JPWO2011070983A1 - Tablet manufacturing method - Google Patents
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- JPWO2011070983A1 JPWO2011070983A1 JP2011545196A JP2011545196A JPWO2011070983A1 JP WO2011070983 A1 JPWO2011070983 A1 JP WO2011070983A1 JP 2011545196 A JP2011545196 A JP 2011545196A JP 2011545196 A JP2011545196 A JP 2011545196A JP WO2011070983 A1 JPWO2011070983 A1 JP WO2011070983A1
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- 238000004519 manufacturing process Methods 0.000 title claims abstract description 26
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 39
- 239000000126 substance Substances 0.000 claims abstract description 37
- 239000007787 solid Substances 0.000 claims abstract description 35
- 239000013078 crystal Substances 0.000 claims abstract description 18
- 239000000203 mixture Substances 0.000 claims abstract description 16
- ZKQDCIXGCQPQNV-UHFFFAOYSA-N Calcium hypochlorite Chemical group [Ca+2].Cl[O-].Cl[O-] ZKQDCIXGCQPQNV-UHFFFAOYSA-N 0.000 claims description 17
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 claims description 6
- 238000002425 crystallisation Methods 0.000 claims description 6
- 230000008025 crystallization Effects 0.000 claims description 6
- 229920006395 saturated elastomer Polymers 0.000 claims description 3
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 7
- 239000000460 chlorine Substances 0.000 description 7
- 229910052801 chlorine Inorganic materials 0.000 description 7
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 6
- 239000003795 chemical substances by application Substances 0.000 description 5
- 239000000645 desinfectant Substances 0.000 description 5
- DIZPMCHEQGEION-UHFFFAOYSA-H aluminium sulfate (anhydrous) Chemical compound [Al+3].[Al+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O DIZPMCHEQGEION-UHFFFAOYSA-H 0.000 description 4
- 238000002156 mixing Methods 0.000 description 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 229910021538 borax Inorganic materials 0.000 description 3
- 239000011575 calcium Substances 0.000 description 3
- 150000001875 compounds Chemical class 0.000 description 3
- 230000007774 longterm Effects 0.000 description 3
- 238000000465 moulding Methods 0.000 description 3
- 239000004328 sodium tetraborate Substances 0.000 description 3
- 235000010339 sodium tetraborate Nutrition 0.000 description 3
- 230000002269 spontaneous effect Effects 0.000 description 3
- YRIZYWQGELRKNT-UHFFFAOYSA-N 1,3,5-trichloro-1,3,5-triazinane-2,4,6-trione Chemical compound ClN1C(=O)N(Cl)C(=O)N(Cl)C1=O YRIZYWQGELRKNT-UHFFFAOYSA-N 0.000 description 2
- CSNNHWWHGAXBCP-UHFFFAOYSA-L Magnesium sulfate Chemical compound [Mg+2].[O-][S+2]([O-])([O-])[O-] CSNNHWWHGAXBCP-UHFFFAOYSA-L 0.000 description 2
- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical compound [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 description 2
- 229940037003 alum Drugs 0.000 description 2
- 150000001639 boron compounds Chemical class 0.000 description 2
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 description 2
- 239000000920 calcium hydroxide Substances 0.000 description 2
- 229910001861 calcium hydroxide Inorganic materials 0.000 description 2
- 238000002485 combustion reaction Methods 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- UQGFMSUEHSUPRD-UHFFFAOYSA-N disodium;3,7-dioxido-2,4,6,8,9-pentaoxa-1,3,5,7-tetraborabicyclo[3.3.1]nonane Chemical compound [Na+].[Na+].O1B([O-])OB2OB([O-])OB1O2 UQGFMSUEHSUPRD-UHFFFAOYSA-N 0.000 description 2
- 239000008187 granular material Substances 0.000 description 2
- QWPPOHNGKGFGJK-UHFFFAOYSA-N hypochlorous acid Chemical compound ClO QWPPOHNGKGFGJK-UHFFFAOYSA-N 0.000 description 2
- 230000001590 oxidative effect Effects 0.000 description 2
- 244000052769 pathogen Species 0.000 description 2
- 230000001717 pathogenic effect Effects 0.000 description 2
- 238000004659 sterilization and disinfection Methods 0.000 description 2
- 230000008961 swelling Effects 0.000 description 2
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 241000224489 Amoeba Species 0.000 description 1
- 241000193738 Bacillus anthracis Species 0.000 description 1
- 241000894006 Bacteria Species 0.000 description 1
- 241000588724 Escherichia coli Species 0.000 description 1
- 241000193096 Human adenovirus B3 Species 0.000 description 1
- 241000588652 Neisseria gonorrhoeae Species 0.000 description 1
- 206010037660 Pyrexia Diseases 0.000 description 1
- 241000293871 Salmonella enterica subsp. enterica serovar Typhi Species 0.000 description 1
- 241000607768 Shigella Species 0.000 description 1
- 239000004115 Sodium Silicate Substances 0.000 description 1
- 229910052783 alkali metal Inorganic materials 0.000 description 1
- 229910052910 alkali metal silicate Inorganic materials 0.000 description 1
- 150000001340 alkali metals Chemical class 0.000 description 1
- 229910052784 alkaline earth metal Inorganic materials 0.000 description 1
- 150000001342 alkaline earth metals Chemical class 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 229940065181 bacillus anthracis Drugs 0.000 description 1
- 230000003115 biocidal effect 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
- 229910052791 calcium Inorganic materials 0.000 description 1
- 239000012320 chlorinating reagent Substances 0.000 description 1
- 230000006835 compression Effects 0.000 description 1
- 238000007906 compression Methods 0.000 description 1
- 150000007973 cyanuric acids Chemical class 0.000 description 1
- CEJLBZWIKQJOAT-UHFFFAOYSA-N dichloroisocyanuric acid Chemical compound ClN1C(=O)NC(=O)N(Cl)C1=O CEJLBZWIKQJOAT-UHFFFAOYSA-N 0.000 description 1
- 239000010840 domestic wastewater Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 206010014599 encephalitis Diseases 0.000 description 1
- 238000007496 glass forming Methods 0.000 description 1
- 230000020169 heat generation Effects 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000010842 industrial wastewater Substances 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 229910052943 magnesium sulfate Inorganic materials 0.000 description 1
- WRUGWIBCXHJTDG-UHFFFAOYSA-L magnesium sulfate heptahydrate Chemical compound O.O.O.O.O.O.O.[Mg+2].[O-]S([O-])(=O)=O WRUGWIBCXHJTDG-UHFFFAOYSA-L 0.000 description 1
- 229940061634 magnesium sulfate heptahydrate Drugs 0.000 description 1
- 235000019341 magnesium sulphate Nutrition 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 238000000034 method Methods 0.000 description 1
- 244000005700 microbiome Species 0.000 description 1
- 238000013508 migration Methods 0.000 description 1
- 230000005012 migration Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000007800 oxidant agent Substances 0.000 description 1
- IFIDXBCRSWOUSB-UHFFFAOYSA-N potassium;1,3-dichloro-1,3,5-triazinane-2,4,6-trione Chemical compound [K+].ClN1C(=O)NC(=O)N(Cl)C1=O IFIDXBCRSWOUSB-UHFFFAOYSA-N 0.000 description 1
- 239000012925 reference material Substances 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 150000004760 silicates Chemical class 0.000 description 1
- 235000017557 sodium bicarbonate Nutrition 0.000 description 1
- 229910000030 sodium bicarbonate Inorganic materials 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
- 230000001954 sterilising effect Effects 0.000 description 1
- 229950009390 symclosene Drugs 0.000 description 1
Classifications
-
- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N25/00—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests
- A01N25/34—Shaped forms, e.g. sheets, not provided for in any other sub-group of this main group
-
- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N59/00—Biocides, pest repellants or attractants, or plant growth regulators containing elements or inorganic compounds
- A01N59/06—Aluminium; Calcium; Magnesium; Compounds thereof
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/50—Treatment of water, waste water, or sewage by addition or application of a germicide or by oligodynamic treatment
Landscapes
- Life Sciences & Earth Sciences (AREA)
- General Health & Medical Sciences (AREA)
- Health & Medical Sciences (AREA)
- Dentistry (AREA)
- Pest Control & Pesticides (AREA)
- Plant Pathology (AREA)
- Engineering & Computer Science (AREA)
- Agronomy & Crop Science (AREA)
- Wood Science & Technology (AREA)
- Zoology (AREA)
- Environmental Sciences (AREA)
- Toxicology (AREA)
- Chemical & Material Sciences (AREA)
- Inorganic Chemistry (AREA)
- Glanulating (AREA)
- Agricultural Chemicals And Associated Chemicals (AREA)
Abstract
本発明は、示差走査熱量計で測定される吸熱量が相互に異なり、且つ双方とも結晶水を保持することができる２種以上の固体物質を少なくとも含有する混合物を用意し、該混合物を打錠圧２５０ｋｇｆ／ｃｍ2〜１１５０ｋｇｆ／ｃｍ2で打錠することを含む錠剤の製造方法に関する。The present invention provides a mixture containing at least two or more kinds of solid substances having different endothermic amounts measured by a differential scanning calorimeter and both capable of retaining crystal water, and compressing the mixture The present invention relates to a tablet production method including tableting at a pressure of 250 kgf / cm 2 to 1150 kgf / cm 2.
Description
本発明は、錠剤の製造方法に関する。より詳細に、本発明は、自然発火による火災の発生が抑制された水用殺菌消毒剤等に好適な、自己崩壊し難い錠剤を得るための製造方法に関する。 The present invention relates to a method for producing a tablet. In more detail, this invention relates to the manufacturing method for obtaining the tablet which is suitable for the disinfection agent for water etc. with which generation | occurrence | production of the fire by spontaneous ignition was suppressed, and which is hard to self-disintegrate.
水用殺菌消毒剤として、次亜塩素酸カルシウムを主成分とする白色、固体の塩素剤が知られている。この塩素剤は、錠剤や顆粒の形で市販されている。これらの塩素剤は、水に溶解した際の不溶解分がほとんどない。顆粒のものはプール等の水中に散布すると速やかに溶解する。錠剤のものはプール等に投入しておくとしだいに溶解して、徐々に有効塩素濃度が上がるので、特別な装置を使用しなくても有効塩素の補給が手軽に行えるという特徴がある。また、塩素水注入装置を用いて、水中の塩素剤の濃度を一定にすることもできる。
水和次亜塩素酸カルシウムは強力な酸化剤であり、それ自体が激しく発熱し、また接触する可燃性物質の燃焼を引き起こすことがある。この酸化力は、その水用殺菌消毒剤の輸送及び貯蔵の両方において問題をもたらす可能性がある。また、次亜塩素酸カルシウムを含む物質の燃焼は非常に激しい。例えば、次亜塩素酸カルシウムを包装した可燃性のシート（例えばプラスチック、ボール紙）は、着火すると激しく燃焼する。As a water disinfectant, a white and solid chlorine agent mainly composed of calcium hypochlorite is known. This chlorinating agent is commercially available in the form of tablets and granules. These chlorine agents have almost no insoluble content when dissolved in water. Granules dissolve quickly when sprayed into water such as pools. Tablets dissolve as soon as they are put into a pool and the like, and the effective chlorine concentration gradually increases. Therefore, effective chlorine can be easily replenished without using a special device. Moreover, the density | concentration of the chlorine agent in water can also be made constant using a chlorine water injection | pouring apparatus.
Hydrated calcium hypochlorite is a powerful oxidant, which itself generates intense heat and can cause combustion of combustible materials in contact with it. This oxidizing power can cause problems in both transport and storage of the water disinfectant. In addition, combustion of substances containing calcium hypochlorite is very intense. For example, a combustible sheet (for example, plastic or cardboard) packaged with calcium hypochlorite burns violently when ignited.
次亜塩素酸カルシウムの発熱を抑える方法として様々な提案がなされている。例えば、特許文献１には、次亜塩素酸カルシウムにアルカリ金属やアルカリ土類金属の水和塩を配合し、水を３〜１３重量％含有させることが記載されている。特許文献２には、次亜塩素酸カルシウムと硫酸マグネシウム七水和物とを配合し、水を少なくとも約１７重量％含有させることが記載されている。特許文献３には、次亜塩素酸カルシウムなどの殺生成分と、ホウ素化合物やアルカリケイ酸塩などのガラス形成性成分と、塩基性硫酸アルミニウム（ミョウバン）などの凝集剤とを含有する組成物が記載されている。また、特許文献４には、トリクロロ−ｓ−トリアジントリオン、四ホウ酸ナトリウムおよび塩基性硫酸アルミニウムを含有する組成物が記載されている。 Various proposals have been made as methods for suppressing the heat generation of calcium hypochlorite. For example, Patent Document 1 describes that calcium hypochlorite is mixed with a hydrated salt of an alkali metal or an alkaline earth metal and contains 3 to 13% by weight of water. Patent Document 2 describes that calcium hypochlorite and magnesium sulfate heptahydrate are blended to contain at least about 17% by weight of water. Patent Document 3 discloses a composition containing a biocidal component such as calcium hypochlorite, a glass-forming component such as a boron compound or an alkali silicate, and a flocculant such as basic aluminum sulfate (alum). Have been described. Patent Document 4 describes a composition containing trichloro-s-triazinetrione, sodium tetraborate and basic aluminum sulfate.
ところが、双方とも結晶水を保持することができる２種以上の固体物質の混合物を加圧成形して錠剤を得たときに、該錠剤が長期間保存において、膨潤等により自己崩壊することがあった。
そこで本発明の目的は、自然発火による火災の発生が抑制された水用殺菌消毒剤等として好適な、自己崩壊し難い錠剤を得るための製造方法を提供することにある。However, when a tablet is obtained by press-molding a mixture of two or more solid substances capable of retaining crystal water in both cases, the tablet may self-disintegrate due to swelling or the like during long-term storage. It was.
Accordingly, an object of the present invention is to provide a production method for obtaining a tablet that is suitable as a water disinfectant and the like, in which the occurrence of fire due to spontaneous ignition is suppressed, and that is difficult to self-disintegrate.
本発明者は、前記目的を達成するために鋭意検討した結果、示差走査熱量計で測定される吸熱量が相互に異なり且つ双方とも結晶水を保持することができる２種以上の固体物質を少なくとも含有する混合物を打錠すると、結晶水が吸熱量の大きい固体物質から吸熱量の小さい固体物質に移行すること；この結晶水の移行量が多くなりすぎると結晶水を受け取った固体物質が膨潤等を起こすこと；および、この結晶水の移行しやすさが、打錠圧と相関を有することを見出した。そして、これらの知見に基づいてさらに検討した結果、錠剤の自己崩壊を防ぐことができる新たな錠剤の製造方法を発明するに至ったのである。 As a result of intensive studies to achieve the above object, the present inventor has at least two or more kinds of solid substances having different endotherms measured by a differential scanning calorimeter and capable of holding crystal water. When tablets containing the mixture are tableted, the crystal water shifts from a solid substance with a large endotherm to a solid substance with a small endotherm; if the amount of crystal water transferred is too large, the solid substance that has received crystal water will swell, etc. And the ease of migration of the crystal water was found to correlate with the tableting pressure. As a result of further studies based on these findings, a new tablet production method that can prevent the tablet from self-disintegrating has been invented.
すなわち、本発明は下記の製造方法に関する。
〈１〉 示差走査熱量計で測定される吸熱量が相互に異なり且つ双方とも結晶水を保持することができる２種以上の固体物質を少なくとも含有する混合物を用意し、該混合物を打錠圧２５０ｋｇｆ／ｃｍ2〜１１５０ｋｇｆ／ｃｍ2で打錠することを含む錠剤の製造方法。
〈２〉 前記２種以上の固体物質の少なくとも一つは、結晶水が飽和状態または不飽和状態にあり、少なくとも一つは結晶水が不飽和状態にある、前記〈１〉に記載の錠剤の製造方法。
〈３〉 前記２種以上の固体物質の少なくとも一つは結晶水を有している、前記〈１〉又は〈２〉に記載の錠剤の製造方法。
〈４〉 前記２種以上の固体物質の一つが硫酸バンドであり、一つが次亜塩素酸カルシウムである、前記〈１〉に記載の錠剤の製造方法。That is, this invention relates to the following manufacturing method.
<1> A mixture containing at least two kinds of solid substances having different endotherms measured by a differential scanning calorimeter and capable of holding water of crystallization is prepared, and the mixture is compressed into a tableting pressure of 250 kgf. / cm 2 method for producing a tablet comprising tabletting in ～1150Kgf / cm 2.
<2> The tablet according to <1>, wherein at least one of the two or more solid substances is a crystal water in a saturated or unsaturated state, and at least one of the crystal water is in an unsaturated state. Production method.
<3> The method for producing a tablet according to <1> or <2>, wherein at least one of the two or more kinds of solid substances has water of crystallization.
<4> The method for producing a tablet according to <1>, wherein one of the two or more solid substances is a sulfate band and one is calcium hypochlorite.
本発明の製造方法で得られる錠剤は、膨潤等による自己崩壊をし難く、形状が安定している。本発明の製造方法で得られる錠剤は、自然発火による火災の発生が抑制され、安全性が高いため、生活排水、産業排水、プール循環水、浴場循環湯などの水の雑菌消毒処理を効果的に行うことができる水用殺菌消毒剤として好適である。
本発明によってこのような顕著な効果を奏する理由は定かで無いが、打錠圧が高すぎると吸熱量の大きい固体物質から吸熱量の小さい固体物質に結晶水が移動しやすくなり、その結果、結晶水を受け取った吸熱量の小さい固体物質が膨潤して、錠剤を自己崩壊に導くのであろうと推測される。一方打錠圧が低すぎると固体物質間の結着力が不足するので錠剤としての強度が不十分になると考えられる。The tablet obtained by the production method of the present invention is hardly self-disintegrating due to swelling or the like, and has a stable shape. Since the tablet obtained by the production method of the present invention suppresses the occurrence of fire due to spontaneous ignition and is highly safe, it is effective to disinfect bacteria such as domestic wastewater, industrial wastewater, pool circulating water, bathhouse circulating hot water, etc. It is suitable as a disinfectant for water that can be used for
The reason why such a remarkable effect is achieved by the present invention is not clear, but if the tableting pressure is too high, the crystal water easily moves from a solid substance having a large endotherm to a solid substance having a small endotherm, and as a result, It is presumed that the solid substance with low endotherm that has received crystal water will swell and lead the tablet to self-disintegration. On the other hand, if the tableting pressure is too low, the binding force between the solid substances is insufficient, so that the strength as a tablet is considered to be insufficient.
本発明に係る錠剤の製造方法は、示差走査熱量計で測定される吸熱量が相互に異なり且つ双方とも結晶水を保持することができる２種以上の固体物質を少なくとも含有する混合物を用意し、該混合物を打錠圧２５０ｋｇｆ／ｃｍ2〜１１５０ｋｇｆ／ｃｍ2で打錠することを含むものである。The tablet production method according to the present invention provides a mixture containing at least two or more kinds of solid substances that have mutually different endotherms measured by a differential scanning calorimeter and are capable of retaining crystal water. Tableting the mixture at a tableting pressure of 250 kgf / cm 2 to 1150 kgf / cm 2 .
本発明に用いられる混合物は、２種以上の固体物質を少なくとも混合してなるものである。該２種以上の固体物質は、示差走査熱量計で測定される吸熱量が相互に異なり且ついずれも結晶水を保持することができるものである。 The mixture used in the present invention is a mixture of at least two kinds of solid substances. The two or more kinds of solid substances have different endothermic amounts as measured by a differential scanning calorimeter, and both can hold crystal water.
吸熱量は、示差走査熱量計で測定される値である。示差走査熱量計は、試料と熱特性が既知である標準物質（おもにα−アルミナ）を温度可変炉にいれ、その雰囲気温度を一定速度で上昇もしくは下降させながら、両者の温度を熱電対を用いて測り、温度差が生じないようにヒーター電流を制御し、試料に供給する熱量速度を記録することができる計測装置である。 The endothermic amount is a value measured with a differential scanning calorimeter. A differential scanning calorimeter uses a thermocouple to move the temperature of the sample and a reference material (mainly α-alumina) with known thermal properties into a temperature-variable furnace, while raising or lowering the ambient temperature at a constant rate. It is a measuring device that can record the heat rate that is supplied to the sample by controlling the heater current so that no temperature difference occurs.
本発明における、吸熱量の示差走査熱量計による測定条件は、昇温速度が１０℃／分、測定温度範囲が２０℃〜２００℃、測定試料の重量が約２０ｍｇである。 The measurement conditions of the endothermic amount with a differential scanning calorimeter in the present invention are a heating rate of 10 ° C./min, a measuring temperature range of 20 ° C. to 200 ° C., and a weight of a measuring sample of about 20 mg.
２種以上の固体物質は、吸熱量の最大差が、好ましくは１００ｍＪ／ｍｇ以上、より好ましくは２００ｍＪ／ｍｇ〜５００ｍＪ／ｍｇである。吸熱量の差が小さすぎる場合には、本発明に係る製造方法の特長が発揮され難い。 Two or more kinds of solid substances have a maximum difference in endothermic amount of preferably 100 mJ / mg or more, more preferably 200 mJ / mg to 500 mJ / mg. When the difference in endothermic amount is too small, the features of the production method according to the present invention are hardly exhibited.
本発明の製造方法では、前記２種以上の固体物質の少なくとも一つは結晶水が飽和状態または不飽和状態にあり、少なくとも一つは結晶水が不飽和状態にあることが好ましい。
また、本発明の製造方法では、前記２種以上の固体物質の少なくとも一つは結晶水を有していることが好ましい。
さらに本発明の製造方法では、前記２種以上の固体物質の一が硫酸バンドであり、一つが次亜塩素酸カルシウムであることが特に好ましい。In the production method of the present invention, it is preferable that at least one of the two or more solid substances has crystal water in a saturated or unsaturated state and at least one of the crystal water is in an unsaturated state.
In the production method of the present invention, it is preferable that at least one of the two or more kinds of solid substances has crystal water.
Furthermore, in the production method of the present invention, it is particularly preferable that one of the two or more solid substances is a sulfate band and one is calcium hypochlorite.
次亜塩素酸カルシウムは、化学式ＣａＣｌ（ＣｌＯ）・Ｈ2ＯまたはＣａ（ＣｌＯ）2で表される化合物である。次亜塩素酸カルシウムの吸熱量は約３３６ｍＪ／ｍｇである。次亜塩素酸カルシウムは、塩素消毒剤の主成分として用いられているものであれば、特に制限されない。次亜塩素酸カルシウムを水に溶解させると次亜塩素酸と水酸化カルシウムに分解する。次亜塩素酸は、大腸菌、アデノビールス３型（プール熱病原菌）、赤痢アメーバ菌、好気性悍菌、チフス菌、コサッキッビールスＡ２型（無菌脳膜炎病原体）、炭疽菌、などの水中微生物を殺滅し、水の消毒を行うことができる。Calcium hypochlorite is a compound represented by the chemical formula CaCl (ClO) .H 2 O or Ca (ClO) 2 . The endothermic amount of calcium hypochlorite is about 336 mJ / mg. Calcium hypochlorite is not particularly limited as long as it is used as a main component of a chlorine disinfectant. When calcium hypochlorite is dissolved in water, it decomposes into hypochlorous acid and calcium hydroxide. Hypochlorous acid is an aquatic microorganism such as Escherichia coli, Adenovirus type 3 (Pool fever pathogen), Shigella Amoeba, Aerobic Neisseria gonorrhoeae, Salmonella typhi, Cossackievirus A2 type (Aseptic encephalitis pathogen), Bacillus anthracis, etc. Can be killed and water disinfected.
硫酸バンドは、アルミニウムの硫酸塩である。硫酸アルミニウムは、化学式Ａｌ2Ｓ3Ｏ12またはＡｌ2（ＳＯ4）3で表される化合物であるが、該化合物は、通常、結晶水を包含する。硫酸アルミニウムの水和物としては、９水和物、１０水和物、１４〜１６水和物、１８水和物、２７水和物などがある。硫酸バンドは、通常、１４〜１６水和物を主成分とするものである。硫酸バンドの吸熱量は約７１２ｍＪ／ｍｇである。The sulfate band is a sulfate of aluminum. Aluminum sulfate is a compound represented by the chemical formula Al 2 S 3 O 12 or Al 2 (SO 4 ) 3 , and the compound usually includes crystal water. Examples of the hydrate of aluminum sulfate include 9 hydrate, 10 hydrate, 14 to 16 hydrate, 18 hydrate, and 27 hydrate. The sulfuric acid band is usually composed mainly of 14 to 16 hydrate. The endothermic amount of the sulfuric acid band is about 712 mJ / mg.
本発明において、吸熱量の大きい固体物質と吸熱量の小さい固体物質との混合比（質量比）は、該固体物質中の結晶水を除いた状態における質量の比として、好ましくは５：９５〜９５：５、より好ましくは１０：９０〜４０：６０、さらに好ましくは１０：９０〜２０：８０である。硫酸バンドと次亜塩素酸カルシウムとの場合には、Ａｌ2（ＳＯ4）3：Ｃａ（ＣｌＯ）2の質量比において、好ましくは１０：９０〜４０：６０、より好ましくは１０：９０〜２０：８０、特に好ましくは１５：８５である。In the present invention, the mixing ratio (mass ratio) of the solid substance having a large endothermic amount and the solid substance having a small endothermic amount is preferably 5:95 to the mass ratio in a state excluding crystallization water in the solid substance. It is 95: 5, More preferably, it is 10: 90-40: 60, More preferably, it is 10: 90-20: 80. In the case of a sulfate band and calcium hypochlorite, the mass ratio of Al 2 (SO 4 ) 3 : Ca (ClO) 2 is preferably 10:90 to 40:60, more preferably 10:90 to 20 : 80, particularly preferably 15:85.
吸熱量の大きい固体物質と吸熱量の小さい固体物質との混合は、例えば、乾燥固形の吸熱量の大きい固体物質と乾燥固形の吸熱量の小さい固体物質とを公知の混合装置に投入して行うことができる。 The mixing of the solid substance having a large endothermic amount and the solid substance having a small endothermic amount is performed, for example, by introducing a solid substance having a large dry endotherm and a solid substance having a small endothermic amount into a known mixing apparatus. be able to.
本発明に係る製造方法では、該混合物を打錠圧２５０ｋｇｆ／ｃｍ2〜１１５０ｋｇｆ／ｃｍ2、好ましくは７００ｋｇｆ／ｃｍ2〜９００ｋｇｆ／ｃｍ2で打錠する。打錠圧がこの範囲である場合には、得られる錠剤は破壊強度が十分にあり且つ長期保存による自己崩壊を起こさなくなる。ここで、打錠圧とは、固体物質に掛かる圧力Ｙ［ｋｇｆ／ｃｍ2］である。すなわち、プレス機の圧力がＸ［ｋｇｆ／ｃｍ2］で、プレス機のシリンダー径がＤ1で、錠剤成形金型のシリンダー径がＤ2であるとき、錠剤成形金型に充填された固体物質に掛かる圧力Ｙ［ｋｇｆ／ｃｍ2］は、Ｘ×Ｄ1 2／Ｄ2 2で算出される。In accordance with the present invention, a tableting pressure of 250kgf / cm 2 ~1150kgf / cm 2 The mixture, preferably tableted at 700kgf / cm 2 ~900kgf / cm 2 . When the tableting pressure is within this range, the obtained tablet has sufficient breaking strength and does not cause self-disintegration due to long-term storage. Here, the tableting pressure is a pressure Y [kgf / cm 2 ] applied to the solid substance. That is, when the pressure of the press is X [kgf / cm 2 ], the cylinder diameter of the press is D 1 , and the cylinder diameter of the tablet molding die is D 2 , the solid substance filled in the tablet molding die The pressure Y [kgf / cm 2 ] applied to is calculated by X × D 1 2 / D 2 2 .
本発明の製造方法によって得られる錠剤には、トリクロロイソシアヌル酸、ジクロロイソシアヌル酸ナトリウム、ジクロロイソシアヌル酸カリウムなど塩素化イソシアヌル酸；水酸化ナトリウム、炭酸水素ナトリウム、水酸化カルシウムなどのアルカリ剤；ホウ酸、ホウ砂、四ホウ酸ナトリウムなどのホウ素化合物；ケイ酸ナトリウムなどのケイ酸塩；硫酸マグネシウム、ミョウバンなどが含まれていてもよい。 Tablets obtained by the production method of the present invention include chlorinated isocyanuric acids such as trichloroisocyanuric acid, sodium dichloroisocyanurate and potassium dichloroisocyanurate; alkaline agents such as sodium hydroxide, sodium hydrogencarbonate and calcium hydroxide; boric acid, Boron compounds such as borax and sodium tetraborate; silicates such as sodium silicate; magnesium sulfate, alum and the like may be included.
本発明の製造方法で得られる錠剤は、その形によって特に制限されない。例えば、高さが２ｃｍ〜５ｃｍ、直径が１ｃｍ〜１０ｃｍの円柱または円盤状のタブレットにすることができる。 The tablet obtained by the production method of the present invention is not particularly limited by its shape. For example, it can be a cylindrical or disk-shaped tablet having a height of 2 cm to 5 cm and a diameter of 1 cm to 10 cm.
本発明の製造方法で得られる錠剤は、自然発火などを生じ難いが、湿気などを避けて冷暗所に保存貯蔵することが好ましい。また長期間保存後においても殺菌性能に変化はない。 The tablet obtained by the production method of the present invention is unlikely to spontaneously ignite, but is preferably stored and stored in a cool and dark place avoiding moisture. In addition, the sterilization performance does not change even after long-term storage.
次に、実施例を挙げて、本発明を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して解釈されるものでない。 EXAMPLES Next, although an Example is given and this invention is demonstrated further in detail, this invention is limited to only these Examples and is not interpreted.
実施例１
硫酸バンドと次亜塩素酸カルシウムとをＡｌ2（ＳＯ4）3：Ｃａ（ＣｌＯ）2の混合比（質量比）において１５：８５となる割合で混ぜ合わせた。該混合物を、打錠圧８１０ｋｇｆ／ｃｍ2で加圧成形して、高さ３０ｍｍ、直径５０ｍｍの円柱状の錠剤を得た。錠剤の破壊強度は１５００Ｎを超え、強度的には十分であった。この錠剤を、４０℃の環境下に、４週間放置した。その結果、錠剤に変化は見られなかった。Example 1
The sulfuric acid band and calcium hypochlorite were mixed at a ratio of 15:85 in the mixing ratio (mass ratio) of Al 2 (SO 4 ) 3 : Ca (ClO) 2 . The mixture was compression molded at a tableting pressure of 810 kgf / cm 2 to obtain a cylindrical tablet having a height of 30 mm and a diameter of 50 mm. The breaking strength of the tablet exceeded 1500 N, and the strength was sufficient. The tablet was left in an environment of 40 ° C. for 4 weeks. As a result, no change was seen in the tablets.
比較例１
打錠圧を２１０ｋｇｆ／ｃｍ2に変更した以外は実施例１と同じ手法で錠剤を得た。錠剤の破壊強度は５００Ｎ以下となり、強度不足な錠剤となった。Comparative Example 1
Tablets were obtained in the same manner as in Example 1 except that the tableting pressure was changed to 210 kgf / cm 2 . The breaking strength of the tablet was 500 N or less, and the tablet was insufficient in strength.
比較例２
打錠圧を１２００ｋｇｆ／ｃｍ2に変更した以外は実施例１と同じ手法で錠剤を得た。錠剤の破壊強度は１５００Ｎを超え、強度的には十分であった。この錠剤を、４０℃の環境下に、４週間放置した。錠剤が膨潤して自己崩壊した。Comparative Example 2
Tablets were obtained in the same manner as in Example 1 except that the tableting pressure was changed to 1200 kgf / cm 2 . The breaking strength of the tablet exceeded 1500 N, and the strength was sufficient. The tablet was left in an environment of 40 ° C. for 4 weeks. The tablet swelled and self-disintegrated.
本発明を詳細に、また特定の実施態様を参照して説明したが、本発明の精神と範囲を逸脱することなく、様々な修正や変更を加えることができることは、当業者にとって明らかである。
本出願は、２００９年１２月７日出願の日本特許出願２００９−２７７９３８に基づくものであり、その内容はここに参照として取り込まれる。Although the invention has been described in detail and with reference to specific embodiments, it will be apparent to those skilled in the art that various modifications and variations can be made without departing from the spirit and scope of the invention.
This application is based on Japanese Patent Application No. 2009-277738 filed on Dec. 7, 2009, the contents of which are incorporated herein by reference.
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| PCT/JP2010/071739 WO2011070983A1 (en) | 2009-12-07 | 2010-12-03 | Method for producing tablet |
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| JPS5154097A (en) * | 1974-11-06 | 1976-05-12 | Olin Corp | Funmuryujokanyoru ryujojiaensosankarushiumu |
| JPS6323812A (en) * | 1986-07-16 | 1988-02-01 | Kao Corp | Production of tablet |
| JPS6330304A (en) * | 1986-07-25 | 1988-02-09 | Tosoh Corp | Method for tableting calcium hypochlorite composition |
| JPH02500256A (en) * | 1986-08-07 | 1990-02-01 | ピーピージー・インダストリーズ・インコーポレイテッド | Calcium hypochlorite composition |
| JPH03502199A (en) * | 1988-06-30 | 1991-05-23 | ピーピージー・インダストリーズ・インコーポレイテッド | Halogen-containing solid composition and method for producing the same |
| JP2006521995A (en) * | 2003-04-02 | 2006-09-28 | アーチ ケミカルズ，インコーポレイテッド | Tablets blended with calcium hypochlorite |
| JP2006522805A (en) * | 2003-04-14 | 2006-10-05 | ブローミン コンパウンズ リミテッド | Solid biocide |
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2010
- 2010-12-03 WO PCT/JP2010/071739 patent/WO2011070983A1/en active Application Filing
- 2010-12-03 JP JP2011545196A patent/JP5643962B2/en not_active Expired - Fee Related
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5154097A (en) * | 1974-11-06 | 1976-05-12 | Olin Corp | Funmuryujokanyoru ryujojiaensosankarushiumu |
| JPS6323812A (en) * | 1986-07-16 | 1988-02-01 | Kao Corp | Production of tablet |
| JPS6330304A (en) * | 1986-07-25 | 1988-02-09 | Tosoh Corp | Method for tableting calcium hypochlorite composition |
| JPH02500256A (en) * | 1986-08-07 | 1990-02-01 | ピーピージー・インダストリーズ・インコーポレイテッド | Calcium hypochlorite composition |
| JPH03502199A (en) * | 1988-06-30 | 1991-05-23 | ピーピージー・インダストリーズ・インコーポレイテッド | Halogen-containing solid composition and method for producing the same |
| JP2006521995A (en) * | 2003-04-02 | 2006-09-28 | アーチ ケミカルズ，インコーポレイテッド | Tablets blended with calcium hypochlorite |
| JP2006522805A (en) * | 2003-04-14 | 2006-10-05 | ブローミン コンパウンズ リミテッド | Solid biocide |
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