容量３０ｍＬの円柱形状のＰＰ製のマルエム容器Ｎｏ．６（マルエム製）に入れた。こ次に、自転公転式ミキサーのあわとり練太郎ＡＲＥ−３１０（ＴＨＩＮＫＹ製）を用いて、７００ｒｐｍで３分間回転撹拌した。次に、レーザ回折／散乱式粒子径分布測定装置ＬＡ−９５０−Ｖ２（ＨＯＲＩＢＡ製）を用いて、前処理剤の水希釈液に含まれる凝集二次粒子の粒度分布を２３℃で測定した。このとき、溶媒としては、蒸留水を使用した。
[Particle size distribution of aggregated secondary particles contained in the water diluent of the pretreatment agent]
After mixing 0.5 g of the pretreatment agent and 10 g of distilled water, a columnar PP Maruem container No. 3 having an inner diameter of 3.1 cm and a height of 5.5 cm and a capacity of 30 mL. It was put in 6 (made by Maruem). Next, using a rotating and revolving mixer, Awatori Rentaro ARE-310 (manufactured by THINKY), the mixture was rotated and stirred at 700 rpm for 3 minutes. Next, the particle size distribution of the aggregated secondary particles contained in the aqueous dilute solution of the pretreatment agent was measured at 23 ° C. using a laser diffraction / scattering type particle size distribution measuring device LA-950-V2 (manufactured by HORIBA). At this time, distilled water was used as the solvent.
表２に、前処理剤の水希釈液に含まれる凝集二次粒子の粒度分布の測定結果を示す。 Table 2 shows the measurement results of the particle size distribution of the aggregated secondary particles contained in the aqueous diluent of the pretreatment agent.
［吐出性］
内径１１ｍｍ、容量３．６ｍｌのシリンジに前処理剤を充填した後、シリンジの吐出部に蓋をした状態で、２３℃の環境下、２４時間以上静置し、恒温化した。次に、シリンジの吐出部に吐出用チップ（ＩＳＯ ９６２６に準拠したゲージサイズ２５Ｇ）を装着した。次に、万能試験機ＡＧ−ＩＳ（ＳＨＩＭＡＤＺＵ製）を用いて、プランジャー部をクロスヘッドスピード１０ｍｍ／ｍｉｎで押し出し、押し出し抵抗の最大値を記録し、前処理剤の吐出性を評価した。
[Dischargeability]
After filling a syringe having an inner diameter of 11 mm and a capacity of 3.6 ml with a pretreatment agent, the syringe was allowed to stand for 24 hours or more in an environment of 23 ° C. with a lid on the discharge portion of the syringe to keep the temperature constant. Next, a ejection tip (gauge size 25G conforming to ISO 9626) was attached to the ejection portion of the syringe. Next, using a universal testing machine AG-IS (manufactured by SHIMADZU), the plunger portion was extruded at a crosshead speed of 10 mm / min, the maximum value of the extruding resistance was recorded, and the ejection property of the pretreatment agent was evaluated.
［シリンジに装着した吐出用チップの目詰まり］
内径１１ｍｍ、容量３．６ｍｌのシリンジに前処理剤を充填した後、シリンジの吐出部に蓋をした状態で、２３℃の環境下、２４時間以上静置し、恒温化した。次に、シリンジの吐出部に吐出用チップ（ＩＳＯ ９６２６に準拠したゲージサイズ３０Ｇ）を装着した。次に、プランジャー部を押し出し、目詰まりの有無を確認した。
[Clogged discharge tip attached to syringe]
After filling a syringe having an inner diameter of 11 mm and a capacity of 3.6 ml with a pretreatment agent, the syringe was allowed to stand for 24 hours or more in an environment of 23 ° C. with a lid on the discharge portion of the syringe to keep the temperature constant. Next, a ejection tip (gauge size 30G conforming to ISO 9626) was attached to the ejection portion of the syringe. Next, the plunger section was extruded and the presence or absence of clogging was confirmed.
［液分離］
内径１１ｍｍ、容量３．６ｍｌのシリンジに前処理剤を充填した後、シリンジの吐出部に蓋をした状態で、２３℃の環境下、２４時間以上静置し、恒温化した。次に、卓上遠心機Ｈ−２８Ｆ（コクサン製）を用いて、６００ｇ、９０ｓｅｃの条件で、遠心分離した。次に、シリンジから前処理剤を吐出させて、前処理剤の液分離の有無を観察した。
[Liquid separation]
After filling a syringe having an inner diameter of 11 mm and a capacity of 3.6 ml with a pretreatment agent, the syringe was allowed to stand for 24 hours or more in an environment of 23 ° C. with a lid on the discharge portion of the syringe to keep the temperature constant. Next, using a desktop centrifuge H-28F (manufactured by Koksan), centrifugation was performed under the conditions of 600 g and 90 sec. Next, the pretreatment agent was discharged from the syringe, and the presence or absence of liquid separation of the pretreatment agent was observed.
表３に、前処理剤の吐出性、操作性、液分離の評価結果を示す。 Table 3 shows the evaluation results of the dischargeability, operability, and liquid separation of the pretreatment agent.
これに対して、比較例１、２、４の前処理剤は、アルミナ粒子を含まないため、液分離が発生する。 On the other hand, since the pretreatment agents of Comparative Examples 1, 2 and 4 do not contain alumina particles, liquid separation occurs.
比較例３の前処理剤は、アルミナ粒子を含まず、水希釈液に含まれる凝集二次粒子の体積平均粒径が２９．７μｍであるため、シリンジに装着した吐出用チップの目詰まり及び液分離が発生する。 The pretreatment agent of Comparative Example 3 does not contain alumina particles, and the volume average particle diameter of the aggregated secondary particles contained in the water-diluted solution is 29.7 μm. Therefore, the discharge tip attached to the syringe is clogged and the liquid is clogged. Separation occurs.
比較例５、６の前処理剤は、アルミナ粒子を含まず、水希釈液に含まれる凝集二次粒子中の粒径が５０μｍ以上である凝集二次粒子の含有量が２８．２体積％、２２．５体積％であるため、シリンジに装着した吐出用チップの目詰まり及び液分離が発生する。 The pretreatment agents of Comparative Examples 5 and 6 did not contain alumina particles, and the content of the aggregated secondary particles having a particle size of 50 μm or more in the water-diluted solution was 28.2% by volume. Since it is 22.5% by volume, clogging of the discharge tip attached to the syringe and liquid separation occur.
比較例７の前処理剤は、シリカ粒子を含まないため、液分離が発生する。なお、比較例７の前処理剤は、粘度が低いため、吐出性を評価することができなかった。 Since the pretreatment agent of Comparative Example 7 does not contain silica particles, liquid separation occurs. Since the pretreatment agent of Comparative Example 7 had a low viscosity, the ejection property could not be evaluated.
Claims (2)
前記凝集二次粒子は、シリカ粒子及びアルミナ粒子が凝集している凝集二次粒子を含み、
当該歯科用前処理剤の水希釈液に含まれる凝集二次粒子は、体積平均粒径が０．１〜２０μｍであり、粒径が５０μｍ以上である凝集二次粒子の含有量が２０体積％以下であることを特徴とする歯科用前処理剤。 A dental pretreatment agent in which silica particles and / or agglomerated secondary particles in which alumina particles are agglomerated are dispersed in an aqueous acid solution.
The aggregated secondary particles include silica particles and aggregated secondary particles in which alumina particles are aggregated.
The aggregated secondary particles contained in the aqueous diluent of the dental pretreatment agent have a volume average particle size of 0.1 to 20 μm, and the content of the aggregated secondary particles having a particle size of 50 μm or more is 20% by volume. A dental pretreatment agent characterized by the following.
前記シリカ粒子、前記アルミナ粒子及び前記酸水溶液を硬練りする工程を含むことを特徴とする歯科用前処理剤の製造方法。 The method for producing the dental pretreatment agent according to claim 1.
The silica particles, method for producing a dental pretreatment agent comprising said alumina particles and a step of hard kneading the aqueous acid solution.
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