JP5660170B2 - Particulate composition containing nitrate and method for producing the same - Google Patents
Particulate composition containing nitrate and method for producing the same Download PDFInfo
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- JP5660170B2 JP5660170B2 JP2013165370A JP2013165370A JP5660170B2 JP 5660170 B2 JP5660170 B2 JP 5660170B2 JP 2013165370 A JP2013165370 A JP 2013165370A JP 2013165370 A JP2013165370 A JP 2013165370A JP 5660170 B2 JP5660170 B2 JP 5660170B2
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- particulate composition
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- 239000000203 mixture Substances 0.000 title claims description 81
- 238000004519 manufacturing process Methods 0.000 title claims description 12
- 229910002651 NO3 Inorganic materials 0.000 title description 3
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 title description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 172
- 238000012360 testing method Methods 0.000 claims description 114
- IWOUKMZUPDVPGQ-UHFFFAOYSA-N barium nitrate Chemical compound [Ba+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O IWOUKMZUPDVPGQ-UHFFFAOYSA-N 0.000 claims description 82
- DHEQXMRUPNDRPG-UHFFFAOYSA-N strontium nitrate Chemical compound [Sr+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O DHEQXMRUPNDRPG-UHFFFAOYSA-N 0.000 claims description 80
- 239000000377 silicon dioxide Substances 0.000 claims description 77
- 230000002209 hydrophobic effect Effects 0.000 claims description 48
- 238000000034 method Methods 0.000 claims description 35
- 230000035945 sensitivity Effects 0.000 claims description 30
- 239000011521 glass Substances 0.000 claims description 28
- 238000002156 mixing Methods 0.000 claims description 17
- 239000002994 raw material Substances 0.000 claims description 17
- 238000007254 oxidation reaction Methods 0.000 claims description 3
- 230000008569 process Effects 0.000 claims description 3
- 238000002485 combustion reaction Methods 0.000 description 40
- 230000000052 comparative effect Effects 0.000 description 26
- 238000004880 explosion Methods 0.000 description 23
- 239000002245 particle Substances 0.000 description 23
- 239000000126 substance Substances 0.000 description 18
- 238000012790 confirmation Methods 0.000 description 16
- 239000007787 solid Substances 0.000 description 15
- 239000000463 material Substances 0.000 description 11
- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Chemical compound [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 description 10
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 9
- 229910002012 Aerosil® Inorganic materials 0.000 description 8
- 230000001590 oxidative effect Effects 0.000 description 8
- XWNSFEAWWGGSKJ-UHFFFAOYSA-N 4-acetyl-4-methylheptanedinitrile Chemical compound N#CCCC(C)(C(=O)C)CCC#N XWNSFEAWWGGSKJ-UHFFFAOYSA-N 0.000 description 6
- 239000004153 Potassium bromate Substances 0.000 description 6
- 239000013056 hazardous product Substances 0.000 description 6
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 6
- 229940094037 potassium bromate Drugs 0.000 description 6
- 235000019396 potassium bromate Nutrition 0.000 description 6
- 239000004323 potassium nitrate Substances 0.000 description 5
- 235000010333 potassium nitrate Nutrition 0.000 description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 5
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 4
- 229910000831 Steel Inorganic materials 0.000 description 4
- 239000001913 cellulose Substances 0.000 description 4
- 229920002678 cellulose Polymers 0.000 description 4
- 229910017604 nitric acid Inorganic materials 0.000 description 4
- VKJKEPKFPUWCAS-UHFFFAOYSA-M potassium chlorate Chemical compound [K+].[O-]Cl(=O)=O VKJKEPKFPUWCAS-UHFFFAOYSA-M 0.000 description 4
- 239000010959 steel Substances 0.000 description 4
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 description 3
- 239000000919 ceramic Substances 0.000 description 3
- 239000003795 chemical substances by application Substances 0.000 description 3
- AXZAYXJCENRGIM-UHFFFAOYSA-J dipotassium;tetrabromoplatinum(2-) Chemical compound [K+].[K+].[Br-].[Br-].[Br-].[Br-].[Pt+2] AXZAYXJCENRGIM-UHFFFAOYSA-J 0.000 description 3
- 238000002844 melting Methods 0.000 description 3
- 230000008018 melting Effects 0.000 description 3
- 239000003960 organic solvent Substances 0.000 description 3
- 229910052697 platinum Inorganic materials 0.000 description 3
- 229910001487 potassium perchlorate Inorganic materials 0.000 description 3
- 229910000077 silane Inorganic materials 0.000 description 3
- 235000012239 silicon dioxide Nutrition 0.000 description 3
- 238000003860 storage Methods 0.000 description 3
- 229910002016 Aerosil® 200 Inorganic materials 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 2
- 229920004482 WACKER® Polymers 0.000 description 2
- AYJRCSIUFZENHW-UHFFFAOYSA-L barium carbonate Chemical compound [Ba+2].[O-]C([O-])=O AYJRCSIUFZENHW-UHFFFAOYSA-L 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000011156 evaluation Methods 0.000 description 2
- 239000002360 explosive Substances 0.000 description 2
- 238000007667 floating Methods 0.000 description 2
- 235000013312 flour Nutrition 0.000 description 2
- 229910021485 fumed silica Inorganic materials 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 239000000383 hazardous chemical Substances 0.000 description 2
- FFUAGWLWBBFQJT-UHFFFAOYSA-N hexamethyldisilazane Chemical compound C[Si](C)(C)N[Si](C)(C)C FFUAGWLWBBFQJT-UHFFFAOYSA-N 0.000 description 2
- BDAGIHXWWSANSR-NJFSPNSNSA-N hydroxyformaldehyde Chemical compound O[14CH]=O BDAGIHXWWSANSR-NJFSPNSNSA-N 0.000 description 2
- 230000006872 improvement Effects 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 239000011259 mixed solution Substances 0.000 description 2
- 230000003472 neutralizing effect Effects 0.000 description 2
- 238000004321 preservation Methods 0.000 description 2
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 description 2
- 229910052710 silicon Inorganic materials 0.000 description 2
- 239000010703 silicon Substances 0.000 description 2
- 238000010583 slow cooling Methods 0.000 description 2
- VWDWKYIASSYTQR-UHFFFAOYSA-N sodium nitrate Chemical compound [Na+].[O-][N+]([O-])=O VWDWKYIASSYTQR-UHFFFAOYSA-N 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 239000010421 standard material Substances 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- 229910000018 strontium carbonate Inorganic materials 0.000 description 2
- 239000004094 surface-active agent Substances 0.000 description 2
- 230000002194 synthesizing effect Effects 0.000 description 2
- 239000002023 wood Substances 0.000 description 2
- 229920006310 Asahi-Kasei Polymers 0.000 description 1
- 239000006087 Silane Coupling Agent Substances 0.000 description 1
- 239000004115 Sodium Silicate Substances 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 239000003905 agrochemical Substances 0.000 description 1
- 150000004996 alkyl benzenes Chemical class 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 238000000137 annealing Methods 0.000 description 1
- CJDPJFRMHVXWPT-UHFFFAOYSA-N barium sulfide Chemical compound [S-2].[Ba+2] CJDPJFRMHVXWPT-UHFFFAOYSA-N 0.000 description 1
- 229940092714 benzenesulfonic acid Drugs 0.000 description 1
- 230000005540 biological transmission 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
- 238000005352 clarification Methods 0.000 description 1
- 238000007596 consolidation process Methods 0.000 description 1
- 238000010924 continuous production Methods 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 239000002537 cosmetic Substances 0.000 description 1
- 230000008878 coupling Effects 0.000 description 1
- 238000010168 coupling process Methods 0.000 description 1
- 238000005859 coupling reaction Methods 0.000 description 1
- 235000014113 dietary fatty acids Nutrition 0.000 description 1
- 239000004205 dimethyl polysiloxane Substances 0.000 description 1
- 235000013870 dimethyl polysiloxane Nutrition 0.000 description 1
- LIKFHECYJZWXFJ-UHFFFAOYSA-N dimethyldichlorosilane Chemical compound C[Si](C)(Cl)Cl LIKFHECYJZWXFJ-UHFFFAOYSA-N 0.000 description 1
- 239000002270 dispersing agent Substances 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 238000004043 dyeing Methods 0.000 description 1
- 239000003995 emulsifying agent Substances 0.000 description 1
- NKSJNEHGWDZZQF-UHFFFAOYSA-N ethenyl(trimethoxy)silane Chemical compound CO[Si](OC)(OC)C=C NKSJNEHGWDZZQF-UHFFFAOYSA-N 0.000 description 1
- 239000000194 fatty acid Substances 0.000 description 1
- 229930195729 fatty acid Natural products 0.000 description 1
- 150000004665 fatty acids Chemical class 0.000 description 1
- 239000010419 fine particle Substances 0.000 description 1
- 238000005187 foaming Methods 0.000 description 1
- 238000000915 furnace ionisation nonthermal excitation spectrometry Methods 0.000 description 1
- 239000003721 gunpowder Substances 0.000 description 1
- 230000003301 hydrolyzing effect Effects 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 238000005342 ion exchange Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- GBMDVOWEEQVZKZ-UHFFFAOYSA-N methanol;hydrate Chemical compound O.OC GBMDVOWEEQVZKZ-UHFFFAOYSA-N 0.000 description 1
- 239000006060 molten glass Substances 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 229910001120 nichrome Inorganic materials 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- GHBKQPVRPCGRAQ-UHFFFAOYSA-N octylsilicon Chemical compound CCCCCCCC[Si] GHBKQPVRPCGRAQ-UHFFFAOYSA-N 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 description 1
- 229920001296 polysiloxane Polymers 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 239000010453 quartz Substances 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 238000002407 reforming Methods 0.000 description 1
- 239000004576 sand Substances 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000010865 sewage Substances 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
- 125000005372 silanol group Chemical group 0.000 description 1
- -1 silicon alkoxide Chemical class 0.000 description 1
- 150000003377 silicon compounds Chemical class 0.000 description 1
- 239000004317 sodium nitrate Substances 0.000 description 1
- 235000010344 sodium nitrate Nutrition 0.000 description 1
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 description 1
- 229910052911 sodium silicate Inorganic materials 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 229910001631 strontium chloride Inorganic materials 0.000 description 1
- AHBGXTDRMVNFER-UHFFFAOYSA-L strontium dichloride Chemical compound [Cl-].[Cl-].[Sr+2] AHBGXTDRMVNFER-UHFFFAOYSA-L 0.000 description 1
- UUCCCPNEFXQJEL-UHFFFAOYSA-L strontium dihydroxide Chemical compound [OH-].[OH-].[Sr+2] UUCCCPNEFXQJEL-UHFFFAOYSA-L 0.000 description 1
- 229910001866 strontium hydroxide Inorganic materials 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 239000012756 surface treatment agent Substances 0.000 description 1
- 239000000271 synthetic detergent Substances 0.000 description 1
- 239000012808 vapor phase Substances 0.000 description 1
- 238000004065 wastewater treatment Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F11/00—Compounds of calcium, strontium, or barium
- C01F11/36—Nitrates
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F11/00—Compounds of calcium, strontium, or barium
- C01F11/36—Nitrates
- C01F11/44—Concentrating; Crystallisating; Dehydrating; Preventing the absorption of moisture or caking
-
- 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
- C03C1/00—Ingredients generally applicable to manufacture of glasses, glazes, or vitreous enamels
- C03C1/02—Pretreated ingredients
- C03C1/026—Pelletisation or prereacting of powdered raw materials
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Inorganic Chemistry (AREA)
- Geology (AREA)
- General Chemical & Material Sciences (AREA)
- Materials Engineering (AREA)
- Geochemistry & Mineralogy (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Silicon Compounds (AREA)
- Glass Compositions (AREA)
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
- Catalysts (AREA)
- Glass Melting And Manufacturing (AREA)
- Cosmetics (AREA)
Description
本発明は、硝酸塩を含有する粒子状組成物、その製造方法、該粒子状組成物から形成されたガラス、及び硝酸塩の保存方法に関する。 The present invention relates to a particulate composition containing nitrate, a method for producing the same, a glass formed from the particulate composition, and a method for storing nitrate.
硝酸ストロンチウムや硝酸バリウムは、火薬や発炎筒の原料として用いられている。また硝酸ストロンチウムに関しては、自動車のエアバッグのガス発生剤としても使用されている（例えば特許文献１）。 Strontium nitrate and barium nitrate are used as raw materials for gunpowder and flame tubes. Strontium nitrate is also used as a gas generating agent for automobile airbags (for example, Patent Document 1).
硝酸ストロンチウムや硝酸バリウムは、可燃物を酸化して、激しい燃焼や爆発を起こすおそれがあることから、日本国の消防法においては酸化性固体として危険物に指定されている物質である。このような危険物は、それを取り扱う作業員を危険に曝すこととなり、安全性の問題がある。また工場などで取り扱う際には防火あるいは防爆設備の設置や保有空地の確保が必要となり、コスト面でも不利である。法令上も、危険物は製造、運搬、貯蔵等の面において厳しい規制を受ける。 Strontium nitrate and barium nitrate are substances that are designated as hazardous materials as oxidizable solids in the Japanese Fire Service Act because they can oxidize combustible materials and cause severe combustion and explosion. Such dangerous goods endanger the workers who handle them, and there is a safety problem. In addition, when handling in factories, it is necessary to install fireproof or explosion-proof equipment and secure an open space, which is disadvantageous in terms of cost. In accordance with laws and regulations, dangerous goods are subject to strict regulations in terms of manufacturing, transportation and storage.
また、硝酸ストロンチウムや硝酸バリウムは、火薬用途に限らず、セラミックスやガラスの原料としても期待されている材料である。セラミックスやガラスの原料として用いる場合には、その酸化性は成形・取扱いの際における安全を脅かすおそれがある。このように、セラミックスやガラスの原料としては、危険性を排除した、より安全性の高い材料への改質が求められている。 In addition, strontium nitrate and barium nitrate are not only used for explosives but are also expected as raw materials for ceramics and glass. When used as a raw material for ceramics and glass, its oxidizability may threaten safety during molding and handling. Thus, as a raw material for ceramics and glass, there is a demand for reforming the material into a safer material that eliminates danger.
これまでにも、硝酸ストロンチウムや硝酸バリウムを改質する方法として、微粒子珪酸を適量含有させることにより、粒子の固結を防止する方法が開示されている（特許文献２）。しかしながら、一般的な微粒子珪酸では爆発や燃焼の危険性を減少させるには不十分であった。 So far, as a method for modifying strontium nitrate or barium nitrate, a method for preventing particle consolidation by containing an appropriate amount of fine particle silicic acid has been disclosed (Patent Document 2). However, general particulate silicic acid has been insufficient to reduce the risk of explosion and combustion.
爆発や燃焼の危険性を低減させる従来の方法としては、アルキルベンゼンスルホン酸を添加する方法がある。界面活性剤であるアルキルベンゼンスルホン酸は家庭用及び業務用の合成洗剤（洗濯用、台所用）として使用され、また染色助剤、農薬乳化剤、精錬剤、分散剤や化粧品としても使用されている。一方で河川や下水処理場での発泡や、他の一般的な界面活性剤に比べて生分解性が低いといった問題があり、工業的な生産において排水処理を考慮した場合、添加剤としては適さない。 As a conventional method for reducing the risk of explosion or combustion, there is a method of adding alkylbenzenesulfonic acid. Alkyl benzene sulfonic acid, which is a surfactant, is used as a synthetic detergent for household and commercial use (for laundry and kitchen use), and is also used as a dyeing assistant, agricultural chemical emulsifier, refining agent, dispersant and cosmetics. On the other hand, there are problems such as foaming in rivers and sewage treatment plants and low biodegradability compared to other general surfactants, which are suitable as additives when wastewater treatment is considered in industrial production. Absent.
また粒子を粗大化させることで危険性を低減させることも可能であるが、工業的な大量・連続生産には不向きであり、各種用途での使用の面でも均一混合が難しいといった問題がある。 In addition, although it is possible to reduce the risk by coarsening the particles, it is not suitable for industrial mass production and continuous production, and there is a problem that uniform mixing is difficult in terms of use in various applications.
本発明の目的の一つは、安全性が高く、取り扱い易い、硝酸ストロンチウム又は硝酸バリウムを含有する材料を提供することにある。具体的には、消防法上、危険物に該当しない、安全性の高い硝酸ストロンチウム又は硝酸バリウムを含有する材料を提供することにある。 One object of the present invention is to provide a material containing strontium nitrate or barium nitrate that is highly safe and easy to handle. Specifically, an object of the present invention is to provide a material containing strontium nitrate or barium nitrate that does not fall under the category of hazardous materials and is highly safe.
すなわち本発明の第１の態様は、硝酸ストロンチウム及び／又は硝酸バリウムと、疎水性シリカとを含有し、日本国消防法の危険物第一類の燃焼試験及び落球式打撃感度試験で危険物に該当しない粒子状組成物に関する。前記疎水性シリカは、好ましくは、そのＢＥＴ比表面積が５０〜４００ｍ２／ｇである。 That is, the first aspect of the present invention contains strontium nitrate and / or barium nitrate and hydrophobic silica, and is classified as a dangerous substance in the fire test and the falling ball hitting sensitivity test of the first class of dangerous goods of the Japanese Fire Service Act. It relates to a particulate composition not applicable. The hydrophobic silica preferably has a BET specific surface area of 50 to 400 m 2 / g.
上記粒子状組成物は、好ましくは国連勧告・試験マニュアル「Ｒｅｃｏｍｍｅｎｄａｔｉｏｎ ｏｎ ｔｈｅ ＴＲＡＮＳＰＯＲＴ ＯＦ ＤＡＮＧＥＲＯＵＳ ＧＯＯＤＳ −Ｍａｎｕａｌ ｏｆ Ｔｅｓｔｓ ａｎｄ Ｃｒｉｔｅｒｉａ− Ｔｈｉｒｄ ｒｅｖｉｓｅｄ ｅｄｉｔｉｏｎ」に準拠した、国連勧告によるＣＬＡＳＳ ５−Ｄｉｖｉｓｉｏｎ ５．１（酸化性固体）の燃焼試験で危険物に該当しないものである。 The particulate composition is preferably a CLASS oxidization 5 test according to the UN recommendation 5 according to the UN recommendation and test manual "Recommendation on the TRANSPORT OF DANGEROUS GOODS-Manual of Tests and Criteria- Third revised edition". Solid) combustion test does not fall under dangerous goods.
上記粒子状組成物は、好ましくは上記硝酸ストロンチウム又は硝酸バリウムを９５．０〜９９．８質量％含有するものである。 The particulate composition preferably contains 95.0 to 99.8% by mass of the strontium nitrate or barium nitrate.
上記粒子状組成物は、ガラス原料として好適に使用することができる。 The particulate composition can be suitably used as a glass raw material.
また上記粒子状組成物は、好ましくは上記疎水性シリカを０．１〜３．０質量％含有する（但し、粒子状組成物の全質量は１００質量％である）ものである。 The particulate composition preferably contains 0.1 to 3.0% by mass of the hydrophobic silica (however, the total mass of the particulate composition is 100% by mass).
本発明の第２の態様は硝酸ストロンチウム及び／又は硝酸バリウムと、疎水性シリカとを混合する工程を含む粒子状組成物の製造方法に関する。 The 2nd aspect of this invention is related with the manufacturing method of the particulate composition including the process of mixing strontium nitrate and / or barium nitrate, and hydrophobic silica.
本発明の第３の態様は粒子状組成物から作製されるガラスに関する。 A third aspect of the present invention relates to glass made from a particulate composition.
本発明の第４の態様は疎水性シリカを混合する硝酸ストロンチウム及び／又は硝酸バリウムの保存方法に関する。 The fourth aspect of the present invention relates to a method for preserving strontium nitrate and / or barium nitrate mixed with hydrophobic silica.
本発明は、特定のシリカの作用により、本来消防法上の危険物である硝酸ストロンチウム及び／又は硝酸バリウムの燃焼性や爆発性を抑制させ危険性を低減することができ、日本国消防法上の危険物に該当しないものとすることができる。これにより、使用や保存、輸送等における安全性を高めることができる。また防爆設備等が不要となることから製造設備の面においてもコストダウンに寄与することができる。 The present invention can reduce the risk by suppressing the flammability and explosiveness of strontium nitrate and / or barium nitrate, which are inherently dangerous materials under the Fire Service Act, by the action of specific silica. May not fall under the category of dangerous goods. Thereby, the safety | security in use, a preservation | save, transportation, etc. can be improved. In addition, since no explosion-proof equipment or the like is required, it is possible to contribute to cost reduction in terms of manufacturing equipment.
（硝酸ストロンチウム及び硝酸バリウム）
本発明の粒子状組成物は硝酸ストロンチウム及び／又は硝酸バリウムを含有する。本発明で用いる硝酸ストロンチウムとしては特に制限はなく、合成したものを用いてもよいし、市販のものを用いてもよい。硝酸ストロンチウムを合成する方法としては、特に限定されないが、例えば水酸化ストロンチウムと硝酸の中和反応による方法や、炭酸ストロンチウムと硝酸を反応させることにより、硝酸ストロンチウムと炭酸に変換する方法、塩化ストロンチウムの濃厚溶液に硝酸ナトリウムを添加して反応させる方法などが挙げられる。
(Strontium nitrate and barium nitrate)
The particulate composition of the present invention contains strontium nitrate and / or barium nitrate. There is no restriction | limiting in particular as strontium nitrate used by this invention, What was synthesize | combined may be used and a commercially available thing may be used. The method for synthesizing strontium nitrate is not particularly limited. For example, a method of neutralizing strontium hydroxide and nitric acid, a method of converting strontium carbonate and nitric acid by reacting strontium carbonate and nitric acid, strontium chloride For example, a method in which sodium nitrate is added to the concentrated solution and reacted is used.
本発明で用いる硝酸バリウムについても特に制限はなく、合成したものを用いてもよいし、市販のものを用いてもよい。硝酸バリウムを合成する方法としては、特に限定されないが、例えば炭酸バリウム又は硫化バリウムに硝酸を作用させる方法などが挙げられる。 There is no restriction | limiting in particular also about the barium nitrate used by this invention, What was synthesize | combined may be used and a commercially available thing may be used. The method for synthesizing barium nitrate is not particularly limited, and examples thereof include a method of causing nitric acid to act on barium carbonate or barium sulfide.
（シリカ）
通常のシリカはその固体表面にシラノール基（Ｓｉ−Ｏ−Ｈ）が存在することから、水との親和性が高い。このようなシリカは「親水性シリカ」と呼ばれている。これに対し、シラン処理、シランカップリング処理などの疎水化処理をシリカの表面に施すことにより、表面を疎水性に改質したものは「疎水性シリカ」と呼ばれている。本発明においては「疎水性シリカ」を用いる。
(silica)
Since ordinary silica has silanol groups (Si—O—H) on its solid surface, it has a high affinity for water. Such silica is called “hydrophilic silica”. On the other hand, the surface of the silica that has been subjected to hydrophobic treatment such as silane treatment or silane coupling treatment to make the surface hydrophobic is called “hydrophobic silica”. In the present invention, “hydrophobic silica” is used.
疎水化処理を施す前の原体シリカに制限はなく、公知の方法によって得られたシリカが使用される。例えば、ヒュームドシリカ、湿式シリカなどが代表的である。 There is no restriction | limiting in the original silica before performing a hydrophobization process, The silica obtained by the well-known method is used. For example, fumed silica, wet silica and the like are typical.
ヒュームドシリカとしては、珪素化合物や金属珪素を酸水素火炎中で燃焼させて得られる気相法シリカが挙げられる。 Examples of fumed silica include vapor phase method silica obtained by burning a silicon compound or metal silicon in an oxyhydrogen flame.
湿式シリカとしては、珪酸ソーダを中和することによって溶液中でシリカを析出させる沈殿法シリカが挙げられる。 Examples of wet silica include precipitated silica that precipitates silica in a solution by neutralizing sodium silicate.
また珪素のアルコキシドを含水有機溶媒中で加水分解させて得られる、ゾル−ゲル法シリカなども用いることができる。 Also, sol-gel silica obtained by hydrolyzing silicon alkoxide in a water-containing organic solvent can be used.
疎水性シリカは、親水性シリカの表面を、ジメチルジクロロシラン、ヘキサメチルジシラザン、オクチルシラン等のシラン、ビニルトリメトキシシラン等のシランカップリング剤、ジメチルポリシロキサン、メチルハイドロジェンポリシロキサン、脂肪酸等の表面処理剤によって処理することにより得られるものが好ましい。但し表面処理剤はこれに限定されるものではない。 Hydrophobic silica, the surface of hydrophilic silica, silane such as dimethyldichlorosilane, hexamethyldisilazane, octylsilane, silane coupling agents such as vinyltrimethoxysilane, dimethylpolysiloxane, methylhydrogenpolysiloxane, fatty acid, etc. What is obtained by processing with the surface treating agent of is preferable. However, the surface treatment agent is not limited to this.
本発明における疎水性シリカは、疎水化度が２０％以上であるのが好ましく、３０％以上であるのがより好ましく、５０％以上であるのがさらに好ましい。また、親水性シリカは、疎水化度がほぼ０％を示すものである。ここで「疎水化度」とは、疎水性シリカを水中に分散させ、有機溶媒（例えばメタノール）を滴下することにより浮遊する疎水性シリカが全量沈んだ時点における有機溶媒−水混合溶液中の有機溶媒の質量分率（質量％）をいう。測定は、例えば、イオン交換水５０ｍｌに疎水性シリカ０．２ｇを加えマグネティックスターラーで攪拌しながらビュレットからメタノールを滴下することにより行うことができる。浮遊する疎水性シリカが徐々に沈降していき、その全量が沈んだ終点におけるメタノール−水混合溶液中のメタノールの質量分率（％）が「疎水化度」である。 The hydrophobic silica in the present invention preferably has a degree of hydrophobicity of 20% or more, more preferably 30% or more, and even more preferably 50% or more. Hydrophilic silica has a hydrophobization degree of almost 0%. Here, the “hydrophobic degree” means that the hydrophobic silica is dispersed in water and the organic solvent (for example, methanol) is added dropwise to the organic solvent in the organic solvent-water mixed solution at the time when the floating hydrophobic silica is completely precipitated. It refers to the mass fraction (% by mass) of the solvent. The measurement can be performed, for example, by adding 0.2 g of hydrophobic silica to 50 ml of ion exchange water and dropping methanol from the burette while stirring with a magnetic stirrer. The floating hydrophobic silica gradually settles, and the mass fraction (%) of methanol in the methanol-water mixed solution at the end point when the total amount of the silica is sinked is the “hydrophobization degree”.
本発明における疎水性シリカは、上記の条件を満たす市販品を使用することができる。疎水性シリカの例としては、ＡＥＲＯＳＩＬ（Ｒ）（エボニックインダストリーズ社製、例えばＡＥＲＯＳＩＬ（Ｒ）Ｒ９７２、Ｒ９７４、Ｒ１０４、Ｒ１０６、Ｒ２０２、Ｒ８０５、Ｒ８１２、Ｒ８１２Ｓ、Ｒ８１６、Ｒ７２００、Ｒ８２００、及びＲ９２００）、ＣＡＢ−Ｏ−ＳＩＬ（Ｒ）（キャボット社製、例えばＣＡＢ−Ｏ−ＳＩＬ（Ｒ）ＴＧ−Ｃ４１３、ＴＧ−３１８０、ＴＧ−７１２０、ＴＧ−８１８Ｆ、ＴＧ−８２０Ｆ、ＴＧ−Ｃ３９０、ＴＧ−Ｃ１２２、ＴＧ−Ｃ１９０、ＴＧ−Ｃ２４３、ＴＳ−３８２、ＴＳ−５３０、ＴＳ−６１０、ＴＳ−６３０、及びＴＳ−７２０）、レオロシール（Ｒ）（株式会社トクヤマ製、例えばレオロシール（Ｒ）ＤＭ−１０、ＤＭ−２０、ＤＭ−３０、ＭＴ−１０及びＭＴ−２０）、ＷＡＣＫＥＲ（Ｒ）（旭化成ワッカーシリコーン株式会社製、ＷＡＣＫＥＲ（Ｒ）ＨＤＫ−Ｈ１５、ＨＤＫ−Ｈ１８、ＨＤＫ−Ｈ２０、及びＨＤＫ−Ｈ３０）、ニップシール（Ｒ）（東ソー・シリカ株式会社製、ニップシール（Ｒ）ＳＳ−１０、ＳＳ−３０Ｓ、ＳＳ−３０Ｐ、ＳＳ−５０、及びＳＳ−５０Ｆ）等が挙げられる。 The hydrophobic silica in this invention can use the commercial item which satisfy | fills said conditions. Examples of hydrophobic silica include AEROSIL (R) (Evonik Industries, for example, AEROSIL (R) R972, R974, R104, R106, R202, R805, R812, R812S, R816, R7200, R8200, and R9200), CAB -O-SIL (R) (manufactured by Cabot, for example, CAB-O-SIL (R) TG-C413, TG-3180, TG-7120, TG-818F, TG-820F, TG-C390, TG-C122, TG -C190, TG-C243, TS-382, TS-530, TS-610, TS-630, and TS-720), Leoro Seal (R) (manufactured by Tokuyama Corporation, for example, Leoro Seal (R) DM-10, DM- 20, DM-30, MT-10 and MT-20), WAC ER (R) (Asahi Kasei Wacker Silicone Co., Ltd., WACKER (R) HDK-H15, HDK-H18, HDK-H20, and HDK-H30), Nip Seal (R) (Tosoh Silica Co., Ltd., Nip Seal (R) SS-10, SS-30S, SS-30P, SS-50, and SS-50F).
上記疎水性シリカは、そのＢＥＴ比表面積が、好ましくは５０〜４００ｍ２／ｇ、より好ましくは７５〜３００ｍ２／ｇである。ＢＥＴ比表面積は、窒素吸着ＢＥＴ１点法により測定した値をいう。測定手順はＪＩＳ Ｚ ８８３０の規定に準ずる。 The hydrophobic silica has a BET specific surface area of preferably 50 to 400 m 2 / g, more preferably 75 to 300 m 2 / g. The BET specific surface area is a value measured by a nitrogen adsorption BET one-point method. The measurement procedure is in accordance with JIS Z 8830.
（粒子状組成物）
本発明の粒子状組成物は、硝酸ストロンチウム及び／又は硝酸バリウムと、疎水性シリカとを含有する。
(Particulate composition)
The particulate composition of the present invention contains strontium nitrate and / or barium nitrate and hydrophobic silica.
本発明の粒子状組成物は、特に限定されないが、硝酸ストロンチウム及び／又は硝酸バリウムと、疎水性シリカとをそれぞれ所要量加えて混合することで粒子状組成物を得ることができる。また、各成分の添加順については特に限定はない。混合するための手段としては特に限定されず、公知の回転固体混合機を適宜選択することができる。上記回転固体混合機としては、例えばリボン型、単軸ローター式、Ｖ型、ナウタ型、二重円錐型、円筒型などが挙げられる。
また、硝酸ストロンチウム及び／又は硝酸バリウムと、疎水性シリカとは均一に混合することが好ましく、硝酸ストロンチウム粒子及び／又は硝酸バリウム粒子の破砕が起こり難いソフトな混合が好ましい。硝酸ストロンチウム粒子及び／又は硝酸バリウム粒子の破砕が進むと、粒子状組成物の固結の発生や、疎水性シリカによる安全性の向上が期待できない場合がある。
Although the particulate composition of the present invention is not particularly limited, the particulate composition can be obtained by adding and mixing required amounts of strontium nitrate and / or barium nitrate and hydrophobic silica. Moreover, there is no limitation in particular about the addition order of each component. The means for mixing is not particularly limited, and a known rotating solid mixer can be appropriately selected. Examples of the rotating solid mixer include a ribbon type, a single-axis rotor type, a V type, a nauta type, a double cone type, and a cylindrical type.
In addition, strontium nitrate and / or barium nitrate and hydrophobic silica are preferably mixed uniformly, and soft mixing is preferred in which crushing of strontium nitrate particles and / or barium nitrate particles hardly occurs. When the strontium nitrate particles and / or barium nitrate particles are crushed, it may be impossible to expect the solidified composition of the particulate composition or the improvement of safety due to the hydrophobic silica.
粒子状組成物中の硝酸ストロンチウム又は硝酸バリウムの量は、特に限定されないが、好ましくは９５〜９９．８質量％、さらに好ましくは９７〜９９．５質量％である。 The amount of strontium nitrate or barium nitrate in the particulate composition is not particularly limited, but is preferably 95 to 99.8% by mass, more preferably 97 to 99.5% by mass.
粒子状組成物中の疎水性シリカの量は、特に限定されないが、好ましくは０．１〜３．０質量％、より好ましくは０．３〜２．０質量％、特に好ましくは０．４〜１．８質量％である。但し、硝酸ストロンチウム、硝酸バリウム、及び疎水性シリカの合計量は１００質量％を超えることはない。上記疎水性シリカの量が３．０質量％を超えると、硝酸ストロンチウム又は硝酸バリウムと均一に混合されず、その結果、分離や容器への付着、粉塵発生等の問題を生じさせるおそれがある。特にガラス原料として使用される場合には、成分が均一に混合されていないとガラス組成に影響を及ぼすおそれがある。また疎水性シリカの量が少なすぎると、疎水性シリカによる安全性の向上が期待できない場合がある。 The amount of hydrophobic silica in the particulate composition is not particularly limited, but is preferably 0.1 to 3.0% by mass, more preferably 0.3 to 2.0% by mass, and particularly preferably 0.4 to 1.8% by mass. However, the total amount of strontium nitrate, barium nitrate, and hydrophobic silica does not exceed 100% by mass. When the amount of the hydrophobic silica exceeds 3.0% by mass, it is not uniformly mixed with strontium nitrate or barium nitrate, and as a result, problems such as separation, adhesion to a container, and generation of dust may occur. In particular, when used as a glass raw material, the glass composition may be affected unless the components are uniformly mixed. In addition, if the amount of hydrophobic silica is too small, the improvement of safety by hydrophobic silica may not be expected.
本発明の粒子状組成物は、日本国の消防法の危険物第一類の燃焼試験及び落球式打撃感度試験で危険物に該当しないものである。ここで、「日本国消防法の危険物第一類の燃焼試験及び落球式打撃感度試験」とは、以下の手順で行う試験である。 The particulate composition of the present invention does not correspond to a dangerous substance in the combustion test and the falling ball hitting sensitivity test of the first dangerous substance of the Fire Service Act of Japan. Here, the “combustion test and the falling ball hitting sensitivity test for dangerous goods No. 1 of the Japanese Fire Service Act” is a test performed in the following procedure.
（燃焼試験）
燃焼試験とは試験試料の酸化力の潜在的な危険性を分類する試験である。作業手順としては、まず試験試料を粉粒状にしたものと木粉とを質量比１：１及び４：１で、両者の合計が３０ｇとなるように混合し、円錐状の堆積をつくる。この堆積の基部に１０００℃に加熱したニクロム線を接触させ、この試験混合試料が燃焼するか確認するとともに、燃焼する場合にはその燃焼時間を測定する。
(Combustion test)
A combustion test is a test that classifies the potential danger of the oxidizing power of a test sample. As a work procedure, first, a powdered test sample and wood flour are mixed at a mass ratio of 1: 1 and 4: 1 so that the total of both becomes 30 g, thereby forming a conical deposit. A nichrome wire heated to 1000 ° C. is brought into contact with the base of the deposit to check whether or not the test mixed sample burns, and when burning, the burning time is measured.
このようにして測定した各混合試料の燃焼時間のうち時間の短い方の燃焼時間を、標準混合試料［標準物質（過塩素酸カリウム又は臭素酸カリウム）と木粉とを質量比１：１で混合したもの］の燃焼時間と比較する。試験混合試料の燃焼時間が、臭素酸カリウムの標準混合試料の燃焼時間以下のものを「ランク１」、臭素酸カリウムの標準混合試料の燃焼時間を超え過塩素酸カリウムの標準混合試料の燃焼時間以下のものを「ランク２」、過塩素酸カリウムの標準混合試料の燃焼時間を超えるものを「ランク３」とする。 The burning time of the shorter burning time of each of the mixed samples measured in this way is determined as the standard mixing sample [standard substance (potassium perchlorate or potassium bromate) and wood flour at a mass ratio of 1: 1. Compared with the combustion time of [mixed]. The burn time of the test mixed sample is less than the burn time of the standard mixed sample of potassium bromate “rank 1”, the burn time of the standard mixed sample of potassium perchlorate exceeds the burn time of the standard mixed sample of potassium bromate “Rank 2” is the following sample, and “Rank 3” is the sample that exceeds the combustion time of the standard mixed sample of potassium perchlorate.
（落球式打撃感度試験）
落球式打撃感度試験とは、試験試料の衝撃に対する敏感性を分類する試験である。作業手順としては、まず標準物質（塩素酸カリウム又は硝酸カリウム）と赤リンとの混合物に対し、それぞれ鋼球をある高さから落下させ、爆・不爆に応じて落下高さを上下させて５０％爆点（５０％の確率で爆発する高さ）を求める。試験試料と赤リンとの混合物に対して、それぞれの５０％爆点から鋼球を落下させる同様の試験を１０又は４０回行い爆・不爆を評価する。本願明細書においては、標準物質として塩素酸カリウムを用いる場合を「塩素酸カリウム法」、硝酸カリウムを用いる場合を「硝酸カリウム法」と呼ぶ。
(Falling ball hitting sensitivity test)
The falling ball hitting sensitivity test is a test for classifying the sensitivity of a test sample to impact. The work procedure is as follows. First, a steel ball is dropped from a certain height against a mixture of standard material (potassium chlorate or potassium nitrate) and red phosphorus, and the drop height is raised or lowered according to the explosion or non-explosion. Find the% explosion point (height to explode with 50% probability). A similar test of dropping a steel ball from each 50% explosion point is performed 10 or 40 times on the mixture of the test sample and red phosphorus, and the explosion / non-explosion is evaluated. In the present specification, the case where potassium chlorate is used as a standard substance is called “potassium chlorate method”, and the case where potassium nitrate is used is called “potassium nitrate method”.
塩素酸カリウム法により５０％爆点から鋼球を落下させる１０回の試験を行い、１０回全てで「爆」となった場合は「ランク１」とする。１０回の試験で「爆」「不爆」の両方が生じた場合はさらに３０回の試験を行い、合計４０回の試験で「爆」が２０回以上の場合は「ランク１」、「爆」が２０回未満の場合は「ランク２」とする。最初の１０回の試験で全て「不爆」となった場合は、さらに硝酸カリウム法での試験を行い評価する。 Ten tests are conducted to drop a steel ball from the 50% explosion point by the potassium chlorate method. If both “explosion” and “non-explosion” occur in 10 tests, perform 30 more tests. If “explosion” exceeds 20 times in a total of 40 tests, “rank 1”, “explosion” "Is less than 20 times," Rank 2 ". If all of the first 10 tests result in “non-explosive”, further test by the potassium nitrate method is performed.
硝酸カリウム法により５０％爆点から鋼球を落下させる１０回の試験で全て「爆」となった場合は「ランク２」、全て「不爆」となった場合は「ランク３」とする。１０回の試験で「爆」「不爆」の両方が生じた場合はさらに３０回の試験を行い、合計４０回の試験で「爆」が２０回以上の場合は「ランク２」、「爆」が２０回未満の場合は「ランク３」とする。 If all of the 10 tests in which the steel ball is dropped from the 50% explosion point by the potassium nitrate method is “explosion”, it is “rank 2”, and if all are “non-explosion”, it is “rank 3”. If both “explosion” and “non-explosion” occur in 10 tests, 30 more tests are performed. If “explosion” exceeds 20 in a total of 40 tests, “rank 2”, “explosion” "Is less than 20 times," Rank 3 ".
（危険性評価）
燃焼試験及び落球式打撃感度試験の結果より、試験試料の危険物としての種別を決定する。燃焼試験又は落球式打撃感度試験で「ランク１」となったものは第１種酸化性固体、燃焼試験及び落球式打撃感度試験でともに「ランク２」となったものは第２種酸化性固体、燃焼試験又は落球式打撃感度試験の一方が「ランク２」で、かつもう一方が「ランク３」となったものは第３種酸化性固体、燃焼試験及び落球式打撃感度試験でともに「ランク３」となったものは非危険物と分類される。
(Danger assessment)
The classification of the test sample as a dangerous substance is determined based on the results of the combustion test and the falling ball hitting sensitivity test. Those that were ranked “Rank 1” in the combustion test or the falling ball impact sensitivity test were the first type oxidizable solid, and those that were both “rank 2” in the combustion test and the falling ball impact sensitivity test were the second type oxidizable solid. One of the combustion test or the falling ball hit sensitivity test is “rank 2” and the other is “rank 3”. Those marked “3” are classified as non-dangerous goods.
危険物としての種別が大きくなるほど消防法で定められる指定数量は大きくなり、同一敷地・同一設備で製造、運搬、貯蔵可能な数量も多くなる。危険物に該当しない場合には製造、運搬、貯蔵における消防法上の規制を受けない。 The larger the classification as dangerous goods, the larger the specified quantity stipulated by the Fire Service Act, and the more quantity that can be manufactured, transported and stored in the same site and equipment. If it does not fall under dangerous goods, it is not subject to regulations under the Fire Service Act in manufacturing, transportation or storage.
本発明の粒子状組成物は、国連勧告・試験マニュアル「Ｒｅｃｏｍｍｅｎｄａｔｉｏｎ ｏｎ ｔｈｅ ＴＲＡＮＳＰＯＲＴ ＯＦ ＤＡＮＧＥＲＯＵＳ ＧＯＯＤＳ −Ｍａｎｕａｌ ｏｆ Ｔｅｓｔｓ ａｎｄ Ｃｒｉｔｅｒｉａ− Ｔｈｉｒｄ ｒｅｖｉｓｅｄ ｅｄｉｔｉｏｎ」に準拠した、国連勧告によるＣＬＡＳＳ ５−Ｄｉｖｉｓｉｏｎ ５．１（酸化性固体）の燃焼試験で危険物に該当しないものであることが好ましい。ここで、「国連勧告によるＣＬＡＳＳ ５−Ｄｉｖｉｓｉｏｎ ５．１（酸化性固体）の燃焼試験」とは、以下の通りである。 The particulate composition of the present invention is a CLASS oxidization test according to the UN recommendation 5 according to the UN recommendation and test manual “Recommendation on the TRANSPORT OF DANGEROUS GOODS-Manual of Tests and Criteria-Third revised edition”. It is preferable that it is not a hazardous material in a solid) combustion test. Here, the “combustion test of CLASS 5-Division 5.1 (oxidizing solid) according to the UN recommendation” is as follows.
（燃焼試験）
燃焼試験とは試験試料の酸化力の潜在的な危険性を分類する試験である。作業手順としては、試験試料を粉粒状にしたものとセルロースとを重量比１：１及び４：１で、両者の合計が３０ｇとなるように混合し、円錐状の堆積をつくる。この堆積と断熱板の間に挟みこんだ点火装置で、完全に着火するか、あるいは全く着火しないことが明らかになるまで最大３分間印加させる。各試験混合試料が燃焼するか確認するとともに、燃焼する場合には各試験混合試料の平均燃焼時間を、標準物質（臭素酸カリウム）とセルロースとを重量比３：２、２：３、３：７で混合した標準混合試料の燃焼時間と比較する。
(Combustion test)
A combustion test is a test that classifies the potential danger of the oxidizing power of a test sample. As a work procedure, a test sample in powder form and cellulose are mixed at a weight ratio of 1: 1 and 4: 1 so that the total of both is 30 g, thereby forming a conical deposit. With an igniter sandwiched between the deposit and the heat insulating plate, it is applied for a maximum of 3 minutes until it becomes clear that it is completely ignited or not ignited at all. It is confirmed whether each test mixed sample burns, and when burning, the average burning time of each test mixed sample is set to a weight ratio of standard material (potassium bromate) to cellulose: 3: 2, 2: 3, 3: Compare with the burning time of the standard mixed sample mixed in 7.
（危険性評価）
各試験混合試料の平均燃焼時間が、臭素酸カリウムとセルロースとの混合重量比３：２の標準混合試料の燃焼時間以下のものは「容器等級１」、混合重量比３：２の標準混合試料の燃焼時間を超え、混合重量比２：３の標準混合試料の燃焼時間以下のものは「容器等級２」、混合重量比２：３の標準混合試料の燃焼時間を超え、混合重量比３：７の標準混合試料の燃焼時間以下のものは「容器等級３」と分類される。臭素酸カリウムとセルロースとの混合重量比３：７の標準混合試料の燃焼時間を超えるものはＣＬＡＳＳ ５−Ｄｉｖｉｓｉｏｎ ５．１（酸化性固体）に該当しない。
(Danger assessment)
The average burning time of each test mixed sample is less than the burning time of the standard mixed sample with a mixing weight ratio of 3: 3 of potassium bromate and cellulose, and the standard mixed sample with a mixing weight ratio of 3: 2 The combustion time of the standard mixed sample with a mixing weight ratio of 2: 3 is less than the burning time of the standard mixed sample with a mixing weight ratio of 2: 3, and the burning time of the standard mixed sample with a mixing weight ratio of 2: 3 is exceeded and the mixing weight ratio of 3: Those with a burning time of 7 standard mixed samples or less are classified as “container grade 3”. What exceeds the burning time of a standard mixed sample having a mixing weight ratio of 3: 7 of potassium bromate and cellulose does not correspond to CLASS 5-Division 5.1 (oxidizing solid).
（ガラス）
本発明は上記粒子状組成物を原料として含有するガラスにも関する。ガラスの製造において、その調合原料の選定は重要であり、硝酸ストロンチウム及び／又は硝酸バリウムを用いる場合は原料の溶解性が良く、清澄性の点でも優れている。本発明のガラスを製造する方法としては、特に限定されないが、公知の方法（例えば溶融法）を用いる事ができる。すなわち、本発明のガラスが酸化物基準で表わされた所定の組成となるように珪砂、アルミナ、ホウ酸、及び本願発明の硝酸ストロンチウム及び／又は硝酸バリウム、並びに他の必要な成分を含有するガラス原料を、石英または白金等からなる坩堝へ充填する。その後、電気炉、ガス炉等の溶融炉で加熱溶融する。溶融後、必要に応じ清澄、撹拌を行いガラスを均質化させ、その後成形型に溶融ガラスを流しこみ急冷することによって成形、徐冷炉において徐冷する。
(Glass)
The present invention also relates to a glass containing the above particulate composition as a raw material. In the production of glass, selection of the raw material for preparation is important, and when strontium nitrate and / or barium nitrate is used, the raw material has good solubility and is excellent in terms of clarity. Although it does not specifically limit as a method to manufacture the glass of this invention, A well-known method (for example, melting method) can be used. That is, the glass of the present invention contains silica sand, alumina, boric acid, strontium nitrate and / or barium nitrate of the present invention, and other necessary components so as to have a predetermined composition expressed on an oxide basis. A glass material is filled into a crucible made of quartz or platinum. Thereafter, it is heated and melted in a melting furnace such as an electric furnace or a gas furnace. After melting, clarification and stirring are performed as necessary to homogenize the glass, and then the molten glass is poured into a mold and rapidly cooled to form and slowly cool in a slow cooling furnace.
徐冷炉から取り出したガラスは必要に応じて切断、研削、研磨を行うことで、各種基板材、構造部材、透過光学系材料を得ることができる。 The glass taken out from the slow cooling furnace can be cut, ground, and polished as necessary to obtain various substrate materials, structural members, and transmission optical system materials.
（保存方法）
本発明は、硝酸ストロンチウム及び／又は硝酸バリウムの保存方法にも関する。
硝酸ストロンチウムや硝酸バリウムは、可燃物を酸化して、激しい燃焼や爆発を起こすおそれがある。
硝酸ストロンチウムや硝酸バリウムを保存する際に、疎水性シリカを混合することにより、上記の激しい燃焼や爆発の危険性を低減することができ、安全性の高い硝酸ストロンチウム及び／又は硝酸バリウムとして取り扱うことができる。
本発明の保存方法により保存された硝酸ストロンチウムや硝酸バリウムは、ガラス原料として好適に使用することができる。
(Preservation method)
The present invention also relates to a method for preserving strontium nitrate and / or barium nitrate.
Strontium nitrate and barium nitrate can oxidize combustibles and cause severe combustion and explosion.
When storing strontium nitrate and barium nitrate, mixing with hydrophobic silica can reduce the risk of the above intense combustion and explosion, and handle it as highly safe strontium nitrate and / or barium nitrate Can do.
Strontium nitrate and barium nitrate stored by the storage method of the present invention can be suitably used as a glass raw material.
以下に本発明を実施例に基づいてさらに詳細に説明するが、本発明はこれらの実施例のみに限定されるものではない。なお下記実施例・比較例において、特に断りの無い限り、「％」は「質量％」を意味する。 The present invention will be described below in more detail based on examples, but the present invention is not limited only to these examples. In Examples and Comparative Examples below, “%” means “% by mass” unless otherwise specified.
（燃焼試験）
日本国の消防法又は国連勧告・試験マニュアルに準拠した上述の方法に従い、燃焼試験を行った。
(Combustion test)
A combustion test was conducted according to the above-mentioned method in accordance with the Japanese Fire Service Act or the UN Recommendation / Test Manual.
（落球式打撃感度試験）
日本国の消防法に準拠した上述の方法に従い、落球式打撃感度試験を行った。
(Falling ball hitting sensitivity test)
In accordance with the method described above in accordance with the Japanese Fire Service Law, a falling ball hitting sensitivity test was conducted.
（硝酸ストロンチウムを含有する粒子の評価）
（実施例１）
硝酸ストロンチウム５００ｋｇに対し、疎水性シリカとしての添加量が粒子総質量の０．５質量％となるようＡＥＲＯＳＩＬ Ｒ９７２（表面処理疎水性シリカ、疎水化度３５％、比表面積１１０ｍ２／ｇ、エボニックインダストリーズ社製）を２．５１ｋｇ加え、リボンブレンダーで混合することにより粒子状組成物１を作製した。得られた粒子状組成物１について、危険物第一類の燃焼試験と落球式打撃感度試験を行った。消防法上の危険物としての確認試験の結果、および国連勧告の危険物としての確認試験の結果を表１に示す。
(Evaluation of particles containing strontium nitrate)
Example 1
AEROSIL R972 (surface-treated hydrophobic silica, hydrophobization degree 35%, specific surface area 110 m 2 / g, Evonik Industries, so that the amount added as hydrophobic silica is 0.5% by mass with respect to 500 kg of strontium nitrate. A particulate composition 1 was prepared by adding 2.51 kg of the same) and mixing with a ribbon blender. About the obtained particulate composition 1, the burning test of the dangerous goods 1st class and the falling ball type impact sensitivity test were done. Table 1 shows the results of confirmation tests as dangerous goods under the Fire Service Act and the results of confirmation tests as dangerous goods as recommended by the United Nations.
（実施例２）
ＡＥＲＯＳＩＬ Ｒ９７２の添加量を粒子総質量の０．７５質量％に変更した以外は実施例１と同様にして、粒子状組成物２を作製した。得られた粒子状組成物２について、危険物第一類の燃焼試験と落球式打撃感度試験を行った。消防法上の危険物としての確認試験の結果を表１に示す。
(Example 2)
A particulate composition 2 was produced in the same manner as in Example 1 except that the amount of AEROSIL R972 added was changed to 0.75% by mass of the total mass of the particles. The obtained particulate composition 2 was subjected to a dangerous substance first class combustion test and a falling ball hitting sensitivity test. Table 1 shows the results of confirmation tests as dangerous goods under the Fire Service Law.
（実施例３）
ＡＥＲＯＳＩＬ Ｒ９７２の添加量を粒子総質量の１．０質量％に変更した以外は実施例１と同様にして、粒子状組成物３を作製した。得られた粒子状組成物３について、危険物第一類の燃焼試験と落球式打撃感度試験を行った。消防法上の危険物としての確認試験の結果を表１に示す。
Example 3
A particulate composition 3 was produced in the same manner as in Example 1 except that the amount of AEROSIL R972 added was changed to 1.0% by mass of the total particle mass. The obtained particulate composition 3 was subjected to a first dangerous substance combustion test and a falling ball hitting sensitivity test. Table 1 shows the results of confirmation tests as dangerous goods under the Fire Service Law.
（実施例４）
疎水性シリカの種類をニップシールＳＳ−３０Ｐ（表面処理疎水性シリカ、疎水化度６０％、比表面積１２５ｍ２／ｇ、東ソー・シリカ株式会社製）に変更した以外は実施例１と同様にして、粒子状組成物４を作製した。得られた粒子状組成物４について、危険物第一類の燃焼試験を行った。その結果を表１に示す。
Example 4
Except for changing the type of hydrophobic silica to nip seal SS-30P (surface-treated hydrophobic silica, hydrophobization degree 60%, specific surface area 125 m 2 / g, manufactured by Tosoh Silica Co., Ltd.), the same as in Example 1, A particulate composition 4 was produced. The obtained particulate composition 4 was subjected to a first hazardous material combustion test. The results are shown in Table 1.
（実施例５）
疎水性シリカの種類をニップシールＳＳ−５０Ｆ（表面処理疎水性シリカ、疎水化度６０％、比表面積８２ｍ２／ｇ、東ソー・シリカ株式会社製）に変更した以外は実施例１と同様にして、粒子状組成物５を作製した。得られた粒子状組成物５について、危険物第一類の燃焼試験を行った。その結果を表１に示す。
(Example 5)
Except for changing the type of hydrophobic silica to nip seal SS-50F (surface-treated hydrophobic silica, hydrophobization degree 60%, specific surface area 82 m 2 / g, manufactured by Tosoh Silica Co., Ltd.), the same as in Example 1, A particulate composition 5 was produced. The obtained particulate composition 5 was subjected to a first hazardous material combustion test. The results are shown in Table 1.
（実施例６）
疎水性シリカの種類をニップシールＳＳ−３０Ｐに、その添加量を粒子総質量の１．０質量％に変更した以外は実施例１と同様にして、粒子状組成物６を作製した。得られた粒子状組成物６について、危険物第一類の燃焼試験を行った。その結果を表１に示す。
(Example 6)
A particulate composition 6 was prepared in the same manner as in Example 1 except that the type of hydrophobic silica was changed to Nipseal SS-30P and the addition amount was changed to 1.0% by mass of the total particle mass. The obtained particulate composition 6 was subjected to a combustion test of the first hazardous material. The results are shown in Table 1.
（実施例７）
疎水性シリカの種類をニップシールＳＳ−５０Ｆに、その添加量を粒子総質量の１．０質量％に変更した以外は実施例１と同様にして、粒子状組成物７を作製した。得られた粒子状組成物７について、危険物第一類の燃焼試験を行った。その結果を表１に示す。
(Example 7)
A particulate composition 7 was produced in the same manner as in Example 1 except that the type of hydrophobic silica was changed to Nipseal SS-50F and the addition amount was changed to 1.0 mass% of the total particle mass. The obtained particulate composition 7 was subjected to a first hazardous material combustion test. The results are shown in Table 1.
（比較例１）
シリカを用いない以外は実施例１と同様にして、比較粒子状組成物１を作製した。得られた比較粒子状組成物１について、危険物第一類の燃焼試験と落球式打撃感度試験を行った。消防法上の危険物としての確認試験の結果を表２に示す。
(Comparative Example 1)
Comparative particulate composition 1 was produced in the same manner as in Example 1 except that silica was not used. The obtained comparative particulate composition 1 was subjected to a first dangerous substance combustion test and a falling ball hitting sensitivity test. Table 2 shows the results of confirmation tests as dangerous goods under the Fire Service Law.
（比較例２）
シリカの種類をＡＥＲＯＳＩＬ ２００（親水性シリカ、疎水化度０％、比表面積２００ｍ２／ｇ、エボニックインダストリーズ社製）に変更した以外は実施例１と同様にして、比較粒子状組成物２を作製した。得られた比較粒子状組成物２について、危険物第一類の燃焼試験と落球式打撃感度試験を行った。消防法上の危険物としての確認試験の結果を表２に示す。
(Comparative Example 2)
Comparative particulate composition 2 was prepared in the same manner as in Example 1 except that the type of silica was changed to AEROSIL 200 (hydrophilic silica, hydrophobization degree 0%, specific surface area 200 m 2 / g, manufactured by Evonik Industries). did. The obtained comparative particulate composition 2 was subjected to a dangerous substance first class combustion test and a falling ball hitting sensitivity test. Table 2 shows the results of confirmation tests as dangerous goods under the Fire Service Law.
（比較例３）
シリカの種類をニップシールＬＰ（親水性シリカ、疎水化度０％、比表面積２１０ｍ２／ｇ、東ソー・シリカ株式会社製）に変更した以外は実施例１と同様にして、比較粒子状組成物３を作製した。得られた比較粒子状組成物３について、危険物第一類の燃焼試験と落球式打撃感度試験を行った。消防法上の危険物としての確認試験の結果を表２に示す。
(Comparative Example 3)
Comparative particulate composition 3 in the same manner as in Example 1 except that the type of silica was changed to nip seal LP (hydrophilic silica, hydrophobization degree 0%, specific surface area 210 m 2 / g, manufactured by Tosoh Silica Co., Ltd.) Was made. The obtained comparative particulate composition 3 was subjected to a first dangerous substance combustion test and a falling ball hitting sensitivity test. Table 2 shows the results of confirmation tests as dangerous goods under the Fire Service Law.
（比較例４）
シリカの種類をニップシールＬＰに、その添加量を粒子総質量の３．０質量％に変更した以外は実施例１と同様にして、比較粒子状組成物４を作製した。得られた比較粒子状組成物４について、危険物第一類の燃焼試験と落球式打撃感度試験を行った。消防法上の危険物としての確認試験の結果を表２に示す。
(Comparative Example 4)
Comparative particulate composition 4 was prepared in the same manner as in Example 1 except that the type of silica was changed to nip seal LP and the addition amount was changed to 3.0% by mass of the total particle mass. The obtained comparative particulate composition 4 was subjected to a first dangerous substance combustion test and a falling ball hitting sensitivity test. Table 2 shows the results of confirmation tests as dangerous goods under the Fire Service Law.
（比較例５）
シリカの種類をＭＫ Ｓｉｌｉｃａ ＦＩＮＥＳ（硝子原料高純度シリカ、疎水化度０％、平均粒径４０μｍ、共立マテリアル株式会社製）に、その添加量を粒子総質量の３０質量％に変更した以外は実施例１と同様にして、比較粒子状組成物５を作製した。得られた比較粒子状組成物５について、危険物第一類の燃焼試験と落球式打撃感度試験を行った。消防法上の危険物としての確認試験の結果を表２に示す。
(Comparative Example 5)
Implemented except that the type of silica was changed to MK Silica FINES (glass raw material high-purity silica, hydrophobization degree 0%, average particle size 40 μm, manufactured by Kyoritsu Materials Co., Ltd.), and the addition amount was changed to 30% by mass of the total particle mass Comparative particulate composition 5 was produced in the same manner as in Example 1. The obtained comparative particulate composition 5 was subjected to a dangerous substance first class combustion test and a falling ball hitting sensitivity test. Table 2 shows the results of confirmation tests as dangerous goods under the Fire Service Law.
（比較例６）
シリカの種類をＭＫ Ｓｉｌｉｃａ ２０／２５０（硝子原料高純度シリカ、疎水化度０％、平均粒径１２０μｍ、共立マテリアル株式会社製）に、その添加量を粒子総質量の３０質量％に変更した以外は実施例１と同様にして比較粒子状組成物６を作製した。得られた比較粒子状組成物６について、危険物第一類の燃焼試験と落球式打撃感度試験を行った。消防法上の危険物としての確認試験の結果を表２に示す。
(Comparative Example 6)
The type of silica was changed to MK Silica 20/250 (glass raw material high purity silica, hydrophobization degree 0%, average particle size 120 μm, manufactured by Kyoritsu Material Co., Ltd.), and the addition amount was changed to 30% by mass of the total particle mass Produced a comparative particulate composition 6 in the same manner as in Example 1. The obtained comparative particulate composition 6 was subjected to a first dangerous substance combustion test and a falling ball hitting sensitivity test. Table 2 shows the results of confirmation tests as dangerous goods under the Fire Service Law.
表１の結果より、硝酸ストロンチウムと疎水性シリカとを含有する本発明の粒子状組成物（実施例１〜７）は、消防法上の第一類酸化性固体の確認試験における燃焼試験においてはいずれもランク３の条件を満たし、酸化力の潜在的な危険性が低いことが分かった。また、実施例１においては、国連勧告のＣＬＡＳＳ ５−Ｄｉｖｉｓｉｏｎ ５．１（酸化性固体）の確認試験においても同様に酸化力の潜在的な危険性が低いことが分かった。さらに消防法上の第一類酸化性固体の確認試験に基づく落球式打撃感度試験によっても、衝撃に対する敏感性が低いことが分かった。一方、表２の結果より、疎水性シリカを含有しない粒子組成物（比較例１〜６）では危険性を排除する効果は認められなかった。このように、上記結果から、本発明の粒子状組成物は、危険性が排除され、より安全性が高い点で優れていることが明らかとなった。 From the results of Table 1, the particulate compositions of the present invention (Examples 1 to 7) containing strontium nitrate and hydrophobic silica were used in the combustion test in the confirmation test of the first kind of oxidizable solid under the Fire Service Act. All met the requirements of rank 3 and were found to have a low potential risk of oxidizing power. In Example 1, it was also found that the potential risk of oxidizing power was low in the confirmation test of CLASS 5-Division 5.1 (oxidizing solid) recommended by the United Nations. Furthermore, the ball-ball hitting sensitivity test based on the confirmation test for the first kind of oxidizable solids under the Fire Service Law revealed that the sensitivity to impact was low. On the other hand, from the results shown in Table 2, the particle composition containing no hydrophobic silica (Comparative Examples 1 to 6) did not show the effect of eliminating the danger. Thus, from the above results, it became clear that the particulate composition of the present invention is superior in terms of eliminating safety and higher safety.
（硝酸バリウムを含有する粒子の評価）
（実施例８）
硝酸バリウム５００ｋｇに対し、疎水性シリカとしての添加量が粒子総質量の０．７５質量％となるようＡＥＲＯＳＩＬ Ｒ９７２を３．７８ｋｇ加え、リボンブレンダーで混合することにより粒子状組成物８を作製した。得られた粒子状組成物８について、危険物第一類の落球式打撃感度試験を行った。その結果を表３に示す。
(Evaluation of particles containing barium nitrate)
(Example 8)
A particulate composition 8 was prepared by adding 3.78 kg of AEROSIL R972 to 500 kg of barium nitrate so that the amount added as hydrophobic silica was 0.75 mass% of the total particle mass, and mixing with a ribbon blender. The obtained particulate composition 8 was subjected to a falling ball-type impact sensitivity test of the first dangerous material. The results are shown in Table 3.
（実施例９）
ＡＥＲＯＳＩＬ Ｒ９７２の添加量を粒子総質量の１．０質量％に変更した以外は実施例８と同様にして、粒子状組成物９を作製した。得られた粒子状組成物９について、危険物第一類の燃焼試験を行った。その結果を表３に示す。
Example 9
A particulate composition 9 was produced in the same manner as in Example 8, except that the amount of AEROSIL R972 added was changed to 1.0% by mass of the total particle mass. The obtained particulate composition 9 was subjected to a first hazardous material combustion test. The results are shown in Table 3.
（実施例１０）
ＡＥＲＯＳＩＬ Ｒ９７２の添加量を粒子総質量の１．５質量％に変更した以外は実施例８と同様にして、粒子状組成物１０を作製した。得られた粒子状組成物１０について、危険物第一類の燃焼試験と落球式打撃感度試験を行った。消防法上の危険物としての確認試験の結果を表３に示す。
(Example 10)
A particulate composition 10 was produced in the same manner as in Example 8, except that the amount of AEROSIL R972 added was changed to 1.5% by mass of the total particle mass. The obtained particulate composition 10 was subjected to a first dangerous substance combustion test and a falling ball hitting sensitivity test. Table 3 shows the results of confirmation tests as dangerous goods under the Fire Service Law.
（比較例７）
シリカを用いない以外は実施例８と同様にして、比較粒子状組成物７を作製した。得られた比較粒子状組成物７について、危険物第一類の燃焼試験と落球式打撃感度試験を行った。消防法上の危険物としての確認試験の結果を表３に示す。
(Comparative Example 7)
Comparative particulate composition 7 was produced in the same manner as in Example 8 except that silica was not used. The obtained comparative particulate composition 7 was subjected to a first dangerous substance combustion test and a falling ball hitting sensitivity test. Table 3 shows the results of confirmation tests as dangerous goods under the Fire Service Law.
（比較例８）
シリカの種類をＡＥＲＯＳＩＬ ２００に、その添加量を粒子総質量の３０質量％に変更した以外は実施例８と同様にして、比較粒子状組成物８を作製した。得られた粒子状組成物８について、危険物第一類の燃焼試験と落球式打撃感度試験を行った。消防法上の危険物としての確認試験の結果を表３に示す。
(Comparative Example 8)
Comparative particulate composition 8 was produced in the same manner as in Example 8 except that the type of silica was changed to AEROSIL 200 and the addition amount was changed to 30% by mass of the total particle mass. The obtained particulate composition 8 was subjected to a first dangerous substance combustion test and a falling ball hitting sensitivity test. Table 3 shows the results of confirmation tests as dangerous goods under the Fire Service Law.
硝酸バリウムは通常、危険物第一類の第２種酸化性固体として分類される。表３の結果より、硝酸バリウムと疎水性シリカとを含有する本発明の粒子状組成物（実施例８〜１０）は、消防法上の第一類酸化性固体としての酸化力の潜在的な危険性と、衝撃に対する敏感性を抑制し、危険性を低減した、より安全性の高い材料へ改質された点で優れている。疎水性シリカを含有しない粒子組成物（比較例７・８）では危険性を低減する効果は認められなかった。 Barium nitrate is usually classified as a second class oxidizable solid of the first class of dangerous goods. From the results of Table 3, the particulate compositions of the present invention (Examples 8 to 10) containing barium nitrate and hydrophobic silica have potential for oxidizing power as the first kind of oxidizable solid under the Fire Service Act. It is superior in that it has been improved to a safer material that has reduced danger and reduced sensitivity to shock and sensitivity. In the particle composition containing no hydrophobic silica (Comparative Examples 7 and 8), the effect of reducing the risk was not recognized.
硝酸ストロンチウム及び／又は硝酸バリウムと、疎水性シリカとを含有する、危険性を低減した粒子状組成物を原料として含有するガラスは、消防法上の規制を受けない製造工程で生産することが可能である。また硝酸ストロンチウム及び／又は硝酸バリウムと、疎水性シリカとを含有する粒子状組成物を原料として含有するガラスは、従来の硝酸ストロンチウム及び／又は硝酸バリウムを原料として含有するガラスと比較して、品質的に差異のないガラスを得ることができる。 Glass containing strontium nitrate and / or barium nitrate and hydrophobic silica as a raw material and a particulate composition with reduced risk can be produced in a manufacturing process that is not subject to fire regulations. It is. Further, the glass containing a particulate composition containing strontium nitrate and / or barium nitrate and hydrophobic silica as a raw material has a higher quality than a glass containing conventional strontium nitrate and / or barium nitrate as a raw material. Glass with no difference can be obtained.
（ガラスの作製例）
表４の調合原料（組成の数値は重量部）を良く混合し、白金坩堝に入れ白金の蓋を被せる。坩堝を電気炉に入れ、１５００〜１６８０℃程度に加熱、溶融、撹拌し、均質化、清澄を行った後、鋳型に流し込み、ガラスが固化後、ガラスの徐冷点近くに加熱しておいた電気炉に移し、室温まで徐冷することによりガラス組成物を作製することができる。
(Example of glass production)
The prepared raw materials in Table 4 (composition values are parts by weight) are mixed well, placed in a platinum crucible and covered with a platinum lid. The crucible was put in an electric furnace, heated to about 1500 to 1680 ° C., melted, stirred, homogenized and clarified, poured into a mold, and after the glass solidified, it was heated near the annealing point of the glass. The glass composition can be produced by transferring to an electric furnace and gradually cooling to room temperature.
Claims (7)
疎水性シリカと
を含有し、
日本国消防法の危険物第一類の燃焼試験及び落球式打撃感度試験で危険物に該当しない
粒子状組成物。 Strontium nitrate and / or barium nitrate;
Containing hydrophobic silica,
Particulate composition that does not fall under the category of dangerous goods in the fire test of the first class of dangerous goods under the Japanese Fire Service Act and the falling ball hitting sensitivity test.
請求項１又は２記載の粒子状組成物。 The particulate composition according to claim 1 or 2, comprising 95.0 to 99.8 mass% of the strontium nitrate or barium nitrate.
請求項１〜３のいずれか一項記載の粒子状組成物。 The particulate composition according to any one of claims 1 to 3, wherein the particulate composition is used as a glass raw material.
請求項１〜４のいずれか一項記載の粒子状組成物。 0.1 to 3.0% by mass of the hydrophobic silica (however, the total mass of the particulate composition is 100% by mass)
The particulate composition according to any one of claims 1 to 4.
請求項１〜５のいずれか一項記載の粒子状組成物。 The particulate composition according to any one of claims 1 to 5, wherein the hydrophobic silica has a BET specific surface area of 50 to 400 m 2 / g.
The manufacturing method of the particulate composition as described in any one of Claims 1-6 including the process of mixing strontium nitrate and / or barium nitrate, and hydrophobic silica.
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