JP2005350276A - Method for producing porous granular ammonium nitrate - Google Patents
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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。詳しくは嵩比重のより小さい多孔質粒状硝酸アンモニウムの製造方法に関する。 The present invention relates to a method for producing porous granular ammonium nitrate. Specifically, the present invention relates to a method for producing porous granular ammonium nitrate having a smaller bulk specific gravity.
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、嵩比重がより小さく、硬く粉化し難いものが望まれている。 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 material having a smaller bulk specific gravity and hard and difficult to powder is desired.
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、水または界面活性剤を添加した後、加熱して乾燥させる方法が開示されている。 As a method for producing such porous granular ammonium nitrate, Patent Document 1 discloses a method in which water or a surfactant is added to ammonium nitrate particles obtained by drying droplets of an aqueous ammonium nitrate solution and then heated and dried. ing.
しかしながら、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よりさらに嵩比重が小さいものが望まれている。
そこで本発明者は、より小さな嵩比重の多孔質粒状硝酸アンモニウムを製造する方法について鋭意検討した結果、界面活性剤を含む水溶液を硝酸アンモニウム粒子に加え、次いで加熱、乾燥させて多孔質粒状硝酸アンモニウムを製造する際に、界面活性剤を含む水溶液に低級アルコール等の水溶性有機溶媒を添加して行うことによって、嵩比重を小さくできることを見出し、本発明に至った。 Therefore, as a result of intensive studies on a method for producing a porous granular ammonium nitrate having a smaller bulk specific gravity, the present inventors added an aqueous solution containing a surfactant to the ammonium nitrate particles, and then heated and dried to produce porous granular ammonium nitrate. At this time, the inventors have found that the bulk specific gravity can be reduced by adding a water-soluble organic solvent such as a lower alcohol to an aqueous solution containing a surfactant, and have reached the present invention.
すなわち本発明は、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、界面活性剤および水溶性有機溶媒を含む水溶液を硝酸アンモニウム粒子に添加し、次いで加熱、乾燥することを特徴とする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。 That is, the present invention provides a porous material characterized in that an aqueous solution containing a surfactant and a water-soluble organic solvent is added to ammonium nitrate particles obtained by drying droplets of an aqueous ammonium nitrate solution, and then heated and dried. A method for producing granular ammonium nitrate is provided.
本発明の製造方法によれば、同じ硬度でより小さい嵩比重の多孔質粒状硝酸アンモニウムを製造することができる。 According to the production method of the present invention, porous granular ammonium nitrate having the same hardness and a smaller bulk specific gravity can be produced.
界面活性剤および水溶性有機溶媒を含む水溶液を添加する硝酸アンモニウム粒子は、濃度が約９２〜９６重量％、温度が約１０５〜１６０℃であ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して得る。硝酸アンモニウム水溶液の濃度が約９２重量％未満では、十分な硬さの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。また約９６重量％を超えると、嵩比重が小さくならない傾向にある。 Ammonium nitrate particles to which an aqueous solution containing a surfactant and a water-soluble organic solvent is added are formed by dropping an aqueous ammonium nitrate solution having a concentration of about 92 to 96% by weight and a temperature of about 105 to 160 ° C. to evaporate water and drying. Get. When the concentration of the aqueous ammonium nitrate solution is less than about 92% by weight, there is a tendency that granular ammonium nitrate having sufficient hardness cannot be obtained. If it exceeds about 96% by weight, the bulk specific gravity tends not to be reduced.
かかる硝酸アンモニウム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、水分を蒸発させる。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が得られる。硝酸アンモニウム粒子の水分含有量は約０．２重量％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約０．２重量％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約０．２重量％以下とするのが好ましい。さらに乾燥するには、約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約０．１〜５ｍｍである。 In order to dry the ammonium nitrate aqueous solution droplets, for example, using a natural ventilation granulation tower, water is evaporated while the aqueous solution is sprayed from the top of the tower and dropped as droplets. By evaporating water from the droplets, the droplets are concentrated and ammonium nitrate particles are obtained. The water content of the ammonium nitrate particles is preferably about 0.2% by weight or less. In some cases, the water content may exceed about 0.2% by weight by simply drying the droplets using a naturally ventilated granulation tower. The content is preferably 2% by weight or less. For further drying, it may be heated to a temperature of about 100 ° C. or lower, or air-dried. The particle diameter of the ammonium nitrate particles thus obtained is about 0.1 to 5 mm.
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りことができる。
界面活性剤の中では、アルキルアミンの塩、中でもオクタデシルアミン酢酸塩が好ましく用いられる。
水溶液中の界面活性剤の濃度は約０．５〜５重量％である。この濃度以上にすると溶解度に応じて水溶液の温度を高くすることが必要になり、水溶液の温度が高くなると嵩比重が小さくならない傾向にあるので好ましくない。
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 can be used alone or in combination of two or more.
Among the surfactants, alkylamine salts, particularly octadecylamine acetate, are preferably used.
The concentration of the surfactant in the aqueous solution is about 0.5-5% by weight. If the concentration is higher than this, it is necessary to increase the temperature of the aqueous solution in accordance with the solubility. If the temperature of the aqueous solution is increased, the bulk specific gravity tends not to decrease, such being undesirable.
水溶性有機溶媒としては、低級アルコール、アセトンやエチルメチルケトン等のケトン類、ジオキサン等のエーテル類等が挙げられるが、取扱い易さの点から低級アルコールが好ましく用いられる。
低級アルコールとしては、メチルアルコール、エチルアルコール、ｎ−プロピルアルコール、イソプロピルアルコール、ｎ−ブチルアルコール、sec−ブチルアルコール、ｔ−ブチルアルコール等が挙げられるが、溶解性、コスト等の観点からメチルアルコール、エチルアルコール、イソプロピルアルコールが好ましく用いられる。
水溶液中の水溶性有機溶媒の濃度は約１〜１０重量％である。この濃度以上にすると硝酸アンモニウム粒子に添加する水溶液の量が少なくなり、均一に添加し難くなり好ましくない。水溶液を多く添加してもよいが、水溶性有機溶媒を必要以上に多く添加するだけであって好ましくない。
Examples of the water-soluble organic solvent include lower alcohols, ketones such as acetone and ethyl methyl ketone, ethers such as dioxane, and the like, but lower alcohols are preferably used from the viewpoint of ease of handling.
Examples of the lower alcohol include methyl alcohol, ethyl alcohol, n-propyl alcohol, isopropyl alcohol, n-butyl alcohol, sec-butyl alcohol, t-butyl alcohol, etc., but from the viewpoint of solubility, cost, etc., methyl alcohol, Ethyl alcohol and isopropyl alcohol are preferably used.
The concentration of the water-soluble organic solvent in the aqueous solution is about 1 to 10% by weight. If this concentration is exceeded, the amount of the aqueous solution added to the ammonium nitrate particles decreases, and it becomes difficult to add uniformly, which is not preferable. Although a large amount of the aqueous solution may be added, it is not preferable because the water-soluble organic solvent is only added more than necessary.
界面活性剤および水溶性有機溶媒を含む水溶液を得られた硝酸アンモニウム粒子に加える。加える水溶液の温度は約５０〜７０℃であり、水溶性有機溶媒を加えない場合に比較して低い温度にすることができる。温度が低くなると界面活性剤が析出するようになり、また高過ぎると嵩比重が小さくならない傾向になる。
水溶液の添加量は、乾燥硝酸アンモニウム粒子１００重量部あたり約０．５〜５重量部である。硝酸アンモニウム粒子に加える界面活性剤の量は約２５〜２５００ｐｐｍ、水溶性有機溶媒の量は約５０〜５０００ｐｐｍとなる。これらの添加量は少ないと嵩比重を小さくする効果が得難く、多過ぎてもそれに見合った効果は得られない。
An aqueous solution containing a surfactant and a water-soluble organic solvent is added to the resulting ammonium nitrate particles. The temperature of the aqueous solution to be added is about 50 to 70 ° C., and can be lowered as compared with the case where no water-soluble organic solvent is added. When the temperature is lowered, the surfactant is precipitated, and when it is too high, the bulk specific gravity tends not to be reduced.
The amount of aqueous solution added is about 0.5 to 5 parts by weight per 100 parts by weight of dry ammonium nitrate particles. The amount of the surfactant added to the ammonium nitrate particles is about 25 to 2500 ppm, and the amount of the water-soluble organic solvent is about 50 to 5000 ppm. If these addition amounts are small, it is difficult to obtain the effect of reducing the bulk specific gravity.
硝酸アンモニウム粒子に界面活性剤および水溶性有機溶媒を含む水溶液を加えた後、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て行われる。本発明の製造方法では、約９０℃以上に加熱して水分含有量を約０．２重量％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。温度を約９０℃以上としても水分含有量が約０．２重量％を超えていたり、水分含有量が約０．２重量％以下であっても温度が約９０℃未満であったりすると、硬さが十分とはならない傾向にある。また、温度が約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、通常は温度を約１２０℃以下とするのが好ましい。 An aqueous solution containing a surfactant and a water-soluble organic solvent is added to the ammonium nitrate particles, and then heated and dried. 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, This is done using a tunnel furnace. In the production method of the present invention, the water content is set to about 0.2% by weight or less by heating to about 90 ° C. or higher. You may dry to such an extent that moisture content is 0 and does not contain water substantially. If the water content exceeds about 0.2% by weight even if the temperature is about 90 ° C. or higher, or if the temperature is less than about 90 ° C. even if the water content is about 0.2% by weight or less, Tend not to be sufficient. Moreover, since the porous granular ammonium nitrate obtained will be easy to aggregate when temperature exceeds about 120 degreeC, it is usually preferable to make temperature into about 120 degrees C or less.
かくして得られる多孔質粒状硝酸アンモニウムの嵩比重は、硬度によって変わるが、同じ硬度で比較した場合、水溶性有機溶媒を添加しないで製造した従来の多孔質粒状硝酸アンモニウムに比べ、約０．０１〜０．０１５ｇ／ｃｍ3小さいものである。 The bulk specific gravity of the porous granular ammonium nitrate thus obtained varies depending on the hardness. However, when compared with the same hardness, the bulk specific gravity is about 0.01 to about 0.000 compared to the conventional porous granular ammonium nitrate produced without adding a water-soluble organic solvent. 015 g / cm 3 is small.
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。 The resulting porous granular ammonium nitrate 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, salts of linear aliphatic monoamines, magnesium aluminate silicate, ethylene bisstearamide, and alkaline earth metal salts of aliphatic carboxylic acids that are commonly used. Can be mentioned.
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。
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。
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（重量比）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。
EXAMPLES Hereinafter, although an Example demonstrates this invention in detail, this invention is not limited by this Example.
In addition, the porous granular ammonium nitrate obtained in the following examples was evaluated by the following method.
The hardness is large enough to pass through a 35 mesh (aperture 0.4 mm) sieve by applying an impact at a purge air pressure of 0.4 MPa (about 4 atm) to about 100 g of porous granular ammonium nitrate using a loading tester. It is the ratio (weight ratio) finely pulverized.
The bulk specific gravity was measured by the method described in JIS K-6721.
実施例１
自然通気型造粒塔を用いて塔頂から濃度９４重量％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重量％以下の硝酸アンモニウム粒子を得た。
水にオクタデシルアミン酢酸塩を２重量％、エチルアルコールを３重量％添加して７０℃で溶解して水溶液を得た。
この水溶液（６０℃）６ｇを上記の硝酸アンモニウム粒子３００ｇに噴霧して添加し、これを内径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℃まで昇温して水分含有量が約０．１重量％になるまで乾燥した。
得られた多孔質粒状硝酸アンモニウムの水分は０．１５８重量％、嵩比重は０．６１５ｇ／ｃｍ3、硬度は２６．２％であった。
更に３回、同様に行い多孔質粒状硝酸アンモニウムを得た。
結果を表１および図１に示す。
Example 1
Using a naturally ventilated granulation tower, water droplets were evaporated while dropping droplets of a 94 wt% ammonium nitrate aqueous solution (temperature about 150 ° C.) from the top of the tower to form a granular material, which was further dried to obtain a particle size of approximately 0 Ammonium nitrate particles having a water content of 0.1% by weight or less at 0.4 mm to 1.7 mm were obtained.
2% by weight of octadecylamine acetate and 3% by weight of ethyl alcohol were added to water and dissolved at 70 ° C. to obtain an aqueous solution.
6 g of this aqueous solution (60 ° C.) is sprayed and added to 300 g of the above ammonium nitrate particles, and this is put into a cylindrical drying container having an inner diameter of 400 mm, a length of 600 mm and a wall surface heated to 100 ° C., and the wall surface temperature is set to 100 ° C. While maintaining, the mixture was heated while rotating naturally at 4 revolutions per minute, and the ammonium nitrate particles were heated to 97 ° C. and dried until the water content became about 0.1% by weight.
The obtained porous granular ammonium nitrate had a water content of 0.158% by weight, a bulk specific gravity of 0.615 g / cm 3 and a hardness of 26.2%.
Further, the same procedure was repeated three times to obtain porous granular ammonium nitrate.
The results are shown in Table 1 and FIG.
比較例１
水にエチルアルコールを添加せず、オクタデシルアミン酢酸塩のみ２重量％を添加して８５℃まで加熱して溶解して水溶液を得た。
この水溶液（７５℃）を硝酸アンモニウム粒子に噴霧した以外は実施例１と同様に行った。
得られた多孔質粒状硝酸アンモニウムの水分は０．１５２重量％、嵩比重は０．６３１ｇ／ｃｍ3、硬度は２５．８％であった。
更に３回、同様に行い多孔質粒状硝酸アンモニウムを得た。
結果を表１および図１に示す。
Comparative Example 1
Without adding ethyl alcohol to water, only 2% by weight of octadecylamine acetate was added and heated to 85 ° C. to dissolve to obtain an aqueous solution.
The same procedure as in Example 1 was performed except that this aqueous solution (75 ° C.) was sprayed onto the ammonium nitrate particles.
The obtained porous granular ammonium nitrate had a water content of 0.152% by weight, a bulk specific gravity of 0.631 g / cm 3 and a hardness of 25.8%.
Further, the same procedure was repeated three times to obtain porous granular ammonium nitrate.
The results are shown in Table 1 and FIG.
図１から明らかなように、エチルアルコールを添加して行うことによって、同じ硬度でより小さい嵩比重の多孔質粒状硝酸アンモニウムを得ることができる。 As can be seen from FIG. 1, porous granular ammonium nitrate having the same hardness and a smaller bulk specific gravity can be obtained by adding ethyl alcohol.
Claims (7)
The production method according to claim 1, wherein the amount of the aqueous solution containing the surfactant and the water-soluble organic solvent added to the ammonium nitrate particles is 0.5 to 5 parts by weight with respect to 100 parts by weight of the ammonium nitrate particles.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GR1005557B (en) * | 2006-05-26 | 2007-06-12 | Κωνσταντινος Μουντζουριδης | Method for obtaining porous ammonium nitrate (nh4no3) |
| JP2009155153A (en) * | 2007-12-26 | 2009-07-16 | Daicel Chem Ind Ltd | Porous gunpowder and method for producing the same |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GR1005557B (en) * | 2006-05-26 | 2007-06-12 | Κωνσταντινος Μουντζουριδης | Method for obtaining porous ammonium nitrate (nh4no3) |
| JP2009155153A (en) * | 2007-12-26 | 2009-07-16 | Daicel Chem Ind Ltd | Porous gunpowder and method for producing the same |
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