JPS59169914A - Production of ammonium sulfamate - Google Patents
Production of ammonium sulfamateInfo
- Publication number
- JPS59169914A JPS59169914A JP4127983A JP4127983A JPS59169914A JP S59169914 A JPS59169914 A JP S59169914A JP 4127983 A JP4127983 A JP 4127983A JP 4127983 A JP4127983 A JP 4127983A JP S59169914 A JPS59169914 A JP S59169914A
- Authority
- JP
- Japan
- Prior art keywords
- ammonium
- liquid
- sulfamate
- liquid phase
- waste water
- 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.)
- Pending
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B21/00—Nitrogen; Compounds thereof
- C01B21/082—Compounds containing nitrogen and non-metals and optionally metals
- C01B21/087—Compounds containing nitrogen and non-metals and optionally metals containing one or more hydrogen atoms
- C01B21/093—Compounds containing nitrogen and non-metals and optionally metals containing one or more hydrogen atoms containing also one or more sulfur atoms
- C01B21/096—Amidosulfonic acid; Salts thereof
Abstract
Description
【発明の詳細な説明】
この発明は、コークス炉の湿式脱硫工程から排出される
脱硫廃液中の、チオ硫酸アンモニウム。DETAILED DESCRIPTION OF THE INVENTION The present invention relates to ammonium thiosulfate in desulfurization waste liquid discharged from a wet desulfurization process of a coke oven.
硫黄酸素酸アンモニウム（以下、チオ硫酸アンモニウム
等といつ）から、スルファミン酸アンモニウムを製造す
る方法に関する。The present invention relates to a method for producing ammonium sulfamate from ammonium sulfur oxyate (hereinafter referred to as ammonium thiosulfate, etc.).
コークス炉ガス中には、通常シアン化水素１．０〜１．
３ｇ／ＮＷＬ３．硫化水素４〜９ ｇ／Ｎｍ３．アンモ
ニア８〜１０ｆＩ／Ｎｍ３などの成分が含まれているの
で、公害防止上、これらを除去し、精製ガスとして燃料
等に供用している。Coke oven gas usually contains 1.0 to 1.0% hydrogen cyanide.
3g/NWL3. Hydrogen sulfide 4-9 g/Nm3. Since it contains components such as 8 to 10 fI/Nm3 of ammonia, these are removed to prevent pollution and used as purified gas for fuel, etc.
上記シアン化水素、硫化水素の除去方法としては、キノ
ン糸触媒を使用するタカハックス法、ピクリン酸触媒を
使用するフマックス法などが、湿式脱硫法と呼ばれて、
広く実用化されている。Methods for removing hydrogen cyanide and hydrogen sulfide include the Takahax method using a quinone thread catalyst and the Fumax method using a picric acid catalyst, which are called wet desulfurization methods.
It has been widely put into practical use.
これら湿式脱硫法によって、シアン化水素ないし硫化水
素を吸収して、脱硫工程から排出されるいわゆる脱硫廃
液中には、通常、チオシアン酸アンモニウム６０〜２０
０ｆ／１！ 、チオ硫酸アンモニウム等５０〜２００ｇ
／’１１ 粉度が含有されているほか、前記脱硫触媒が
含有されていて深赤色ないし゛濃褐色を呈している。こ
の脱硫廃液は、上記イｊ価成分を含有しているとは云え
、そ′の回収が高価につくので、活性汚泥法によって無
害化したのち河海に放流するか、濃縮後焼却し、その燃
焼排ガスから、せいぜいＳ０２をｆ？ｆ Ｒｅや石・）
：ｆの形で回収するにすぎない。この回収物は安価であ
り乍ら、回収設備は高価であるから、有利な脱硫廃液の
利用方法とは云い鈍い。チオ硫酸アンモニウムの利用法
として、特公昭４５−’８０９５号記載の発明では、ヂ
オ硫南アンモニウムと遊離のアンモニア８モル／ＩＩ
以上を含む水溶液を１００〜１１０°Ｃで、酸素圧７
５１ｃｑ／ｃｍ２で液相酸化することによってスルファ
ミン酸アンモニウムの製造を提案しているが、その明細
ｄ）に示される出発原料は何れも、チオシアン酸アンモ
ニウムを含まない溶液であって、湿式ｊ児硫廃液中のチ
オ硫酸アンモニウムを折角該法でスルファミン酸アンモ
ニウムに転化させても、共存するチオシアン酸アンモニ
ウムと分離することが困難であるという難点がｔ、す、
湿式脱硫廃液Ｇ−そのま一適用することは出来ない。By these wet desulfurization methods, hydrogen cyanide or hydrogen sulfide is absorbed, and the so-called desulfurization waste liquid discharged from the desulfurization process usually contains 60 to 20% ammonium thiocyanate.
0f/1! , ammonium thiosulfate, etc. 50-200g
/'11 In addition to containing fineness, it also contains the desulfurization catalyst, giving it a deep red to deep brown color. Although this desulfurization waste liquid contains the above-mentioned I-value components, it is expensive to recover, so it is either rendered harmless by the activated sludge method and then discharged into rivers and seas, or it is concentrated and then incinerated. From combustion exhaust gas, at most S02 is f? f Reya stone)
: It is simply recovered in the form of f. Although this recovered product is inexpensive, the recovery equipment is expensive, so it is not an advantageous method of utilizing the desulfurization waste liquid. As a method of utilizing ammonium thiosulfate, in the invention described in Japanese Patent Publication No. 1983-8095, ammonium diosulfate and free ammonia 8 mol/II
An aqueous solution containing the above was heated at 100 to 110°C with an oxygen pressure of 7.
The company proposes the production of ammonium sulfamate by liquid phase oxidation at 51 cq/cm2, but the starting materials shown in specification d) are all ammonium thiocyanate-free solutions and cannot be processed by wet oxidation. Even if ammonium thiosulfate in the waste liquid is converted to ammonium sulfamate by this method, the problem is that it is difficult to separate it from the coexisting ammonium thiocyanate.
Wet desulfurization waste liquid G - cannot be applied as is.
本発明は如上観点から、処分に窮する湿式脱硫廃液中の
チオ硫酸アンモニウム等に着目し、これをスルファミン
酸アンモニウムとして回収する合理的な方法を提供する
ものであって、上述した湿式脱硫廃液中の脱硫触媒を除
去したのち、酸化触媒の存在下、遊離アンモニアの濃度
を２モル／ｌにＷ１１整し、酸素加圧下に、まず約１０
０°Ｃ前後で液相酸化し、それによってチオ硫酸アンモ
ニウム等をスルファミン酸生成率、ニウムに転化し、つ
いで反応温度を１８０°Ｃ前後に昇温して、引きつ！い
て液相酸化し、それによってチオシアン酸アンモニウム
を硫酸アンモニウムに酸化分解し、得られた酸化分解後
の反応液から、相互溶解度の差を利用して硫酸アンモニ
ウムを固相分離し、分離された液相から、スルファミン
酸アンモニウムを回収する方法である。From this perspective, the present invention focuses on ammonium thiosulfate, etc. in the wet desulfurization waste liquid, which is difficult to dispose of, and provides a rational method for recovering this as ammonium sulfamate. After removing the desulfurization catalyst, the concentration of free ammonia was adjusted to 2 mol/l in the presence of an oxidation catalyst, and the concentration of free ammonia was adjusted to about 10 mol/l under oxygen pressure.
Liquid phase oxidation is carried out at around 0°C, thereby converting ammonium thiosulfate, etc. to sulfamic acid production rate and nium, and then the reaction temperature is raised to around 180°C, and then! ammonium thiocyanate is oxidatively decomposed into ammonium sulfate, ammonium sulfate is separated in the solid phase from the resulting reaction solution after oxidative decomposition by utilizing the difference in mutual solubility, and ammonium sulfate is separated from the separated liquid phase. , is a method for recovering ammonium sulfamate.
本発明方法がｉｌｈ用される湿式脱硫廃液とは、既述し
たコークス炉ガスのタカハックス法（髄公昭３９−１０
１５号）もしくけ７マツクス法（特公昭３３−７０８４
号）などの脱硫廃液を指称する。この廃液中には、チオ
シアン酸アンモニウム、チオ（＋ＷＨ’ｉ？アンモニウ
ム等のほかに、０．５％未満のピクリン酸、ナフトキノ
ンスルフォン酸等の脱°硫触媒が含まれている。本発明
方法では、まずこの触媒を除去するのであるが、除去手
段としては、活性炭吸着法が実用的である。即ち、廃液
に対し、粉末状活性炭ｘｓｙ／ｌ稈度添加し、常温下数
分攪拌後、これを戸去すればよい。得られたρ液は淡黄
色透明である。もしも、触媒を除去することなく、酸化
工程を実施すれば、最終製品たるスルファミン酸アンモ
ニウムも亦着色してくるので、その精製が面倒となる。The wet desulfurization waste liquid to which the method of the present invention is applied is the Takahax method of coke oven gas described above (Mino Kosho 39-10).
No. 15) Moshike 7 Max Method (Special Publication No. 33-7084
This refers to desulfurization waste liquid such as No. This waste liquid contains not only ammonium thiocyanate and thio(+WH'i?ammonium), but also less than 0.5% of desulfurization catalysts such as picric acid and naphthoquinone sulfonic acid. First, this catalyst is removed, and the activated carbon adsorption method is a practical method for removing it.That is, xsy/l powdered activated carbon is added to the waste liquid, and after stirring for several minutes at room temperature, this The ρ solution obtained is pale yellow and transparent.If the oxidation step is carried out without removing the catalyst, the final product, ammonium sulfamate, will also become colored. Refining becomes troublesome.
本発明方法にあっては、ついでｒ液中のアンモニア量を
２モル／１以上に調整する。調整と述べたの沙、ρ液中
にアンモニアが含有されている場合には、その緻をも考
慮してという程の意味であるが、通常は、その量は極め
て微量であるので、実際にはアンモニアを添加すること
になろう。その量が２モル／ｅ以上というのけ、廃液中
のチオ硫酸濃度が、はぼ０．５〜１．０モル／ｌで下式
に示すとおり、遊離アンモニアはその２倍モル必要であ
るからである。In the method of the present invention, the amount of ammonia in the r liquid is then adjusted to 2 mol/1 or more. When I say "adjustment", I mean that if ammonia is contained in the rho solution, we should take into consideration its density, but normally the amount is extremely small, so in reality would add ammonia. Although the amount is 2 mol/e or more, the concentration of thiosulfate in the waste liquid is approximately 0.5 to 1.0 mol/l, and as shown in the formula below, twice the amount of free ammonia is required. It is.
（ＮＨ４）２Ｓ２０３ ＋ ２０２ ＋ ２ＮＨ３＋
Ｈ２Ｏ−ｖ ２（ＮＨ４）２Ｓ０４遊７４ｆアンモニア
の添加量は、多いほどスルファミン酸生成率が向上する
ので望ましいか、８〜１４モル／ｌ程度が実際的である
。アンモニアに代えて、水酸化ナトリウムや水酸化カル
シウムのような他のアルカリを使用しても、チオ硫酸ア
ンモニウム等のスルファミン酸の転化率は向上するが、
酸化反応後の反応液から、スルファミン酸以外の成分を
合理的に分離回収し雌い。(NH4)2S203 + 202 + 2NH3+
The amount of H2O-v2(NH4)2S04 free 74f ammonia to be added is preferably about 8 to 14 mol/l, since the larger the amount, the higher the sulfamic acid production rate. Using other alkalis such as sodium hydroxide or calcium hydroxide in place of ammonia also improves the conversion of sulfamic acids such as ammonium thiosulfate, but
Components other than sulfamic acid are rationally separated and recovered from the reaction solution after the oxidation reaction.
既述した通り、本発明液相酸化工程は、チオ硫酸アンモ
ニウム等ヲスルファミン酸アンモニウムに酸化する前段
工程と、こ＼に得られたスルファミン酸アンモニウムと
チオシアン酸アンモニウムとの混合溶液を、さらに湿式
酸化してチオシアン酸アンモニウムを硫酸アンモニウム
＼１に酸化する後段工程とに分けられるのであるが、そ
れは両工程が最適条件を異にするがためである。As mentioned above, the liquid phase oxidation process of the present invention includes a first step of oxidizing ammonium thiosulfate to ammonium sulfamate, and a further wet oxidation of the resulting mixed solution of ammonium sulfamate and ammonium thiocyanate. The process is divided into a subsequent step in which ammonium thiocyanate is oxidized to ammonium sulfate\1, and this is because the optimal conditions for both processes are different.
とくに後＆ 酸化は、スルファミン酸アンモニウムの分
解が少く、シかもチオシアン酸アンモニウムの硫酸アン
モニウムへの転化の早い条件を選択しなければならない
。In particular, post-oxidation conditions must be selected so that the decomposition of ammonium sulfamate is small and the conversion of ammonium thiocyanate to ammonium sulfate is quick.
本発明方法において、液相酸化というのは、オートクレ
ーブのような密閉容器内においで、加圧下に攪拌しっ！
反応を行わしめることをハ、味し、加圧条件は、前後段
とも同じ＜ １０ｋｇ １０１１２前後で充分である。In the method of the present invention, liquid phase oxidation is carried out in a closed container such as an autoclave and stirred under pressure.
To ensure that the reaction takes place, it is sufficient that the pressurization conditions are the same for both the front and rear stages, <10 kg <10112.
温度条件は、前段が１００±２０’Ｃ前後、後段が２０
０部５０°Ｃ程度が望ましい。The temperature conditions are around 100±20'C in the first stage and 20°C in the second stage.
The temperature is preferably about 50°C.
上述した２段の酸化を行った後の反応液は、スルファミ
ン酸アンモニウムと硫酸アンモニウムとの混合液である
。したがって本発明では両者の相互溶解度の差、例えば
濃縮などの操作によって、両者を分離するのである。さ
きの後段液相酸化の反応温度は１８０°Ｃ前後の高温で
あるので、これを濃縮しながら７０〜８０ ′Ｃ程度に
冷却することによって、まず溶解度の低い硫酸アンモニ
アを晶出させ、これを１５別することによってスルファ
ミン酸アンモニウムの含有量の高い水溶液を得ることが
できる。The reaction solution after performing the two-stage oxidation described above is a mixed solution of ammonium sulfamate and ammonium sulfate. Therefore, in the present invention, the two are separated based on the difference in their mutual solubility, for example, by operations such as concentration. The reaction temperature of the latter stage liquid phase oxidation is a high temperature of around 180°C, so by cooling it to around 70-80'C while concentrating it, ammonia sulfate with low solubility is first crystallized, and then this is An aqueous solution with a high content of ammonium sulfamate can be obtained by separating the mixture into 15 parts.
晶析分熱した硫酸アンモニウムは、再結晶法。Ammonium sulfate that has been crystallized is recrystallized.
硫酸分解法などの公知操作を加えることによって容易に
肥料規格を充足する品質の硫酸アンモニウムとして回収
することができる。しかし、コークス炉ガス精製工程中
に副生硫安製造設備が設けられている場合には、この設
備の中へ導入して、本来の副生硫安の一部に組み入れて
しまうがよい。By adding known operations such as sulfuric acid decomposition method, ammonium sulfate of a quality that satisfies fertilizer standards can be easily recovered. However, if by-product ammonium sulfate production equipment is provided during the coke oven gas purification process, it is better to introduce it into this equipment and incorporate it into a part of the original by-product ammonium sulfate.
硫酸アンモニウムを分離したあとの溶液から、目的とす
るスルファミン酸アンモニウムヲ回収するには、冷却、
濃縮等の手段を併用して効率的にスルファミン酸アンモ
ニアを晶出せしめ沖別同収するのである。To recover the desired ammonium sulfamate from the solution after separating ammonium sulfate, cooling,
By using means such as concentration, ammonia sulfamate is efficiently crystallized and collected at the same time.
実施例
７マツクス法脱硫廃液に、粉末活性炭を１５ｆ／１添加
攪拌後沖別して、淡黄色透明なｒ液を得た。Example 7 15 f/1 powdered activated carbon was added to the Maxx process desulfurization waste liquid, stirred, and separated to obtain a pale yellow and transparent R liquid.
このものは、ＮＨ４ＳＣＮ ０．９９３ ％ ル／ （
１、（ＮＨ４）２ｓ０３０．４９０モル／ｌを含有して
いた。This stuff contains NH4SCN 0.993% le/(
1, (NH4)2s030.490 mol/l.
このものに、触媒としてｃｓｓｏ４ 、 ＺｎＳＯ４を
それぞれ０．０５モル／ｌ添加し、がっＮＨ３を添加し
て、その濃度を１４モル／ｌに調整して反応液とした。To this, csso4 and ZnSO4 were added as catalysts at 0.05 mol/l each, and NH3 was added to adjust the concentration to 14 mol/l to prepare a reaction solution.
この反応液５００ ｒｔｔｌを、容積２．ＯＩ！の攪拌
機っきチタン製オートクレーブに入れて、第１段の液相
酸化に服せしめた。該酸化条件は、温度１００°±５°
Ｃ１常圧換算酸素圧力１０±１ｋｑ／ｃｍ２． ｆｆｔ
拌機０回転数を４００Ｔ−Ｐ−ｍで、反応時間は１２０
分でる。500 rttl of this reaction solution was added to a volume of 2. OI! The sample was placed in a stirrer-plated titanium autoclave and subjected to the first stage liquid phase oxidation. The oxidation conditions are a temperature of 100°±5°
C1 Normal pressure equivalent oxygen pressure 10±1kq/cm2. fft
The 0 rotation speed of the stirrer was 400 T-P-m, and the reaction time was 120
I understand.
この間３０分毎にサンプリングして５２０３ＳＯ３ＮＨ
２１３よび５ＣＮ−の濃度を測定した。During this period, sample every 30 minutes and 5203SO3NH
The concentrations of 213 and 5CN- were measured.
つぎに第２段の液相酸化に服せしめるため、器内温度を
１８０部５°Ｃに昇温すると共に、攪拌機の回転数をも
１１０００ｒ−ｐ−に高めた。酸素圧力は、依然１０±
１ｋｇ／（７）２に維持した。反応によって００２が発
生するので３０分毎にガス抜きを行い、また３０分毎に
サンプリングを行って５Ｏ３ＮＨ２およびＳＣＮ 濃
度を測定した。Next, in order to subject the mixture to the second stage of liquid phase oxidation, the temperature inside the vessel was raised to 180 parts at 5°C, and the rotational speed of the stirrer was also increased to 11,000 rpm. Oxygen pressure is still 10±
It was maintained at 1 kg/(7)2. Since 002 is generated by the reaction, degassing was performed every 30 minutes, and sampling was performed every 30 minutes to measure the 5O3NH2 and SCN concentrations.
上記測定した各成分濃度と経過時間への関係は、第１図
に示した通りである。この図から明らかな通り、約１０
０分間で（ＮＨ４）２５２０３は完全に酸化消失し、Ｎ
Ｈ４ＳＣＮは、８０分間の第２段の液相酸化段において
酸化消失する。The relationship between the concentration of each component measured above and the elapsed time is as shown in FIG. As is clear from this figure, approximately 10
In 0 minutes, (NH4)25203 is completely oxidized and disappeared, and N
H4SCN is oxidized and lost in the second liquid phase oxidation stage for 80 minutes.
２１２階の上記液相１ψ化終了後の内容液を分析したと
ころ、５Ｏ３ＮＨ２０，５１０モル／ｌ 、 ＳＣＮ
Ｏ，０１４モル／ ｌ、 ５０４ １．．５４モル／
ｌであった。したがって、５Ｏ３ＮＨ２の選択率は５２
．０４％、 ５ＣＮ−の分解率は９８％以上という好成
績である。Analysis of the content liquid on the 212th floor after completing the liquid phase conversion to 1ψ revealed that 5O3NH20,510 mol/l, SCN
O, 014 mol/l, 504 1. ．． 54 mol/
It was l. Therefore, the selectivity of 5O3NH2 is 52
．． 04%, and the decomposition rate of 5CN- was over 98%, which is a good result.
このような酸化後の反応液、つまりスルファミン酸アン
モニウム−硫酸アンモニウム沖合溶液５０００部をとり
、これに常法通りキレート樹脂を添加して、金属類を除
去したのち、７０°Ｃで減圧濃縮し、スルファミン酸ア
ンモニウム２９１部、硫酸アンモニウム１０２３部、水
７８部を含む溶＃１３９２部を得た。Take 5000 parts of the reaction solution after such oxidation, that is, the ammonium sulfamate-ammonium sulfate offshore solution, add a chelate resin to it in the usual manner to remove metals, and then concentrate under reduced pressure at 70°C to obtain sulfamine. A solution #1,392 containing 291 parts of ammonium acid, 1,023 parts of ammonium sulfate, and 78 parts of water was obtained.
ついで、同じ７０ ”Ｃで遠心分離することによって粗
結晶硫酸アンモニウム（その内訳は、スルファミン酸ア
ンモニウム３０部、硫酸アンモニウム１００．４部、水
２０部）’１０５４部と、−液（その内訳は、スルファ
ミン酸アンモニウム２６１部、硫隋アンモニウム１９部
、水５９部）３３９部を得た。Then, by centrifuging at the same 70"C, 1054 parts of crude crystalline ammonium sulfate (30 parts of ammonium sulfamate, 100.4 parts of ammonium sulfate, 20 parts of water) and 1054 parts of crude crystalline ammonium sulfate (30 parts of ammonium sulfamate, 100.4 parts of ammonium sulfate, 20 parts of water) 339 parts of ammonium (261 parts of ammonium, 19 parts of ammonium sulfate, 59 parts of water) were obtained.
この遠心分用ト沖液を３０℃に冷却することによって晶
析して来た結晶を沖別分離し乾燥した。このものは、純
度９７．０％のスルファミン酸アンモニウムの１３５部
であった。晶析物を沖別した諷液の量は１９９部であっ
て、その組成は、スルファミン酸アンモニウム１３０部
、硫酸アンモニウム１５部、水５４部であった。このも
のは、前記減圧濃縮工程、もしくは液相酸化工程へ返戻
して回収することができる。The centrifugal liquid was cooled to 30°C, and the crystals were separated and dried. This was 135 parts of ammonium sulfamate with a purity of 97.0%. The amount of liquid obtained by separating the crystallized product was 199 parts, and its composition was 130 parts of ammonium sulfamate, 15 parts of ammonium sulfate, and 54 parts of water. This material can be recovered by returning to the vacuum concentration step or liquid phase oxidation step.
なお、粗コークス炉ガスの湿式脱硫が、タカ／・ツクス
法によって行われた場合の脱硫廃液についても、上記フ
マックス法脱硫廃液の場合と、全く同様にしてスルファ
ミン酸アンモニウムを取ｉすることができた。In addition, ammonium sulfamate can be obtained from the desulfurization waste liquid obtained when wet desulfurization of crude coke oven gas is carried out by the Taka/Tokus method in exactly the same manner as in the case of the desulfurization waste liquid using the FMAX method. Ta.
添付第１図は、実施例記載の、液相酸化経過時間におけ
る分析値および温度を示す実測図である。
出願人 住金化工株式会社
代理人 弁理土石間壬生弥
（ほか１名）
第１図
一経過癖却浴）Attached FIG. 1 is an actual measurement diagram showing analytical values and temperatures during the elapsed time of liquid phase oxidation described in Examples. Applicant: Sumikin Chemical Co., Ltd. Agent: Patent Attorney Mibuya Tsuchishima (and 1 other person) Figure 1.
Claims (1)
廃液中の脱硫触媒を除去したのち、自交イし触媒の存在
下、辺ｆＩＭアンモニア濃度を２モル／β以上に調整し
、酸素加圧下に、液相酸イヒして、チオ硫酸アンモニウ
ムおよび硫黄酸素酸アンモニウムをスルファミン酸アン
モニウムに転化し、ついで１８０°Ｃ前後に昇温して、
引続き液相酸化して、チオシアン酸アンモニウムを硫酸
アンモニウムに酸化分解し、酸化分解後の反応液から、
相ｈ：浴解・（の差により（祇（調アンモニウムを分離
したのち、ルファミン酸アンモニウムを回収することを
特徴とするスルファミン酸アンモニウムの製造力法After removing the desulfurization catalyst from the wet desulfurization waste liquid discharged from the wet desulfurization process of coke oven gas, the side fIM ammonia concentration was adjusted to 2 mol/β or more in the presence of an autocrossing catalyst, and the mixture was heated under oxygen pressure. , convert ammonium thiosulfate and ammonium sulfur oxyate to ammonium sulfamate by immersion in liquid phase, and then raise the temperature to around 180°C,
Subsequently, ammonium thiocyanate is oxidatively decomposed into ammonium sulfate by liquid phase oxidation, and from the reaction liquid after oxidative decomposition,
Phase h: A method for producing ammonium sulfamate, which is characterized by recovering ammonium sulfamate after separating ammonium in a bath.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP4127983A JPS59169914A (en) | 1983-03-11 | 1983-03-11 | Production of ammonium sulfamate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP4127983A JPS59169914A (en) | 1983-03-11 | 1983-03-11 | Production of ammonium sulfamate |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPS59169914A true JPS59169914A (en) | 1984-09-26 |
Family
ID=12604005
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP4127983A Pending JPS59169914A (en) | 1983-03-11 | 1983-03-11 | Production of ammonium sulfamate |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS59169914A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US7807124B2 (en) * | 2006-07-13 | 2010-10-05 | Carbodeon Ltd. Oy | Carbon nitride preparation method |
| CN108779008A (en) * | 2016-03-11 | 2018-11-09 | 株式会社片山化学工业研究所 | The inorganic agent of cyanide containing wastewater and the method for handling cyanide containing wastewater with it |
-
1983
- 1983-03-11 JP JP4127983A patent/JPS59169914A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US7807124B2 (en) * | 2006-07-13 | 2010-10-05 | Carbodeon Ltd. Oy | Carbon nitride preparation method |
| CN108779008A (en) * | 2016-03-11 | 2018-11-09 | 株式会社片山化学工业研究所 | The inorganic agent of cyanide containing wastewater and the method for handling cyanide containing wastewater with it |
| CN108779008B (en) * | 2016-03-11 | 2021-08-24 | 株式会社片山化学工业研究所 | Cyanide-containing wastewater treatment agent and method for treating cyanide-containing wastewater by using same |
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