JPS60103022A - Manufacture of granular ammonium sulfate - Google Patents
Manufacture of granular ammonium sulfateInfo
- Publication number
- JPS60103022A JPS60103022A JP20676083A JP20676083A JPS60103022A JP S60103022 A JPS60103022 A JP S60103022A JP 20676083 A JP20676083 A JP 20676083A JP 20676083 A JP20676083 A JP 20676083A JP S60103022 A JPS60103022 A JP S60103022A
- Authority
- JP
- Japan
- Prior art keywords
- mother liquor
- ammonium sulfate
- metals
- contg
- crystallization
- 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
- BFNBIHQBYMNNAN-UHFFFAOYSA-N ammonium sulfate Chemical compound N.N.OS(O)(=O)=O BFNBIHQBYMNNAN-UHFFFAOYSA-N 0.000 title claims abstract description 46
- 229910052921 ammonium sulfate Inorganic materials 0.000 title claims abstract description 46
- 235000011130 ammonium sulphate Nutrition 0.000 title claims abstract description 46
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 5
- 239000012452 mother liquor Substances 0.000 claims abstract description 45
- 229910052751 metal Inorganic materials 0.000 claims abstract description 21
- 239000002184 metal Substances 0.000 claims abstract description 21
- 239000013078 crystal Substances 0.000 claims abstract description 16
- 150000002739 metals Chemical class 0.000 claims abstract description 15
- 238000002425 crystallisation Methods 0.000 claims abstract description 13
- 230000008025 crystallization Effects 0.000 claims abstract description 13
- 229920005989 resin Polymers 0.000 claims abstract description 13
- 239000011347 resin Substances 0.000 claims abstract description 13
- 239000013522 chelant Substances 0.000 claims abstract description 11
- 239000003607 modifier Substances 0.000 claims abstract description 8
- 239000002253 acid Substances 0.000 claims description 6
- 239000000203 mixture Substances 0.000 claims description 4
- 150000003839 salts Chemical class 0.000 claims description 4
- 230000003750 conditioning effect Effects 0.000 claims description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 abstract description 11
- 239000000571 coke Substances 0.000 abstract description 7
- -1 coke oven gas Chemical compound 0.000 abstract description 5
- 229910052742 iron Inorganic materials 0.000 abstract description 5
- 229910021529 ammonia Inorganic materials 0.000 abstract description 4
- 239000006227 byproduct Substances 0.000 abstract description 4
- 229910052802 copper Inorganic materials 0.000 abstract description 2
- NBZBKCUXIYYUSX-UHFFFAOYSA-N iminodiacetic acid Chemical compound OC(=O)CNCC(O)=O NBZBKCUXIYYUSX-UHFFFAOYSA-N 0.000 abstract description 2
- LNOPIUAQISRISI-UHFFFAOYSA-N n'-hydroxy-2-propan-2-ylsulfonylethanimidamide Chemical compound CC(C)S(=O)(=O)CC(N)=NO LNOPIUAQISRISI-UHFFFAOYSA-N 0.000 abstract description 2
- 230000000051 modifying effect Effects 0.000 abstract 2
- 230000007774 longterm Effects 0.000 abstract 1
- 238000002360 preparation method Methods 0.000 abstract 1
- IIACRCGMVDHOTQ-UHFFFAOYSA-M sulfamate Chemical compound NS([O-])(=O)=O IIACRCGMVDHOTQ-UHFFFAOYSA-M 0.000 abstract 1
- VYECFMCAAHMRNW-UHFFFAOYSA-N sulfamic acid Chemical compound NS(O)(=O)=O.NS(O)(=O)=O VYECFMCAAHMRNW-UHFFFAOYSA-N 0.000 abstract 1
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 6
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 5
- 239000007788 liquid Substances 0.000 description 5
- 239000000243 solution Substances 0.000 description 5
- PAWQVTBBRAZDMG-UHFFFAOYSA-N 2-(3-bromo-2-fluorophenyl)acetic acid Chemical compound OC(=O)CC1=CC=CC(Br)=C1F PAWQVTBBRAZDMG-UHFFFAOYSA-N 0.000 description 4
- 239000003795 chemical substances by application Substances 0.000 description 4
- 238000002156 mixing Methods 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 3
- 235000013339 cereals Nutrition 0.000 description 3
- 238000000034 method Methods 0.000 description 3
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 2
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 2
- 241000209094 Oryza Species 0.000 description 2
- 235000007164 Oryza sativa Nutrition 0.000 description 2
- 239000004793 Polystyrene Substances 0.000 description 2
- JUJWROOIHBZHMG-UHFFFAOYSA-N Pyridine Chemical compound C1=CC=NC=C1 JUJWROOIHBZHMG-UHFFFAOYSA-N 0.000 description 2
- 235000011114 ammonium hydroxide Nutrition 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 230000002401 inhibitory effect Effects 0.000 description 2
- 229910017604 nitric acid Inorganic materials 0.000 description 2
- 229920002223 polystyrene Polymers 0.000 description 2
- 229910052700 potassium Inorganic materials 0.000 description 2
- 235000009566 rice Nutrition 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- GEHMBYLTCISYNY-UHFFFAOYSA-N Ammonium sulfamate Chemical compound [NH4+].NS([O-])(=O)=O GEHMBYLTCISYNY-UHFFFAOYSA-N 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- 239000004698 Polyethylene Substances 0.000 description 1
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 230000004720 fertilization Effects 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 230000002452 interceptive effect Effects 0.000 description 1
- 238000005342 ion exchange Methods 0.000 description 1
- 235000014413 iron hydroxide Nutrition 0.000 description 1
- NCNCGGDMXMBVIA-UHFFFAOYSA-L iron(ii) hydroxide Chemical compound [OH-].[OH-].[Fe+2] NCNCGGDMXMBVIA-UHFFFAOYSA-L 0.000 description 1
- 238000006386 neutralization reaction Methods 0.000 description 1
- 238000012261 overproduction Methods 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 229920000573 polyethylene Polymers 0.000 description 1
- 229920005990 polystyrene resin Polymers 0.000 description 1
- 239000011591 potassium Substances 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- UMJSCPRVCHMLSP-UHFFFAOYSA-N pyridine Natural products COC1=CC=CN=C1 UMJSCPRVCHMLSP-UHFFFAOYSA-N 0.000 description 1
- 239000012047 saturated solution Substances 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 239000006228 supernatant Substances 0.000 description 1
Landscapes
- Fertilizers (AREA)
Abstract
Description
【発明の詳細な説明】
この発明は、コークス炉ガスからバルクブレンド用に適
した粒状硫安を製造する方法に関する。DETAILED DESCRIPTION OF THE INVENTION The present invention relates to a process for producing granular ammonium sulfate suitable for bulk blending from coke oven gas.
国内における硫安の需給は、生産過剰で国内需要の余剰
分は輸出にたよっている。しかし、粒状のリン、カリ成
分とバラ状のまま任意に、しかも迅速に配合して施肥す
る方法に使用されるバルクブレンド用の粒状硫安は、生
産量が少な（、常に不足している状況にある。Domestic supply and demand for ammonium sulfate is due to overproduction, with surplus domestic demand relying on exports. However, granular ammonium sulfate for bulk blending, which is used for fertilization by arbitrarily and quickly mixing granular phosphorus and potassium components in their bulk form, is produced in small quantities (and is constantly in short supply). be.
上記バルクブレンド用の粒状硫安としては、粒度１〜８
正程度の粒の揃ったサイコロ状１球状。The granular ammonium sulfate for the above bulk blend has a particle size of 1 to 8.
A dice-like ball with uniform grains.
米粒状のものが要゛ｎされている。Rice grain-like grains are required.
飽和器で遊離硫酸を含む母液とアンモニアから硫安母液
を生成さトｋ、これを結晶槽に導入して濃縮することに
よって粒状硫安を製造せんとしても、得られる硫安結晶
は柱状あるいは板状であって、リーイコロ状９球状、米
粒状の粒状硫安を製造することができなかった。Even if ammonium sulfate mother liquor is produced from mother liquor containing free sulfuric acid and ammonia in a saturator and granular ammonium sulfate is produced by introducing this into a crystallization tank and concentrating it, the ammonium sulfate crystals obtained are columnar or plate-shaped. Therefore, it was not possible to produce granular ammonium sulfate in the shape of 9 spheres and rice grains.
この対策として、硫安母液から晶析装置を経て粒状硫安
をｌＩｌ’Ｊ ｉ＋’ｆ ｔＪ−る工程において、硫安
母液に媒晶剤として硝酸または硝酸アンモニウムを硝酸
アンモニウム換算値で１〜１０％添加して晶析する方法
（特開昭５６−１０９８１４） 、硫安母液に媒晶剤と
してスルファミノ酸またはスルファミノ酸アンモニウム
をスルフ゛ｒミン酸換算値で０．５〜５−ｔ！ｌ）添加
して晶析すル）ｊ ＩＩＥ （特開昭５６−１０９８１
５）、あるいは硫安母液に媒晶剤として硝酸または硝酸
アンモニウムを硝酸アンモニウムの形で１〜１０係及び
スルファミン酸またはスルファミン酸アンモニツムをス
ルファミノ酸アンモニウムの形で０，５〜５饅の範囲で
添加し晶析する方法（特開昭５６−１０９８１６）等の
提案も行なわれでいるが、媒晶剤の添加率、バルクブレ
ンド用の収率等必ずしも満足できるものではない。As a countermeasure for this, in the step of producing granular ammonium sulfate from the ammonium sulfate mother liquor through a crystallizer, nitric acid or ammonium nitrate is added as a crystallizing agent to the ammonium sulfate mother liquor in an amount of 1 to 10% in terms of ammonium nitrate. (Japanese Unexamined Patent Publication No. 56-109814), sulfamino acid or ammonium sulfamino acid is added as a modifier to ammonium sulfate mother liquor in an amount of 0.5 to 5 tons in terms of sulfuric acid! l) Addition and crystallization l)j IIE (Japanese Unexamined Patent Publication No. 10981-1981)
5) Or crystallize by adding nitric acid or ammonium nitrate as a modifier to the ammonium sulfate mother liquor in the range of 1 to 10 in the form of ammonium nitrate, and sulfamic acid or ammonium sulfamate in the form of ammonium sulfaminate in the range of 0.5 to 5. Although proposals have been made such as a method to do this (Japanese Unexamined Patent Publication No. 56-109816), the addition rate of the crystal modifier and the yield for bulk blending are not necessarily satisfactory.
本来、スルファミノ酸またはその塩の媒晶効果は著シい
が、コークス炉ガスからの副生硫安１１Ｅ中には、媒晶
剤の媒晶効果を阻害する鉄、グロＡ。Originally, the modulating effect of sulfamino acid or its salt is significant, but ammonium sulfate 11E, a by-product from coke oven gas, contains iron and glomerate A, which inhibits the modulating effect of the modifier.
銅などが溶存してくることがある。このようｆ、Ｋ １
ｉ１１害金属を系内に入れないことが重要であるが、硫
安母液にこれらが混入した場合、スルファミノ酸または
その塩類の存在にもかかわらず、結晶形状の悪化を招（
。従来、この対策としては、阻害金属が硫安結晶に付着
して系外へ排出されるのを待つか、あるいは硫安母液を
廃棄して新しい母液を調製するなどの方法が採られてい
る。Copper, etc. may be dissolved. Like this f, K 1
It is important not to introduce harmful metals into the system, but if they are mixed into the ammonium sulfate mother liquor, the crystal shape may deteriorate (despite the presence of sulfamino acid or its salts).
. Conventionally, countermeasures against this problem include waiting for the inhibiting metal to adhere to ammonium sulfate crystals and being discharged from the system, or discarding the ammonium sulfate mother liquor and preparing a new mother liquor.
この発明は上記小情に鑑みなされたもので、スルファミ
ノ酸またはその塩類を含む硫安母液から晶析装置を経て
粒状硫安を製造する方法において、媒晶剤の媒晶能阻害
金属混入時、硫安１す液の一部を系外に抜き出し、ＰＨ
２，５〜５に調整した後、キレート樹脂により含有金属
類を除去し、再度系内に導入して晶析せしめることを要
旨とする。This invention was made in view of the above-mentioned circumstances, and in a method for producing granular ammonium sulfate from an ammonium sulfate mother liquor containing sulfamino acid or its salts through a crystallizer, when a metal that inhibits the modulating ability of the crystallizing agent is mixed, ammonium sulfate 1 A part of the liquid is extracted from the system, and the pH is
After adjusting to 2.5 to 5, the contained metals are removed using a chelate resin, and the metals are reintroduced into the system for crystallization.
硫安融液のＰＹｉ調整は、アンモニアガスまたはコーク
ス炉ガス等ｒンモニアを含むガス、あるいはアンモニア
水を用いることができる。ＰＨは２．５以−ヒが必要で
、８以ｌ−が望ましく、ＰＨ２，５未満では、キレート
樹脂とのイオン交換が十分でない。To adjust the PYi of the ammonium sulfate melt, ammonia gas, a gas containing ammonia such as coke oven gas, or ammonia water can be used. The pH is required to be 2.5 or higher, preferably 8 or higher; if the pH is lower than 2.5, ion exchange with the chelate resin is not sufficient.
また、ＰＨは＋ｌ’ｔｉい方が望ましいが、５以上では
水酸化鉄の沈澱が生じ好ましくない。したがって最適範
囲としては、ＰＨ８〜４．５程度が望ましい。一方、コ
ークス炉ガス副生硫安設備では、硫安母液から中和によ
ってピリジン等のタール塩基を回収することが行なわれ
ているが、このピリジン回収後の硫安母液の場合、これ
に未処理硫安母液を混合してＰＨｉ整した硫安母液をキ
レート樹脂により処理すればよく、経済的に有利である
。Further, it is desirable that the pH value is +l'ti, but if it is 5 or more, precipitation of iron hydroxide occurs, which is not preferable. Therefore, the optimum range is preferably about PH8 to 4.5. On the other hand, in coke oven gas by-product ammonium sulfate facilities, tar bases such as pyridine are recovered from ammonium sulfate mother liquor by neutralization. The ammonium sulfate mother liquor mixed and adjusted to PHi may be treated with a chelate resin, which is economically advantageous.
この発明によれば、媒晶剤の媒晶能を阻害する金属類が
硫安母液に混入時、硫安＠液の一部を系外へ抜き出し、
ＰＨ調整後キレート樹脂により脱金属処理して再ぽ系内
へ導入せしめるから、短期間で明害金属が除去され、阻
害金属が硫安結晶に付着して系外へ排出されるまで長期
間待つ必要もなく、また、硫安＠液を廃棄して新しい母
液を調製する必要もない。According to this invention, when metals that inhibit the modulating ability of the crystal modifier are mixed into the ammonium sulfate mother liquor, a part of the ammonium sulfate solution is extracted out of the system,
After adjusting the pH, the metal is demetallized using a chelate resin and introduced into the repo system, so it is necessary to wait for a long time until the harmful metals are removed in a short period of time and the interfering metals adhere to the ammonium sulfate crystals and are discharged from the system. There is no need to discard the ammonium sulfate solution and prepare a new mother liquor.
実施例
第１図に示す試験装置を用い゛Ｃコークス炉ガス副生硫
安設備からの硫安母液を脱金属処理した。EXAMPLE Using the test apparatus shown in FIG. 1, ammonium sulfate mother liquor from a coke oven gas by-product ammonium sulfate facility was subjected to metal removal treatment.
すなわち、ポリスチレン系の樹脂にキレート基としてイ
ミノジ酢酸を付加したキレート樹脂を、２Ｑ Ｑ １．
７ｍφＸ１７７１のむラム（４）にそれぞれ２０．６充
填し、２水筒列に接続して使用した。Ｓ−１／ −ｌ・
樹脂のコンディショニングとして、２係硫酸約４０４に
て洗浄したのち、水６０〜８ｏｌにて水洗し、つぎに３
係アンモニア水をカラム（４）の出１」流出液が十分ア
ルカリ性となるまで通液し、最後に１−分に水洗を行な
った。That is, a chelate resin in which iminodiacetic acid is added as a chelate group to a polystyrene resin is 2Q Q1.
Rams (4) each measuring 7 mφ x 1771 mm were filled with 20.6 liters of water and used by connecting them to two rows of water bottles. S-1/-l・
To condition the resin, wash it with about 404 liters of dihydric sulfuric acid, then wash it with 60 to 8 ol of water, and then
Aqueous ammonia was passed through the column (4) until the effluent became sufficiently alkaline, and finally washed with water for 1 minute.
容ｉ１ｉのポリスチレンタンク（１）に硫安ＩＩＪ液９
００召を入れ、Ｉχ拌しながらアンモニアガスを吹き込
み、ＰＨを３．８に調整した。このとき分離浮上した若
干の油分を除去したのら、ポンプ（２）により約２ｄ／
ｍｉｎの流量でフィルター（３）を介し゛Ｃキレート樹
脂のカーツム（４）に通液し脱金属処理した。Add ammonium sulfate IIJ solution 9 to a polystyrene tank (1) with a capacity of 1i.
Ammonia gas was blown into the flask while stirring to adjust the pH to 3.8. After removing some of the oil that separated and floated at this time, pump (2)
The solution was passed through the filter (3) at a flow rate of min. to the C chelate resin cartridge (4) for metal removal treatment.
処理母液はカラム（４）の出口にて鉄イオンをチェック
し、鉄イオンが検出されるまで通液した。ｌ同の母液処
理量は、３００〜３５０１であった。鉄イオンが検出さ
れるとキレート樹脂は、上記コンディショニング方法に
よって再生し使用した。なお、処理母液は容腓１ｍ’の
ポリスチレンタンク（５）に収容した。The treated mother liquor was checked for iron ions at the outlet of the column (4), and the solution was passed until iron ions were detected. The amount of mother liquor treated was 300-3501. When iron ions were detected, the chelate resin was regenerated by the above conditioning method and used. The treated mother liquor was stored in a 1 m' polystyrene tank (5).
未処理母液および脱金属処理母液の金ｊζ弓分析値を第
１表に示づ−０
小１表
（ｎ１ｙ／ ｌ ）
上記により脱金属処理した母液は、遊離硫酸分を４．５
％に調整したのち、第２図に示すオス口型晶析実験装置
１１を用いて晶析実験を行なった。すなわち、母液槽α
力に脱金属処理した母液９０Ｍと硫安結晶８０ ｋｙを
入れ、スチームヒーター（１）により母液槽０℃内を４
０℃一定に保持し、攪拌機（ハ）で攪拌しながら溶解せ
しめた。この飽和溶液にスルファミノ酸アンモニウムを
０．８％添加し、循環ポンプＱうにより上洛母液を母液
クーラーＱｅで約３５℃程度に冷却して高さ２．７ｍ、
容積３９．２４のオス口型結晶槽０Ｑに２５ｎ／ｍｉｎ
で供給し、オーバーフローしたものは、母液槽Ｑｌ）に
戻しながら、種晶（２０メツシユ以下）ｓｏｏ、ｙを母
液槽ａηに投入し、晶析を開始した。結晶が成長して結
晶槽θΦ内の保存層が所定量となったのち、１時間毎に
抜き出し、これを遠心分離後乾燥し、結晶の大きさおよ
び形状が安定した時点で、硫安結晶をヌケールルーぺを
用いてランダムに測定し、結晶成長軸を８． ａに直行
する軸をｂとして形状係数（ａ／ｂ ）を算出した。同
様に未処理母液についても同条件で晶析試験を実施した
。その結果を第２表に示す。The gold jζ arc analysis values of the untreated mother liquor and the demetallized mother liquor are shown in Table 1.
%, a crystallization experiment was conducted using a male-end crystallization experiment apparatus 11 shown in FIG. In other words, mother liquid tank α
Add 90 M of demetallized mother liquor and 80 ky of ammonium sulfate crystals to the tank, and heat the mother liquor tank to 0°C using a steam heater (1).
The mixture was maintained at a constant temperature of 0° C. and dissolved while stirring with a stirrer (c). 0.8% ammonium sulfaminate was added to this saturated solution, and the supernatant mother liquor was cooled to about 35°C with a mother liquor cooler Qe using a circulation pump Q.
25n/min in a male-end crystal tank 0Q with a volume of 39.24
While the overflow was returned to the mother liquid tank Ql), seed crystals (20 mesh or less) soo, y were put into the mother liquid tank aη to start crystallization. After the crystals grow and the storage layer in the crystallization tank θΦ reaches a predetermined amount, they are extracted every hour, centrifuged and dried, and when the size and shape of the crystals have stabilized, the ammonium sulfate crystals are placed in Nucair Ru. The crystal growth axis was measured randomly using 8. The shape factor (a/b) was calculated by setting the axis perpendicular to a as b. Similarly, a crystallization test was conducted on the untreated mother liquor under the same conditions. The results are shown in Table 2.
−６２−表
第１表Ｉこ示ｒと＆ｉす、−？レート樹脂で税金ｌ処Ｊ
Ｉ Ｌ、た母液中の全１ｔ１！含有社は、未処理母液に
叱し°Ｃ極めて僅かとなるから、これを再度系内に導入
ぜしめることｌこよって順次硫安母液中の媒品剤の媒晶
能を阻害する金属類の含有；Ａを低減せしめろことがで
きるから、阻害金属が硫安結晶に付着して系外へ排出さ
れるのを待つ必要がなく、また、硫安母液を廃棄しＣ新
しい母液を調製ｒる必要もない。-62-Table 1 Table I shows r and &i, -? Tax treatment with rate resin J
I L, total 1t1 in the mother liquor! The company that contains the untreated mother liquor has to re-introduce it into the system because the temperature is extremely low.Thus, the content of metals that inhibit the modulating ability of the medium agent in the ammonium sulfate mother liquor is gradually reduced. ; Since A can be reduced, there is no need to wait for inhibiting metals to adhere to ammonium sulfate crystals and be discharged from the system, and there is no need to discard the ammonium sulfate mother liquor and prepare a new mother liquor. .
第１図は実施例で使用した脱金属試験装置の系統図、第
２図は同じく晶析装置の系統図である。
１．５・・・ポリエチレンタンク、２・・・ポンプ、３
・・・フィルター、４・・・カラム、１１・・・ｌｔＪ
： 液Ａ４Ｖ 、１２・・・スチームヒーター、１３・
・・攪拌機、１４・・・循環ポンプ、１５・・・母液ク
ーラー、１６・・・結晶槽。
出願人 住金化工株式会社
代理人 押 １） 良 久し１〕FIG. 1 is a system diagram of the demetallization test apparatus used in the examples, and FIG. 2 is a system diagram of the crystallization apparatus. 1.5...Polyethylene tank, 2...Pump, 3
...filter, 4...column, 11...ltJ
: Liquid A4V, 12...Steam heater, 13.
... Stirrer, 14... Circulation pump, 15... Mother liquor cooler, 16... Crystallization tank. Applicant Sumikin Chemical Co., Ltd. Agent Oshi 1) Ryo Hisashi 1]
Claims (1)
晶析装置を経て粒状硫安を製造する方法において、媒晶
剤の媒晶能阻害金属混入時、硫安母液の一部を系外に抜
き出し、ＰＨ２，５〜５に調腎した後、キレート樹脂に
より含有金属類を除去し、再度系内に導入して晶析せし
めることを特徴とする粒状硫安の製造法。1 In a method for producing granular ammonium sulfate from an ammonium sulfate mother liquor containing sulfamino acid or its salts through a crystallizer, when a metal that inhibits the modulating ability of the crystal modifier is mixed, a part of the ammonium sulfate mother liquor is extracted from the system and the pH is adjusted to 2.5. A method for producing granular ammonium sulfate, which comprises conditioning the mixture to a temperature of 1 to 5, removing metals contained therein using a chelate resin, and reintroducing the mixture into the system for crystallization.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP20676083A JPS60103022A (en) | 1983-11-01 | 1983-11-01 | Manufacture of granular ammonium sulfate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP20676083A JPS60103022A (en) | 1983-11-01 | 1983-11-01 | Manufacture of granular ammonium sulfate |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPS60103022A true JPS60103022A (en) | 1985-06-07 |
Family
ID=16528631
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP20676083A Pending JPS60103022A (en) | 1983-11-01 | 1983-11-01 | Manufacture of granular ammonium sulfate |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS60103022A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2002193614A (en) * | 2000-12-22 | 2002-07-10 | Nippon Steel Chem Co Ltd | Method of producing granular ammonium sulfate |
| JP2014237566A (en) * | 2013-06-07 | 2014-12-18 | Ｊｆｅケミカル株式会社 | Method for producing granular ammonium sulfate |
-
1983
- 1983-11-01 JP JP20676083A patent/JPS60103022A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2002193614A (en) * | 2000-12-22 | 2002-07-10 | Nippon Steel Chem Co Ltd | Method of producing granular ammonium sulfate |
| JP2014237566A (en) * | 2013-06-07 | 2014-12-18 | Ｊｆｅケミカル株式会社 | Method for producing granular ammonium sulfate |
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