JPH0675681B2 - Regeneration method of ion exchange resin - Google Patents
Regeneration method of ion exchange resinInfo
- Publication number
- JPH0675681B2 JPH0675681B2 JP1185997A JP18599789A JPH0675681B2 JP H0675681 B2 JPH0675681 B2 JP H0675681B2 JP 1185997 A JP1185997 A JP 1185997A JP 18599789 A JP18599789 A JP 18599789A JP H0675681 B2 JPH0675681 B2 JP H0675681B2
- Authority
- JP
- Japan
- Prior art keywords
- exchange resin
- ion exchange
- water
- organic solvent
- resin layer
- 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 - Lifetime
Links
- NWUYHJFMYQTDRP-UHFFFAOYSA-N 1,2-bis(ethenyl)benzene;1-ethenyl-2-ethylbenzene;styrene Chemical compound C=CC1=CC=CC=C1.CCC1=CC=CC=C1C=C.C=CC1=CC=CC=C1C=C NWUYHJFMYQTDRP-UHFFFAOYSA-N 0.000 title claims description 68
- 239000003456 ion exchange resin Substances 0.000 title claims description 65
- 229920003303 ion-exchange polymer Polymers 0.000 title claims description 65
- 238000011069 regeneration method Methods 0.000 title claims description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 47
- 239000007788 liquid Substances 0.000 claims description 40
- 239000003960 organic solvent Substances 0.000 claims description 31
- 238000000034 method Methods 0.000 claims description 19
- 230000008929 regeneration Effects 0.000 claims description 16
- 238000007664 blowing Methods 0.000 claims description 10
- 238000005406 washing Methods 0.000 claims description 10
- 238000009835 boiling Methods 0.000 claims description 9
- 239000011347 resin Substances 0.000 claims description 9
- 229920005989 resin Polymers 0.000 claims description 9
- 230000001172 regenerating effect Effects 0.000 claims description 6
- 150000001450 anions Chemical class 0.000 claims description 5
- 150000001768 cations Chemical class 0.000 claims description 5
- 150000002500 ions Chemical class 0.000 claims description 2
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 33
- 238000005342 ion exchange Methods 0.000 description 16
- 239000000243 solution Substances 0.000 description 11
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 10
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 6
- 239000000203 mixture Substances 0.000 description 6
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 5
- 239000003729 cation exchange resin Substances 0.000 description 5
- 238000011049 filling Methods 0.000 description 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 238000010793 Steam injection (oil industry) Methods 0.000 description 3
- 239000003957 anion exchange resin Substances 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- 238000004140 cleaning Methods 0.000 description 2
- 238000009833 condensation Methods 0.000 description 2
- 230000005494 condensation Effects 0.000 description 2
- 229910001873 dinitrogen Inorganic materials 0.000 description 2
- 238000000605 extraction Methods 0.000 description 2
- -1 hydrogen ions Chemical class 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 239000012492 regenerant Substances 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 239000002253 acid Substances 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 229940023913 cation exchange resins Drugs 0.000 description 1
- 239000003518 caustics Substances 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 238000002242 deionisation method Methods 0.000 description 1
- 238000000635 electron micrograph Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 235000010755 mineral Nutrition 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 235000011121 sodium hydroxide Nutrition 0.000 description 1
- 229910001415 sodium ion Inorganic materials 0.000 description 1
Landscapes
- Treatment Of Water By Ion Exchange (AREA)
Description
【発明の詳細な説明】 〔産業上の利用分野〕 本発明はイオン交換樹脂の改良された再生方法に関する
ものである。DETAILED DESCRIPTION OF THE INVENTION [Field of Industrial Application] The present invention relates to an improved method for regenerating an ion exchange resin.
イオン交換樹脂には陽イオン交換樹脂と陰イオン交換樹
脂とがあり、陽イオンまたは陰イオンを含有する溶液
（以下、「処理液」と言う）を、イオン交換樹脂を充填
したカラム（イオン交換塔）に通液すると、処理液中の
陽イオンまたは陰イオンは、イオン交換樹脂中の他のイ
オンたとえば水素イオンまなたは水酸基イオンと交換し
除去される。The ion exchange resin includes a cation exchange resin and an anion exchange resin, and a solution containing a cation or an anion (hereinafter referred to as “treatment liquid”) is a column packed with the ion exchange resin (ion exchange tower). ), The cations or anions in the treatment liquid are exchanged with other ions in the ion exchange resin, for example, hydrogen ions or hydroxyl ions to be removed.
したがって、このイオン交換能力は処理液の通液の経過
と共に次第に低下し、遂にはイオン交換しなくなるの
で、適当な時点でイオン交換樹脂を再生しなければなら
ない。Therefore, this ion exchange capacity gradually decreases with the passage of the processing solution, and finally ion exchange is stopped. Therefore, the ion exchange resin must be regenerated at an appropriate time.
イオン交換樹脂の再生は通常次の方法で行われる。即ち
処理液の通液停止、処理液の抜液、再生前の洗浄、洗浄
水の抜液、再生、再生液の抜液、再生後の洗浄、洗浄水
の抜液、処理液の通液の順序に従って行われる。Regeneration of the ion exchange resin is usually performed by the following method. That is, stopping the passage of the treatment liquid, draining the treatment liquid, washing before regeneration, draining the washing water, regeneration, draining the regeneration liquid, washing after regeneration, draining the washing water, passing the treatment liquid. It is done in order.
再生前の洗浄は、イオン交換樹脂に含浸している処理液
を回収するのが目的で、通常水をイオン交換塔へ通水ま
たは水張・抜水する操作を数回繰返し、処理液を回収
後、必要に応じ更に水洗を続行（水洗後は廃棄）する方
法で行われる。然しこの方法は処理液の回収の目的は達
するものの、希薄な処理液を相当量生ずる。この希薄な
処理液は、何れかの方法で濃縮しなければならず、エネ
ルギーの損失は無視出来ない。The purpose of cleaning before regeneration is to recover the treatment liquid that has been impregnated in the ion exchange resin.Normally, water is passed through the ion exchange tower or the operation of filling and draining water is repeated several times to collect the treatment liquid. After that, if necessary, further washing with water is continued (discarding after washing). However, although this method achieves the purpose of recovering the processing liquid, it produces a considerable amount of dilute processing liquid. This dilute processing liquid must be concentrated by any method, and the energy loss cannot be ignored.
この問題を解消するため、処理液の回収を多段で行う方
法もある。この方法は上記方法に比較して希薄な処理液
の発生量はある程度減少するものの、洗浄時間が長くな
るという欠点がある。In order to solve this problem, there is also a method of collecting the processing liquid in multiple stages. Although this method reduces the amount of dilute treatment liquid generated to some extent as compared with the above method, it has the drawback of increasing the cleaning time.
そこで本発明者らは先に希薄な処理液の発生をなくし、
再生前の所要時間を削減した再生方法、すなわち処理液
をイオン交換樹脂層に通液して処理液中の陽イオンまた
は陰イオンを脱イオンした後のイオン交換樹脂を再生す
る際、処理液を該イオン交換樹脂層から抜液後、該イオ
ン交換樹脂層へ水蒸気を樹脂層下部より吹き込む方法を
発明した（特開昭62-42748号）。しかし、この方法は残
存有機溶媒を全量水蒸気により蒸発させなければならな
いため、多量の水蒸気を必要とする欠点があった。ま
た、水蒸気を可能な限り減らすためには、予め抜液操作
が必要であった。Therefore, the present inventors first eliminated the generation of a dilute processing liquid,
A regeneration method that reduces the time required before regeneration, that is, when the treatment liquid is passed through the ion-exchange resin layer and the cations or anions in the treatment liquid are deionized, the treatment liquid is regenerated. After draining the ion-exchange resin layer, a method of injecting water vapor into the ion-exchange resin layer from below the resin layer was invented (JP-A-62-42748). However, this method has a drawback that a large amount of water vapor is required because the entire amount of residual organic solvent must be evaporated by water vapor. Further, in order to reduce the water vapor as much as possible, it was necessary to perform a draining operation in advance.
本発明者等はイオン交換樹脂の再生に当り、使用する水
蒸気量を極力減少させる方法について、鋭意検討した結
果、イオン交換樹脂層に水蒸気を吹込む際、イオン交換
樹脂層の上部より吹き込めば使用水蒸気量を大幅に削減
出来ることを見出し、本発明を完成するに至ったもので
ある。The present inventors have diligently studied a method of reducing the amount of water vapor used in regenerating the ion exchange resin, and as a result, when injecting water vapor into the ion exchange resin layer, if it is blown from above the ion exchange resin layer, it is used. The inventors have found that the amount of water vapor can be significantly reduced, and have completed the present invention.
即ち本発明のイオン交換樹脂の再生方法は、水可溶性で
沸点が水より低い有機溶媒を含む溶液（処理液）をイオ
ン交換樹脂層に通液して該処理液中の陽イオンまたは陰
イオンを脱イオンした後、該イオン交換樹脂を再生する
方法であって、該イオン交換樹脂層上部より水蒸気を吹
き込むことを特徴とするイオン交換樹脂の再生方法であ
る。That is, the method for regenerating an ion exchange resin of the present invention is a solution (treatment liquid) containing a water-soluble organic solvent having a boiling point lower than that of water, which is passed through the ion exchange resin layer to remove cations or anions in the treatment liquid. A method of regenerating the ion exchange resin after deionization, which is characterized in that steam is blown from the upper portion of the ion exchange resin layer.
本発明を更に具体的に説明する。 The present invention will be described more specifically.
本発明におけるイオン交換樹脂の再生順序は通常次の通
り実施される。The regeneration order of the ion exchange resin in the present invention is usually carried out as follows.
１）イオン交換樹脂層への処理液の通液を停止する。1) Stop passing the treatment liquid through the ion exchange resin layer.
２）イオン交換樹脂層への水蒸気を上部より吹き込む。2) Blow steam into the ion exchange resin layer from above.
３）イオン交換樹脂層へ再生液を通液し、イオン交換樹
脂を再生する。3) The regenerant is passed through the ion exchange resin layer to regenerate the ion exchange resin.
４）再生後はイオン交換塔内の再生液を抜液する。4) After regeneration, drain the regeneration liquid in the ion exchange tower.
５）イオン交換樹脂層へ通水しイオン交換樹脂を洗浄す
る。5) Water is passed through the ion exchange resin layer to wash the ion exchange resin.
６）イオン交換塔内の水を抜水する。6) Drain the water in the ion exchange tower.
７）イオン交換樹脂層へ処理液を通液する。7) Pass the treatment liquid through the ion exchange resin layer.
本発明の対象とする処理液は、水可溶性で沸点が水より
低い有機溶媒を含む溶液である（以下特に明記しない限
り水可溶性で沸点が水より低い有機溶媒を単に有機溶媒
と記す）。即ち、有機溶媒と水及び溶質からなる三成分
系、または有機溶媒と溶質からなる二成分系の溶液であ
る。The treatment liquid targeted by the present invention is a solution containing a water-soluble organic solvent having a lower boiling point than water (hereinafter, a water-soluble organic solvent having a lower boiling point than water is simply referred to as an organic solvent unless otherwise specified). That is, it is a three-component system solution consisting of an organic solvent, water and a solute, or a two-component system solution comprising an organic solvent and a solute.
溶質が不揮発性または水より沸点の高い物質である場合
は、次の工程であるイオン交換樹脂層への水蒸気の吹き
込みによって、イオン交換樹脂層に含浸している有機溶
媒は回収されるものの溶質は回収されないので、溶質の
完全な回収を図るためには、イオン交換樹脂層への水蒸
気の吹き込みに先立ってイオン交換樹脂層を有機溶媒で
洗浄するのが好ましく、この洗浄する有機溶媒は処理液
中に含まれる有機溶媒と同一のものであれば更に好まし
い。When the solute is a non-volatile substance or a substance having a boiling point higher than that of water, by blowing water vapor into the ion exchange resin layer in the next step, the organic solvent impregnated in the ion exchange resin layer is recovered but the solute is Since it is not collected, in order to recover the solute completely, it is preferable to wash the ion exchange resin layer with an organic solvent prior to blowing the water vapor into the ion exchange resin layer. More preferably, it is the same as the organic solvent contained in.
またこの洗浄した有機溶媒をそのまま利用出来る場合は
好適である。この様な好適な例として後述する実施例に
示す如く、有機溶媒による湿式燐酸精製プロセスが挙げ
られる。Further, it is suitable when the washed organic solvent can be used as it is. As such a suitable example, a wet phosphoric acid refining process using an organic solvent can be mentioned as shown in Examples described later.
イオン交換樹脂層の有機溶媒での洗浄は、ダウンフロー
にて行う。The washing of the ion exchange resin layer with the organic solvent is performed by a down flow.
尚溶質の沸点が水より低い場合は、後述するイオン交換
樹脂層への水蒸気の吹き込みによって、溶質は有機溶媒
と共に蒸発し回収出来るので、上記有機溶媒での洗浄は
必要ないが、処理液中の有機溶媒の含有量が少ない場合
は有機溶媒で洗浄した方が、後の工程であるイオン交換
樹脂層への水蒸気の吹き込み操作がやりやすい。When the boiling point of the solute is lower than that of water, by blowing water vapor into the ion exchange resin layer described later, the solute can be evaporated and recovered together with the organic solvent, so washing with the organic solvent is not necessary, but in the treatment liquid. When the content of the organic solvent is small, it is easier to wash with the organic solvent in the subsequent step, which is a step of blowing water vapor into the ion exchange resin layer.
本発明における水蒸気の吹き込みについて説明する。The blowing of steam in the present invention will be described.
イオン交換樹脂層への処理液の通液を停止後、水蒸気を
イオン交換樹脂塔の塔頂より吹き込むと、水蒸気の圧力
により塔内の処理液は塔底より押し出される。次に樹脂
層上部が水蒸気により加熱され、樹脂中に含浸している
有機溶媒は蒸発する。この有機溶媒蒸気は下部の樹脂に
熱を伝え凝縮し、更に下部の樹脂に熱を伝えながら流出
する。この様にして樹脂に含浸している有機溶媒は水蒸
気により一旦、蒸発するが下方に熱交換できる樹脂層が
ある間は凝縮液として抜き出すことができる。しかし、
塔底の樹脂温度が上昇してくると、有機溶媒蒸気は塔内
で凝縮されないため、系外の凝縮器を用いて回収する。When water vapor is blown from the top of the ion exchange resin column after stopping the passage of the treatment liquid through the ion exchange resin layer, the treatment liquid in the column is pushed out from the bottom by the pressure of the water vapor. Next, the upper part of the resin layer is heated by steam, and the organic solvent impregnated in the resin is evaporated. The organic solvent vapor transfers heat to the lower resin and condenses, and then flows out while transferring heat to the lower resin. In this way, the organic solvent impregnated in the resin is once evaporated by water vapor, but can be extracted as a condensate while there is a resin layer below which heat exchange is possible. But,
When the temperature of the resin at the bottom of the column rises, the organic solvent vapor is not condensed inside the column, so it is recovered using a condenser outside the system.
この様にして、イオン交換樹脂層に水蒸気を吹き込んで
行くと、始めはイオン交換樹脂層上部に含浸している有
機溶媒が蒸発するが、すぐに凝縮し凝縮液として回収さ
れるので、イオン交換塔の塔底で回収される気体部分の
温度は変化しない。その後、該部分の温度は有機溶媒と
水との共沸点を示す。更に続け、有機溶媒が蒸発してし
まうと該部分の温度は急に上昇する。この時点で水蒸気
の吹き込みを停止すればよい。In this way, when water vapor is blown into the ion-exchange resin layer, the organic solvent impregnated in the upper part of the ion-exchange resin layer evaporates at first, but it immediately condenses and is recovered as a condensate. The temperature of the gas part recovered at the bottom of the column does not change. Then, the temperature of the portion shows the azeotropic point of the organic solvent and water. Further, when the organic solvent evaporates, the temperature of the portion suddenly rises. At this point, the blowing of steam may be stopped.
イオン交換樹脂層へ吹き込む水蒸気の圧力はゲージ圧力
で0.5Kg/cm2・Ｇ〜5Kg/cm2・Ｇ程度が好ましい。圧力が
0.5Kg/cm2・Ｇ未満では、イオン交換樹脂に含浸してい
る有機溶媒が十分蒸発されないので好ましくなく、また
圧力があまり高過ぎると水蒸気の吹込量が調節しにくい
ので好ましくない。The pressure of the steam blown to the ion exchange resin layer is 0.5Kg / cm 2 · G~5Kg / cm 2 · about G is preferably a gauge pressure. Pressure is
If it is less than 0.5 Kg / cm 2 · G, the organic solvent impregnated in the ion exchange resin is not sufficiently evaporated, and if the pressure is too high, it is difficult to control the amount of steam blown, which is not preferable.
イオン交換樹脂への水蒸気の吹き込み量はイオン交換樹
脂の粒径により若干異なるが、イオン交換樹脂層１m2当
たり、200〜300Kg/h程度が好ましい。これより多いと精
溜効果が薄れ、得られる有機溶媒濃度が低くなるので好
ましくなく、また、これより少ないと所要時間が長くな
るので好ましくない。The amount of water vapor blown into the ion exchange resin varies slightly depending on the particle size of the ion exchange resin, but is preferably about 200 to 300 kg / h per 1 m 2 of the ion exchange resin layer. If it is more than this range, the rectification effect will be weakened and the concentration of the organic solvent obtained will be low, which is not preferable.
イオン交換樹脂の再生は、陽イオン交換樹脂にあっては
濃度５〜10重量％の硫酸、塩酸などの鉱酸水溶液を、陰
イオン交換樹脂にあっては濃度５〜10重量％の苛性ソー
ダなどの苛性アルカリを、イオン交換塔へ通液するそれ
自体公知の方法で実施される。Regeneration of the ion exchange resin is carried out by using an aqueous solution of mineral acid such as sulfuric acid and hydrochloric acid having a concentration of 5 to 10% by weight for the cation exchange resin and caustic soda having a concentration of 5 to 10% by weight for the anion exchange resin. It is carried out by a method known per se in which caustic is passed through an ion exchange column.
かくしてイオン交換樹脂層への水蒸気の吹込みが終了す
れば、イオン交換樹脂はそれ自体公知の方法により再生
液による再生及び再生後の水洗を行えば良い。When the blowing of water vapor into the ion-exchange resin layer is completed in this way, the ion-exchange resin may be regenerated with a regenerant and washed with water after regeneration by a method known per se.
尚本発明はこの様にイオン交換樹脂層へ水蒸気を吹込む
ので、イオン交換樹脂は当然100℃以上の耐熱性のある
ものであることが好ましい。この様な耐熱性のあるイオ
ン交換樹脂としては、陽イオン交換樹脂では西独バイエ
ル社製レバチットSP-112、レバチットSP-120、栗田工業
（株）製C-111、C-132、陰イオン交換樹脂では栗田工業
（株）製A-168等がある。Since the present invention blows water vapor into the ion-exchange resin layer in this manner, it is preferable that the ion-exchange resin has heat resistance of 100 ° C. or higher. Examples of such heat-resistant ion-exchange resins include cation-exchange resins such as Levitit SP-112, Levatit SP-120 manufactured by Bayer in Germany, C-111, C-132, anion-exchange resins manufactured by Kurita Water Industries Ltd. Then there is A-168 etc. made by Kurita Water Industries Ltd.
以下実施例及び比較例により本発明を具体的に説明す
る。尚実施例及び比較例において％は重量％を示す。The present invention will be specifically described below with reference to Examples and Comparative Examples. In the examples and comparative examples,% means% by weight.
実施例１ P2O5濃度54.3％の湿式燐酸液にイソプロピルアルコール
を加え、湿式燐酸中の遊離燐酸分を抽出して第１表に示
す組成の抽出液を得た。Example 1 Isopropyl alcohol was added to a wet phosphoric acid solution having a P 2 O 5 concentration of 54.3% to extract free phosphoric acid in the wet phosphoric acid to obtain an extract solution having the composition shown in Table 1.
陽イオン交換樹脂レバチットSP-112（西独バイエル社
製）を充填した塔径1.5m、塔高6.4mのイオン交換塔（イ
オン交換樹脂充填高さ4.5m）に、第１表に示す組成の抽
出液を16m3/hの流量でアップフローにて通液し、含有す
るNaイオンを脱イオン処理した。7.5時間通液したとこ
ろでイオン交換処理能力が低下したので通液をストップ
した。 Extraction of the composition shown in Table 1 into an ion exchange column (ion exchange resin filling height of 4.5 m) with a column diameter of 1.5 m and a tower height of 6.4 m packed with cation exchange resin Levatit SP-112 (manufactured by Bayer, West Germany) The liquid was passed through the upflow at a flow rate of 16 m 3 / h, and the contained Na ions were deionized. When the solution had been passed for 7.5 hours, the ion exchange treatment capacity deteriorated, so the flow was stopped.
その後、濃度87％のイソプロピルアルコールを用い、15
m3/hの流量でダウンフローにて２時間イオン交換樹脂を
洗浄した。次いで、イオン交換塔の上部からゲージ圧力
1.5Kg/cm2・Ｇの水蒸気を500kg/hの流量で吹き込み、イ
オン交換塔下部出口に設置した気液分離器により分離し
流出液９m3と、蒸気を冷却器で凝縮した液１m3を回収し
た。気液分離器の蒸気部の温度は、始め50℃であった
が、水蒸気吹き込み開始後30分の時点より80℃となり、
70分後の時点ではこの温度が95℃に達したので水蒸気の
吹き込みを中止した（水蒸気使用量約580kg）。Then, using isopropyl alcohol with a concentration of 87%,
The ion exchange resin was washed for 2 hours with down flow at a flow rate of m 3 / h. Then from the top of the ion exchange tower, gauge pressure
Blows 1.5 Kg / cm 2 · G of water vapor at a flow rate of 500 kg / h and separates 9 m 3 of effluent separated by a gas-liquid separator installed at the lower outlet of the ion exchange tower and 1 m 3 of liquid condensed by a cooler. Recovered. The temperature of the vapor part of the gas-liquid separator was 50 ° C. at the beginning, but it became 80 ° C. from 30 minutes after the start of steam injection,
After 70 minutes, this temperature reached 95 ° C, so blowing of steam was stopped (steam usage of about 580 kg).
上記凝縮により回収した液の組成はイソプロピルアルコ
ール濃度83％（残余は水）、気液分離器より流出した液
の組成はイソプロピルアルコール濃度87％（残余は水）
であった。尚この回収したイソプロピルアルコールは、
湿式燐酸の抽出用溶媒として再利用できた。The composition of the liquid recovered by the above condensation is 83% isopropyl alcohol concentration (the rest is water), and the composition of the liquid flowing out from the gas-liquid separator is 87% isopropyl alcohol concentration (the rest is water).
Met. The recovered isopropyl alcohol is
It could be reused as a solvent for extraction of wet phosphoric acid.
次いでイオン交換塔へ、アップフローで水張りした後、
濃度9.5％の硫酸水溶液16m3をダウンフローで20m3/hの
速度で50分間通液させ、イオン交換樹脂の再生を行っ
た。再生後のイオン交換樹脂は上水で十分洗浄した。尚
再生後の再生液中にはイソプロピルアルコールは殆んど
存在しなく、イソプロピルアルコールの損失は無視出来
る程度であった。Then, after filling the ion exchange tower with upflow,
An ion exchange resin was regenerated by passing 16 m 3 of a 9.5% concentration aqueous sulfuric acid solution through the downflow at a rate of 20 m 3 / h for 50 minutes. The regenerated ion exchange resin was thoroughly washed with clean water. Almost no isopropyl alcohol was present in the regenerated liquid after regeneration, and the loss of isopropyl alcohol was negligible.
かくして再生した陽イオン交換樹脂の１部を電子顕微鏡
写真撮影で観察したが、イオン交換樹脂の粒子の形状に
変化は認められなかった。A part of the cation exchange resin thus regenerated was observed by electron micrograph photography, but no change was observed in the shape of the particles of the ion exchange resin.
比較例１ 実施例１と同様にして抽出液の通液をストップした。そ
の後、濃度87％のイソプロピルアルコールを用い、15m3
/hの流量でダウンフローにて２時間イオン交換樹脂を洗
浄した後、窒素ガスを用い、イオン交換塔内のイソプロ
ピルアルコールを溶媒タンクへ抜液した（抜液所要時間
30分）。Comparative Example 1 In the same manner as in Example 1, the passage of the extract was stopped. Then, using isopropyl alcohol with a concentration of 87%, 15m 3
After washing the ion exchange resin for 2 hours at a flow rate of / h, the isopropyl alcohol in the ion exchange tower was drained to the solvent tank using nitrogen gas (required draining time
Half an hour).
次いでイオン交換樹脂塔の下部からゲージ圧力1.5Kg/cm
2・Ｇの水蒸気を1200Kg/hの流量で吹込み、イオン交換
塔頂部より発生した蒸気を冷却器で凝縮させ回収した。Next, from the bottom of the ion exchange resin tower, a gauge pressure of 1.5 Kg / cm
2. G water vapor was blown at a flow rate of 1200 kg / h, and the vapor generated from the top of the ion exchange column was condensed by a cooler and collected.
イオン交換塔頂部の温度は、始め80℃でイソプロピルア
ルコールと水との共沸組成物の沸点を示した。この温度
が95℃に達し、水蒸気の吹き込みを中止したのは水蒸気
吹込開始後約70分の時点であった（水蒸気使用量約1400
kg）。The temperature at the top of the ion exchange column was initially 80 ° C., and the boiling point of the azeotropic composition of isopropyl alcohol and water was shown. It was about 70 minutes after the start of the steam injection that the temperature reached 95 ° C and the steam injection was stopped.
kg).
上記凝縮により回収した液の組成はイソプロピルアルコ
ール濃度約86％（残余は水）であった。The composition of the liquid recovered by the above condensation had an isopropyl alcohol concentration of about 86% (the balance was water).
次いで実施例１と同様にしてイオン交換塔へ、アップフ
ローで水張りした後、濃度9.5％の硫酸水溶液16m3をダ
ウンフローで20m3/hの速度で50分間通液させ、イオン交
換樹脂の再生を行った。再生後のイオン交換樹脂は上水
で十分洗浄した 〔発明の効果〕 以上詳細に述べた様に、本発明の方法により、イオン交
換樹脂の再生の際、従来多量に必要であった水蒸気の使
用量を大幅に削減することができた。又、水蒸気の吹き
込み前に必要であった抜液操作が省略できたため、その
際使用していた窒素ガスが必要なくなった。Then, in the same manner as in Example 1, after filling the ion exchange column with upflow, 16 m 3 of a 9.5% concentration aqueous sulfuric acid solution was passed through the downflow at a rate of 20 m 3 / h for 50 minutes to regenerate the ion exchange resin. I went. The ion-exchange resin after regeneration was thoroughly washed with clean water [Effect of the invention] As described in detail above, according to the method of the present invention, when regenerating the ion-exchange resin, the use of a large amount of steam, which was conventionally required, was used. The amount could be reduced significantly. Further, since the draining operation required before the blowing of the steam can be omitted, the nitrogen gas used at that time is no longer necessary.
すなわち、本発明は大幅なコスト削減を行い、然もイオ
ン交換樹脂再生の所要時間を短縮したもので、その経済
的な効果大なるものがある。That is, the present invention significantly reduces the cost and shortens the time required to regenerate the ion exchange resin, and has a great economical effect.
Claims (3)
む溶液（処理液）をイオン交換樹脂層に通液して該処理
液中の陽イオンまたは陰イオンを脱イオンした後、該イ
オン交換樹脂層に再生液を通液し該イオン交換樹脂を再
生する方法において、再生液を通液する前に該イオン交
換樹脂層上部より水蒸気を吹き込むことを特徴とするイ
オン交換樹脂の再生方法。1. A solution (treatment liquid) containing a water-soluble organic solvent having a boiling point lower than that of water is passed through an ion exchange resin layer to deionize cations or anions in the treatment liquid, and then the ion A method for regenerating an ion exchange resin by passing a regeneration liquid through an exchange resin layer, characterized in that steam is blown from above the ion exchange resin layer before the regeneration liquid is passed through.
先立って該イオン交換樹脂を水可溶性で沸点が水より低
い有機溶媒で洗浄することを特徴とする特許請求の範囲
第１項記載の方法。2. The method according to claim 1, wherein the ion exchange resin is washed with an organic solvent which is water-soluble and has a boiling point lower than that of water, prior to blowing the water vapor into the ion exchange resin layer. .
が水より低い有機溶媒が処理液中に含まれる有機溶媒と
同一の有機溶媒であることを特徴とする特許請求の範囲
第２項記載の方法。3. The water-soluble organic solvent having a boiling point lower than that of water for washing the ion exchange resin is the same organic solvent as the organic solvent contained in the treatment liquid. the method of.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP1185997A JPH0675681B2 (en) | 1989-07-20 | 1989-07-20 | Regeneration method of ion exchange resin |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP1185997A JPH0675681B2 (en) | 1989-07-20 | 1989-07-20 | Regeneration method of ion exchange resin |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH0352649A JPH0352649A (en) | 1991-03-06 |
| JPH0675681B2 true JPH0675681B2 (en) | 1994-09-28 |
Family
ID=16180565
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP1185997A Expired - Lifetime JPH0675681B2 (en) | 1989-07-20 | 1989-07-20 | Regeneration method of ion exchange resin |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH0675681B2 (en) |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP6481424B2 (en) * | 2014-03-20 | 2019-03-13 | 三菱ケミカル株式会社 | How to remove the catalyst |
| JP7543741B2 (en) | 2020-07-10 | 2024-09-03 | 日産化学株式会社 | Method for producing coating film-forming composition for lithography |
-
1989
- 1989-07-20 JP JP1185997A patent/JPH0675681B2/en not_active Expired - Lifetime
Also Published As
| Publication number | Publication date |
|---|---|
| JPH0352649A (en) | 1991-03-06 |
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