JPH0791071B2 - Glass precursor containing non-heat-resistant specimen and manufacturing method thereof - Google Patents
Glass precursor containing non-heat-resistant specimen and manufacturing method thereofInfo
- Publication number
- JPH0791071B2 JPH0791071B2 JP4146936A JP14693692A JPH0791071B2 JP H0791071 B2 JPH0791071 B2 JP H0791071B2 JP 4146936 A JP4146936 A JP 4146936A JP 14693692 A JP14693692 A JP 14693692A JP H0791071 B2 JPH0791071 B2 JP H0791071B2
- Authority
- JP
- Japan
- Prior art keywords
- phosphoric acid
- heat
- silane compound
- general formula
- precursor containing
- 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 17
- 239000002243 precursor Substances 0.000 title claims description 9
- 238000004519 manufacturing process Methods 0.000 title claims description 8
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 50
- -1 alkyl silicate Chemical compound 0.000 claims description 39
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 25
- 229910000077 silane Inorganic materials 0.000 claims description 18
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 claims description 7
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 claims description 7
- 150000001875 compounds Chemical class 0.000 claims description 6
- 125000003545 alkoxy group Chemical group 0.000 claims description 5
- 238000002444 silanisation Methods 0.000 claims description 2
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 claims 1
- 239000000499 gel Substances 0.000 description 14
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 9
- 239000000243 solution Substances 0.000 description 9
- 239000002904 solvent Substances 0.000 description 7
- 239000007788 liquid Substances 0.000 description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 6
- 238000006482 condensation reaction Methods 0.000 description 4
- 238000001879 gelation Methods 0.000 description 4
- 229920000592 inorganic polymer Polymers 0.000 description 4
- 238000000034 method Methods 0.000 description 4
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 3
- 229910004298 SiO 2 Inorganic materials 0.000 description 3
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 description 3
- 239000007795 chemical reaction product Substances 0.000 description 3
- BFXIKLCIZHOAAZ-UHFFFAOYSA-N methyltrimethoxysilane Chemical compound CO[Si](C)(OC)OC BFXIKLCIZHOAAZ-UHFFFAOYSA-N 0.000 description 3
- 238000002156 mixing Methods 0.000 description 3
- 238000003980 solgel method Methods 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 238000009834 vaporization Methods 0.000 description 3
- 230000008016 vaporization Effects 0.000 description 3
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 2
- 125000000217 alkyl group Chemical group 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 239000012153 distilled water Substances 0.000 description 2
- 238000000465 moulding Methods 0.000 description 2
- 150000004756 silanes Chemical class 0.000 description 2
- 230000007704 transition Effects 0.000 description 2
- 239000011240 wet gel Substances 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 241000238631 Hexapoda Species 0.000 description 1
- 239000004698 Polyethylene Substances 0.000 description 1
- 150000001298 alcohols Chemical class 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 239000002518 antifoaming agent Substances 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000003086 colorant Substances 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000008602 contraction Effects 0.000 description 1
- 230000018044 dehydration Effects 0.000 description 1
- 238000006297 dehydration reaction Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 239000011256 inorganic filler Substances 0.000 description 1
- 229910003475 inorganic filler Inorganic materials 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000000049 pigment Substances 0.000 description 1
- 238000006068 polycondensation reaction Methods 0.000 description 1
- 229920000573 polyethylene Polymers 0.000 description 1
- 229920000137 polyphosphoric acid Polymers 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 229910000029 sodium carbonate Inorganic materials 0.000 description 1
- 235000017550 sodium carbonate Nutrition 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 1
Landscapes
- Glass Melting And Manufacturing (AREA)
- Glass Compositions (AREA)
- Silicon Polymers (AREA)
Description
【０００１】[0001]
【産業上の利用分野】本発明は非耐熱性標本入りガラス
先駆体とその製造方法に関する。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a glass precursor containing a non-heat resistant specimen and a method for producing the same.
【０００２】[0002]
【従来の技術】従来、ガラスは、原料となるシリカやソ
ーダ灰などを溶融してガラス化しこれを所定の型に流し
込むか、成型することによって作られてきているが、こ
の方法では、ガラス製造工程で数１００℃以上の高温を
必要とするため大量の熱エネルギーを消費し、経済的に
好ましくないのに加え、成型加工も熟練を要するなど多
くの問題がある。2. Description of the Related Art Conventionally, glass has been produced by melting a raw material such as silica or soda ash and making it into a glass, and then pouring it into a predetermined mold or molding it. Since the process requires a high temperature of several hundreds of degrees Celsius or more, a large amount of heat energy is consumed, which is not economically preferable, and there are many problems such as the molding process requires skill.
【０００３】これに対し、近年、ゾル・ゲル法と呼ばれ
るガラスの低温での製造方法が注目されている。ゾル・
ゲル法は、一般式Ｓｉ（ＯＲ）4 （ここでＲは、メチル
またはエチル基）で示されるアルキルシリケートを主成
分とし、これに水、溶剤、触媒などを加えたゾルを加水
分解・重縮合によってゲル化させ、さらに乾燥させて乾
燥ゲルとしこれを加熱焼結してガラスを得る方法であ
る。On the other hand, in recent years, a method for producing glass at a low temperature, which is called a sol-gel method, has attracted attention. Sol
The gel method is based on an alkyl silicate represented by the general formula Si (OR) 4 (where R is a methyl or ethyl group) as a main component, and water, a solvent, a catalyst, etc. are added to the resulting sol for hydrolysis / polycondensation. This is a method of obtaining a glass by gelling and further drying to obtain a dried gel, which is heat-sintered.
【０００４】[0004]
【発明が解決しようとする課題】ゾル・ゲル法によるガ
ラス製造においては、ゾルが乾燥ゲルに移行する段階
で、溶剤や縮合反応生成物の気散のために、その分の容
積が減ることによりクラックやワレを生じやすいという
問題があり、また、加熱焼結してガラス化するものであ
るから、非耐熱性の標本、例えば生花，ドライフラワ
ー，昆虫，装飾品等を封じ込めことができなかったし、
特に大型のに成型することは困難であった。In the production of glass by the sol-gel method, the volume of the sol is reduced due to the vaporization of the solvent and the condensation reaction product at the stage when the sol shifts to the dry gel. There is a problem that cracks and cracks tend to occur, and because it is heated and sintered to vitrify, non-heat resistant specimens such as fresh flowers, dried flowers, insects, ornaments, etc. could not be contained. Then
In particular, it was difficult to mold it into a large size.
【０００５】本発明は、ゾル・ゲル法によるガラス製造
におけるかかる欠点を改善することを目的としてなされ
た。The present invention has been made with the object of remedying such drawbacks in the production of glass by the sol-gel method.
【０００６】[0006]
【課題を解決するための手段】この発明は、アルキルシ
リケート及びシラン化合物、または、シラン化合物をリ
ン酸と低級アルコールを溶剤として共縮合させることに
よって、上記の問題を解決することを知見し完成に至っ
たもので、さらに詳しくは、一般式（１）で示されるア
ルキルシリケート及び一般式（２）で示されるシラン化
合物をリン酸と、または、一般式（２）で示されるシラ
ン化合物をリン酸と、低級アルコールを溶剤として共縮
合させ、その共縮合物中に非耐熱性標本を没入し、かつ
その全体を密閉状態で静置してゲル化することを内容と
する。 Ｓｉ（ＯＲ）４ （１） ここで、Ｒはメチルまたはエチル基を表す。 Ｒ′ｎＳｉ（ＯＲ″）４−ｎ （２） ここで、Ｒ′、Ｒ″はメチルまたはエチル基、ｎは１ま
たは２を表す。The present invention is directed to an alkyl group.
It has been completed by discovering that the above problems can be solved by co-condensing a silicate and a silane compound or a silane compound with phosphoric acid and a lower alcohol as a solvent. More specifically, the general formula (1) Indicated by
Rutile silicate and silanization represented by general formula (2)
The compound is phosphoric acid, or the sila represented by the general formula (2)
Compounds with phosphoric acid and lower alcohols as solvents
The contents are to immerse the non-heat-resistant specimen in the co-condensate, and leave the whole in a closed state to gel. Si (OR) 4 (1) Here, R represents a methyl or ethyl group. R'n Si (OR ") 4-n (2) Here, R'and R" represent a methyl or ethyl group, and n represents 1 or 2.
【０００７】アルキルシリケート（１）及びシラン化合
物（２）に対するリン酸の割合、または、シラン化合物
（２）に対するリン酸の割合は、アルコキシ（ＯＲ基）
または（ＯＲ″基）の１モルに対してリン酸が１／３〜
１モルの範囲で組み合わされる。リン酸が少なければゲ
ル化に長い時間を要し、多くなればゲル化時間が短くな
る。Ratio of phosphoric acid to alkyl silicate (1) and silane compound (2) or silane compound
The ratio of phosphoric acid to (2) is alkoxy (OR group)
Or phosphoric acid is 1/3 to 1 mol of (OR "group)
Combined in the range of 1 mole. If the amount of phosphoric acid is small, it takes a long time to gel, and if it is large, the gelling time is short.
【０００８】シラン化合物（γ−グリシドキシプロピル
トリアルコキシシラン及び／又はメチルトリメトキシシ
ラン）６０％とエチルシルケートの加水分解物（ＳｉＯ
2 として１０％含む）４０％の混合液をＸ液とする。一
方、８５％リン酸１０％とイソプロピルアルコール９０
％との混合物をＹ液とする。Ｘ液及びＹ液それぞれの比
率によってゾルから湿潤ゲルまでの時間は表１のように
変化した。60% of a silane compound (γ-glycidoxypropyltrialkoxysilane and / or methyltrimethoxysilane) and a hydrolyzate of ethyl silicate (SiO 2
A mixed solution of 40% (including 10% as 2 ) is designated as solution X. On the other hand, 85% phosphoric acid 10% and isopropyl alcohol 90
The mixture with 10% is referred to as liquid Y. The time from the sol to the wet gel changed as shown in Table 1 depending on the ratio of each of the X liquid and the Y liquid.
【０００９】[0009]
【表１】 [Table 1]
【００１０】リン酸としては化学用純８５％リン酸が好
ましいが７５％、８９％、１００％のリン酸や１０５
％、１１５〜１１６％のポリリン酸も使用できる。Chemically pure 85% phosphoric acid is preferred as phosphoric acid, but 75%, 89%, 100% phosphoric acid or 105
%, 115-116% polyphosphoric acid can also be used.
【００１１】アルキルシリケート（１）及びシラン化合
物（２）、または、シラン化合物（２）に対するリン酸
の反応は複雑で正確な表現は困難であるが、例えぱ、ア
ルキルシリケート（１）及びシラン化合物（２）のアル
コキシ基とリン酸が反応して Alkyl silicate (1) and silane compound
The reaction of phosphoric acid with the compound (2) or the silane compound (2) is complicated and accurate expression is difficult, but, for example, the alkoxy group of the alkyl silicate (1) and the silane compound (2) and phosphoric acid are React
【００１２】これが、さらにアルキルシリケート（１）
及びシラン化合物（２）のアルコキシ基と反応して、 This is the alkyl silicate (1)
And it reacts with the alkoxy groups of the silane compound (2),
【００１３】また、さらにリン酸と反応して、 のような反応が繰り返されることによって、次式の構造
を含む無機ポリマーが完成されるものと考えられる。Further, by further reacting with phosphoric acid, It is considered that the inorganic polymer containing the structure of the following formula is completed by repeating the above reaction.
【００１４】 [0014]
【００１５】本発明において、必要に応じて染料、顔料
などの着色剤、無機フィラー、あるいは消泡剤、チクソ
性付与剤などを併用することもできる。In the present invention, a coloring agent such as a dye or a pigment, an inorganic filler, an antifoaming agent, a thixotropy-imparting agent, or the like can be used in combination, if necessary.
【００１６】[0016]
【作用】本発明によれば、アルキルシリケート及びシラ
ン化合物、または、シラン化合物をリン酸と共縮合さ
せ、その共縮合物中に非耐熱性標本を没入し、かつその
全体を密閉状態で静置してゲル化することにより、当該
非標本入りガラス先駆体を製造できるもので、ゲル化す
るまでの時間を調節することができ、しかも、乾燥ゲル
に移行する段階ではゲル中の溶剤や縮合反応生成物の気
散に起因するクラックやワレを生じにくく、したがっ
て、大型に成型することもできる。本発明の共縮合物
は、水溶性物質の縮合反応で得られる物質であるため、
適当な解析手段がなく、上記クラックやワレが生じにく
くなる理由が、今のところ立証できる程に明らかではな
いが、次のように推測される。すなわち、本発明の共縮
合物は、前記のように若干のアルキル基を有する極めて
親水性の無機ポリマーとなっており、したがって、本発
明のゲル体は、イ）水溶性無機ポリマーから溶媒の水が
揮発してゆくようなメカニズムで脱水・脱アルコールが
進行して乾燥ゲルが得られ、ロ）無機ポリマーの親水度
が高いために、ゲル中の水が完全には取り除けないが、
このような含有水状態でも見かけ上、乾燥した状態にな
っていると考えられ、クラックやワレを生じにくくす
る。According to the present invention, alkyl silicates and silas
Co-condensation of silane compounds or silane compounds with phosphoric acid, immersing the non-heat-resistant specimen in the co-condensate, and allowing the whole to stand still in a sealed state and gelate It is a product that can manufacture glass precursors, the time until gelation can be adjusted, and further, cracks and cracks caused by the solvent in the gel and the vaporization of condensation reaction products at the stage of transition to dry gel. It does not easily occur, and therefore can be molded into a large size. Cocondensate of the present invention
Is a substance obtained by the condensation reaction of a water-soluble substance,
The above cracks and cracks are unlikely to occur because there is no suitable analysis method.
The reason why
However, it is supposed as follows . That is, the contraction of the present invention
The compound has very few alkyl groups as described above.
Since it is a hydrophilic inorganic polymer,
The bright gel body is a) The water of the solvent from the water-soluble inorganic polymer
Dehydration and dealcoholization are carried out by a mechanism that evaporates.
Progresses to dry gel, b) hydrophilicity of inorganic polymer
The water in the gel cannot be completely removed due to the high
Even with such water content, it appears to be dry.
It is thought that the cracks and cracks are less likely to occur
It
【００１７】[0017]
【実施例】実施例１ γ−グリシドキシプロピルトリアルコキシシラン４００
ｇにメチルトリメトキシシラン１００ｇを加え良く撹拌
・混合した（Ａ液という）。一方、エチルシリケートの
加水分解物（ＳｉＯ2 として１０％含む）３００ｇと８
５％リン酸１００ｇをＩＰＡ（イソプロピルアルコー
ル）１００ｇに溶解した（Ｂ液という）。EXAMPLES Example 1 γ-glycidoxypropyltrialkoxysilane 400
100 g of methyltrimethoxysilane was added to g and well mixed and stirred (referred to as solution A). On the other hand, 300 g of a hydrolyzate of ethyl silicate (containing 10% as SiO 2 ) and 8
100 g of 5% phosphoric acid was dissolved in 100 g of IPA (isopropyl alcohol) (referred to as solution B).
【００１８】Ａ液とＢ液を静かに混合して得られたゾル
を、密閉のできるガラスあるいはポリエチレン等の透明
容器に入れるとともに、その中に新鮮な生花一輪を下向
きにして没入設置して室温に静置した。ゾルは４８時間
後にはゲル化し流動性がなくなった。その後、透明容器
の蓋の一部に穴を開けることによってこの容器を外部に
対して開放し、室温で４週間静置することにより湿潤ゲ
ルを乾燥ゲルとした。その乾燥ゲルを容器から取り出し
た。上記生花一輪は上記没入時の新鮮さ及び立体的状態
をそのまま保持している様子を外部から見ることができ
た。The sol obtained by gently mixing the liquids A and B is placed in a hermetically-sealed transparent container such as glass or polyethylene, and a fresh flower arrangement is placed in the container so that the sol is placed at room temperature. It was left still. The sol gelled after 48 hours and disappeared. After that, this container was opened to the outside by making a hole in a part of the lid of the transparent container, and left at room temperature for 4 weeks to make the wet gel a dry gel. The dry gel was removed from the container. It could be seen from the outside that the above-mentioned flower arrangement retains the freshness and the three-dimensional state as it was when it was immersed.
【００１９】実施例２ 蒸留水９９ｇに酢酸１ｇを加えて撹拌し、これをγ−グ
リシドキシプロピルトリアルコキシシラン４００ｇに滴
下し、撹拌混合した（Ａ2 液という）。一方、８５％リ
ン酸１００ｇを蒸留水４００ｇに溶解した（Ｂ2 液とい
う）。Ａ2 液とＢ2 液を静かに混合して得られたゾル
を、実施例１と同様に、透明容器に入れ、かつその中に
新鮮な生花一輪を下向きにして没入設置して室温に静置
した。ゾルは７２時間後にはゲル化し流動性がなくなっ
た。Example 2 1 g of acetic acid was added to 99 g of distilled water and stirred, which was added dropwise to 400 g of γ-glycidoxypropyltrialkoxysilane and mixed by stirring (referred to as A 2 solution). On the other hand, 100 g of 85% phosphoric acid was dissolved in 400 g of distilled water (referred to as solution B 2 ). The sol obtained by gently mixing the solution A 2 and the solution B 2 was placed in a transparent container in the same manner as in Example 1, and a fresh flower arrangement was placed downwardly in the container to allow it to stand at room temperature. I put it. The sol gelled after 72 hours and lost fluidity.
【００２０】実施例３ γ−グリシドキシプロピルトリアルコキシシラン４００
ｇにメチルトリメトキシシラン１００ｇを加え、良く撹
拌・混合した（Ａ3 液という）。一方、エチルシリケー
トの加水分解物（ＳｉＯ2 として１０％含む）４８０ｇ
に８５％リン酸８０ｇを良く混合撹拌した（Ｂ3 液とい
う）。Ａ3 液とＢ3 液を静かに混合して得られたゾル
を、実施例１と同様に、透明容器に入れ、かつその中に
ドライフラワーを下向きにして没入設置して室温に静置
した。ゾルは３６時間後にはゲル化し流動性がなくなっ
た。Example 3 γ-glycidoxypropyltrialkoxysilane 400
100 g of methyltrimethoxysilane was added to g, and well stirred and mixed (referred to as A 3 solution). On the other hand, ethyl silicate hydrolyzate (containing 10% as SiO 2 ) 480 g
80 g of 85% phosphoric acid was thoroughly mixed and stirred (referred to as solution B 3 ). The sol obtained by gently mixing the liquid A 3 and the liquid B 3 was placed in a transparent container in the same manner as in Example 1, and the dried flower was immersed therein with the dried flower facing downward and allowed to stand at room temperature. . The sol gelled after 36 hours and lost its fluidity.
【００２１】[0021]
【発明の効果】以上述べたところから明らかなように、
本発明によれば、アルキルシリケート及びシラン化合
物、または、シラン化合物をリン酸と共縮合させ、その
共縮合物中に非耐熱性標本を没入し、かつその全体を密
閉状態で静置してゲル化することにより、当該標本入り
ガラス先駆体を製造できるもので、ゲル化するまでの時
間を調節することができ、しかも、乾燥ゲルに移行する
段階ではゲル中の溶剤や縮合反応生成物の気散に起因す
るクラックやワレを生じにくく、したがってまた、大型
に成型することもできる。その上、本発明ガラス先駆体
は、透明度が高く当該標本を外部からよく見ることがで
きるとともに、その封じ込みも完全であるから当該標本
の長期保存に有効である。As is apparent from the above description,
According to the invention, an alkyl silicate and a silane compound
Substance or a silane compound is co-condensed with phosphoric acid, the non-heat-resistant specimen is immersed in the co-condensate, and the entire specimen is allowed to stand in a sealed state for gelation to give a glass precursor containing the specimen. The body can be manufactured, the time until gelation can be adjusted, and at the stage of transition to dry gel, cracks and cracks due to solvent in the gel and vaporization of condensation reaction products are less likely to occur. Therefore, it can also be molded into a large size. In addition, the glass precursor of the present invention is highly transparent and allows the sample to be seen well from the outside, and since it is completely contained, it is effective for long-term storage of the sample.
Claims (4)
ト及び一般式（２）で示されるシラン化合物とリン酸と
の共縮合物中、または、一般式（２）で示されるシラン
化合物とリン酸との共縮合物中に非耐熱性標本を封じ込
んでなることを特徴とする非耐熱性標本入りガラス先駆
体。 Ｓｉ（ＯＲ）４ （１） ここで、Ｒはメチルまたはエチル基を表す。 Ｒ′ｎＳｉ（ＯＲ″）４−ｎ （２） ここで、Ｒ′、Ｒ″はメチルまたはエチル基、ｎは１ま
たは２を表す。1. An alkyl silicate represented by the general formula (1) :
And a silane compound represented by the general formula (2) and phosphoric acid
In the co-condensate of silane or represented by the general formula (2)
A glass precursor containing a non-heat-resistant specimen, comprising a non-heat-resistant specimen enclosed in a cocondensate of a compound and phosphoric acid . Si (OR) 4 (1) Here, R represents a methyl or ethyl group. R'n Si (OR ") 4-n (2) Here, R'and R" represent a methyl or ethyl group, and n represents 1 or 2.
ト及び一般式（２）で示されるシラン化合物をリン酸と
共縮合させ、または、一般式（２）で示されるシラン化
合物をリン酸と共縮合させ、得られた共縮合物中に非耐
熱性標本を没入し、かつ、その全体を密閉状態で静置し
てゲル化することを特徴とする非耐熱性標本入りガラス
先駆体の製造方法。 Ｓｉ（ＯＲ）４ （１） ここで、Ｒはメチルまたはエチル基を表す。 Ｒ′ｎＳｉ（ＯＲ″）４−ｎ （２） ここで、Ｒ′、Ｒ″はメチルまたはエチル基、ｎは１ま
たは２を表す。2. An alkyl silicate represented by the general formula (1) :
And a silane compound represented by the general formula (2) with phosphoric acid
Cocondensation or silanization represented by the general formula (2)
A non-heat-resistant specimen characterized by co-condensing a compound with phosphoric acid , immersing the non-heat-resistant specimen in the obtained co-condensate, and allowing the whole to stand in a sealed state to gel. Manufacturing method of glass precursor containing glass. Si (OR) 4 (1) Here, R represents a methyl or ethyl group. R'n Si (OR ") 4-n (2) Here, R'and R" represent a methyl or ethyl group, and n represents 1 or 2.
たは、シラン化合物のアルコキシ基１モルに対してリン
酸が１／３〜１モルである請求項１記載の共縮合物から
なる非耐熱性標本入りガラス先駆体。3. An alkyl silicate and a silane compound, or
Alternatively, the glass precursor containing a non-heat-resistant specimen comprising the cocondensate according to claim 1, wherein phosphoric acid is 1/3 to 1 mol per 1 mol of the alkoxy group of the silane compound .
たは、シラン化合物のアルコキシ基１モルに対してリン
酸が１／３〜１モルである請求項２記載の非耐熱性標本
入りガラス先駆体の製造方法。4. An alkyl silicate and a silane compound, or
The method for producing a glass precursor containing a non-heat resistant specimen according to claim 2, wherein the phosphoric acid is 1/3 to 1 mol per 1 mol of the alkoxy group of the silane compound .
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP4146936A JPH0791071B2 (en) | 1992-05-13 | 1992-05-13 | Glass precursor containing non-heat-resistant specimen and manufacturing method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP4146936A JPH0791071B2 (en) | 1992-05-13 | 1992-05-13 | Glass precursor containing non-heat-resistant specimen and manufacturing method thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH05319862A JPH05319862A (en) | 1993-12-03 |
| JPH0791071B2 true JPH0791071B2 (en) | 1995-10-04 |
Family
ID=15418924
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP4146936A Expired - Lifetime JPH0791071B2 (en) | 1992-05-13 | 1992-05-13 | Glass precursor containing non-heat-resistant specimen and manufacturing method thereof |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH0791071B2 (en) |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE69328963T2 (en) * | 1992-12-16 | 2000-12-07 | Shiseido Co. Ltd., Tokio/Tokyo | DRY FLOWER AND METHOD FOR PRODUCING THE SAME |
| US20090029064A1 (en) * | 2007-07-25 | 2009-01-29 | Carlton Maurice Truesdale | Apparatus and method for making nanoparticles using a hot wall reactor |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS6225616A (en) * | 1985-07-24 | 1987-02-03 | Shimizu Constr Co Ltd | Auger excavator with built-in blade |
-
1992
- 1992-05-13 JP JP4146936A patent/JPH0791071B2/en not_active Expired - Lifetime
Also Published As
| Publication number | Publication date |
|---|---|
| JPH05319862A (en) | 1993-12-03 |
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