JP4378973B2 - Method for producing porous granular ammonium nitrate - Google Patents
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【０００１】
【発明の属する技術分野】
本発明は、多孔質粒状硝酸アンモニウムの製造方法に関する。
【０００２】
【従来の技術】
多孔質粒状硝酸アンモニウムは、爆薬組成物の原料として有用である。例えば多孔質粒状アンモニウムに燃料油を吸収させたものは、硝酸アンモニウム燃料油爆薬（ＡＮＦＯ爆薬）として広く用いられている。かかる多孔質粒状硝酸アンモニウムとしては、細孔容積がより大きく、より硬いものが望まれている。
【０００３】
かかる多孔質粒状硝酸アンモニウムの製造方法として、特許文献１（特公昭４４−１８５７３号公報）には、硝酸アンモニウム水溶液の液滴を乾燥させて得た硝酸アンモニウム粒子に、常温の水を添加した後、加熱して乾燥させる方法が開示されている。
【０００４】
しかし、かかる従来の製造方法により得られる多孔質粒状硝酸アンモニウムは、細孔容積が十分に大きなものではないか、または十分に硬いものではないという問題があった。
【０００５】
【特許文献１】
特公昭４４−１８５７３号公報
【０００６】
【発明が解決しようとする課題】
そこで本発明者は、十分な大きさの細孔容積を有しつつ、十分な硬さの多孔質粒状硝酸アンモニウムを製造し得る方法を開発するべく鋭意検討した結果、濃度９２〜９６質量％の硝酸アンモニウム水溶液の液滴を乾燥させて得た硝酸アンモニウム粒子に、７０℃以上の水を加え、次いで９０℃以上に加熱して水分含有量０．２質量％以下まで乾燥させることで、より大きな細孔容積を有し、十分に硬い多孔質粒状硝酸アンモニウムを製造し得ることを見出し、本発明に至った。
【０００７】
【課題を解決するための手段】
すなわち本発明は、濃度９２質量％以上９６質量％以下の硝酸アンモニウム水溶液の液滴を乾燥させて得た硝酸アンモニウム粒子を原料として用いて、該硝酸アンモニウム粒子と同じ粒子径の多孔質粒状硝酸アンモニウムを製造する方法であり、前記硝酸アンモニウム粒子に、７０℃以上の水を硝酸アンモニウム粒子１００質量部あたり０．５質量部以上５質量部以下加え、
次いで９０℃以上に加熱して水分含有量０．２質量％以下に乾燥させることを特徴とする前記多孔質粒状硝酸アンモニウムの製造方法を提供するものである。
【０００８】
【発明の実施の形態】
本発明の製造方法では、濃度９２質量％以上９６質量％以下の硝酸アンモニウム水溶液から得た硝酸アンモニウム粒子を用いる。かかる濃度の硝酸アンモニウム水溶液の温度は通常１０５℃以上１６０℃以下である。かかる硝酸アンモニウム水溶液を液滴とし、水分を蒸発させて乾燥することで、硝酸アンモニウム粒子を得る。硝酸アンモニウム水溶液の濃度が９２質量％未満では、十分な硬さの多孔質粒状硝酸アンモニウムを得ることができない傾向にある。また９６質量％を超えると、細孔容積が十分に大きくならない傾向にある。
【０００９】
かかる水溶液の液滴を乾燥するには、例えば自然通気型造粒塔を用いて、塔頂から水溶液を噴霧して液滴として落下させながら、水分を蒸発させればよい。液滴から水分を蒸発させることで、液滴が濃縮されて、硝酸アンモニウム粒子を得ることができる。硝酸アンモニウム粒子の水分含有量は０．２質量％以下であることが好ましい。自然通気型造粒塔を用いて液滴を乾燥させただけでは水分含有量が０．２質量％を超える場合もあるが、その場合には、さらに乾燥して水分含有量を０．２質量％以下としてもよい。さらに乾燥するには、１００℃以下の温度に加熱してもよいし、風乾してもよい。かくして得られる硝酸アンモニウム粒子の粒子径は通常０．１ｍｍ以上５ｍｍ以下程度である。
【００１０】
得られた硝酸アンモニウム粒子に、水を加える。加える水の温度は７０℃以上であり、通常は１００℃以下である。加える水の温度が７０℃未満であると、より大きな細孔容積とすることができず、また十分な硬さとはならない傾向にある。水の添加量は、乾燥硝酸アンモニウム粒子１００質量部あたり通常は０．５質量部以上５質量部以下である。
【００１１】
加える水は、界面活性剤を含んでいてもよい。界面活性剤としては、アニオン系界面活性剤、カチオン系界面活性剤などを用いることができる。アニオン系界面活性剤としては、例えば高級脂肪酸の塩、アルキルベンゼンスルホン酸の塩、アルキルナフタレンスルホン酸の塩、高級アルコール硫酸エステルの塩などが、アニオン系界面活性剤としては、例えばアルキルアミンの塩などが挙げられる。これらの界面活性剤はそれぞれ単独でまたは２種以上を組み合わせて用いられる。水が界面活性剤を含む場合、その濃度は通常０．５質量％以上５質量％以下程度である。
【００１２】
硝酸アンモニウム粒子に７０℃以上の水を加えた後、加熱して乾燥させる。加熱して乾燥させるには、例えば棚段式加熱炉、内燃型回転式加熱炉、外熱型回転式加熱炉、振動通風式加熱炉、縦型通風式加熱炉、振動外熱式加熱炉、トンネル式加熱炉などを用いればよい。本発明の製造方法では、９０℃以上に加熱し水分含有量を０．２質量％以下とする。水分含有量が０で、実質的に水を含まない程度まで乾燥してもよい。温度を９０℃以上としても水分含有量が０．２質量％を超えていたり、水分含有量が０．２質量％以下であっても温度が９０℃未満であると、硬さが十分とはならない傾向にある。また、温度が１２０℃を超えると得られる多孔質粒状硝酸アンモニウムが凝集し易くなるため、通常は温度を１２０℃以下とする。
【００１３】
かくして硝酸アンモニウム粒子に空隙が生じて、目的の多孔質粒状硝酸アンモニウムが得られるが、その粒子径は、用いた硝酸アンモニウム粒子と同じ粒子径、具体的には０．１ｍｍ以上５ｍｍ以下程度の粒子径の粒状硝酸アンモニウムを用いた場合には０．１ｍｍ以上５ｍｍ以下程度であって、その全細孔容積は０．２５ｃｍ3／ｇ以上０．４ｃｍ3／ｇ以下程度であり、平均細孔半径は５μｍ以上程度であり、硬度は３０％以下程度であり、嵩比重は０．７ｇ／ｃｍ3以下程度である。
【００１４】
かかる多孔質粒状硝酸アンモニウムは、内層と、この内層よりも緻密な構造の最外層とを含む多層構造であることが、機械的強度により優れる点で、好ましい。かかる多層構造の多孔質粒状硝酸アンモニウムは、例えば硝酸アンモニウム粒子に７０℃以上の水を加えた後の硝酸アンモニウム粒子を容器中で撹拌しながら容器壁面を加熱する方法で得ることができる。かかる方法によれば、硝酸アンモニウム粒子が水の存在下に壁面と接触しながら表面から加熱されるので、内部に空隙の多い内層が形成されると共に、表面には空隙の少ない緻密な層が形成される。かくして形成される最外層の厚みは粒子径の１／４０以上１／１０以下程度である。
【００１５】
かかる多層構造の多孔質粒状硝酸アンモニウムは、例えば加熱して乾燥させて得られた多孔質粒状硝酸アンモニウムに硝酸アンモニウムの微細な粒子を添加して、撹拌することで得ることもできる。かかる方法によれば、添加された微細な粒子が表面で互いに密着して緻密な最外層を形成する。
【００１６】
加熱して乾燥させて得られた多孔質粒状硝酸アンモニウムに高濃度の硝酸アンモニウム水溶液を添加し、乾燥させる方法により、多層構造の多孔質粒状硝酸アンモニウムを得ることもできる。かかる方法によれば、表面に付着した高濃度の硝酸アンモニウム水溶液が緻密な最外層を形成する。高濃度の硝酸アンモニウム水溶液は通常、噴霧して添加される。
【００１７】
かくして得られた多孔質粒状硝酸アンモニウムは、加熱して乾燥された後、冷却しながら、または冷却した後に固結防止剤を添加されてもよい。固結防止剤は、多孔質粒状硝酸アンモニウムが互いに凝集して固結することを防止するために添加されるものである。固結防止剤としては、通常用いられると同様の直鎖脂肪族モノアミン、直鎖脂肪族モノアミンの塩、珪酸アルミン酸マグネシウム、エチレンビスステアロアマイド、脂肪族カルボン酸のアルカリ土類金属塩などが挙げられる。
【００１８】
【発明の効果】
本発明の製造方法によれば、より大きな細孔容積を示し、比較的硬い多孔質粒状硝酸アンモニウムを製造することができる。
【００１９】
【実施例】
以下、実施例によって本発明をより詳細に説明するが、本発明はかかる実施例によって限定されるものではない。
【００２０】
なお、以下の実施例において得られた多孔質粒状硝酸アンモニウムは、以下の方法によって評価した。
全細孔容積および平均細孔半径は、水銀圧入法によって測定した。硬度は、ローディング試験機を用いて、多孔質粒状硝酸アンモニウム約１００ｇにパージ空気圧０．４ＭＰａ（約４気圧）にて衝撃を加えることで、３５メッシュ（目開き０．４ｍｍ）の篩を通過する大きさに微粉化した割合（質量比）であり、値が小さいほど硬いことを示す。嵩比重は、ＪＩＳ Ｋ−６７２１に記載の方法により測定した。
【００２１】
実施例１
自然通気型造粒塔を用いて塔頂から濃度９４質量％の硝酸アンモニウム水溶液（温度約１５０℃）の液滴を落下させながら水分を蒸発させて粒状物とし、さらに乾燥させて粒子径が概ね０．４ｍｍ〜１．７ｍｍで水分含有量０．１質量％以下の硝酸アンモニウム粒子を得た。この乾燥硝酸アンモニウム粒子（温度は約２０℃）１００質量部に、濃度２質量％のステアリン酸塩（高級脂肪酸の塩）の水溶液（９０℃）２質量部を添加し、次いで温風により加熱して１０１℃まで昇温して水分含有量０．１質量％以下まで乾燥させて、粒子径が概ね０．４ｍｍ〜１．７ｍｍの多孔質粒状硝酸アンモニウムを得た。この多孔質粒状硝酸アンモニウムの細孔容積は０．３０ｃｍ3／ｇ、平均細孔半径は８μｍ、硬度は２２％、嵩密度は０．６６ｇ／ｃｍ3であった。
【００２２】
実施例２
実施例１と同様に操作して得た硝酸アンモニウム粒子（水分含有量は０．１質量％以下、温度は約２０℃）１００質量部に、濃度３質量％のステアリン酸塩水溶液（８０℃）３．５質量部を添加した。次いで、内径４００ｍｍ、長さ６００ｍｍで壁面を１００℃に加熱した円筒形状の乾燥容器に、このステアリン酸水溶液を加えた後の硝酸アンモニウム粒子６６０ｇ（水溶液を含む状態の質量）を入れ、壁面温度を１００℃に維持しつつ、毎分４回転で回転させつつ自然通気しながら加熱して、硝酸アンモニウム粒子を９７℃まで昇温して乾燥させて水分含有量０．１質量％以下の多孔質粒状硝酸アンモニウム（粒子径は概ね０．４ｍｍ〜１．７ｍｍ）を得た。この多孔質粒状硝酸アンモニウムの細孔容積は０．３８ｃｍ3／ｇ、平均細孔半径は１２μｍ、硬度は３０％、嵩密度は０．５７ｇ／ｃｍ3であった。
【００２３】
実施例３
実施例１と同様に操作して得た硝酸アンモニウム粒子（水分含有量は０．１質量％以下、温度は約２０℃）１００質量部に、濃度３質量％のステアリン酸塩水溶液（８０℃）２質量部を添加した。次いで実施例２で用いたと同様に操作して加熱し、９０℃まで昇温して乾燥させて水分含有量０．１質量％以下の多孔質粒状硝酸アンモニウム（粒子径は概ね０．４ｍｍ〜１．７ｍｍ）を得た。この多孔質粒状硝酸アンモニウムの細孔容積は０．３８ｃｍ3／ｇ、平均細孔半径は１２μｍ、硬度は３０％、嵩密度は０．５７ｇ／ｃｍ3であった。得られた多孔質粒状硝酸アンモニウムのうちの一つ（粒子径は２．０ｍｍ）について、その断面を走査型電子顕微鏡（ＳＥＭ）により観察したところ、空隙の多い内層と、この内層よりも空隙が少なく緻密な最外層（厚みは１００μｍ程度）との２層構造であった。
【００２４】
実施例４
実施例１と同様に操作して得た硝酸アンモニウム粒子（水分含有量は０．１質量％以下、温度は約３０℃）１００質量部に、濃度２質量％のステアリン酸塩（高級脂肪酸の塩）の水溶液（８０℃）３質量部を添加し、次いで棚段式熱風加熱炉により加熱して９５℃まで昇温して水分含有量０．１質量％以下まで乾燥させて、多孔質粒状硝酸アンモニウム（粒子径は概ね０．４〜１．７ｍｍ）を得た。この多孔質粒状硝酸アンモニウムの細孔容積は０．２８ｃｍ3／ｇ、平均細孔半径は９μｍ、硬度は２５％、嵩密度は０．６８ｇ／ｃｍ3であった。
【００２５】
比較例１
自然通気型造粒塔を用いて塔頂から濃度９６質量％の硝酸アンモニウム水溶液（温度約１５０℃）の液滴を落下させながら水分を蒸発させて粒状物とし、さらに乾燥させて粒子径が概ね０．４ｍｍ〜１．７ｍｍで水分含有量０．１質量％以下の硝酸アンモニウム粒子を得た。この乾燥硝酸アンモニウム粒子（温度は約２０℃）１００質量部に、濃度２質量％のステアリン酸塩水溶液（６０℃）３質量部を添加し、次いで加熱して９５℃まで昇温して乾燥させて水分含有量０．１質量％以下の多孔質粒状硝酸アンモニウム（粒子径は概ね０．４ｍｍ〜１．７ｍｍ）を得た。この多孔質粒状硝酸アンモニウムの細孔容積は０．２３ｃｍ3／ｇ、平均細孔半径は２０μｍ、硬度は２５％、嵩密度は０．７７ｇ／ｃｍ3であった。
【００２６】
比較例２
比較例１と同様にして得た乾燥硝酸アンモニウム粒子（温度は約２０℃）１００質量部に、濃度２質量％のステアリン酸塩水溶液（９０℃）３質量部を添加し、次いで加熱して７５℃まで昇温して乾燥させて水分含有量０．１質量％以下の多孔質粒状硝酸アンモニウム（粒子径は概ね０．４ｍｍ〜１．７ｍｍ）を得た。この多孔質粒状硝酸アンモニウムの細孔容積は０．２３ｃｍ3／ｇ、平均細孔半径は８μｍ、硬度は１８％、嵩密度は０．７８ｇ／ｃｍ3であった。
【００２７】
比較例３
比較例１と同様にして得た乾燥硝酸アンモニウム粒子（温度は約２０℃）１００質量部に、濃度２質量％のステアリン酸塩水溶液（９０℃）４．６質量部を添加し、次いで加熱して６０℃まで昇温して乾燥させて水分含有量０．１質量％以下の多孔質粒状硝酸アンモニウム（粒子径は概ね０．４ｍｍ〜１．７ｍｍ）を得た。この多孔質粒状硝酸アンモニウムの細孔容積は０．２８ｃｍ3／ｇ、平均細孔半径は９μｍ、硬度は４３％、嵩密度は０．６６ｇ／ｃｍ3であった。[0001]
BACKGROUND OF THE INVENTION
The present invention relates to a method for producing porous granular ammonium nitrate.
[0002]
[Prior art]
Porous granular ammonium nitrate is useful as a raw material for explosive compositions. For example, porous particulate ammonium in which fuel oil is absorbed is widely used as an ammonium nitrate fuel oil explosive (ANFO explosive). As such porous granular ammonium nitrate, a harder one having a larger pore volume is desired.
[0003]
As a method for producing such porous granular ammonium nitrate, Patent Document 1 (Japanese Patent Publication No. 44-18573) discloses that water at room temperature is added to ammonium nitrate particles obtained by drying droplets of an aqueous ammonium nitrate solution, followed by heating. And a method of drying is disclosed.
[0004]
However, the porous granular ammonium nitrate obtained by such a conventional production method has a problem that the pore volume is not sufficiently large or not sufficiently hard.
[0005]
[Patent Document 1]
Japanese Examined Patent Publication No. 44-18573 [0006]
[Problems to be solved by the invention]
Therefore, the present inventor has intensively studied to develop a method capable of producing a porous granular ammonium nitrate having a sufficiently large pore volume and having a sufficient hardness, and as a result, has a concentration of 92 to 96% by mass of ammonium nitrate. By adding water of 70 ° C. or higher to ammonium nitrate particles obtained by drying droplets of an aqueous solution, then heating to 90 ° C. or higher and drying to a water content of 0.2% by mass or less, a larger pore volume It was found that a sufficiently hard porous granular ammonium nitrate can be produced, and the present invention has been achieved.
[0007]
[Means for Solving the Problems]
That is, the present invention is a method for producing porous granular ammonium nitrate having the same particle diameter as that of ammonium nitrate particles using, as a raw material, ammonium nitrate particles obtained by drying droplets of an ammonium nitrate aqueous solution having a concentration of 92% by mass or more and 96% by mass or less. , and the said ammonium nitrate particle, 0.5 parts by mass or more 5 parts by weight added per 100 parts by weight of ammonium nitrate particles 70 ° C. or more water,
Next, the present invention provides a method for producing the porous granular ammonium nitrate, which is heated to 90 ° C. or more and dried to a water content of 0.2% by mass or less.
[0008]
DETAILED DESCRIPTION OF THE INVENTION
In the production method of the present invention, ammonium nitrate particles obtained from an aqueous ammonium nitrate solution having a concentration of 92% by mass to 96% by mass are used. The temperature of the aqueous ammonium nitrate solution having such a concentration is usually 105 ° C. or higher and 160 ° C. or lower. The ammonium nitrate aqueous solution is made into droplets, and moisture is evaporated and dried to obtain ammonium nitrate particles. When the concentration of the aqueous ammonium nitrate solution is less than 92% by mass, there is a tendency that porous granular ammonium nitrate having sufficient hardness cannot be obtained. Moreover, when it exceeds 96 mass%, it exists in the tendency for a pore volume not to become large enough.
[0009]
In order to dry the droplets of the aqueous solution, for example, using a natural ventilation granulation tower, the aqueous solution may be evaporated while spraying the aqueous solution from the top of the tower and dropping it as droplets. By evaporating water from the droplets, the droplets are concentrated and ammonium nitrate particles can be obtained. The water content of the ammonium nitrate particles is preferably 0.2% by mass or less. In some cases, the moisture content may exceed 0.2% by mass by simply drying the droplets using a natural ventilation granulation tower. In that case, the moisture content is further dried to a moisture content of 0.2% by mass. % Or less. Further drying may be performed by heating to a temperature of 100 ° C. or lower, or air drying. The particle diameter of the ammonium nitrate particles thus obtained is usually about 0.1 mm to 5 mm.
[0010]
Water is added to the obtained ammonium nitrate particles. The temperature of the added water is 70 ° C. or higher, and is usually 100 ° C. or lower. If the temperature of the water to be added is less than 70 ° C., a larger pore volume cannot be obtained and the hardness tends not to be sufficient. The amount of water added is usually 0.5 parts by mass or more and 5 parts by mass or less per 100 parts by mass of the dried ammonium nitrate particles.
[0011]
The water to be added may contain a surfactant. As the surfactant, an anionic surfactant, a cationic surfactant, or the like can be used. Examples of the anionic surfactant include salts of higher fatty acids, salts of alkylbenzene sulfonic acids, salts of alkyl naphthalene sulfonic acids, salts of higher alcohol sulfates, and examples of anionic surfactants include salts of alkyl amines. Is mentioned. These surfactants are used alone or in combination of two or more. When water contains surfactant, the density | concentration is 0.5 to 5 mass% normally.
[0012]
Water of 70 ° C. or higher is added to the ammonium nitrate particles, and then heated to dry. In order to heat and dry, for example, a shelf type heating furnace, an internal combustion type rotary heating furnace, an external heating type rotary heating furnace, a vibration ventilation type heating furnace, a vertical type ventilation heating furnace, a vibration type external heating heating furnace, A tunnel heating furnace or the like may be used. In the manufacturing method of this invention, it heats to 90 degreeC or more and makes water content 0.2 mass% or less. You may dry to such an extent that moisture content is 0 and does not contain water substantially. Even if the temperature is 90 ° C. or higher, the moisture content exceeds 0.2% by mass, or the hardness is sufficient if the temperature is less than 90 ° C. even if the moisture content is 0.2% by mass or less There is a tendency not to become. Moreover, since the porous granular ammonium nitrate obtained will become easy to aggregate when temperature exceeds 120 degreeC, normally temperature shall be 120 degrees C or less.
[0013]
Thus, voids are generated in the ammonium nitrate particles, and the desired porous granular ammonium nitrate is obtained. The particle diameter is the same as the ammonium nitrate particles used, specifically, a granular having a particle diameter of about 0.1 mm to 5 mm. when using ammonium nitrate is a much more 5mm or less 0.1 mm, the total pore volume is on the order 0.25 cm 3 / g or more 0.4 cm 3 / g or less, the degree average pore radius 5μm or more The hardness is about 30% or less, and the bulk specific gravity is about 0.7 g / cm 3 or less.
[0014]
The porous granular ammonium nitrate preferably has a multilayer structure including an inner layer and an outermost layer having a denser structure than the inner layer in terms of excellent mechanical strength. Such porous granular ammonium nitrate having a multilayer structure, for example ammonium nitrate particles after the addition of 70 ° C. or more water ammonium nitrate particles can be obtained by a method of heating the vessel wall with stirring in a vessel. According to this method, the ammonium nitrate particles are heated from the surface in contact with the wall surface in the presence of water, so that an inner layer with many voids is formed inside, and a dense layer with few voids is formed on the surface. The The thickness of the outermost layer thus formed is about 1/40 to 1/10 of the particle diameter.
[0015]
Such porous granular ammonium nitrate having a multilayer structure can also be obtained, for example, by adding fine particles of ammonium nitrate to porous granular ammonium nitrate obtained by heating and drying and stirring. According to such a method, the added fine particles adhere to each other on the surface to form a dense outermost layer.
[0016]
A porous granular ammonium nitrate having a multilayer structure can also be obtained by adding a high concentration aqueous ammonium nitrate solution to the porous granular ammonium nitrate obtained by heating and drying, and then drying. According to this method, a high concentration ammonium nitrate aqueous solution adhering to the surface forms a dense outermost layer. A high concentration ammonium nitrate aqueous solution is usually added by spraying.
[0017]
The porous granular ammonium nitrate thus obtained may be added with an anti-caking agent while being cooled or cooled after being heated and dried. The anti-caking agent is added to prevent the porous granular ammonium nitrate from aggregating and caking together. Examples of anti-caking agents include linear aliphatic monoamines, linear aliphatic monoamine salts, magnesium aluminate silicate, ethylene bisstearamide, and alkaline earth metal salts of aliphatic carboxylic acids that are commonly used. Can be mentioned.
[0018]
【The invention's effect】
According to the production method of the present invention, porous granular ammonium nitrate that exhibits a larger pore volume and is relatively hard can be produced.
[0019]
【Example】
EXAMPLES Hereinafter, although an Example demonstrates this invention in detail, this invention is not limited by this Example.
[0020]
In addition, the porous granular ammonium nitrate obtained in the following examples was evaluated by the following method.
Total pore volume and average pore radius were measured by the mercury intrusion method. The hardness is large enough to pass through a 35 mesh (aperture 0.4 mm) sieve by applying an impact to about 100 g of porous granular ammonium nitrate at a purge air pressure of 0.4 MPa (about 4 atm) using a loading tester. It is the ratio (mass ratio) that was finely divided, and the smaller the value, the harder it is. The bulk specific gravity was measured by the method described in JIS K-6721.
[0021]
Example 1
Using a naturally ventilated granulation tower, droplets of an aqueous solution of ammonium nitrate (temperature: about 150 ° C.) having a concentration of 94% by mass are dropped from the top of the tower to evaporate the water into granules and then dried to obtain a particle size of approximately 0 Ammonium nitrate particles having a water content of 0.1% by mass or less at 0.4 mm to 1.7 mm were obtained. This dry ammonium nitrate particles (temperature about 20 ° C.) 100 parts by weight, was added an aqueous solution (90 ° C.) 2 parts by weight of the concentration of 2 wt% salt of stearic acid (salts of higher fatty acids), then heated by hot air The temperature was raised to 101 ° C. and dried to a water content of 0.1% by mass or less to obtain porous granular ammonium nitrate having a particle size of approximately 0.4 mm to 1.7 mm. The porous granular ammonium nitrate had a pore volume of 0.30 cm 3 / g, an average pore radius of 8 μm, a hardness of 22%, and a bulk density of 0.66 g / cm 3 .
[0022]
Example 2
In the same manner as in Example 1 operating-obtained ammonium nitrate particles (moisture content 0.1 wt% or less, the temperature is about 20 ° C.) to 100 parts by weight, concentration of 3 wt% of stearic acid salt aqueous solution (80 ° C.) 3 .5 parts by weight were added. Next, 660 g of ammonium nitrate particles (mass in a state containing the aqueous solution) after addition of this stearic acid aqueous solution was put into a cylindrical dry container having an inner diameter of 400 mm and a length of 600 mm and the wall surface heated to 100 ° C., and the wall surface temperature was set to 100. While maintaining at ℃, heated with natural aeration while rotating at 4 revolutions per minute, the ammonium nitrate particles were heated to 97 ℃ and dried to form porous granular ammonium nitrate having a water content of 0.1 mass% or less ( The particle diameter was approximately 0.4 mm to 1.7 mm. The porous granular ammonium nitrate had a pore volume of 0.38 cm 3 / g, an average pore radius of 12 μm, a hardness of 30%, and a bulk density of 0.57 g / cm 3 .
[0023]
Example 3
In the same manner as in Example 1 operating-obtained ammonium nitrate particles (moisture content 0.1 wt% or less, the temperature is about 20 ° C.) to 100 parts by weight, concentration of 3 wt% of stearic acid salt aqueous solution (80 ° C.) 2 Part by weight was added. Subsequently, the same operation as in Example 2 was performed, followed by heating, heating up to 90 ° C., drying, and porous granular ammonium nitrate having a water content of 0.1% by mass or less (particle diameter is approximately 0.4 mm to 1. 7 mm). The porous granular ammonium nitrate had a pore volume of 0.38 cm 3 / g, an average pore radius of 12 μm, a hardness of 30%, and a bulk density of 0.57 g / cm 3 . About one of the obtained porous granular ammonium nitrates (particle diameter is 2.0 mm), the cross section thereof was observed with a scanning electron microscope (SEM). As a result, an inner layer with many voids and fewer voids than the inner layer. It was a two-layer structure with a dense outermost layer (thickness of about 100 μm).
[0024]
Example 4
In the same manner as in Example 1 operating-obtained ammonium nitrate particles (moisture content 0.1 wt% or less, the temperature is about 30 ° C.) to 100 parts by weight, concentration of 2 wt% salt of stearic acid (salts of higher fatty acids) 3 parts by weight of an aqueous solution (80 ° C.), heated by a shelf-type hot air heating furnace, heated to 95 ° C. and dried to a water content of 0.1% by mass or less, and porous granular ammonium nitrate ( The particle diameter was approximately 0.4 to 1.7 mm. The porous granular ammonium nitrate had a pore volume of 0.28 cm 3 / g, an average pore radius of 9 μm, a hardness of 25%, and a bulk density of 0.68 g / cm 3 .
[0025]
Comparative Example 1
Using a naturally ventilated granulation tower, water droplets are evaporated to drop a droplet of a 96 mass% aqueous ammonium nitrate solution (temperature: about 150 ° C.) from the top of the tower to form a granular material, which is further dried to obtain a particle size of approximately 0. Ammonium nitrate particles having a water content of 0.1% by mass or less at 0.4 mm to 1.7 mm were obtained. This dry ammonium nitrate particles (temperature about 20 ° C.) 100 parts by weight, concentration of 2 wt% of stearic acid salt aqueous solution (60 ° C.) 3 parts by weight was added, then dried and heated to heated to 95 ° C. A porous granular ammonium nitrate having a water content of 0.1% by mass or less (particle diameter is approximately 0.4 mm to 1.7 mm) was obtained. The porous granular ammonium nitrate had a pore volume of 0.23 cm 3 / g, an average pore radius of 20 μm, a hardness of 25%, and a bulk density of 0.77 g / cm 3 .
[0026]
Comparative Example 2
Dry ammonium nitrate particles obtained in the same manner as in Comparative Example 1 (temperature of about 20 ° C.) to 100 parts by weight, was added to a concentration of 2 wt% of stearic acid salt aqueous solution (90 ° C.) 3 parts by mass, then heated to 75 ° C. And dried to obtain porous granular ammonium nitrate having a water content of 0.1% by mass or less (particle diameter is approximately 0.4 mm to 1.7 mm). The porous granular ammonium nitrate had a pore volume of 0.23 cm 3 / g, an average pore radius of 8 μm, a hardness of 18%, and a bulk density of 0.78 g / cm 3 .
[0027]
Comparative Example 3
Dry ammonium nitrate particles obtained in the same manner as in Comparative Example 1 (temperature of about 20 ° C.) to 100 parts by weight, was added to a concentration of 2 wt% of stearic acid salt aqueous solution (90 ° C.) 4.6 parts by mass, then heated to The temperature was raised to 60 ° C. and dried to obtain porous granular ammonium nitrate having a water content of 0.1% by mass or less (particle diameter was approximately 0.4 mm to 1.7 mm). The porous granular ammonium nitrate had a pore volume of 0.28 cm 3 / g, an average pore radius of 9 μm, a hardness of 43%, and a bulk density of 0.66 g / cm 3 .
Claims (5)
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