JPH0676233B2 - Glass ampoule or tube bottle and method for manufacturing the same - Google Patents
Glass ampoule or tube bottle and method for manufacturing the sameInfo
- Publication number
- JPH0676233B2 JPH0676233B2 JP2138239A JP13823990A JPH0676233B2 JP H0676233 B2 JPH0676233 B2 JP H0676233B2 JP 2138239 A JP2138239 A JP 2138239A JP 13823990 A JP13823990 A JP 13823990A JP H0676233 B2 JPH0676233 B2 JP H0676233B2
- Authority
- JP
- Japan
- Prior art keywords
- hot
- glass
- ampoule
- glass ampoule
- tube
- 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.)
- Expired - Lifetime
Links
- 239000011521 glass Substances 0.000 title claims description 34
- 239000003708 ampul Substances 0.000 title claims description 26
- 238000004519 manufacturing process Methods 0.000 title claims description 14
- 238000000034 method Methods 0.000 title claims description 14
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 37
- 239000000377 silicon dioxide Substances 0.000 claims description 19
- 239000012071 phase Substances 0.000 claims description 11
- -1 silyl isocyanate compound Chemical class 0.000 claims description 8
- 239000012808 vapor phase Substances 0.000 claims description 6
- 238000001816 cooling Methods 0.000 claims description 4
- 238000000465 moulding Methods 0.000 claims description 4
- 238000000151 deposition Methods 0.000 claims description 3
- 239000007788 liquid Substances 0.000 claims description 3
- 239000000047 product Substances 0.000 description 20
- 238000010828 elution Methods 0.000 description 13
- 239000007789 gas Substances 0.000 description 11
- 239000003513 alkali Substances 0.000 description 9
- 150000003377 silicon compounds Chemical class 0.000 description 9
- BUZRAOJSFRKWPD-UHFFFAOYSA-N isocyanatosilane Chemical compound [SiH3]N=C=O BUZRAOJSFRKWPD-UHFFFAOYSA-N 0.000 description 5
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 4
- 239000012159 carrier gas Substances 0.000 description 4
- 239000003814 drug Substances 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 239000005388 borosilicate glass Substances 0.000 description 2
- 239000006227 byproduct Substances 0.000 description 2
- 239000001569 carbon dioxide Substances 0.000 description 2
- 229910002092 carbon dioxide Inorganic materials 0.000 description 2
- 238000007796 conventional method Methods 0.000 description 2
- 229910001873 dinitrogen Inorganic materials 0.000 description 2
- 229940079593 drug Drugs 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 230000007062 hydrolysis Effects 0.000 description 2
- 238000006460 hydrolysis reaction Methods 0.000 description 2
- 238000003860 storage Methods 0.000 description 2
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- BFNBIHQBYMNNAN-UHFFFAOYSA-N ammonium sulfate Chemical compound N.N.OS(O)(=O)=O BFNBIHQBYMNNAN-UHFFFAOYSA-N 0.000 description 1
- 229910052921 ammonium sulfate Inorganic materials 0.000 description 1
- 235000011130 ammonium sulphate Nutrition 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 description 1
- 239000004327 boric acid Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 125000001181 organosilyl group Chemical group [SiH3]* 0.000 description 1
- 125000004430 oxygen atom Chemical group O* 0.000 description 1
- 238000003672 processing method Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000000682 scanning probe acoustic microscopy Methods 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 229920002050 silicone resin Polymers 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 239000011593 sulfur Substances 0.000 description 1
- 238000005211 surface analysis Methods 0.000 description 1
- 238000004448 titration Methods 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Landscapes
- Surface Treatment Of Glass (AREA)
- Re-Forming, After-Treatment, Cutting And Transporting Of Glass Products (AREA)
Description
【発明の詳細な説明】 ［産業上の利用分野］ 本発明は、主に医療・理化学の分野において薬品や検査
試料の保存容器等として使用される、ガラス管から成形
されたガラスアンプルまたは管瓶、及びその製造方法に
関する。DETAILED DESCRIPTION OF THE INVENTION [Industrial application] The present invention is mainly used in the fields of medicine and physics and chemistry as a storage container for chemicals and test samples, and the like, and is a glass ampoule or tube bottle molded from a glass tube. And a manufacturing method thereof.
［従来の技術］ 医療・理化学の分野において薬品や検査試料の保存容器
等として使用されるガラスアンプルまたは管瓶を製造す
る方法として、ガラス管をバーナー火炎によりアンプル
または管瓶の形状に加熱溶融成形し、その成形品を徐冷
する工程を経る方法が知られている。[Prior Art] As a method of manufacturing a glass ampoule or a tube bottle used as a storage container for medicines or test samples in the fields of medical science and physics, a glass tube is heated and melt-molded into a shape of an ampoule or a tube bottle by a burner flame. Then, a method is known in which the molded product is gradually cooled.
ガラスは、主原料としてまたは融剤として、アルカリ成
分を含むものが多く、上記ガラス管の加熱溶融成形の際
に、ガラス中に含まれているアルカリホウ酸等のアルカ
リ成分が揮発し、これが成形品の内壁に付着・凝縮す
る。この付着・凝縮したアルカリ成分は、通常の洗浄に
よっては殆ど除去できない。従って、こうして製造され
たガラスアンプルまたは管瓶は、内面からのアルカリ溶
出が極めて高いものとなっている。このようなガラスア
ンプルまたは管瓶に薬品や検査試料を保存すると、アル
カリ溶出によって内容液が変質してしまう。Many glass contains an alkaline component as a main raw material or as a fluxing agent, and when the glass tube is heated and melt-molded, an alkaline component such as an alkaline boric acid contained in the glass is volatilized, and this is molded. It adheres and condenses on the inner wall of the product. The adhered and condensed alkaline component can hardly be removed by ordinary washing. Therefore, the glass ampoule or tube bottle manufactured in this way has extremely high alkali elution from the inner surface. When a drug or test sample is stored in such a glass ampoule or a tube bottle, the content liquid is altered due to alkali elution.
上記アルカリ成分の溶出を防止する方法として、得られ
た成形品の内面にシリコーン樹脂を塗布する方法、また
は成形品内面を硫酸アンモニウムによるサルファー処理
に供する方法が行なわれている。これらの処理方法は、
付着したアルカリ成分の溶出を防止するものとして効果
的ではあるが、ガラスアンプルまたは管瓶の製造プロセ
スに別個の工程を付加することとなり、生産性が低く、
コスト高になる。As a method for preventing the elution of the alkaline component, a method of applying a silicone resin to the inner surface of the obtained molded product or a method of subjecting the inner surface of the molded product to a sulfur treatment with ammonium sulfate is performed. These processing methods are
Although it is effective as a means to prevent elution of adhered alkaline components, it adds a separate step to the glass ampoule or tube bottle manufacturing process, resulting in low productivity,
High cost.
なお、アルカリ成分の付着を防止する方法として、バー
ナー火炎の温度を低下してアルカリ成分の揮発を減少さ
せたり、あるいは成形品の口部から加圧空気を通じ、揮
発した成分を排出する方法も行なわれているが、これら
の方法では、アルカリ成分の付着を充分に防止できない
とともに、生産性も低い。As a method of preventing the adhesion of the alkaline component, a method of lowering the temperature of the burner flame to reduce the volatilization of the alkaline component, or a method of discharging the volatilized component by passing pressurized air from the mouth of the molded product is also performed. However, these methods cannot sufficiently prevent the adhesion of alkali components and have low productivity.
［発明が解決しようとする課題］ 従って、本発明は、上記タイプのガラス管から、長期間
に渡ってアルカリ溶出の少ないガラスアンプルまたは管
瓶を効率よく製造するための方法、及びそのようなガラ
スアンプルまたは管瓶を提供することを課題とするもの
である。[Problems to be Solved by the Invention] Accordingly, the present invention provides a method for efficiently producing a glass ampoule or a tube bottle with little alkali elution from a glass tube of the above type for a long period of time, and such a glass. It is an object to provide ampoules or vials.
［課題を解決するための手段］ 上記課題を解決するために、本発明では、ガラス管から
加熱成形した後の熱間成形品の内面をシリコン化合物で
気相処理して安定なシリカ膜を被着させている。[Means for Solving the Problems] In order to solve the above problems, in the present invention, the inner surface of a hot-molded product after being heat-molded from a glass tube is vapor-phase treated with a silicon compound to form a stable silica film. I'm wearing it.
すなわち、本発明は、ガラス管をアンプルまたは管瓶形
状に加熱形成し、徐冷してガラスアンプルまたは管瓶を
製造する方法において、加熱成形後、熱間成形品の内面
をシリコン化合物で気相処理してシリカ膜を被着させる
ことを特徴とするガラスアンプルまたは管瓶の製造方法
を提供する。That is, the present invention is a method of forming a glass tube by heating in the shape of an ampoule or a tube bottle and gradually cooling it to produce a glass ampoule or a tube bottle. Provided is a method for producing a glass ampoule or a vial, which comprises treating and depositing a silica film.
また、本発明は、シリコン化合物の熱間気相処理により
形成されたシリカ膜を内面に有するガラスアンプルまた
は管瓶を提供する。The present invention also provides a glass ampoule or a vial having on its inner surface a silica film formed by a hot vapor phase treatment of a silicon compound.
以下、本発明をさらに詳しく説明する。Hereinafter, the present invention will be described in more detail.
本発明によりガラスアンプルまたは管瓶を製造するに
は、それ自体よく知られた手法により、ガラス（例え
ば、ホウケイ酸ガラス）の管を加熱溶融して、アンプル
または管瓶形状に成形する。加熱温度は、通常、800℃
ないし1000℃程度である。In order to produce a glass ampoule or a vial according to the present invention, a glass (for example, borosilicate glass) tube is heated and melted to form an ampoule or a vial by a method known per se. The heating temperature is usually 800 ℃
To about 1000 ° C.
次に、得られた熱間成形品の内面をシリコン化合物で気
相処理し、その分解（加水分解等）によりシリカ膜を成
形品の内面に堆積・形成させる。Next, the inner surface of the obtained hot-molded product is subjected to a gas phase treatment with a silicon compound, and its decomposition (hydrolysis or the like) causes a silica film to be deposited / formed on the inner surface of the molded product.
本発明で使用されるシリコン化合物は、熱間成形品の内
面を気相処理し、シリカ膜を堆積・形成するものであ
り、シリコンの外に酸素原子を含有する。好ましいシリ
コン化合物は、気相中で、加水分解により、シリカ膜を
形成・堆積し、副生物としては、ガスを生成するシリコ
ン化合物である。このようなシリコン化合物として、シ
リルイソシアネート化合物、特に、シリルテトライソシ
アネート（Si(NCO)4）を挙げることができる。この化合
物は、雰囲気の水分により加水分解してシリカ膜を形成
し、二酸化炭素ガス及び窒素ガスを副生する。The silicon compound used in the present invention is for subjecting the inner surface of a hot-molded product to a vapor phase treatment to deposit and form a silica film, and contains oxygen atoms outside silicon. A preferred silicon compound is a silicon compound which forms and deposits a silica film by hydrolysis in a gas phase, and produces a gas as a byproduct. An example of such a silicon compound is a silyl isocyanate compound, particularly silyl tetraisocyanate (Si (NCO) 4 ). This compound is hydrolyzed by moisture in the atmosphere to form a silica film, and carbon dioxide gas and nitrogen gas are by-produced.
さて、シリコン化合物による熱間成形品内面の気相処理
は、例えば、加熱成形直後で約400〜600℃の温度状態に
ある成形品の内部に液状のシリルイソシアネートを滴下
（例えば、１〜２滴）することによって行なうことがで
きる。滴下されたシリルイソシアネートは、瞬時に揮発
し、気相を形成する。Now, the gas phase treatment of the inner surface of the hot-molded product with the silicon compound is performed by, for example, dropping liquid silylisocyanate inside the molded product in a temperature state of about 400 to 600 ° C. immediately after the heat molding (for example, 1 to 2 drops). ) Can be done. The dropped silyl isocyanate volatilizes instantly to form a gas phase.
あるいは、気相処理は、約100〜200℃に加熱されたシリ
ルイソシアネートに同時に加熱された空気をキャリアガ
スとして通じ（流量例えば、２リットル／分ないし３リ
ットル／分）、そのキャリアガスにシリルイソシアネー
トを同伴させ、このキャリアガスを、加熱成形直後で約
400〜600℃の温度状態にある成形品の内部に通じること
によっても行なうことができる。Alternatively, the gas phase treatment is carried out by passing heated air as a carrier gas at the same time as silyl isocyanate heated to about 100 to 200 ° C. (flow rate, for example, 2 liters / minute to 3 liters / minute), and adding silyl isocyanate to the carrier gas. The carrier gas, and the carrier gas is
It can also be carried out by communicating with the inside of the molded product in the temperature state of 400 to 600 ° C.
これらいずれの方法でも、シリルイソシアネートは、気
相中で雰囲気水分による加水分解されシリカ膜を形成
し、副生成物の二酸化炭素ガス及び窒素ガスは、揮発除
去されるものと考えられる。In any of these methods, it is considered that the silyl isocyanate is hydrolyzed by atmospheric moisture in the gas phase to form a silica film, and carbon dioxide gas and nitrogen gas which are by-products are volatilized and removed.
シリコン化合物による熱間成形品内面の気相処理を行な
った後、成形品を常法により徐冷し、放冷して内面がシ
リカ膜でコートされたガラスアンプルまたは管瓶を得
る。こうして形成されたシリカ膜は、安定であり、長期
間に渡って、ガラスに含まれるアルカリ成分の溶出を防
止できる。After the vapor phase treatment of the inner surface of the hot-molded product with a silicon compound, the molded product is gradually cooled by a conventional method and allowed to cool to obtain a glass ampoule or tube bottle whose inner surface is coated with a silica film. The silica film thus formed is stable and can prevent elution of the alkaline component contained in the glass over a long period of time.
［作用］ 上に述べたように、熱間成形品と気相接触したシリカ化
合物は、加水分解してシリカ膜を成形品内面に堆積し、
このシリカ膜は、アルカリ成分の溶出を長期に渡って防
止する膜として作用する。また、そのシリカ膜の形成
は、通常のガラスアンプルまたは管瓶の一連の製造過程
で行なわれているため、気相処理に要する時間は、その
製造時間に付加されるものでなく、生産性もよい。[Operation] As described above, the silica compound in vapor phase contact with the hot molded product is hydrolyzed to deposit a silica film on the inner surface of the molded product,
This silica film acts as a film that prevents the elution of alkaline components over a long period of time. In addition, since the silica film is formed in a series of ordinary glass ampoule or tube bottle manufacturing process, the time required for the gas phase treatment is not added to the manufacturing time, and the productivity is also improved. Good.
［実施例］ 以下、本発明の実施例を説明する。[Examples] Examples of the present invention will be described below.
実施例１ ホウケイ酸ガラスの管から、以下の表１に示す規格のア
ンプル及び管瓶を加熱成形した。Example 1 Ampoules and tube bottles having the specifications shown in Table 1 below were thermoformed from a borosilicate glass tube.
その加熱成形直後で580℃の温度状態にある各成形品の
内部に、シリルテトライソシアネートを１滴（0.04〜0.
05グラム）滴下し、気相処理を行なった後、徐冷、放冷
して所望のガラスアンプル及び管瓶を得た。 Immediately after the heat-molding, one drop of silyltetraisocyanate (0.04-0.
(05 g) was added dropwise, and a gas phase treatment was performed, followed by gradual cooling and cooling to obtain a desired glass ampoule and tube bottle.
得られた製品の内面をオージェ電子分光法により表面分
析したところ、シリカ膜のみの形成が確認できた。When the inner surface of the obtained product was subjected to surface analysis by Auger electron spectroscopy, formation of only a silica film could be confirmed.
次に、得られたアンプル及び管瓶のアルカリ溶出量を、
製造直後に、0.02N−H2 SO4の消費量（滴定量により測
定した。なお、比較のため、従来の非処理品についても
同様の測定を行なった。結果を以下の表２に示す。Next, the amount of the alkaline elution of the obtained ampoule and tube bottle,
Immediately after production, the consumption of 0.02N-H 2 SO 4 (as measured by titer. For comparison, were measured same applies to conventional non-treated products. The results shown in Table 2 below.
表２に示す結果から明らかなように、本発明のガラスア
ンプル及び管瓶は、従来品に比べ、アルカリ溶出が非常
に少ない。 As is clear from the results shown in Table 2, the glass ampoule and tube bottle of the present invention have much less alkali elution than the conventional products.
また、製造後100日経過した本発明の製品について、同
様にアルカリ溶出量を測定した。結果を、以下の表３に
示す。In addition, the amount of alkali elution was similarly measured for the product of the present invention after 100 days had passed since the production. The results are shown in Table 3 below.
表 ３ 種類 滴定量（ml） ブランク（水のみ） 0.04 アンプル 0.07 管瓶 0.05 表３に示す結果からわかるように、本発明のガラスアン
プル及び管瓶は、長期間に渡ってアルカリの溶出を効果
的に防止することができる。 Table 3 Types Titration (ml) Blank (water only) 0.04 Ampoule 0.07 Tube bottle 0.05 As can be seen from the results shown in Table 3, the glass ampoule and tube bottle of the present invention are effective in elution of alkali over a long period of time. Can be prevented.
［発明の効果］ 以上述べたように、本発明は、従来の方法と異なり、ア
ルカリ溶出防止膜としてのシリカ膜をガラスアンプルま
たは管瓶の通常の製造過程において形成するものである
から、比較的容易にかつ優れた生産性をもってガラス管
からアンプルまたは管瓶を製造することができ、また形
成されたシリカ膜は、長期間に渡ってアルカリ溶出を防
止することができる。[Effects of the Invention] As described above, the present invention is different from the conventional method in that the silica film as the alkali elution preventing film is formed in the normal manufacturing process of the glass ampoule or the tube bottle. Ampoules or vials can be easily manufactured from glass tubes with excellent productivity, and the formed silica film can prevent alkali elution for a long period of time.
Claims (5)
成形し、徐冷する工程を経てガラスアンプルまたは管瓶
を製造する方法において、加熱成形後、熱間成形品の内
面をシリルイソシアネート化合物で気相処理してシリカ
膜を被着させることを特徴とするガラスアンプルまたは
管瓶の製造方法。1. A method for producing a glass ampoule or a vial through a step of heat-molding a glass tube into an ampoule or a tube bottle shape and gradually cooling the glass tube. After the hot molding, the inner surface of the hot-formed product is treated with a silyl isocyanate compound. A method for producing a glass ampoule or a vial, which comprises vapor-depositing and depositing a silica film.
理を熱間成形品の温度約400ないし600℃で行う特許請求
の範囲第１項記載の製造方法。2. The production method according to claim 1, wherein the vapor phase treatment with the silyl isocyanate compound is carried out at a temperature of the hot molded product of about 400 to 600 ° C.
シアネート化合物に同様に加熱された空気を通じて該シ
リルイソシアネート化合物を該空気に同伴させ、これを
熱間成形品の内部に通じることによって気相処理を行う
特許請求の範囲第２項記載の製造方法。3. A silylisocyanate compound heated to about 100 to 200 ° C. is also entrained with the silylisocyanate compound through heated air, which is then passed into the hot-molded article to form a gas phase. The manufacturing method according to claim 2, wherein the treatment is performed.
成形品の内部に滴下することによって気相処理を行う特
許請求の範囲第２項記載の製造方法。4. The method according to claim 2, wherein the gas phase treatment is carried out by dropping a liquid silyl isocyanate compound into the hot-air molded product.
理により形成されたシリカ膜を内面に有するガラスアン
プルまたは管瓶。5. A glass ampoule or a vial having a silica film formed by a hot gas phase treatment of a silyl isocyanate compound on its inner surface.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2138239A JPH0676233B2 (en) | 1990-05-30 | 1990-05-30 | Glass ampoule or tube bottle and method for manufacturing the same |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2138239A JPH0676233B2 (en) | 1990-05-30 | 1990-05-30 | Glass ampoule or tube bottle and method for manufacturing the same |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH0437632A JPH0437632A (en) | 1992-02-07 |
| JPH0676233B2 true JPH0676233B2 (en) | 1994-09-28 |
Family
ID=15217327
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP2138239A Expired - Lifetime JPH0676233B2 (en) | 1990-05-30 | 1990-05-30 | Glass ampoule or tube bottle and method for manufacturing the same |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH0676233B2 (en) |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPWO2006123621A1 (en) * | 2005-05-16 | 2008-12-25 | ニプロ株式会社 | Vials and manufacturing method thereof |
| EP2239237A2 (en) | 2009-04-07 | 2010-10-13 | Nipro Corporation | Method for producing medical glass container and burner for inner surface treatment of medical glass container |
| JP2011001253A (en) * | 2009-05-18 | 2011-01-06 | Nipro Corp | Glass vessel for medical use and method for producing glass vessel for medical use |
| JP2016510288A (en) * | 2012-11-30 | 2016-04-07 | コーニング インコーポレイテッド | Glass container with delamination resistance and improved strength |
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