JPH0679708B2 - Treatment method of desulfurization waste liquids - Google Patents
Treatment method of desulfurization waste liquidsInfo
- Publication number
- JPH0679708B2 JPH0679708B2 JP60189819A JP18981985A JPH0679708B2 JP H0679708 B2 JPH0679708 B2 JP H0679708B2 JP 60189819 A JP60189819 A JP 60189819A JP 18981985 A JP18981985 A JP 18981985A JP H0679708 B2 JPH0679708 B2 JP H0679708B2
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- Japan
- Prior art keywords
- desulfurization waste
- desulfurization
- waste liquid
- cement
- raw material
- 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.)
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Description
【発明の詳細な説明】 ［産業上の利用分野］ この発明は、脱硫廃液類の無害化処理方法に係り、特
に、セメント製造原料予熱仮焼工程に於ける高温排ガス
及びセメント原料・予熱仮焼工程で生成する酸化カルシ
ウムを利用する脱硫廃液の無害化処理方法に関する。Description: TECHNICAL FIELD The present invention relates to a method for detoxifying desulfurization waste liquor, and particularly to high-temperature exhaust gas and cement raw material / preheating calcination in a preheating and calcination process of a cement manufacturing raw material. The present invention relates to a method for detoxifying a desulfurization waste liquid using calcium oxide produced in a process.
［従来の技術］ 石油化学工業、石炭化学工業及び都市ガス工業に於い
て、製造されている燃料ガス及び副生されるオフガスに
は公害規制の対象となる硫化水素、シアン、アンモニア
及びSOxが含まれていることが多く、通常、利用に先だ
ちアルカリを用いた脱硫プロセスで処理されている。こ
の処理の際、プロセス運転の安定維持（閉塞防止等）及
び効率的脱硫の保持の観点から脱硫作動液の一部がパー
ジ液、即ち脱硫廃液として抜き出されている。一般に、
この脱硫廃液はCOD値が非常に高く、且つ酸化硫黄化合
物、チオシアン酸塩等が含まれていることから、自然流
水域へ放流する前に何等かの処理が必要である。[Prior Art] In the petrochemical industry, coal chemical industry, and city gas industry, the fuel gas produced and the off gas produced as a by-product include hydrogen sulfide, cyanide, ammonia, and SOx that are subject to pollution control. In most cases, they are usually treated with a desulfurization process using an alkali prior to use. At the time of this treatment, a part of the desulfurization working liquid is extracted as a purge liquid, that is, a desulfurization waste liquid, from the viewpoint of maintaining stable operation of the process (blocking prevention, etc.) and maintaining efficient desulfurization. In general,
Since this desulfurization waste liquid has a very high COD value and contains a sulfur oxide compound, thiocyanate, etc., some treatment is required before it is discharged into the natural flowing water area.
従来、このような脱硫廃液を無害化する方法としては、
空気率１以下にて還元分解を行い、廃液中に含まれてい
るアルカリを回収して、脱硫プロセスにリサイクルする
還元分解法、湿式酸化して硫安及び硫酸とする湿式酸化
法、酸化燃焼して硫酸とする方法、希釈して活性汚泥法
で処理する方法及び苛性ソーダ又は炭酸ソーダ存在下酸
化燃焼する方法等が実施されている。Conventionally, as a method of detoxifying such desulfurization waste liquid,
Reductive decomposition is performed at an air ratio of 1 or less, and alkali contained in the waste liquid is recovered and recycled to a desulfurization process, a wet oxidation process that wet-oxidizes ammonium sulfate and sulfuric acid, and oxidative combustion is performed. A method of using sulfuric acid, a method of diluting and treating with an activated sludge method, a method of oxidizing and burning in the presence of caustic soda or sodium carbonate, and the like are carried out.
［発明が解決しようとする問題点］ しかしながら、上記各処理方法には夫々問題がある。即
ち、還元分解法には処理すべき脱硫廃液に含まれている
脱硫プロセスに有効なアルカリ分を回収できるという利
点があるものの、還元分解時に多量の燃料が必要な上
に、副生する分解ガス中に硫化水素ガスが含まれている
為、付加的な脱硫設備が必要とされる等、プロセス経済
性の観点から見ると改善の余地がある。湿式酸化法は、
アルカリ源としてアンモニアを利用した脱硫プロセスの
廃液に適用されるものであるが、高温で腐蝕性の硫酸を
取扱う為設備費が高く、且つ回収されるものが硫安と希
硫酸の混合物であり、回収されるものそれ自体では市販
出来るものではなく、通常、アンモニアを用いた硫安飽
和槽、硫安晶析槽及び硫安乾燥設備を備えた一連の設備
を処理システムに組み込む必要があり、システムが複雑
であるという問題点を抱えている。酸化燃焼して硫酸と
する方法は、アルカリ源としてアンモニアを用いる脱硫
プロセスの廃液に適用されているものであり、酸化燃焼
に当り、処理すべき廃液の濃縮プロセスがプロセス経済
上必須であることと、システム内で取扱う流体が腐蝕性
の強い硫酸である為、修繕にかなりの費用がかかるこ
と、更に、回収硫酸の品質が悪いという問題点があっ
た。活性汚泥法は、脱硫廃液を直接処理することが非常
に困難であり、通常、希釈を前提としている上、処理効
率がよくないという問題点を抱えている。又、過剰の苛
性ソーダ又は炭酸ソーダの存在下に酸化燃焼する方法
は、略完全な無害化技術といえるが、燃焼時に付加的な
エネルギーと脱硫の為のアルカリが必要な為に、処理費
が高くつくという問題点があった。[Problems to be Solved by the Invention] However, each of the above processing methods has a problem. That is, although the reductive decomposition method has an advantage that it can recover an alkali content contained in the desulfurization waste liquid to be treated, which is effective for the desulfurization process, it requires a large amount of fuel during the reductive decomposition, and the decomposition gas produced as a byproduct. Since hydrogen sulfide gas is contained therein, additional desulfurization equipment is required, and there is room for improvement from the viewpoint of process economy. Wet oxidation method
It is applied to the waste liquid of the desulfurization process using ammonia as an alkali source, but the facility cost is high because it handles corrosive sulfuric acid at high temperature, and the recovered product is a mixture of ammonium sulfate and dilute sulfuric acid. The product itself is not commercially available and usually requires a series of equipment equipped with ammonium sulfate saturation tank, ammonium sulfate crystallization tank and ammonium sulfate drying equipment to be incorporated into the treatment system, which makes the system complicated. I have a problem. The method of oxidizing and burning to sulfuric acid is applied to the waste liquid of the desulfurization process using ammonia as an alkali source, and the process of concentrating the waste liquid to be treated is essential for the process economy during the oxidative combustion. However, since the fluid handled in the system is highly corrosive sulfuric acid, there is a problem that repair costs a lot and the quality of recovered sulfuric acid is poor. In the activated sludge method, it is very difficult to directly treat the desulfurization waste liquid, and it is usually premised on dilution, and there is a problem that the treatment efficiency is not good. Further, the method of oxidative combustion in the presence of excess caustic soda or sodium carbonate can be said to be a substantially complete detoxification technology, but the treatment cost is high because additional energy and alkali for desulfurization are required at the time of combustion. There was a problem of getting stuck.
［問題点を解決する為の手段及び作用］ 本発明者等は、かかる観点に鑑みて鋭意研究を重ねた結
果、セメント製造原料予熱仮焼工程に於ける高温排ガス
及びセメント原料・予熱仮焼工程で生成する酸化カルシ
ウムを利用する効率的な脱硫廃液類の無害化処理法を見
出し、本発明を完成したものである。[Means and Actions for Solving Problems] The inventors of the present invention have made earnest studies in view of such viewpoints, and as a result, high temperature exhaust gas and cement raw material / preheating calcination step in the cement production raw material preheating calcination step The present invention has been completed by finding an efficient detoxification treatment method of desulfurization waste liquor utilizing the calcium oxide generated in step 2.
即ち、本発明者等は、上記従来法の問題点を解決する為
に種々の基礎的実験を行い、更に、応用研究として工場
実験を重ねた結果、次のような事実を見出し本発明を完
成するに至った。That is, the present inventors conducted various basic experiments in order to solve the problems of the above-mentioned conventional method, and further conducted factory experiments as applied research, and as a result, found the following facts and completed the present invention. Came to do.
（１）研究に当り、無害化する脱硫廃液をいわゆるレド
ックス反応（redox reaction）を利用する湿式脱硫プロ
セスからのパージ液として脱硫廃液に限定することな
く、石油精製工場のスイートニング廃液（Sweetening廃
液）、サワーコンデンセート（Sour condensate）、カ
ーボンブラック工場冷却排水並びにコークス工場排水
（通称安水）等の廃液・排水（以下脱硫廃液類と称す）
についても併せて検討した。その結果、脱硫廃液及び上
記類似脱硫廃液はCOD値が数1000〜数10万ppm（Mn）と非
常に高く、且つ酸化硫黄化合物、硫化物並びにチオシア
ン酸塩を含んでおり、場合によってはシアン化合物、油
分が含まれていることがある。(1) In the research, the desulfurization waste liquid which is made harmless is not limited to the desulfurization waste liquid as the purge liquid from the wet desulfurization process using the so-called redox reaction, and the sweetening waste liquid (Sweetening waste liquid) of the oil refinery plant is used. , Sour condensate, carbon black factory cooling wastewater, coke factory wastewater (commonly known as cheap water), and other waste liquids and wastewater (hereinafter referred to as desulfurization waste liquids)
Was also examined. As a result, the desulfurization waste liquid and the above-mentioned similar desulfurization waste liquid have a very high COD value of several thousand to several hundreds of thousands ppm (Mn), and contain sulfur oxide compounds, sulfides and thiocyanates, and in some cases cyanide compounds. , It may contain oil.
又、一般にアルカリ性である場合が多く、且つ、濃縮可
能であるという共通の特性を有していて、このことから
無害化処理に当って、類似脱硫廃液は湿式脱硫液と同様
な取扱いができる。従って、本発明でいう脱硫廃液類は
脱硫廃液のみならず、上記のような類似脱硫廃液を含む
ものである。Further, in general, it has a common property that it is often alkaline and can be concentrated. Therefore, in the detoxification treatment, the similar desulfurization waste liquid can be handled in the same manner as the wet desulfurization liquid. Therefore, the desulfurization waste liquids referred to in the present invention include not only desulfurization waste liquids but also similar desulfurization waste liquids as described above.
（２）脱硫廃液類中に含まれる酸化硫黄化合物（硫酸
塩、亜硫酸塩、チオン酸塩、チオ硫酸塩等）及び硫化物
は、セメント排ガスで熱分解・酸化されて酸化硫黄（SO
x）となると同時に、セメント原料中の石灰及びセメン
ト製造予熱仮焼工程で生成する酸化カルシウムに化学吸
着される。化学吸着された酸化硫黄はセメント排ガス中
の酸素で酸化され、最終的に硫酸カルシウムとなる。こ
れ等の一連の反応は250〜1000℃の温度範囲にて起こ
る。(2) Sulfur oxide compounds (sulfates, sulfites, thionates, thiosulfates, etc.) and sulfides contained in desulfurization waste liquor are pyrolyzed and oxidized by cement exhaust gas to produce sulfur oxides (SO
Simultaneously with x), it is chemically adsorbed to lime in the cement raw material and calcium oxide generated in the cement preheating calcination step. The chemisorbed sulfur oxide is oxidized by oxygen in the cement exhaust gas, and finally becomes calcium sulfate. These series of reactions occur in the temperature range of 250 to 1000 ° C.
（３）チオシアン酸塩は、石灰及び酸化カルシウムの存
在下セメント排ガス中で熱分解・酸化されて硫酸カルシ
ウム、炭酸ガス及び窒素となり無害化される。この反応
は400〜1000℃で進む。(3) Thiocyanate is pyrolyzed and oxidized in cement exhaust gas in the presence of lime and calcium oxide to become calcium sulfate, carbon dioxide gas and nitrogen, and is rendered harmless. This reaction proceeds at 400 to 1000 ° C.
（４）シアン化合物は熱分解・酸化されて炭酸ガス・窒
素となり無害化される。反応完結には850〜1050℃の温
度が必要である。この範囲の温度では、シアン化合物か
らの窒素酸化物の生成は無視出来る。(4) The cyan compound is thermally decomposed and oxidized to become carbon dioxide gas and nitrogen, and is rendered harmless. A temperature of 850 to 1050 ° C is required for completion of the reaction. At temperatures in this range, the formation of nitrogen oxides from cyanide is negligible.
（５）脱硫廃液類中にアンモニア塩が含まれる場合、セ
メント排ガス中でアンモニアに分解され、最終的には酸
化を受けて窒素と水蒸気になる。この分解・酸化は600
〜1000℃で起こる。又、窒素酸化物が存在すると、この
分解・酸化は促進される。(5) When the desulfurization waste liquor contains an ammonia salt, it is decomposed into ammonia in the cement exhaust gas, and finally is oxidized to be nitrogen and water vapor. This decomposition / oxidation is 600
Occurs at ~ 1000 ° C. Also, the presence of nitrogen oxides accelerates this decomposition / oxidation.
（６）脱硫廃液中のCOD成分には、熱分解・酸化され難
いものが含まれており、無害化には850〜1050℃の温度
が必要である。(6) The COD components in the desulfurization waste liquid include substances that are difficult to thermally decompose and oxidize, and a temperature of 850 to 1050 ° C is required for detoxification.
（７）脱硫廃液を無害化する場合の難易度を含有成分に
ついて比較すると、 COD成分及びシアン化合物＞アンモニウム塩＞チオシア
ン酸塩＞酸化硫黄化合物及び硫化物となり、COD成分及
びシアン化合物の無害化が一番難しい。(7) Comparing the difficulty in detoxifying desulfurization waste liquor with respect to the contained components, COD components and cyan compounds> ammonium salts>thiocyanates> sulfur oxide compounds and sulfides are obtained, and the COD components and cyan compounds are rendered harmless. The most difficult
従って、脱硫廃液類の無害化処理を反応工学的に見る
と、その律速段階はCOD成分ないしシアン化合物の熱分
解・酸化過程にあるものと推定される。又、反応時間的
に見ると、COD成分及びシアン化合物の無害化には850〜
1050℃で１〜３秒の滞留時間が必要である。更に、排ガ
ス中の酸素濃度は1.5％（容積）以上の濃度が望まし
い。これに対して、硫黄酸化物、硫化物、チオシアン酸
塩及びアンモニウム塩は、上記と同一温度範囲の場合、
0.5秒程度の滞留時間で無害化可能である。このような
温度範囲、酸素濃度及び滞留時間が確保され、且つ脱硫
廃液類が熱分解・酸化過程で生成する硫黄酸化物（SO
x）を化学吸着する能力を有する石灰及び酸化カルシウ
ムの存在する過程は、セメント製造プロセスに於いては
予熱仮焼帯に限定される。COD成分及びシアン化合物の
熱分解・酸化の観点から見ると1050℃の温度を越えた温
度範囲のところでの無害化処理も可能であるが、チオシ
アン酸塩及びアンモニウム塩は窒素酸化物の発生源とな
り、好ましくない。脱硫廃液類は、通常、脱硫プロセス
で使用されるアルカリ源になって苛性ソーダを使用する
ナトリウムベース脱硫廃液とアンモニアベース脱硫廃液
とに大別され、本発明による処理方法ではどちらも処理
可能であるが、セメント品質への影響のないアンモニア
ベース脱硫廃液が好ましい。Therefore, from a reaction engineering point of view, the detoxification treatment of desulfurization waste liquor is presumed to be the rate-determining step in the thermal decomposition / oxidation process of the COD component or the cyanide compound. Also, in terms of reaction time, it is 850 ~ for detoxifying COD and cyan compounds.
A residence time of 1 to 3 seconds at 1050 ° C is required. Furthermore, it is desirable that the oxygen concentration in the exhaust gas be at least 1.5% (volume). On the other hand, sulfur oxides, sulfides, thiocyanates and ammonium salts, in the same temperature range as above,
It can be made harmless with a residence time of about 0.5 seconds. Such temperature range, oxygen concentration and residence time are secured, and the sulfur oxides (SO
The presence of lime and calcium oxide with the ability to chemisorb x) is limited to the preheated calcination zone in the cement manufacturing process. From the viewpoint of thermal decomposition and oxidation of COD components and cyan compounds, detoxification treatment is possible in the temperature range exceeding 1050 ° C, but thiocyanate and ammonium salts are sources of nitrogen oxides. , Not preferable. The desulfurization waste liquids are generally roughly divided into sodium-based desulfurization waste liquids that use caustic soda as an alkali source used in the desulfurization process and ammonia-based desulfurization waste liquids, and both can be treated by the treatment method according to the present invention. Ammonia-based desulfurization effluent that does not affect the quality of cement is preferable.
［実施例］ 以下、本発明方法を実施例に基づいて具体的に説明す
る。[Examples] Hereinafter, the method of the present invention will be specifically described based on Examples.
第１表に示す組成及び性状の脱硫廃液１容量部を機械噴
霧によりセメント製造設備の850〜1050℃の原料予熱工
程の排ガス105容量部に装入して、残存酸素濃度２〜３
％で無害化処理を行った。排ガスの性状を第２表に示
す。尚、得られたセメントは還元物質が検出されなかっ
た。1 part by volume of the desulfurization waste liquid having the composition and properties shown in Table 1 was charged by mechanical spraying into 10 5 parts by volume of the exhaust gas of the raw material preheating process at 850 to 1050 ° C. of the cement manufacturing facility, and the residual oxygen concentration was 2-3
Detoxification treatment was performed in%. The properties of the exhaust gas are shown in Table 2. No reducing substance was detected in the obtained cement.
第１表 組 成 COD（Mn） 15×104mg/l チオシアン酸塩 1.48mol/l 硫 酸 塩 0.57mol/l 硫 化 物 0.41mol/l 炭 酸 塩 0.44mol/l 性 状 全アンモニア 4.15mol/l PH（25℃） 9.4 総発熱量 750kcal/l 本実施例は、硫化水素約7g/Nm3，シアン化水素約5g/Nm3
を含むコークス炉ガス（COG）２万Ｎm3をレドックス反
応を利用するタカハックス法で脱硫した場合の脱硫廃液
をセメント製造原料予熱工程で無害化処理したことに相
当するものである。又、第２表の結果は、本発明方法の
副次的効果としてセメント製造時の排ガスの浄化（NOx
低減）に寄与していることを示唆している。更に、セメ
ント製造原料予熱仮焼工程の操業には何等トラブルはな
かった。Table 1 Composition COD (Mn) 15 × 10 4 mg / l Thiocyanate 1.48mol / l Sulfuric acid salt 0.57mol / l Sulfuric acid 0.41mol / l Carbonic acid salt 0.44mol / l Properties Total ammonia 4.15mol / l PH (25 ℃) 9.4 Total calorific value 750kcal / l This example, hydrogen sulfide from about 7 g / Nm 3, hydrogen cyanide of about 5 g / Nm 3
This corresponds to the desulfurization waste liquid obtained by desulfurizing coke oven gas (COG) containing 20,000 Nm 3 by the Takahax method utilizing the redox reaction in the preheating process of the raw material for cement production. In addition, the results in Table 2 show that, as a side effect of the method of the present invention, purification of exhaust gas (NOx
Reduction). Furthermore, there were no troubles in the operation of the preheating and calcination process of the cement manufacturing raw material.
［発明の効果］ 本発明の脱硫廃液処理方法によれば、セメント製造原料
予熱仮焼工程に於ける高温排ガス及びセメント原料・同
工程で生成する酸化カルシウムを利用することにより、
特別な装置、付加的なエネルギー及びアルカリを使用す
ることなく極めて経済的に脱硫廃液の無害化処理を行う
ことが出来る。[Effect of the Invention] According to the desulfurization waste liquid treatment method of the present invention, by utilizing the high temperature exhaust gas in the preheating calcination step of the cement manufacturing raw material and the cement raw material and the calcium oxide produced in the same step,
The desulfurization waste liquid can be detoxified very economically without using special equipment, additional energy and alkali.
───────────────────────────────────────────────────── フロントページの続き (56)参考文献 特開 昭49−63654（ＪＰ，Ａ) 造水技術編集企画委員会「造水技術−水 処理のすべて−」（昭和58−５−10）造水 促進センター，Ｐ．123−125 ─────────────────────────────────────────────────── ─── Continuation of the front page (56) References JP-A-49-63654 (JP, A) Water-making technology editorial planning committee “Water-making technology-all about water treatment-” (Showa 58-5-10) Water Promotion Center, P. 123-125
Claims (3)
ント製造原料予熱仮焼工程に脱硫廃液を装入し、セメン
ト焼成排ガス及びセメント原料予熱仮焼工程で生成する
酸化カルシウムと接触させることを特徴とする脱硫廃液
類の処理方法。1. Detoxification treatment of desulfurization waste liquor, charging desulfurization waste liquor to the cement production raw material preheating calcination step, and contacting it with cement calcination exhaust gas and calcium oxide produced in the cement raw material preheating calcination step. A method for treating desulfurization waste liquors, characterized by:
0℃の範囲である特許請求の範囲第１項記載の脱硫廃液
類の処理方法。2. The temperature range in which desulfurization waste liquid is charged is 850 to 105.
The method for treating desulfurization waste liquor according to claim 1, which is in the range of 0 ° C.
許請求の範囲第１項又は第２項記載の脱硫廃液類の処理
方法。3. The method for treating desulfurization waste liquid according to claim 1 or 2, wherein the desulfurization waste liquid contains an ammonium salt.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP60189819A JPH0679708B2 (en) | 1985-08-30 | 1985-08-30 | Treatment method of desulfurization waste liquids |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP60189819A JPH0679708B2 (en) | 1985-08-30 | 1985-08-30 | Treatment method of desulfurization waste liquids |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS6253784A JPS6253784A (en) | 1987-03-09 |
| JPH0679708B2 true JPH0679708B2 (en) | 1994-10-12 |
Family
ID=16247735
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP60189819A Expired - Lifetime JPH0679708B2 (en) | 1985-08-30 | 1985-08-30 | Treatment method of desulfurization waste liquids |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH0679708B2 (en) |
Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP4181682B2 (en) * | 1999-02-19 | 2008-11-19 | 太平洋セメント株式会社 | Factory waste liquid treatment method |
| AT500744B8 (en) * | 2005-03-11 | 2007-02-15 | Montanuniv Leoben | USE OF AN AMMONIA-RELATED RESIDUE |
| CN109913275B (en) * | 2019-03-13 | 2024-06-18 | 中冶焦耐上海工程技术有限公司 | Vacuum sodium carbonate desulfurization fine desulfurization and waste liquid comprehensive treatment process |
| CN109824019A (en) * | 2019-03-22 | 2019-05-31 | 扬州康龙环保工程有限公司 | The method of sodium sulfocyanate, sodium thiosulfate and sodium sulphate is extracted in oven gas alkali desulphurization waste liquid |
| CN115672369B (en) * | 2022-10-19 | 2024-02-06 | 中钢集团鞍山热能研究院有限公司 | Preparation method of super-structure carbon material for catalytic oxidation and decoloration of desulfurization waste liquid |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS525313B2 (en) * | 1972-10-23 | 1977-02-12 |
-
1985
- 1985-08-30 JP JP60189819A patent/JPH0679708B2/en not_active Expired - Lifetime
Non-Patent Citations (1)
| Title |
|---|
| 造水技術編集企画委員会「造水技術−水処理のすべて−」（昭和５８−５−１０）造水促進センター，Ｐ．１２３−１２５ |
Also Published As
| Publication number | Publication date |
|---|---|
| JPS6253784A (en) | 1987-03-09 |
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| Date | Code | Title | Description |
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| EXPY | Cancellation because of completion of term |