JPS5935022A - Preparation of ammonium nitrate - Google Patents
Preparation of ammonium nitrateInfo
- Publication number
- JPS5935022A JPS5935022A JP14248282A JP14248282A JPS5935022A JP S5935022 A JPS5935022 A JP S5935022A JP 14248282 A JP14248282 A JP 14248282A JP 14248282 A JP14248282 A JP 14248282A JP S5935022 A JPS5935022 A JP S5935022A
- Authority
- JP
- Japan
- Prior art keywords
- ammonium nitrate
- ammonia
- melt
- contact
- value
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- PAWQVTBBRAZDMG-UHFFFAOYSA-N 2-(3-bromo-2-fluorophenyl)acetic acid Chemical compound OC(=O)CC1=CC=CC(Br)=C1F PAWQVTBBRAZDMG-UHFFFAOYSA-N 0.000 title claims abstract description 68
- 238000002360 preparation method Methods 0.000 title description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims abstract description 68
- 229910021529 ammonia Inorganic materials 0.000 claims abstract description 33
- 239000011261 inert gas Substances 0.000 claims abstract description 12
- 238000001816 cooling Methods 0.000 claims abstract description 5
- 239000000155 melt Substances 0.000 claims abstract description 5
- 239000007789 gas Substances 0.000 claims abstract 2
- 238000004519 manufacturing process Methods 0.000 claims description 6
- 238000002844 melting Methods 0.000 claims description 3
- 230000008018 melting Effects 0.000 claims description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims 1
- 239000007864 aqueous solution Substances 0.000 abstract description 5
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 7
- 238000006243 chemical reaction Methods 0.000 description 7
- 238000000034 method Methods 0.000 description 7
- 229910017604 nitric acid Inorganic materials 0.000 description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 7
- 239000002360 explosive Substances 0.000 description 4
- 230000000694 effects Effects 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- 239000007787 solid Substances 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- 229910002651 NO3 Inorganic materials 0.000 description 2
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 description 2
- 239000000654 additive Substances 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- 238000005469 granulation Methods 0.000 description 2
- 230000003179 granulation Effects 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 241000283986 Lepus Species 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 1
- 239000003570 air Substances 0.000 description 1
- PRORZGWHZXZQMV-UHFFFAOYSA-N azane;nitric acid Chemical compound N.O[N+]([O-])=O PRORZGWHZXZQMV-UHFFFAOYSA-N 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000000112 cooling gas Substances 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 238000004880 explosion Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 230000007794 irritation Effects 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 208000024891 symptom Diseases 0.000 description 1
- 238000011282 treatment Methods 0.000 description 1
Landscapes
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
Description
【発明の詳細な説明】
本発明は硝酸アンモニウム(以下硝安と略記する)の製
造方法に関し、詳しくはアンモニア含有量の少ない硝安
の爬造法に関する。DETAILED DESCRIPTION OF THE INVENTION The present invention relates to a method for producing ammonium nitrate (hereinafter abbreviated as ammonium nitrate), and more particularly to a method for producing ammonium nitrate with a low ammonia content.
硝安は硝酸とアンモニアとを反応させて製造はれるが、
硝安中に硝酸が存在すると、硝安が分解しやすく、また
爆発の危険性があるので、通常アンモニアが若干過剰と
なるようにして反応が行なわれて、この為一般に硝安は
微量のアンモニアを含有する。か\る硝安は、含水爆薬
、硝安油剤爆薬、ダイナマイト等の添加原$:1など爆
薬用として従来例の痛痒もなく多用されてきたが、近時
、耐固結性、非帯電性、分散性、倣動性等、多様かつ精
細な特性が要求されるに至り、硝安中にアンモニアが存
在すると、爆薬の調製時、種々の添加剤を配合した場合
、アンモニアが添加剤に作用を及ぼして所望の性能が得
られないとか、所望のpH値の製品が得られない等の不
都合を招くことが見出でれた。Ammonium nitrate is produced by reacting nitric acid and ammonia,
If nitric acid exists in ammonium nitrate, the ammonium nitrate will easily decompose and there is a risk of explosion, so the reaction is usually carried out with a slight excess of ammonia, and for this reason ammonium nitrate generally contains a trace amount of ammonia. . Ammonium nitrate has been widely used for explosives such as hydrous explosives, ammonium nitrate oil explosives, and dynamite without causing any pain or irritation. As a result, ammonia is required to have various and precise properties such as elasticity and conformability, and if ammonia is present in ammonium nitrate, when various additives are mixed during the preparation of explosives, the ammonia may have an effect on the additives. It has been found that this causes inconveniences such as not being able to obtain the desired performance or not being able to obtain a product with the desired pH value.
本発明者らは、硝安中のアンモニアを除去する方法につ
き種々研究を重ねた結果、固体の硝安に微量の硝酸を冷
加混合する方法はそのpl(制i卸がむずかしく工業的
に有利でないことを知得した。そして、固体の硝安は加
熱、減圧、通気あるい1171.それら全併用した処理
を行なっても、その硝安中のアンモニアを減少させるこ
とは困141Lであるのtc >Jt、、溶融している
硝安は、不活性ガスと接触させることによって、容易に
その硝安中のアンモニアが除去できることを見出し本発
明を完成した。As a result of various studies on methods for removing ammonia from ammonium nitrate, the present inventors found that the method of cooling and mixing solid ammonium nitrate with a small amount of nitric acid was found to be difficult to control and not industrially advantageous. I learned that solid ammonium nitrate is heated, depressurized, aerated, or all of these treatments are used in combination, but it is difficult to reduce the ammonia in the ammonium nitrate.tc > Jt. The present invention was completed based on the discovery that ammonia in molten ammonium nitrate can be easily removed by contacting it with an inert gas.
すなわち、本発明は、アンモニア含有量が少なく、工業
的価値の大きい硝安全製造することを目的とするもので
あシ、この目r白は、アンモニアを含有する硝安の融液
と、硝安に対して不活性なガスとを接触させて脱アンモ
ニアした後冷却固(ヒさせることによって達成される。That is, the purpose of the present invention is to safely produce a glass having a low ammonia content and a high industrial value. This is achieved by contacting with an inert gas to remove ammonia and then cooling to solidify.
以下、本発明の詳細な説明する。The present invention will be explained in detail below.
アンモニア全含有する硝安の融液としては、硝酸とアン
モニアとをアンモニアが若干過剰となるようにし−C反
応させて得た硝安の融液が代表的なものであるが、これ
に限られるものではなく、別途製造したアンモニアを含
有する固体の硝安全溶融したものでもよい。A typical ammonium nitrate melt containing all ammonia is an ammonium nitrate melt obtained by reacting nitric acid and ammonia with a slight excess of ammonia and C-C, but it is not limited to this. Instead, a separately produced solid sulfate containing ammonia may be used.
硝酸とアンモニアとの反応は発熱反応であり、通常反応
温度は硝安の融点以上となり反応生成物は溶融状、態で
あるので、本発明ではこれ全そのまま不活性ガスとの接
触処理に供するのが得唯である。The reaction between nitric acid and ammonia is an exothermic reaction, and the reaction temperature is usually higher than the melting point of ammonium nitrate, and the reaction product is in a molten state. It's a good deal.
アンモニアを含有する硝安の融液は、/θ屯Pi−係4
!T!Ifi4以下の水を含有していてもよい。水の含
量j’ 、DIがあまシに多いと、脱アンモニアが内錐
となる。好ましくは水含有附は3〜2重用%である。The ammonium nitrate melt containing ammonia is /θtun Pi−4
! T! It may contain water with an Ifi of 4 or less. When the water content j' and DI are too large, deammonization becomes an inner cone. Preferably, the water content is 3 to 2%.
硝安に利して不活性なガスとしては、空気、窒素、炭酸
ガスなどがあげられるが、1tn當空気で十分である。Examples of inert gases that are useful for ammonium nitrate include air, nitrogen, carbon dioxide, etc., but 1 ton of air is sufficient.
硝安の融液と不活性ガスとの接触は1種々のから不活性
ガス全向流または併流で流通させる方法、硝安の融液に
不活性ガスを気泡として流通させる方法などがあげられ
る。The contact between the ammonium nitrate melt and the inert gas can be carried out in various ways, including a method in which the inert gas is passed in full countercurrent or cocurrent flow, and a method in which the inert gas is passed through the ammonium nitrate melt in the form of bubbles.
硝安の融液と不活性ガスとの接触の際の温度は、硝安の
融点以上23θ°C以下の範囲から選ぶことができる。The temperature at which the ammonium nitrate melt and the inert gas are brought into contact can be selected from a range from the melting point of ammonium nitrate to 23θ°C.
例えば、はとんど水を含有しない硝安の場合は760〜
.230°C1好ましくは/70−コθ0 ’O程度、
水の含有量がjN鼠チ程度の硝安の鳴合は730〜.2
30 ’O,好ましくは//=θ〜200 ’o程度を
選ぶのがよい。For example, in the case of ammonium nitrate that does not contain much water, it is 760~
.. 230°C1 preferably about /70-koθ0'O,
The ringing height of ammonium nitric acid with a water content of about 730~. 2
30'O, preferably about //=θ~200'O.
温度が、230°Cよりも高くなると硝安の分解が起る
ようになるので好ましくない。If the temperature is higher than 230°C, decomposition of ammonium nitrate will occur, which is not preferable.
不活性ガスの使用量は、硝安/ kg当り標準状態で7
01以上、好ましくは2θ〜、xoot程IWである。The amount of inert gas used is ammonium nitrate/kg under standard conditions.
01 or more, preferably 2θ~, xoot IW.
この徴があまりに少ないと、アンモニア除去の効果が小
さくなる。逆に量が多いことは特に不都合はないが、多
くしたことによる特別の効果は期待できず、設備、熱的
な面などから得策ではない。If this symptom is too small, the effect of ammonia removal will be reduced. On the other hand, there is no particular disadvantage to having a large amount, but no special effect can be expected from increasing the amount, and it is not a good idea from the standpoint of equipment, heat, etc.
かくしてアンモニアを含有する硝安の融液と不活性ガス
とを接触させるときは、アンモニアをほとんど含まない
硝安の融液を得ることができるので、これを冷却固化し
て製品とする。In this way, when the ammonium nitrate melt containing ammonia is brought into contact with an inert gas, it is possible to obtain an ammonium nitrate melt containing almost no ammonia, which is then cooled and solidified to form a product.
冷却固化の方法としては、硝安の融液を哉拌機を有する
結晶機に導入し、攪拌しながら冷却して粉状硝安とする
方法、硝安の融液′fr:造粒塔の塔頂からスプレーし
、冷却用気体と接触をぜて粒状硝安とする方法などがあ
げられる。As a method of cooling and solidifying, ammonium nitrate melt is introduced into a crystallizer equipped with a stirrer and cooled while stirring to form ammonium nitrate powder.Ammonium nitrate melt 'fr: from the top of a granulation tower Examples include spraying and contacting with cooling gas to form granular ammonium nitrate.
本発明方法によるときは、容易な操作で効率よく硝安中
のアンモニアを除去することかでき、硝安全IO重量%
水溶液にして測足したp)−] 値が、9.θ以下とい
う理論値のり、5に近いものが得られ、か\るp)I値
り、5〜!uO1より好1しくはq、S〜L9というア
ンモニア含量が極小量の硝安は工業的製品として本発明
によって留めて供給することが可能となったものである
。When using the method of the present invention, ammonia in ammonium nitrate can be efficiently removed with easy operation, and the nitrate safety IO weight%
The p)-] value measured in an aqueous solution is 9. The theoretical value of θ or less is close to 5, and the p)I value is 5~! Ammonium nitrate having a minimal ammonia content, q, S to L9, which is more preferable than uO1, can be kept and supplied as an industrial product by the present invention.
そして、この様な硝安は前記した)t11’) % 工
業的利用の種々の局面において各科の条件に円滑に対応
することが可能であり、よって本発明はか\る工業的有
利な硝安全提供し、かつ、その製造方法を提供するもの
である。In addition, such ammonium nitrate can be smoothly adapted to various conditions in various aspects of industrial use, and therefore, the present invention can improve the industrially advantageous nitrate safety. and a method for manufacturing the same.
以下、実施例によって本発明を具体的に説明するが、本
発明はその要旨をこえない限!ll旬下の実施例に限定
てれるもので幻、ない。Hereinafter, the present invention will be specifically explained with reference to examples, but the present invention does not exceed its gist. It is limited to the current example and is not an illusion.
なJ3・、実施例中1%」は「−重用係」を示−す。J3・, 1% in Examples indicates "-Important person".
実施例/
乙3−条硝酸に1理論搦より約/係過剰のアンモニアガ
スを吹き込んで反応を行ないflRl、 D、e /
90℃の硝安の融液を得た。Example/Otsu 3-article Ammonia gas in excess of about 1 stoichiometry is blown into nitric acid to cause a reaction, flRl, D, e/
A melt of ammonium nitrate at 90°C was obtained.
この硝安の副I液は、水含有事り係で、10係水溶液と
して測定したp Hは3.9であった。This sub-I solution of ammonium nitrate contained water and had a pH of 3.9 when measured as a 10% aqueous solution.
この硝安のhi’l!液/θに9を内容田/Stのジャ
ケット加熱式の容器に仕込み、温度f / 7−+’e
に保ちながら標準状態でjθθlの空気を7時間かけて
吹き込み泡出させた。This is hi'l! Pour 9 into a jacket heating type container with inner field/St, and bring the temperature to f/7-+'e.
Air of jθθl was blown into the flask for 7 hours under standard conditions to cause bubbles to form.
次いでこの硝安の融液を、徐々に二+lQbパドル型結
晶機に移しながら、冷却固化させて粉状硝安を得た。Next, the ammonium nitrate melt was gradually transferred to a 2+1Qb paddle type crystallizer and cooled and solidified to obtain powdered ammonium nitrate.
得られた粉状硝安は70%水溶液としてpHを測定した
ところグ、7であった。The pH of the obtained ammonium nitrate powder was measured as a 70% aqueous solution and found to be 7.
実施例
充填層式反応塔に、にJ%硝酸および理論冴より絢、2
%過剰のアンモニアガスを導入しながら連続的に反応を
行なって、温度−〇〇“(3の硝安の融液を製造した。Example: In a packed bed type reaction tower, J% nitric acid and a theoretical value of 2.
The reaction was carried out continuously while introducing % excess ammonia gas to produce a melt of ammonium nitrate at a temperature of -3.
この硝安の融液は、水含有M、グチで、/θ係氷水溶液
しで測定したpHは乙、/であった。This ammonium nitrate melt contained water and had a pH of /θ as measured with an aqueous ice solution.
この硝安の融液/θθkg/ hr f多孔板り段か
らなる脱アンモニア塔の頂部(lこ供給して液滴としで
流下させながら、開基の下部から標準状態でj、θθθ
t/hrの空気を導入し、温度を・/りθ゛Cに保って
硝安の融液と空気とを自流接触をぜた。This ammonium nitrate melt/θθkg/hr was fed to the top of the deammonification tower consisting of a perforated plate stage (l) and allowed to flow down as droplets, while the ammonium nitrate melt was added to the top of the deammonification tower consisting of a perforated plate stage, and the ammonium nitrate melt was added from the bottom of the open group under standard conditions to j, θθθ
Air was introduced at a rate of t/hr, and the temperature was maintained at .theta.C to cause self-flow contact between the ammonium nitrate melt and the air.
塔底かも抜き出した硝安の融液を造粒塔に導き空気の流
通下(てスプレーして冷却固化させ、粒径θ。I〜/、
5胴の粒状硝安全面た。The ammonium nitrate melt extracted from the bottom of the tower is introduced into a granulation tower and sprayed under air circulation to cool and solidify the particle size θ.
5-barrel granulated glass safety face.
得られた粒状硝安は70%水溶液としてpHを測定した
ところ¥57であった。When the pH of the obtained granular ammonium nitrate was measured as a 70% aqueous solution, it was found to be 57 yen.
出願人 三菱化成工業株式会社 代理人 弁理士 長谷用 − (ほか7名) 189Applicant: Mitsubishi Chemical Industries, Ltd. Agent Patent Attorney Hase - (7 others) 189
Claims (3)
、硝酸アンモニウムに対して不活性なガスとを接触させ
て脱アンモニアした後冷却固化させることを特徴とする
硝酸アンモニウムの製造方法。(1) A method for producing ammonium nitrate, which comprises bringing a melt of ammonium nitrate containing ammonia into contact with a gas inert to ammonium nitrate to remove ammonia, and then cooling and solidifying it.
際の温度が、硝酸アンモニウムの融点以上1.230’
o以下である特許請求の範囲第(1)項記載の硝酸アン
モニウムの製造方法。(2) The temperature at which the ammonium nitrate melt and the inert gas come into contact is 1.230' above the melting point of ammonium nitrate.
The method for producing ammonium nitrate according to claim (1), wherein the ammonium nitrate is less than or equal to o.
θを以):(標準状態)流通させて接触2行なう特許請
求の範囲第(11項または第(2)項記載(D (it
’J fW/アンモニウムの製造方法。(3) Add inert gas to ammonium nitrate/kg/
θ): (Standard state) Flowing and contacting 2 (D (it
'J fW/Method for producing ammonium.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP14248282A JPS5935022A (en) | 1982-08-17 | 1982-08-17 | Preparation of ammonium nitrate |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP14248282A JPS5935022A (en) | 1982-08-17 | 1982-08-17 | Preparation of ammonium nitrate |
Publications (2)
Publication Number | Publication Date |
---|---|
JPS5935022A true JPS5935022A (en) | 1984-02-25 |
JPH0424287B2 JPH0424287B2 (en) | 1992-04-24 |
Family
ID=15316342
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
JP14248282A Granted JPS5935022A (en) | 1982-08-17 | 1982-08-17 | Preparation of ammonium nitrate |
Country Status (1)
Country | Link |
---|---|
JP (1) | JPS5935022A (en) |
Families Citing this family (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
WO2011019070A1 (en) * | 2009-08-13 | 2011-02-17 | 株式会社ワコール | Garment with crotch |
-
1982
- 1982-08-17 JP JP14248282A patent/JPS5935022A/en active Granted
Non-Patent Citations (1)
Title |
---|
THE NITROGEN INDUSTRY=1976 * |
Also Published As
Publication number | Publication date |
---|---|
JPH0424287B2 (en) | 1992-04-24 |
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