JPS6012971B2 - Manufacturing method of ammonium sulfate - Google Patents
Manufacturing method of ammonium sulfateInfo
- Publication number
- JPS6012971B2 JPS6012971B2 JP14796080A JP14796080A JPS6012971B2 JP S6012971 B2 JPS6012971 B2 JP S6012971B2 JP 14796080 A JP14796080 A JP 14796080A JP 14796080 A JP14796080 A JP 14796080A JP S6012971 B2 JPS6012971 B2 JP S6012971B2
- Authority
- JP
- Japan
- Prior art keywords
- ammonium sulfate
- mother liquor
- coke oven
- oven gas
- ammonium
- 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.)
- Expired
Links
- BFNBIHQBYMNNAN-UHFFFAOYSA-N ammonium sulfate Chemical compound N.N.OS(O)(=O)=O BFNBIHQBYMNNAN-UHFFFAOYSA-N 0.000 title claims description 58
- 229910052921 ammonium sulfate Inorganic materials 0.000 title claims description 58
- 235000011130 ammonium sulphate Nutrition 0.000 title claims description 58
- 238000004519 manufacturing process Methods 0.000 title claims description 8
- 239000012452 mother liquor Substances 0.000 claims description 42
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 38
- 239000000571 coke Substances 0.000 claims description 20
- 238000002425 crystallisation Methods 0.000 claims description 16
- 230000008025 crystallization Effects 0.000 claims description 16
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 14
- 229910021529 ammonia Inorganic materials 0.000 claims description 13
- 238000000034 method Methods 0.000 claims description 10
- 239000002351 wastewater Substances 0.000 claims description 9
- 238000010521 absorption reaction Methods 0.000 claims description 8
- 238000001816 cooling Methods 0.000 claims description 7
- 238000010438 heat treatment Methods 0.000 claims description 7
- 239000013535 sea water Substances 0.000 description 8
- 239000013078 crystal Substances 0.000 description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 5
- 239000000498 cooling water Substances 0.000 description 3
- 238000009434 installation Methods 0.000 description 2
- 239000002002 slurry Substances 0.000 description 2
- 239000002253 acid Substances 0.000 description 1
- 238000003763 carbonization Methods 0.000 description 1
- 239000003245 coal Substances 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 229910000069 nitrogen hydride Inorganic materials 0.000 description 1
- 239000007800 oxidant agent Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
Landscapes
- Industrial Gases (AREA)
- Fertilizers (AREA)
Description
【発明の詳細な説明】
この発明は、コークス炉ガスの間接冷却に使用したプラ
イマリークーラーの温排水を硫安母液の加熱に利用する
硫安の製造方法に関するものである。DETAILED DESCRIPTION OF THE INVENTION The present invention relates to a method for producing ammonium sulfate in which heated waste water from a primary cooler used for indirect cooling of coke oven gas is used to heat ammonium sulfate mother liquor.
′コークス炉で石炭乾留時に発生
するコークス炉１ガス中のアンモニア（ＮＨ３）は、そ
の精製段階において、一般的に創生硫安として回収する
場合が多く、製品形状としては、結晶で得る方式が採用
されている。'Ammonia (NH3) in the coke oven gas generated during coal carbonization in a coke oven is generally recovered as ammonium sulfate during its refining stage, and the product form is obtained in the form of crystals. has been done.
結晶硫安製造において安定した粒径の結晶を得るために
は、蒸発缶で減圧下硫安母液を蒸発濃縮させ、結晶槽に
て結晶化させる必要がある。In order to obtain crystals with a stable particle size in the production of crystalline ammonium sulfate, it is necessary to evaporate and concentrate the ammonium sulfate mother liquor under reduced pressure in an evaporator and crystallize it in a crystallization tank.
そのためには硫安母液を事前に所定温度まで加熱昇温し
ておく必要があり、通常、この加熱用熱源としてスチー
ムが使用されているが、スチーム使用量が多いため、そ
の硫安製造コストに占める割合が非常に高い。結晶硫安
の製造方法としては、従釆より多くの方法があり、その
一つに、コークス炉ガスを安水で冷却し、さらに冷却水
で冷却してタールを分離除去し、アンモニア吸収塔に導
き、ここで硫安溶液と接触せしめて硫安母液として取出
し、これを晶折槽に導入して硫安を晶出させ、遠′○分
離機で分離し、乾燥して製品硫安とする方法がある。To do this, it is necessary to heat the ammonium sulfate mother liquor to a predetermined temperature in advance, and steam is normally used as the heat source for this heating, but since the amount of steam used is large, the proportion of the ammonium sulfate production cost is is very high. There are many methods for producing crystalline ammonium sulfate, one of which is to cool coke oven gas with ammonium water, further cool it with cooling water to separate and remove tar, and guide it to an ammonia absorption tower. Here, there is a method in which ammonium sulfate is brought into contact with an ammonium sulfate solution and taken out as an ammonium sulfate mother liquor, which is introduced into a crystallization tank to crystallize ammonium sulfate, separated in a far separator, and dried to obtain a product ammonium sulfate.
この方法においては、晶折槽の硫安母液循環ライン又は
硫安母液供給ラインに硫安母液を加熱するための母液ヒ
ーターを設直し、スチームを使って間接加熱する方法が
孫られている。この方法では硫安母液加熱のため１〜２
ノ硫安ｔと多量のスタチームが必要である。又上記母液
ヒーターを改良したものに多重効用缶方式があり、スチ
ーム使用量を０．５ｔ／硫安ｔ程度低減させ得るが、な
おスチーム使用量が多すぎるのである。又スチームを使
用しない方法として、たとえば０袴公昭弘−偲び旨公報
に記載された、アンモニア吸収塔前にガスコンディショ
ナーを設置し、コークス炉ガスと７０〜８０℃の安水を
直接接触させ、コークス炉ガス温度を４５℃以上に昇温
することにより硫安母液を昇温させる方法があるが、こ
の方法夕では硫安母液加熱のためのスチームの使用量を
皆無となし得るが、ガスコンディショナー新設に伴う設
備費、設置場所が必要となり、経済的負担が大きくなる
。In this method, a mother liquor heater for heating the ammonium sulfate mother liquor is reinstalled in the ammonium sulfate mother liquor circulation line or ammonium sulfate mother liquor supply line of the crystallization tank, and steam is used to indirectly heat the mother liquor. In this method, 1 to 2
Ammonium sulfate and a large amount of starzyme are required. An improved version of the mother liquor heater is a multi-effect can system, which can reduce the amount of steam used by about 0.5 t/t of ammonium sulfate, but the amount of steam used is still too large. In addition, as a method that does not use steam, for example, a gas conditioner is installed in front of the ammonia absorption tower, and the coke oven gas is brought into direct contact with ammonium water at 70 to 80 degrees Celsius, as described in the 0 Hakama Kimihiro Memorial Bulletin. There is a method of raising the temperature of the ammonium sulfate mother liquor by raising the furnace gas temperature to 45°C or higher, but with this method, the amount of steam used for heating the ammonium sulfate mother liquor can be completely eliminated, but due to the installation of a new gas conditioner. Equipment costs and installation space are required, which increases the economic burden.
なお、コークス炉から発生するコークス炉ガスは、５０
０〜８０００Ｃの温度があり、通常コレクテイングメィ
ンと上昇管を連結するペンド管において冷却安水と直接
接触して７５〜８５ｏ０に冷却され、その後プライマリ
ークーラーで冷却水により３０℃程度まで冷却される。In addition, the coke oven gas generated from the coke oven is 50
It has a temperature of 0 to 8000C, and is usually cooled to 75 to 85o0 by direct contact with cooling ammonium water in the pend pipe that connects the collecting main and riser pipe, and then cooled to about 30℃ with cooling water in the primary cooler. .
すなわち、コークス炉ガスの顕熱は、安水および冷却水
に移行し、４０〜８５ｑｏの温水として排出されており
、この温排水の熱回収については有効な手段がなかった
。この発明は、創生結晶硫安製造における現状に鑑み、
かかる欠点を排除することを目的とし、コ−クス炉ガス
の間接冷却に使用したプライマリークーラーの塩排水を
、硫安母液の加熱に使用する硫安の製造方法を提案する
ものである。That is, the sensible heat of coke oven gas is transferred to ammonium water and cooling water, and is discharged as hot water of 40 to 85 qo, and there has been no effective means for recovering heat from this hot waste water. This invention was developed in view of the current situation in the production of crystalline ammonium sulfate.
In order to eliminate such drawbacks, we propose a method for producing ammonium sulfate in which salt waste water from a primary cooler used for indirect cooling of coke oven gas is used for heating ammonium sulfate mother liquor.
すなわち、この発明は、コークス炉ガスをアンモニア吸
収塔に導き、硫安溶液と接触せしめて硫安母液として取
出し、該硫安母液を晶析槽に導入して減圧濃縮により硫
安を晶出せしめ、これを分離回収する硫安の製造方法に
おいて、コークス炉ガスの間接冷却に使用したプライマ
リークーラーの温排水を用いて、硫安母液を間接加熱す
ることを特徴とする硫安の製造方法である。That is, in this invention, coke oven gas is introduced into an ammonia absorption tower, brought into contact with an ammonium sulfate solution, and taken out as an ammonium sulfate mother liquor.The ammonium sulfate mother liquor is introduced into a crystallization tank, where ammonium sulfate is crystallized by vacuum concentration, and this is separated. The method for producing ammonium sulfate to be recovered is characterized in that ammonium sulfate mother liquor is indirectly heated using heated waste water from a primary cooler used for indirect cooling of coke oven gas.
コークス炉ガスの間接冷却に使用したプライマリークー
ラーの温排水、すなわち、前段のプラィ、マリークーラ
ーから排出される温排水は、６５〜７５℃で回収される
。The heated waste water from the primary cooler used for indirect cooling of coke oven gas, that is, the heated waste water discharged from the ply and Mary coolers in the previous stage, is recovered at 65 to 75°C.
この発明においては、これを晶析槽へ供給する硫安母液
の供給系あるいは晶折槽の蒸発缶への母液循環系に熱交
換器を設けて導き、硫安母液を前段プライマリークーラ
ーの温排水で間接加熱し、蒸発缶での硫安母液の温度を
４０ｑｏ以上、望ましくは４５ｏｏ以上に昇温せしめる
のである。In this invention, a heat exchanger is installed in the supply system of the ammonium sulfate mother liquor that is supplied to the crystallization tank or in the mother liquor circulation system to the evaporator of the crystallization tank, and the ammonium sulfate mother liquor is indirectly transferred to the heated waste water of the primary cooler in the previous stage. The temperature of the ammonium sulfate mother liquor in the evaporator is raised to 40 qo or more, preferably 45 oo or more.
したがって、この発明方法によれば、従来廃棄されてい
た前段プライマリークーラーの温排水の保有する顕熱を
有効利用でき、しかも硫安母液を加熱するためにスチー
ムを使用する必要がなく、硫安の製品コストを大中に低
減せしめることができる。Therefore, according to the method of this invention, it is possible to effectively utilize the sensible heat possessed by the heated waste water of the front primary cooler, which was conventionally discarded, and there is no need to use steam to heat the ammonium sulfate mother liquor, which reduces the product cost of ammonium sulfate. can be reduced to a large extent.
次に、この発明の実施例を図面に基いて説明する。Next, embodiments of the present invention will be described based on the drawings.
コークス炉１から発生する６００〜８００ｑｏのコーク
ス炉ガスは、コレクテイングメィン２において、安水集
合糟２０からポンプ２１により供給される約８０℃の安
水の噴霧により８５℃まで冷却され、ダウンカマー３で
タール、凝縮水等を含む昇温した熱安水を分離後プライ
マリークーラー４に送られる。Coke oven gas of 600 to 800 qo generated from the coke oven 1 is cooled down to 85°C in the collecting main 2 by spraying of about 80°C ammonium water supplied from the ammonium water collection tank 20 by the pump 21, and then sent to the downcomer. 3, the heated ammonium water containing tar, condensed water, etc. is separated and sent to the primary cooler 4.
ここで冷却用海水により３０℃に冷却され、タール抽出
器５でタールを抽出分離してガスブロワー６を介してア
ンモニア吸収塔７に送られる。このアンモニア吸収塔７
には、母液循環槽８で硫酸ｓを加えて、硫酸濃度３〜５
％に調整された硫安溶液が、ポンプ９を介して循環系ａ
により供給され、コークス炉ガス中のアンモニアは、硫
安溶液中の硫酸と反応して硫安として固定され硫安母液
となる。そして循環系ａ中の硫安母液の一部は、配管ｂ
により晶析槽１０の結晶槽１２に供給される。そして、
結晶層槽２で結晶しなかった硫安母液の一部は、オーバ
ーフロー槽１５、ポンプ１６、配管ｃを経て母液循環槽
８にもどされる。晶析槽１川ま結晶槽１２と蒸発缶１１
の組合せからなり、その間にはポンプ１３、母液ヒータ
ー１４を有する配管よりなる硫安母液循環ラインｄが設
けられている。なお、蒸発缶１１にはコンデンサ１７、
スチームヱジェクター１８が配管接続され、結晶槽１２
の底には、硫安結晶スラリーを図示しない遠Ｄ分離機へ
搬出する配管ｅが設けられている。上記母液ヒーター１
４は、プライマリークーラー前段４から排出する温海水
を熱源とするもので、温海水は、温海水ビット２２、ポ
ンプ２３を介して母液ヒーター１４と配管ｆで接続され
、使用済の海水は配管ｇにより廃棄する。Here, it is cooled to 30° C. with cooling seawater, and the tar is extracted and separated in a tar extractor 5 and sent to an ammonia absorption tower 7 via a gas blower 6. This ammonia absorption tower 7
, add sulfuric acid s in the mother liquor circulation tank 8 to make the sulfuric acid concentration 3 to 5.
Ammonium sulfate solution adjusted to
The ammonia in the coke oven gas reacts with the sulfuric acid in the ammonium sulfate solution and is fixed as ammonium sulfate, forming an ammonium sulfate mother liquor. A part of the ammonium sulfate mother liquor in circulation system a is transferred to pipe b.
It is supplied to the crystallization tank 12 of the crystallization tank 10 by this. and,
A portion of the ammonium sulfate mother liquor that did not crystallize in the crystal bed tank 2 is returned to the mother liquor circulation tank 8 via the overflow tank 15, pump 16, and piping c. Crystallization tank 1, crystallization tank 12 and evaporator 11
An ammonium sulfate mother liquor circulation line d consisting of piping having a pump 13 and a mother liquor heater 14 is provided between them. Note that the evaporator 11 includes a condenser 17,
A steam ejector 18 is connected to the piping, and the crystallization tank 12
A pipe e is provided at the bottom of the tank to carry out the ammonium sulfate crystal slurry to a centrifugal separator (not shown). The above mother liquor heater 1
4 uses warm seawater discharged from the front stage 4 of the primary cooler as a heat source.The warm seawater is connected to the mother liquor heater 14 via a warm seawater bit 22 and a pump 23 via a pipe f, and the used seawater is connected to a pipe g. will be disposed of.
又コレクティングメィン２に供給される安水は、安水集
合槽２０からポンプ２１により配管ｈを経て供給され、
ダウンカマー３からタールデカンター１９に配管ｉを介
して流下し、再び安水集合槽２０‘こもどるよう構成さ
れている。In addition, the ammonium water supplied to the collecting main 2 is supplied from the ammonium water collection tank 20 by a pump 21 through a pipe h,
It is configured to flow down from the downcomer 3 to the tar decanter 19 via a pipe i, and return again to the ammonium water collection tank 20'.
図中２４は離酸器である。上記によりコークス炉より発
生したアンモニアを含有するコークス炉ガスは、冷却さ
れた後、アンモニア吸収塔７で硫安溶液と向流接触し、
アンモニアは硫酸と反応して硫安として固定され硫安母
液となり、晶析槽１０で減圧濃縮して硫安結晶を晶出せ
しめ、硫安スラリーとして抜出すのである。In the figure, 24 is an acid remover. The coke oven gas containing ammonia generated from the coke oven as described above is cooled and then brought into countercurrent contact with the ammonium sulfate solution in the ammonia absorption tower 7.
Ammonia reacts with sulfuric acid and is fixed as ammonium sulfate to form an ammonium sulfate mother liquor, which is concentrated under reduced pressure in a crystallization tank 10 to crystallize ammonium sulfate crystals, which are extracted as ammonium sulfate slurry.
この際硫安母液は、循環ラインｄに設けた母液ヒーター
４において、プライマリークーラー前段４から排出され
る約７ｙｏの溢海水と熱交換して４０℃以上に昇温され
、しかるのち蒸発缶１１に供給して減圧下硫安母液の水
分を蒸発させ、濃厚母液＊＊を結晶槽１２へ降下させ、
硫安の結晶を生成せしめるのである。At this time, the ammonium sulfate mother liquor is heated to 40°C or higher by exchanging heat with about 7yo of overflow water discharged from the primary cooler front stage 4 in the mother liquor heater 4 installed in the circulation line d, and then supplied to the evaporator 11. The water in the ammonium sulfate mother liquor is evaporated under reduced pressure, and the concentrated mother liquor is lowered into the crystallization tank 12.
This causes ammonium sulfate crystals to form.
次に前記硫安母液の加熱用に温海水を使用したこの発明
法の場合とスチームを使用した従来法の場合を対比して
示す。Next, a comparison will be made between the method of the present invention in which warm seawater is used for heating the ammonium sulfate mother liquor and the conventional method in which steam is used.
このようにこの発明によれば、従来廃棄されていたプラ
イマリークーラー前段の温海水の保有する顕熱を有効に
回収できると共に、硫安母液加熱のためのスチーム使用
量を皆無とすることができるので硫安の製品コストを大
中に低減することができる。As described above, according to the present invention, the sensible heat held in the warm seawater in the front stage of the primary cooler, which was conventionally discarded, can be effectively recovered, and the amount of steam used for heating the ammonium sulfate mother liquor can be completely eliminated. The product cost can be significantly reduced.
第１図はこの発明の一実施例におけるフローシートを示
す図表である。
図中、１……コークス炉、２……コレクティングメイン
、３……ダウンカマー、４……プライマリークーラー、
５……タール抽出器、６……ガスプロワー、７・・・・
・・アンモニア吸収塔、８・・・・・・母液循環槽、９
・・・・・・ポンプ、１０・・・・・・晶析槽、１１・
・・・・・蒸発缶、１２・・・・・・結晶槽、１３・・
・・・・ポンプ、１４……母液ヒーター、１５……オー
バーフロー槽、１６……ポンプ、１７……コンデンサ、
１８……エジヱクター、１９……タールデカンター、２
０・…・・安水集合槽、２１・・・・・・ポンプ、２２
・・・・・・温海水ビット、２３・・・・・・ポンプ、
２４…・・・離酸器、ａ・・・・・・循環系、ｂ，ｃ・
・・・・・配管、ｄ・・・・・・硫安母液循環ライン、
ｅ，ｆ，ｇ，ｈ，ｉ…・・・配管、Ｓ．・・・・・硫酸
。
鷺１図FIG. 1 is a chart showing a flow sheet in one embodiment of the present invention. In the diagram, 1...Coke oven, 2...Collecting main, 3...Downcomer, 4...Primary cooler,
5... Tar extractor, 6... Gas blower, 7...
... Ammonia absorption tower, 8 ... Mother liquor circulation tank, 9
...Pump, 10...Crystallization tank, 11.
...Evaporator, 12...Crystallization tank, 13...
... pump, 14 ... mother liquor heater, 15 ... overflow tank, 16 ... pump, 17 ... condenser,
18... Educator, 19... Tar decanter, 2
0...Anonymous water collection tank, 21...Pump, 22
... Warm seawater bit, 23 ... Pump,
24... Oxidizer, a... Circulatory system, b, c.
...Piping, d...Ammonium sulfate mother liquor circulation line,
e, f, g, h, i...Piping, S. ...Sulfuric acid. Heron 1
Claims (1)
と接触させ、アンモニアを硫酸と反応させて硫安母液を
生成し、これを晶析槽に導入して減圧濃縮し、硫安を晶
出分離するコークス炉ガスからの硫安の製造方法におい
て、コークス炉ガスの間接冷却に使用したプライマリー
クーラーの温排水を用いて、硫安母液を間接加熱するこ
とを特徴とする硫安の製造方法。1 Coke oven gas is introduced into an ammonia absorption tower and brought into contact with sulfuric acid, ammonia is reacted with sulfuric acid to produce ammonium sulfate mother liquor, which is introduced into a crystallization tank and concentrated under reduced pressure to crystallize and separate ammonium sulfate. A method for producing ammonium sulfate from furnace gas, the method comprising indirectly heating ammonium sulfate mother liquor using heated waste water from a primary cooler used for indirect cooling of coke oven gas.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP14796080A JPS6012971B2 (en) | 1980-10-21 | 1980-10-21 | Manufacturing method of ammonium sulfate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP14796080A JPS6012971B2 (en) | 1980-10-21 | 1980-10-21 | Manufacturing method of ammonium sulfate |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS5771886A JPS5771886A (en) | 1982-05-04 |
| JPS6012971B2 true JPS6012971B2 (en) | 1985-04-04 |
Family
ID=15441969
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP14796080A Expired JPS6012971B2 (en) | 1980-10-21 | 1980-10-21 | Manufacturing method of ammonium sulfate |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS6012971B2 (en) |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2015218077A (en) * | 2014-05-15 | 2015-12-07 | Ｊｆｅケミカル株式会社 | Production method and production facility of ammonium sulfate, and treatment method of surplus ammoniacal liquor |
| JP6149821B2 (en) * | 2014-08-04 | 2017-06-21 | Ｊｆｅスチール株式会社 | Coke oven gas purification method |
-
1980
- 1980-10-21 JP JP14796080A patent/JPS6012971B2/en not_active Expired
Also Published As
| Publication number | Publication date |
|---|---|
| JPS5771886A (en) | 1982-05-04 |
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