JPH06279063A - Porous glass having alkali resistance - Google Patents
Porous glass having alkali resistanceInfo
- Publication number
- JPH06279063A JPH06279063A JP9197293A JP9197293A JPH06279063A JP H06279063 A JPH06279063 A JP H06279063A JP 9197293 A JP9197293 A JP 9197293A JP 9197293 A JP9197293 A JP 9197293A JP H06279063 A JPH06279063 A JP H06279063A
- Authority
- JP
- Japan
- Prior art keywords
- porous glass
- glass substrate
- silicone oil
- porous
- phase
- 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.)
- Pending
Links
- 239000005373 porous glass Substances 0.000 title claims abstract description 51
- 239000003513 alkali Substances 0.000 title claims abstract description 25
- 239000000758 substrate Substances 0.000 claims abstract description 35
- 229920002545 silicone oil Polymers 0.000 claims abstract description 23
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000011593 sulfur Substances 0.000 claims abstract description 8
- 229910052717 sulfur Inorganic materials 0.000 claims abstract description 8
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 claims abstract description 7
- 150000001875 compounds Chemical class 0.000 claims abstract description 7
- 239000012495 reaction gas Substances 0.000 claims description 12
- 239000011521 glass Substances 0.000 abstract description 19
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 abstract description 10
- 238000000034 method Methods 0.000 abstract description 9
- 238000004519 manufacturing process Methods 0.000 abstract description 8
- 239000011148 porous material Substances 0.000 abstract description 6
- 239000002253 acid Substances 0.000 abstract description 5
- 239000005388 borosilicate glass Substances 0.000 abstract description 5
- 238000010438 heat treatment Methods 0.000 abstract description 5
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 abstract description 4
- 239000011248 coating agent Substances 0.000 abstract description 4
- 238000000576 coating method Methods 0.000 abstract description 4
- 239000000377 silicon dioxide Substances 0.000 abstract description 4
- 238000005191 phase separation Methods 0.000 abstract description 3
- 239000000126 substance Substances 0.000 abstract description 3
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 abstract description 2
- 239000004327 boric acid Substances 0.000 abstract description 2
- 238000002844 melting Methods 0.000 abstract description 2
- 230000008018 melting Effects 0.000 abstract description 2
- 239000004576 sand Substances 0.000 abstract description 2
- 229910000029 sodium carbonate Inorganic materials 0.000 abstract description 2
- 235000017550 sodium carbonate Nutrition 0.000 abstract description 2
- KKCBUQHMOMHUOY-UHFFFAOYSA-N Na2O Inorganic materials [O-2].[Na+].[Na+] KKCBUQHMOMHUOY-UHFFFAOYSA-N 0.000 abstract 2
- 229910052681 coesite Inorganic materials 0.000 abstract 2
- 229910052906 cristobalite Inorganic materials 0.000 abstract 2
- 235000012239 silicon dioxide Nutrition 0.000 abstract 2
- 229910052682 stishovite Inorganic materials 0.000 abstract 2
- 229910052905 tridymite Inorganic materials 0.000 abstract 2
- 238000003756 stirring Methods 0.000 abstract 1
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 15
- 239000007789 gas Substances 0.000 description 6
- 238000012545 processing Methods 0.000 description 6
- 238000012360 testing method Methods 0.000 description 6
- 238000012546 transfer Methods 0.000 description 6
- 229910004298 SiO 2 Inorganic materials 0.000 description 4
- 239000007864 aqueous solution Substances 0.000 description 4
- 239000006121 base glass Substances 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 4
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 description 4
- 239000011734 sodium Substances 0.000 description 4
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 3
- IMNFDUFMRHMDMM-UHFFFAOYSA-N N-Heptane Chemical compound CCCCCCC IMNFDUFMRHMDMM-UHFFFAOYSA-N 0.000 description 3
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 3
- 238000010306 acid treatment Methods 0.000 description 3
- 239000002585 base Substances 0.000 description 3
- 238000007598 dipping method Methods 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 description 2
- LSNNMFCWUKXFEE-UHFFFAOYSA-N Sulfurous acid Chemical compound OS(O)=O LSNNMFCWUKXFEE-UHFFFAOYSA-N 0.000 description 2
- 239000012153 distilled water Substances 0.000 description 2
- 229920001296 polysiloxane Polymers 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 1
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- 150000007513 acids Chemical class 0.000 description 1
- 239000012670 alkaline solution Substances 0.000 description 1
- 235000019270 ammonium chloride Nutrition 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
- 238000007664 blowing Methods 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 238000007865 diluting Methods 0.000 description 1
- 238000010828 elution Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000004744 fabric Substances 0.000 description 1
- 238000007654 immersion Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C23/00—Other surface treatment of glass not in the form of fibres or filaments
- C03C23/008—Other surface treatment of glass not in the form of fibres or filaments comprising a lixiviation step
Landscapes
- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Geochemistry & Mineralogy (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Surface Treatment Of Glass (AREA)
Abstract
Description
【０００１】[0001]
【産業上の利用分野】この発明は耐アルカリ性を具備し
た多孔質ガラスに関する。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a porous glass having alkali resistance.
【０００２】[0002]
【従来の技術】たとえば濾過器などに用いられる一般的
な多孔質ガラスは、ガラス基材を溶融し、分相によって
ケイ素を主体とする骨格相とアルカリ成分を含む可溶相
とに分けるとともに、酸を用いて前記可溶相を除去する
ことによって得られる。2. Description of the Related Art A general porous glass used in, for example, a filter is obtained by melting a glass substrate and separating it into a skeletal phase containing silicon as a main component and a soluble phase containing an alkaline component by phase separation. Obtained by removing the soluble phase with an acid.
【０００３】しかしながら、このような多孔質ガラスに
あっては、前記アルカリ成分に対して侵食されやすいと
いう問題があった。また、多孔質ガラス表面のアルカリ
成分が、経時的にガラス表面に溶出するという問題もあ
る。However, such a porous glass has a problem that it is easily corroded by the alkali component. There is also a problem that the alkaline component on the surface of the porous glass is eluted on the glass surface over time.
【０００４】[0004]
【発明が解決しようとする課題】この発明は、このよう
な問題点に鑑み提案されたものであって、アルカリ液に
対する優れた耐性を有する多孔質ガラスを提供しようと
するものである。SUMMARY OF THE INVENTION The present invention has been proposed in view of the above problems, and it is an object of the present invention to provide a porous glass having excellent resistance to an alkaline solution.
【０００５】[0005]
【課題を解決するための手段】すなわち、この発明は、
硫黄もしくはその化合物または塩化物の反応ガス体によ
って表面のアルカリ成分を除去せしめた多孔質ガラス基
材に、シリコーンオイルが焼付塗着されていることを特
徴とする耐アルカリ性を具備した多孔質ガラスに係る。That is, the present invention is
A porous glass substrate having alkali resistance, characterized in that a silicone oil is baked and applied to a porous glass substrate whose surface alkali components have been removed by a reaction gas of sulfur or its compound or chloride. Pertain.
【０００６】[0006]
【実施例】以下、添付の図面に従ってこの発明を詳細に
説明する。図１はこの発明に用いられる多孔質ガラス基
材の製造例を示す概略図、図２は多孔質ガラス基材の表
面からアルカリ成分を除去する工程の一例を示す断面
図、図３は耐アルカリ性試験の結果を示すグラフであ
る。DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS The present invention will be described in detail below with reference to the accompanying drawings. FIG. 1 is a schematic view showing an example of manufacturing a porous glass substrate used in the present invention, FIG. 2 is a sectional view showing an example of a step of removing an alkaline component from the surface of the porous glass substrate, and FIG. 3 is an alkali resistance. It is a graph which shows the result of a test.
【０００７】この発明の耐アルカリ性を具備した多孔質
ガラスは、表面のアルカリ成分を除去した多孔質ガラス
基材にシリコーンオイルが焼付塗着されてなる。The alkali-resistant porous glass of the present invention is obtained by baking-coating silicone oil on a porous glass substrate from which alkaline components have been removed.
【０００８】この発明に用いられる多孔質ガラス基材
は、広く一般に多用されている多孔質ガラスを用いるこ
とができる。たとえば、ＳｉＯ2 −Ｂ2 Ｏ3 −Ｎａ2 Ｏ
系や、シラス系ではＳｉＯ2 −Ｂ2 Ｏ3 −Ｎａ2 Ｏ−Ｃ
ａＯ−Ａｌ2 Ｏ3 系などから製造される多孔質ガラスで
ある。図１にその多孔質ガラス基材の製造例を示す。な
お、ここでは分相法による多孔質ガラス基材の製法を示
したが、これに限定されることはなく、公知の他の方法
を用いてもよい。まず、あらかじめ適宜の割合で混合し
た硅砂・ソーダ灰・ホウ酸を１２００℃〜１４００℃で
加熱攪拌して溶融し、８００℃〜１１００℃で所望の管
または板などに成形する。そして、図の（Ａ）に示され
るように、得られた未分相のホウ珪酸ガラス１０を、ガ
ラスの分相温度域である５００℃〜６５０℃で数時間か
ら数日間加熱し微細な二相に分相する。この熱処理によ
って、前記ホウ珪酸ガラス１０は（Ｂ）に図示されるよ
うな、ＳｉＯ2 が三次元的に結合した骨格相１１とＢ2
Ｏ−Ｎａ2 Ｏよりなる可溶相１２とに分相される。As the porous glass substrate used in the present invention, porous glass that is widely and commonly used can be used. For example, SiO 2 -B 2 O 3 -Na 2 O
SiO 2 —B 2 O 3 —Na 2 O—C
aO-Al 2 O 3 system is a porous glass produced from such. FIG. 1 shows an example of manufacturing the porous glass substrate. Although the method for producing the porous glass substrate by the phase separation method is shown here, the method is not limited to this and other known methods may be used. First, silica sand, soda ash, and boric acid, which have been mixed in an appropriate ratio in advance, are heated and stirred at 1200 ° C to 1400 ° C to be melted, and molded into a desired tube or plate at 800 ° C to 1100 ° C. Then, as shown in (A) of the figure, the obtained unphased borosilicate glass 10 is heated at a temperature of 500 ° C. to 650 ° C., which is a phase-separating temperature range of the glass, for several hours to several days to obtain a fine two-phase powder. Split into two phases. As a result of this heat treatment, the borosilicate glass 10 and the skeleton phase 11 in which SiO 2 is three-dimensionally bonded and the B 2
It is separated into a soluble phase 12 composed of O—Na 2 O.
【０００９】次いで、前記ホウ珪酸ガラス１０を、約９
０℃に加熱した酸に数時間から数日間接触させる。この
酸処理に用いられる酸としては、硫酸あるいは塩酸など
の一般的な強酸類が好ましく、処理されるガラスに含ま
れる可溶相の割合などによって適宜に選定されて用いら
れる。それによって、この分相されたガラスから前記可
溶相１２が溶出除去されるとともに、当該可溶相１２が
存在した部分が細孔１３として形成され、（Ｃ）に示さ
れるような多孔質ガラス基材１４が得られる。符号１５
は前記細孔１３内に堆積するＳｉＯ2 ゲルである。Next, the borosilicate glass 10 is treated with about 9
Contact with the acid heated to 0 ° C. for several hours to several days. As the acid used for this acid treatment, general strong acids such as sulfuric acid or hydrochloric acid are preferable, and they are appropriately selected and used according to the ratio of the soluble phase contained in the glass to be treated. As a result, the soluble phase 12 is eluted and removed from the phase-separated glass, and the portion where the soluble phase 12 was present is formed as pores 13, and the porous glass as shown in (C). The base material 14 is obtained. Code 15
Is a SiO 2 gel deposited in the pores 13.
【００１０】得られた多孔質ガラス基材１４に、硫黄も
しくはその化合物または塩化物の反応ガス体を接触せし
めて、該ガラス表面のアルカリ成分を除去する。それに
よって、多孔質ガラス基材表面からのアルカリ成分の溶
出を防止し、次工程によって塗着されるシリコーンオイ
ルの塗膜がガラス基材表面と強固に結合することができ
る。The porous glass substrate 14 thus obtained is brought into contact with a reaction gas of sulfur or its compound or chloride to remove the alkaline component on the glass surface. Thereby, the elution of the alkaline component from the surface of the porous glass substrate can be prevented, and the silicone oil coating film applied in the next step can be firmly bonded to the surface of the glass substrate.
【００１１】図２に多孔質ガラス基材からアルカリ成分
を除去する工程の一例を示す。符号２０は処理炉、２１
は移送コンベア、２２はヒーター、２３は反応ガス体の
噴出部である。この工程におけるアルカリ除去処理は、
２５０〜６５０℃の温度域で行われ、処理時間は処理さ
れる多孔質ガラス基材の厚みやガス濃度などによって異
なるが、約１０分〜２時間程度行われる。FIG. 2 shows an example of the step of removing the alkaline component from the porous glass substrate. Reference numeral 20 is a processing furnace, 21
Is a transfer conveyor, 22 is a heater, and 23 is a spouting part of the reaction gas body. The alkali removal treatment in this step is
The treatment is performed in a temperature range of 250 to 650 ° C., and the treatment time is about 10 minutes to 2 hours, varying depending on the thickness of the porous glass substrate to be treated, the gas concentration, and the like.
【００１２】処理炉２０は、前記移送コンベア２１によ
る多孔質ガラス基材Ｇの移送方向に、第１ゾーン２０
Ａ、第２ゾーン２０Ｂ、第３ゾーン２０Ｃ、第４ゾーン
２０Ｄと適宜数の区画に分割されている。実施例では、
このうち第１ゾーン２０Ａがヒーター２２を備えた加熱
ゾーン、第２ゾーン２０Ｂが反応ガス体を噴出する処理
ゾーン、第３ゾーン２０Ｃ以下が脱アルカリ反応を進行
させる反応ゾーンとして構成されている。The processing furnace 20 is provided with a first zone 20 in the transfer direction of the porous glass substrate G by the transfer conveyor 21.
A, the second zone 20B, the third zone 20C, and the fourth zone 20D are divided into an appropriate number of sections. In the example,
Among them, the first zone 20A is configured as a heating zone provided with a heater 22, the second zone 20B is configured as a treatment zone for ejecting a reaction gas, and the third zone 20C and below are configured as reaction zones for promoting dealkalization reaction.
【００１３】図示したように、あらかじめ分相され酸処
理によって多孔化されたガラス基材Ｇが、処理炉２０の
入口より内部の移送コンベア２１上に送り込まれる。符
号２６は前記ガラス基材Ｇをコンベア上に保持するスタ
ンドである。処理炉１０の入口に位置する第１ゾーン２
０Ａにはヒーター２２，２２が設けられていて、アルカ
リ除去処理に好適な温度に多孔質ガラス基材Ｇを加熱す
る。第１ゾーン２０Ａにて加熱された多孔質ガラス基材
Ｇは、移送コンベア２１上を第２ゾーン２０Ｂに送り込
まれる。As shown in the figure, a glass base material G which has been phase-separated in advance and made porous by an acid treatment is fed from an inlet of the processing furnace 20 onto a transfer conveyor 21 inside. Reference numeral 26 is a stand for holding the glass base material G on the conveyor. The first zone 2 located at the entrance of the processing furnace 10
Heaters 22 and 22 are provided at 0A to heat the porous glass substrate G to a temperature suitable for alkali removal treatment. The porous glass substrate G heated in the first zone 20A is sent to the second zone 20B on the transfer conveyor 21.
【００１４】第２ゾーン２０Ｂでは、移送コンベア２１
の上方に反応ガス体の噴出部２３が設けられ、適宜数の
噴出ノズル２４を備えている。この噴出ノズル２４から
前記多孔質ガラス基材Ｇに向かって、硫黄もしくはその
化合物またはその塩化物の反応ガス体が噴出されるよう
に構成されている。前記噴出部２３は一か所でもよい
が、より確実な処理を行うため複数か所設置してもよ
い。このアルカリ除去処理に用いられる反応ガス体とし
ては、硫黄単体または亜硫酸ガスもしくは無水硫酸ガス
の液化ガス、または硫酸アンモニウムもしくは塩化アン
モニウムなどのガス体が用いられる。In the second zone 20B, the transfer conveyor 21
An ejection portion 23 for the reaction gas body is provided above, and an appropriate number of ejection nozzles 24 are provided. A reaction gas of sulfur, a compound thereof, or a chloride thereof is ejected from the ejection nozzle 24 toward the porous glass substrate G. The ejection part 23 may be provided at one place, but may be provided at a plurality of places for more reliable processing. As the reaction gas body used for the alkali removing treatment, a simple substance of sulfur, a liquefied gas of sulfurous acid gas or anhydrous sulfuric acid, or a gas body of ammonium sulfate, ammonium chloride or the like is used.
【００１５】多孔質ガラス基材Ｇが、所定濃度の反応ガ
ス体の雰囲気中を、移動コンベア２１によって第３ゾー
ン２０Ｃから第４ゾーン２０Ｄへと移動していくうち
に、前記反応ガス体が多孔質ガラス基材Ｇの細孔中にも
充満し充分に接触する。そして、そのガラス表面のナト
リウム成分が反応ガス体と接触反応を起こし抽出除去さ
れる。最終ゾーン近辺では、多孔質ガラス基材Ｇを室温
程度まで冷却してアルカリ除去工程が終了する。なお、
実施例の第３ゾーン２０Ｃ以下の処理工程において当該
ゾーンにファン２５を設置して、ゾーン内のガスを対流
させその濃度を均一化することが好ましい。While the porous glass substrate G moves from the third zone 20C to the fourth zone 20D by the moving conveyor 21 in the atmosphere of the reaction gas body having a predetermined concentration, the reaction gas body becomes porous. It also fills the pores of the quality glass substrate G and makes sufficient contact. Then, the sodium component on the glass surface causes a contact reaction with the reaction gas body and is extracted and removed. In the vicinity of the final zone, the porous glass substrate G is cooled to about room temperature and the alkali removing step is completed. In addition,
It is preferable that a fan 25 is installed in the third zone 20C and subsequent processing steps of the embodiment so that the gas in the zone is convected to make the concentration uniform.
【００１６】前記脱アルカリ工程を経て得られた多孔質
ガラスに、シリコーンオイルが焼付塗着される。以下に
その工程例を示す。まず、蒸留水を用いて、前記脱アル
カリ処理工程によって基材ガラス表面に生じたブルーム
（曇り）を洗浄し、洗浄した後、基材ガラスに約１２０
℃の熱風を３０分吹き付けて乾燥し、しかるのち冷風に
切り換えて約３０℃になるまで冷却する。Silicone oil is baked and applied to the porous glass obtained through the dealkalizing step. An example of the process is shown below. First, distilled water is used to wash blooms (cloudiness) generated on the surface of the base glass in the dealkalizing step, and after washing, about 120
It is dried by blowing hot air of ℃ for 30 minutes, and then switched to cold air to cool to about 30 ℃.
【００１７】前記洗浄工程後、前記基材ガラスにシリコ
ーンオイルが塗着される。このシリコーンオイルとして
は、公知のシリコーンオイルが用いられ、実施例では商
品名「ＫＦ８７０」、「ＫＦ９６」、「ＫＦ９９」（い
ずれも信越シリコーン株式会社製）などを使用した。ま
た、前記シリコーンオイルは、その種類や粘度、および
塗着される多孔質ガラスの孔径などによって適宜の濃度
に希釈されて用いられ、その濃度は０．２〜２％が好ま
しいと考えられている。実験によれば、このシリコーン
オイルの濃度が０．２％未満ではアルカリに対する高い
耐性が得られず、２％より高い場合ではコスト高となる
とともに、焼付処理に時間がかかることが判明した。After the cleaning step, silicone oil is applied to the base glass. As this silicone oil, a known silicone oil is used, and in the examples, trade names “KF870”, “KF96”, “KF99” (all manufactured by Shin-Etsu Silicone Co., Ltd.) and the like were used. Further, the silicone oil is used after being diluted to an appropriate concentration depending on the type and viscosity thereof, the pore diameter of the porous glass to be applied, and the like, and the concentration is preferably 0.2 to 2%. . According to experiments, it was found that when the concentration of this silicone oil is less than 0.2%, high resistance to alkali cannot be obtained, and when it is more than 2%, the cost becomes high and the baking process takes time.
【００１８】前記シリコーンオイルを希釈するための溶
剤としては、シリコーンオイルと相溶性を有しかつ多孔
質ガラスに対する高い濡れ特性を有する公知の有機溶剤
が用いられる。好ましくは、ｎ−ヘキサン、ｎ−ヘプタ
ン、ジエチルエーテルなどである。As a solvent for diluting the silicone oil, a known organic solvent which is compatible with the silicone oil and has high wettability with respect to the porous glass is used. Preferred are n-hexane, n-heptane, diethyl ether and the like.
【００１９】前記シリコーンオイルの塗着方法として
は、塗着される基材ガラスの形状や大きさによって適宜
に選定され、スプレー塗着法、浸漬法、刷毛塗り法、布
による塗着法などがあるが、作業性の点から浸漬法が好
適である。The method for applying the silicone oil is appropriately selected according to the shape and size of the base glass to be applied, and includes spray application, dipping, brush application, cloth application and the like. However, the dipping method is preferable from the viewpoint of workability.
【００２０】続いて、前記シリコーンオイルが塗着され
た多孔質ガラス基材が焼付処理される。なお、焼付処理
前に前記シリコーンオイルを希釈した溶剤を完全に除去
するために、前記基材ガラスを５０〜７０℃で放置（風
乾）することが好ましい。Then, the porous glass substrate coated with the silicone oil is baked. In addition, in order to completely remove the solvent diluted with the silicone oil before the baking treatment, it is preferable to leave the base glass at 50 to 70 ° C. (air dry).
【００２１】この焼付処理工程におけるシリコーンオイ
ルの焼付温度は２００〜３５０℃が好ましく、特には２
７０〜３３０℃である。また、焼付時間は、シリコーン
オイルの種類にもよるが５分〜１時間程度が好ましく、
特には２０〜４０分である。それによって、シリコーン
オイルがシロキサン結合するとともに、ガラス表面と反
応して強固に結合する。The baking temperature of the silicone oil in this baking process is preferably 200 to 350 ° C., and particularly 2
It is 70 to 330 ° C. The baking time is preferably about 5 minutes to 1 hour, depending on the type of silicone oil,
Particularly, it is 20 to 40 minutes. As a result, the silicone oil is siloxane-bonded and also reacts with the glass surface to form a strong bond.
【００２２】以下、具体的な製品例を例示し、比較例と
比較して説明する。 〔製造例〕あらかじめ酸処理によって多孔化した多孔質
ガラス基材を、亜硫酸ガス雰囲気下、６００℃で３０分
間加熱しアルカリ除去処理を行った。脱アルカリ処理の
施された多孔質ガラスに０．５％（容量％）に希釈した
シリコーンオイル（ＫＦ−８７０（信越シリコーン社
製））のｎ−ヘキサン溶液を浸漬により塗着し、３００
℃前後で約３０分間加熱して焼付処理を行った。Hereinafter, specific product examples will be illustrated and described in comparison with comparative examples. [Production Example] A porous glass substrate which had been made porous by acid treatment in advance was heated at 600 ° C for 30 minutes in a sulfurous acid gas atmosphere to carry out alkali removal treatment. An n-hexane solution of silicone oil (KF-870 (manufactured by Shin-Etsu Silicone Co., Ltd.)) diluted to 0.5% (volume%) was applied to the porous glass that had been dealkalized by dipping, and 300
A baking process was performed by heating at about 30 ° C. for about 30 minutes.
【００２３】〔比較例〕製造例において、アルカリ除去
処理およびシリコーンオイルの焼付塗着処理をしないほ
かはすべて同様にして多孔質ガラスを得た。Comparative Example A porous glass was obtained in the same manner as in the production example except that the alkali removing treatment and the silicone oil baking treatment were not performed.
【００２４】〔実験例１〕製造例によって得られた多孔
質ガラスを０．０１ＮのＮａＯＨ水溶液に浸漬しその耐
アルカリ性を測定する。結果を図３に示す。[Experimental Example 1] The porous glass obtained by the production example is immersed in a 0.01 N aqueous NaOH solution to measure its alkali resistance. The results are shown in Fig. 3.
【００２５】〔実験例２〕実験例１において、ＮａＯＨ
水溶液を１Ｎにするほかはすべて同様にして耐アルカリ
性を測定する。結果を図３に示す。Experimental Example 2 In Experimental Example 1, NaOH was used.
The alkali resistance is measured in the same manner except that the aqueous solution is 1N. The results are shown in Fig. 3.
【００２６】〔実験例３〕比較例によって得られた多孔
質ガラスを０．０１ＮのＮａＯＨ水溶液に浸漬しその耐
アルカリ性を測定する。結果を図３に示す。[Experimental Example 3] The porous glass obtained by the comparative example is dipped in a 0.01 N NaOH aqueous solution to measure its alkali resistance. The results are shown in Fig. 3.
【００２７】〔実験例４〕比較例１において、ＮａＯＨ
水溶液を１Ｎに調整するほかはすべて同様にして耐アル
カリ性を測定する。結果を図３に示す。Experimental Example 4 In Comparative Example 1, NaOH
The alkali resistance is measured in the same manner except that the aqueous solution is adjusted to 1N. The results are shown in Fig. 3.
【００２８】〔耐アルカリ性測定試験〕 （１）所定濃度に調整した浸漬液（ＮａＯＨ水溶液）を
７０℃に加温し、あらかじめ重量を測定した多孔質ガラ
ス試験片を浸漬する。 （２）一定時間経過後、試験片を取り出して水洗し、希
塩酸で中和洗浄したのち蒸留水でさらに数回洗浄する。 （３）得られた試験片を濾紙にのせ、１２０℃で３０分
乾燥させ室温まで放冷してからその重量を測定する。こ
の作業を繰り返し、その重量変化を観察する。[Alkali Resistance Measurement Test] (1) An immersion liquid (NaOH aqueous solution) adjusted to a predetermined concentration is heated to 70 ° C., and a porous glass test piece whose weight is measured in advance is immersed. (2) After a certain period of time, the test piece is taken out, washed with water, neutralized and washed with dilute hydrochloric acid, and further washed several times with distilled water. (3) The obtained test piece is placed on a filter paper, dried at 120 ° C. for 30 minutes and allowed to cool to room temperature, and then its weight is measured. This operation is repeated and the weight change is observed.
【００２９】図３の実験結果から明らかなように、製品
例によって得られた多孔質ガラスはアルカリ液によって
侵食されにくく、アルカリ成分を除去しない従来の多孔
質ガラスと比して高い耐久性を有している。As is clear from the experimental results shown in FIG. 3, the porous glass obtained by the product example is less likely to be corroded by the alkaline liquid and has a higher durability than the conventional porous glass which does not remove the alkaline component. is doing.
【００３０】[0030]
【発明の効果】以上図示し説明したように、この発明の
耐アルカリ性を具備した多孔質ガラスによれば、硫黄も
しくはその化合物または塩化物の反応ガス体によって、
ガラス基材の表面のアルカリ成分があらかじめ除去され
ているので、ガラス表面にアルカリ成分が溶出すること
がない。この発明ではさらに、ガラス基材からのアルカ
リ成分の溶出がなく、焼付塗着されたシリコーンオイル
の被膜はガラス表面と強固に結合しているので、多孔質
ガラスのアルカリ液に対する耐性をさらに向上させ、そ
の耐久性を著しく向上させることができる。As shown and described above, according to the porous glass having alkali resistance of the present invention, by the reaction gas of sulfur or its compound or chloride,
Since the alkaline component on the surface of the glass substrate has been removed in advance, the alkaline component does not elute on the glass surface. Further, in this invention, the alkali component is not eluted from the glass substrate, and the coating of the silicone oil applied by baking is firmly bonded to the glass surface, further improving the resistance of the porous glass to the alkaline liquid. , Its durability can be remarkably improved.
【図１】この発明に用いられる多孔質ガラス基材の製造
例を示す概略図である。FIG. 1 is a schematic view showing a production example of a porous glass substrate used in the present invention.
【図２】多孔質ガラス基材の表面からアルカリ成分を除
去する工程の一例を示す断面図である。FIG. 2 is a cross-sectional view showing an example of a step of removing an alkaline component from the surface of a porous glass substrate.
【図３】耐アルカリ性試験の結果を示すグラフである。FIG. 3 is a graph showing the results of an alkali resistance test.
１０ ホウ珪酸ガラス １１ 骨格相 １２ 可溶相 １３ 細孔 １４ 多孔質ガラス基材 10 Borosilicate glass 11 Skeletal phase 12 Soluble phase 13 Pore 14 Porous glass substrate
Claims (1)
反応ガス体によって表面のアルカリ成分を除去せしめた
多孔質ガラス基材に、シリコーンオイルが焼付塗着され
ていることを特徴とする耐アルカリ性を具備した多孔質
ガラス。1. Alkali resistance, characterized in that silicone oil is baked and applied to a porous glass substrate from which alkaline components on the surface have been removed by a reaction gas of sulfur or its compound or chloride. Porous glass.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP9197293A JPH06279063A (en) | 1993-03-26 | 1993-03-26 | Porous glass having alkali resistance |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP9197293A JPH06279063A (en) | 1993-03-26 | 1993-03-26 | Porous glass having alkali resistance |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH06279063A true JPH06279063A (en) | 1994-10-04 |
Family
ID=14041450
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP9197293A Pending JPH06279063A (en) | 1993-03-26 | 1993-03-26 | Porous glass having alkali resistance |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH06279063A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2006054313A (en) * | 2004-08-11 | 2006-02-23 | Rohm Co Ltd | Semiconductor light-emitting device |
| JP2011251872A (en) * | 2010-06-01 | 2011-12-15 | Canon Inc | Production method of porous glass |
-
1993
- 1993-03-26 JP JP9197293A patent/JPH06279063A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2006054313A (en) * | 2004-08-11 | 2006-02-23 | Rohm Co Ltd | Semiconductor light-emitting device |
| JP2011251872A (en) * | 2010-06-01 | 2011-12-15 | Canon Inc | Production method of porous glass |
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