JPH02144144A - Method for regenerating ion-exchange resin - Google Patents
Method for regenerating ion-exchange resinInfo
- Publication number
- JPH02144144A JPH02144144A JP29827188A JP29827188A JPH02144144A JP H02144144 A JPH02144144 A JP H02144144A JP 29827188 A JP29827188 A JP 29827188A JP 29827188 A JP29827188 A JP 29827188A JP H02144144 A JPH02144144 A JP H02144144A
- Authority
- JP
- Japan
- Prior art keywords
- exchange resin
- regeneration
- gas
- ion exchange
- resin
- 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.)
- Granted
Links
- 239000003456 ion exchange resin Substances 0.000 title claims abstract description 50
- 229920003303 ion-exchange polymer Polymers 0.000 title claims abstract description 50
- 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 abstract description 48
- 230000001172 regenerating effect Effects 0.000 title claims abstract description 23
- 238000000034 method Methods 0.000 title claims description 19
- 230000008929 regeneration Effects 0.000 claims abstract description 56
- 238000011069 regeneration method Methods 0.000 claims abstract description 56
- XSTXAVWGXDQKEL-UHFFFAOYSA-N Trichloroethylene Chemical group ClC=C(Cl)Cl XSTXAVWGXDQKEL-UHFFFAOYSA-N 0.000 claims abstract description 29
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 21
- UBOXGVDOUJQMTN-UHFFFAOYSA-N trichloroethylene Natural products ClCC(Cl)Cl UBOXGVDOUJQMTN-UHFFFAOYSA-N 0.000 claims abstract description 19
- UOCLXMDMGBRAIB-UHFFFAOYSA-N 1,1,1-trichloroethane Chemical compound CC(Cl)(Cl)Cl UOCLXMDMGBRAIB-UHFFFAOYSA-N 0.000 claims abstract description 15
- 230000018044 dehydration Effects 0.000 abstract description 29
- 238000006297 dehydration reaction Methods 0.000 abstract description 29
- 238000001179 sorption measurement Methods 0.000 abstract description 20
- 239000011347 resin Substances 0.000 abstract description 9
- 229920005989 resin Polymers 0.000 abstract description 9
- 238000009833 condensation Methods 0.000 abstract description 6
- 230000005494 condensation Effects 0.000 abstract description 6
- 230000003134 recirculating effect Effects 0.000 abstract description 3
- 239000007789 gas Substances 0.000 description 42
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 12
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 6
- 238000001816 cooling Methods 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 5
- 238000004064 recycling Methods 0.000 description 5
- 230000007613 environmental effect Effects 0.000 description 4
- 238000005260 corrosion Methods 0.000 description 3
- 230000007797 corrosion Effects 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 229910052757 nitrogen Inorganic materials 0.000 description 3
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 description 2
- 230000002378 acidificating effect Effects 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 2
- 239000001110 calcium chloride Substances 0.000 description 2
- 229910001628 calcium chloride Inorganic materials 0.000 description 2
- 239000003729 cation exchange resin Substances 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 238000000354 decomposition reaction Methods 0.000 description 2
- 239000011261 inert gas Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 150000002739 metals Chemical class 0.000 description 2
- 239000003507 refrigerant Substances 0.000 description 2
- SCYULBFZEHDVBN-UHFFFAOYSA-N 1,1-Dichloroethane Chemical compound CC(Cl)Cl SCYULBFZEHDVBN-UHFFFAOYSA-N 0.000 description 1
- 238000009825 accumulation Methods 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000004063 acid-resistant material Substances 0.000 description 1
- 229910000963 austenitic stainless steel Inorganic materials 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229940023913 cation exchange resins Drugs 0.000 description 1
- HRYZWHHZPQKTII-UHFFFAOYSA-N chloroethane Chemical compound CCCl HRYZWHHZPQKTII-UHFFFAOYSA-N 0.000 description 1
- 238000011437 continuous method Methods 0.000 description 1
- 238000007791 dehumidification Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 229960003750 ethyl chloride Drugs 0.000 description 1
- 238000007710 freezing Methods 0.000 description 1
- 230000008014 freezing Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000004781 supercooling Methods 0.000 description 1
Landscapes
- Treatment Of Liquids With Adsorbents In General (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
Abstract
Description
【発明の詳細な説明】
イ）発明の目的
〔産業上の利用分野〕
本発明は、１，１．１−トリクロロエタンまたはトリク
ロロエチレンをイオン交換樹脂で脱水処理した後の、イ
オン交換樹脂の再生方法に関するものである。Detailed Description of the Invention A) Purpose of the Invention [Field of Industrial Application] The present invention relates to a method for regenerating an ion exchange resin after dehydrating 1,1,1-trichloroethane or trichloroethylene with an ion exchange resin. It is something.
１．１．ｌ−トリクロロエタンまたはトリクロロエチレ
ンは製造工程中、あるいは使用時に水分を吸収し、水分
を含有したｌ、１．１−トリクロロエタンまたはトリク
ロロエチレンは、熱により化学反応を起こして塩酸を生
成し、装置や容器等に用いられている金属を腐食したり
、また製品の品質にも影響を及ぼす。1.1. l-Trichloroethane or trichlorethylene absorbs moisture during the manufacturing process or during use, and the l,1,1-trichloroethane or trichloroethylene that contains moisture causes a chemical reaction with heat to produce hydrochloric acid, which may cause damage to equipment, containers, etc. It corrodes the metals used and also affects the quality of the product.
水分を含有した１、１．１−トリクロロエタンまたはト
リクロロエチレンの脱水方法としては種々の方法がある
が、作業環境上あるいは省エネルギー面より、イオン交
換樹脂による吸着脱水法が用いられることが多い。Although there are various methods for dehydrating 1,1,1-trichloroethane or trichloroethylene containing water, an adsorption dehydration method using an ion exchange resin is often used from the viewpoint of working environment or energy saving.
イオン交換樹脂による吸着脱水法における水分吸着後の
イオン交換樹脂の再生方法としては、例えば特公昭４６
−２８５２２号公報、４５−１１７３号公報記載の方法
があるが、１． １． １−トリクロロエタンまたはト
リクロロエチレンの脱水の場合、効率を高める為にそれ
らの分解温度以」：でイオン交換樹脂の乾燥再生が行な
われるため、水分と共に吸着された付着残留している１
、１゜１− ）リクロロエタンまたはトリクロロエチレ
ンが吸着水分と反応し塩酸を生じ、装置等の腐食の原因
となり、従って高価な素材の装置を用いる必要がある。As a method for regenerating an ion exchange resin after water adsorption in an adsorption dehydration method using an ion exchange resin, for example,
There are methods described in JP-28522 and JP-45-1173, but 1. 1. In the case of dehydration of 1-trichloroethane or trichloroethylene, the ion exchange resin is dried and regenerated at temperatures below their decomposition temperature in order to increase efficiency.
, 1°1-) Lichloroethane or trichloroethylene reacts with adsorbed moisture to produce hydrochloric acid, which causes corrosion of equipment, etc., and therefore requires the use of equipment made of expensive materials.
またイオン交換樹脂を再生した後の再生用循環ガスから
、水分および１，１．１−トリクロロエタンまたはトリ
クロロエチレンを離脱させるため、ガスの冷却処理が行
われるが、冷却後のガス中に残存する１、１．１−トリ
クロロエタンまたはトリクロロエチレンのａ度は高く、
これを大気中に放出すれば環境面で問題となり、またこ
れをｗｉ環使用する連続方式の場合には、循環ガスを更
に除湿をするための除湿吸着器を装備する必要があり、
再生システムが複雑で費用が嵩む等、未だ工業的に満足
する方法は見出されていない。In addition, in order to remove moisture and 1,1.1-trichloroethane or trichloroethylene from the regeneration circulating gas after regenerating the ion exchange resin, a gas cooling process is performed. 1.1-Trichloroethane or trichloroethylene has a high a degree,
If this is released into the atmosphere, it will be an environmental problem, and in the case of a continuous system that uses a wi-ring, it is necessary to equip a dehumidifying adsorption device to further dehumidify the circulating gas.
No industrially satisfactory method has yet been found, as the regeneration system is complicated and expensive.
〔発明が解決しようとする課題〕
本発明者らは、水分を含有した１、ｌ、１−トリクロロ
エタンまたはトリクロロエチレンをイオン交換樹脂で脱
水した後、イオン交換樹脂を再生するにあたり、１，１
．１−トリクロロエタンまたはトリクロロエチレンと水
分との反応を抑制して塩酸の生成を防ぎ、装置、容器等
の金属の腐食を防止し、しかも再生後の循環ガスは簡単
な処置で再生にＶＩｉ環利月利用ことが出来、環境上の
問題もないイオン交換樹脂の再生方法につき鋭意研究し
た結果、本発明を完成した。[Problem to be Solved by the Invention] The present inventors dehydrated 1,1,1-trichloroethane or trichloroethylene containing water using an ion exchange resin, and then regenerated the ion exchange resin by using 1,1
．． It suppresses the reaction between 1-trichloroethane or trichloroethylene and water to prevent the formation of hydrochloric acid, and prevents corrosion of metals such as equipment and containers. Moreover, the circulating gas after regeneration can be used for regeneration with simple treatment. As a result of intensive research into a method for regenerating ion exchange resins that can be used without causing any environmental problems, the present invention was completed.
口）発明の構成
〔！！！！題を解決する為の手段〕
本発明は、水分を含有したｉ、ｌ、ｌ−１リクロロエタ
ンまたはトリクロロエチレンの脱水に使用されたイオン
交換樹脂を、再生用循環ガスにより再生するに際し、１
，１．１−１−リクロロエタンの脱水に使用されたイオ
ン交換樹脂を再生する場合は５０℃〜７０°Ｃの再生用
循環ガスを、またトリクロロエチレンの脱水に使用され
たイオン交換樹脂を再生する場合は７０℃〜９０ ℃の
再生用循環ガスを、それぞれイオン交換樹脂と接触させ
、次いで再生用循環ガスを０℃〜１２゛Ｃに冷却して凝
縮液を分離した後、再生用循環ガスを再度循環しイオン
交換樹脂と接触させることを特徴とするイオン交換樹脂
の再生方法である。口) Structure of the invention [! ! ! ! Means for Solving the Problem] The present invention provides a method for regenerating an ion exchange resin used for dehydrating i, l, l-1 dichloroethane or trichloroethylene containing water using a regeneration circulating gas.
, 1. When regenerating the ion exchange resin used in the dehydration of 1-1-lichloroethane, use the recycling gas at 50°C to 70°C, and regenerate the ion exchange resin used in the dehydration of trichlorethylene. In this case, the regeneration circulating gas at 70°C to 90°C is brought into contact with the ion exchange resin, and then the regenerating circulating gas is cooled to 0°C to 12°C to separate the condensate, and then the regenerating circulating gas is brought into contact with the ion exchange resin. This is a method for regenerating an ion exchange resin, which is characterized by circulating the resin again and bringing it into contact with the ion exchange resin.
本発明方法は吸着脱水に使用される各種のイオン交換樹
脂、例えば強酸性陽イオン交換樹脂等の再生に適用する
ことが出来る。The method of the present invention can be applied to regenerating various ion exchange resins used for adsorption dehydration, such as strongly acidic cation exchange resins.
再生用循環ガスとしては、一般に用いられている窒素等
の不活性ガスや空気が挙げられるが、安全性の面から窒
素等の不活性ガスが好ましい。Examples of the circulating gas for regeneration include commonly used inert gases such as nitrogen and air, and from the viewpoint of safety, inert gases such as nitrogen are preferred.
イオン交換樹脂の再生の際の再生用循環ガスの温度は、
イオン交換樹脂がｌ、ｌ、１−トリクロロエタンの脱水
に使用された場合は、５０℃〜７０°Ｃ５好ましくは５
８℃〜６５°Ｃである。７０°Ｃを超えると塩酸が発生
して装置の腐食が起こり、５０°Ｃ未満では脱水が充分
に行われない。また、イオン交換樹脂がトリクロロエチ
レンの脱水に使用された場合の再生用循環ガスの温度は
、７０℃〜９０°Ｃ１好ましくは７５℃〜８５°Ｃであ
る。９０°Ｃを超えると塩酸が発生し装置の腐食を起こ
し、また７０°Ｃ未満では脱水機能が充分でない。The temperature of the regeneration circulating gas when regenerating the ion exchange resin is
When the ion exchange resin is used for dehydration of 1,1,1-trichloroethane, the temperature is 50°C to 70°C, preferably 5
The temperature is 8°C to 65°C. If the temperature exceeds 70°C, hydrochloric acid will be generated and corrosion of the equipment will occur, and if the temperature is below 50°C, sufficient dehydration will not occur. Further, when the ion exchange resin is used for dehydrating trichlorethylene, the temperature of the recycling gas for regeneration is 70°C to 90°C, preferably 75°C to 85°C. If the temperature exceeds 90°C, hydrochloric acid will be generated and the equipment will corrode, and if the temperature is below 70°C, the dehydration function will not be sufficient.
本発明においては、イオン交ｔＡｔＨ脂と接触後の再生
用循環ガスを０℃〜１２℃、好ましくは３℃〜５℃に冷
却し、ガス中の水分および１．１．１トリクロロエタン
またはトリクロロエチレンを凝縮させ、凝ｍ液の分離を
通常の気液分離操作により行った後、再生用循環ガスを
循環使用する。In the present invention, the regeneration circulating gas after contact with the ion-exchanged tAtH fat is cooled to 0°C to 12°C, preferably 3°C to 5°C, and moisture in the gas and 1.1.1 trichloroethane or trichloroethylene are condensed. After separating the condensed liquid by a normal gas-liquid separation operation, the recycling gas for regeneration is recycled.
冷却温度が０°Ｃ未満では凝縮液中の水分の凍結による
配管の閉塞等の問題が生じ、また装置上経済的に不利と
なり、１２°Ｃを超えると循環する再生用循環ガスの水
分濃度が高すぎ、該循環ガスを用いて連続再生処理を行
う場合、効率的な再生を望めず、また該ｗｉ環ガスを系
外に廃棄する場合は環境上の問題が生じる。If the cooling temperature is less than 0°C, problems such as piping blockage due to freezing of water in the condensate will occur, and it will be economically disadvantageous for the equipment, and if it exceeds 12°C, the water concentration in the circulating regeneration gas will decrease. If the recycling gas is too high and continuous regeneration treatment is performed using the circulating gas, efficient regeneration cannot be expected, and if the circulating gas is disposed of outside the system, environmental problems will occur.
再生用循環ガスを冷却する際、急冷すると局所的に過冷
却され、冷却器へ氷が付着する場合があり、これを避け
るために予備冷却を行うことは、より効率的な方法であ
る。When cooling the regenerating circulating gas, rapid cooling may result in local supercooling and ice may adhere to the cooler.To avoid this, a more efficient method is to pre-cool the gas.
本発明は上記の如く、１，１，１−トリクロロエタンお
よびトリクロロエチレンのイオン交換樹脂による脱水に
おいて、イオン交換樹脂の再生を連続的に有利に行い得
るものであり、例えば従来の方法では、脱水後の再生用
循環ガスの冷却が充分でないため、連続方式で行う場合
は除湿吸着装置を必要とし、複雑な再生システムで行わ
ざる得なかったが、再生後の循環ガスを０℃〜１２℃に
冷却することにより、除湿吸着装置を全く必要とせず、
凝縮液分離後の再生用循環ガスは相対湿度が例えば０．
７〜０．８％程度であり、そのまま加温して再生に用い
ても、再生後のイオン交換樹脂は長時間にわたって高い
脱水能力を維持しており、非常に経済的であり、また環
境上の問題もない。As described above, the present invention enables continuous and advantageous regeneration of the ion exchange resin in the dehydration of 1,1,1-trichloroethane and trichloroethylene using an ion exchange resin. Since the circulating gas for regeneration is not sufficiently cooled, a dehumidification and adsorption device is required when using a continuous method, and a complicated regeneration system has no choice but to cool the circulating gas after regeneration to 0°C to 12°C. This eliminates the need for a dehumidifying adsorption device at all.
After the condensate has been separated, the regenerating recirculating gas has a relative humidity of, for example, 0.
It is approximately 7 to 0.8%, and even if it is heated and regenerated as it is, the regenerated ion exchange resin maintains a high dehydration ability for a long time, making it very economical and environmentally friendly. No problem.
また本発明によれば装置の材質について懸念する必要が
なく、例えばオーステナイト系のステンレス鋼等を用い
れば十分であるが、安定性が比較的低い１，１．１−ト
リクロロエタンの脱水に使用されたイオン交換樹脂を再
生する場合には、吸着塔、凝縮タンクに耐酸処理を施し
たり、冷却器に耐酸材を用いることが好ましい。Furthermore, according to the present invention, there is no need to worry about the material of the equipment; for example, it is sufficient to use austenitic stainless steel, etc.; When regenerating the ion exchange resin, it is preferable to subject the adsorption tower and the condensation tank to acid-resistant treatment, and to use an acid-resistant material in the cooler.
以下、第１図に基づいて本発明を更に詳細に説明する。Hereinafter, the present invention will be explained in more detail based on FIG.
第１図は本発明方法の一実施態様を示すフローシートで
ある。１は吸着塔で、その中に強酸性陽イオン交換樹脂
２が充填されており、脱水操作においては、１，１．１
−トリクロロエタンまたはトリクロロエチレンを導入管
３より吸着塔１に導入し、イオン交換樹脂２により脱水
した後、出口管４より糸外に取り出す。FIG. 1 is a flow sheet showing one embodiment of the method of the present invention. 1 is an adsorption tower filled with a strongly acidic cation exchange resin 2;
- Trichloroethane or trichloroethylene is introduced into the adsorption tower 1 through the inlet pipe 3, dehydrated with the ion exchange resin 2, and then taken out from the thread through the outlet pipe 4.
再生操作においては、再生用循環ガスは再生用循環ガス
供給管５より系内に供給され、ブロワ−６により循環さ
れるが、まずヒーター７により所定の温度に加熱され、
熱風となり吸着塔１中に導かれる。再生用循環ガスの温
度は温度計８にて測定する。In the regeneration operation, the regeneration circulation gas is supplied into the system from the regeneration circulation gas supply pipe 5 and circulated by the blower 6, but is first heated to a predetermined temperature by the heater 7.
It becomes hot air and is guided into the adsorption tower 1. The temperature of the circulating gas for regeneration is measured with a thermometer 8.
吸着塔１に導入された再生用Ｗ１環ガスは、イオン交換
樹脂に吸着されている水分および１．１゜１−） ＋Ｊ
クロロエタンまたはトリクロロエチレンを気化させて
含み、配管９を経由して冷却器１０に導かれ予備冷却さ
れ、ここで一部の水分および１．１．ｉ）リクロロエタ
ンまたはトリクロロエチレンが凝縮液として凝縮タンク
１３中に回収される。一方再生用ｗｉ環ガスはつづいて
冷却器１１に導かれて０℃〜１２℃に冷却され、水分お
よびＩ、Ｉ、ｉ−トリクロロエタンまたはトリクロロエ
チレンが充分に凝縮され、凝縮液として凝縮タンク１３
において分離回収され、再生用循環ガスは配管１４を経
由してブロワ−６により再度イオン交換樹脂の再生にＶ
ｉ１ｍ使用される。なお、冷却された再生用循環ガスの
温度は温度計１２で測定する。The W1 ring gas for regeneration introduced into the adsorption tower 1 contains moisture adsorbed on the ion exchange resin and 1.1°1-) +J
It contains vaporized chloroethane or trichlorethylene, is led to a cooler 10 via piping 9, and is precooled, where it contains some moisture and 1.1. i) Lichloroethane or trichlorethylene is recovered as condensate in the condensation tank 13. On the other hand, the recycling gas is then led to the cooler 11 and cooled to 0°C to 12°C, and water and I, I, i-trichloroethane or trichloroethylene are sufficiently condensed, and the condensed liquid is transferred to the condensation tank 13.
The circulating gas for regeneration is separated and recovered at
i1m is used. Note that the temperature of the cooled regeneration circulating gas is measured with a thermometer 12.
再生終了後は、吸着塔に通ずる再生用循環ガス用配管の
内、吸着塔の入口および出口部分を閉鎖し、吸着塔を脱
水に再使用し、次段階の再生においては前記閉鎖部分を
開放し、同様の再生操作を行えばよい、そうする事によ
り、再生用循環ガスを系外に出さずに脱水と再生を繰り
返す事が出来、再生用循環ガスの演費を防止することが
でき、また再生用ｗｇ環ガスを系外に放出する場合の１
．１゜１−トリクロロエタンまたはトリクロロエチレン
のｔａ失それらの回収操作および環境上の問題も解消さ
れる。After the regeneration is completed, the inlet and outlet portions of the regeneration gas piping leading to the adsorption tower are closed, the adsorption tower is reused for dehydration, and the closed portions are opened for the next stage of regeneration. , the same regeneration operation can be performed. By doing so, dehydration and regeneration can be repeated without letting the regeneration circulating gas out of the system, and the cost of regeneration circulating gas can be prevented. 1 when releasing the regeneration wg ring gas to the outside of the system
．． The loss of 1.1-trichloroethane or trichloroethylene, their recovery operation and environmental problems are also eliminated.
以下実施例、比較例に基づき、本発明をさらに詳細に説
明する。The present invention will be explained in more detail below based on Examples and Comparative Examples.
実施例１〜３、比較例１〜４
第１図と同様な装置を用い、イオン交換樹脂再生を行っ
た。主装置である吸着塔ｌは、イオン交換樹脂（ダイヤ
イオン５Ｋ１ｔ３：三菱化成工業■製）７１が充填され
た内容積１５Ｎの吸着塔である。３２０ＰＰ鍋の水分を
含有した１、１．．１−トリクロロエタンの脱水を９０
Ｉ！／ｈｒの流速で、３５時間供給し脱水を行った後
、イオン交換樹脂の再生を開始した。脱水により吸着し
た水分は約２００ｇ／ｊ！（イオン交換樹脂基準）であ
った、なお脱水および再生装置は５ＵＳ３０４製である
。Examples 1 to 3, Comparative Examples 1 to 4 Ion exchange resin was regenerated using an apparatus similar to that shown in FIG. The adsorption tower 1, which is the main device, has an internal volume of 15N and is filled with 71 ion exchange resins (Diaion 5K1t3, manufactured by Mitsubishi Chemical Corporation). 320PP pot containing moisture 1, 1. ．． Dehydration of 1-trichloroethane to 90%
I! After dehydration was performed at a flow rate of /hr for 35 hours, regeneration of the ion exchange resin was started. The amount of water absorbed through dehydration is approximately 200g/j! (based on ion exchange resin), and the dehydration and regeneration equipment was manufactured by 5US304.
窒累１ ｉ Ｎｍ’／ｈｒを再生用循環ガス供給管５よ
り供給し、ブロワ−６により循環し、ヒーター７ （加
熱源ニスチーム、形式：エロフィン型）で加熱して吸着
塔１に供給した。加熱された再生用循環ガスの温度は温
度計８で測定し、加熱温度は第１表の通りとした。Nitrogen accumulation 1 i Nm'/hr was supplied from a regeneration circulation gas supply pipe 5, circulated by a blower 6, heated by a heater 7 (heating source Nisteam, type: Erofin type), and supplied to the adsorption tower 1. The temperature of the heated circulating gas for regeneration was measured with a thermometer 8, and the heating temperature was as shown in Table 1.
水分および１，１．１−トリクロロエタンを含有した吸
着塔１からの再生用循環ガスを、配管９を経由して冷却
器１０（冷媒：塩化カルシウム水溶液、形式：垂直型多
管式、温度−２０℃）に導き、予備冷却し、ここで一部
の水分および１，１゜１−トリクロロエタンを凝縮分離
させ、凝縮液は凝縮タンク１３に回収した。The circulating gas for regeneration from the adsorption tower 1 containing moisture and 1,1,1-trichloroethane is passed through a pipe 9 to a cooler 10 (refrigerant: calcium chloride aqueous solution, type: vertical multi-tube type, temperature -20 ℃) and pre-cooled, at which time some of the water and 1,1°1-trichloroethane were condensed and separated, and the condensate was collected in the condensation tank 13.
再生用循環ガスは冷却器１１（冷媒：塩化カルシウム水
溶液、形式：垂直型多管式、温度−２０”Ｃ）に導き、
温度計１２で温度を測定しつつ冷却し、水分および１，
１．ｌ−１−リクロロエタンを凝縮させ、凝縮液は凝縮
タンク１３に回収した。The circulating gas for regeneration is led to a cooler 11 (refrigerant: calcium chloride aqueous solution, type: vertical multi-tube type, temperature -20"C),
It is cooled while measuring the temperature with a thermometer 12, and moisture and 1,
1. 1-1-lichloroethane was condensed, and the condensate was collected in a condensation tank 13.
なお、冷却温度は第１表の通りとした。Note that the cooling temperature was as shown in Table 1.
一方再生用循環ガスは配管１４を経てプロワ−６により
ヒーター７に循環し、再度イオン交換樹脂の再生に使用
した。On the other hand, the circulating gas for regeneration was circulated through the pipe 14 to the heater 7 by the blower 6 and used again to regenerate the ion exchange resin.
上記のようにして連続７時間再生を行った後の、装置の
状態またはａＷＩタンク中の水のＰＨを第１表に示す。Table 1 shows the condition of the apparatus or the pH of the water in the aWI tank after 7 hours of continuous regeneration as described above.
また再生が終った後のイオン交換樹脂の脱水能力を調べ
るために、３２０ ｐｐｍの水分を含有した１、ｌ、１
−トリクロロエタンの脱水を流速９゜１／ｈｒで行い、
脱水後の１．１．１−トリクロロエタン中の水分量の経
時変化を測定した。その結果を第２表に示す。In addition, in order to investigate the dehydration ability of the ion exchange resin after the regeneration, 1, 1, 1 containing 320 ppm water was used.
- Dehydration of trichloroethane at a flow rate of 9° 1/hr,
Changes in water content in 1.1.1-trichloroethane after dehydration over time were measured. The results are shown in Table 2.
実施例４〜６、比較例５〜８
２４０ρｐ園の水分を含有したトリクロロエチレンの脱
水を流速１２０ｊ！／ｈｒで３５時間行い〔吸着した水
分量は約２００ｇ／／！（イオン交換樹脂基準）〕、加
熱温度と冷却温度を第２表の通りとした以外は、実施例
１〜３、比較例１〜４と同様にトリクロロエチレンの脱
水およびイオン交換樹脂の再生を行った。Examples 4 to 6, Comparative Examples 5 to 8 Trichlorethylene containing 240p water was dehydrated at a flow rate of 120j! /hr for 35 hours [The amount of water absorbed is about 200g//! (ion exchange resin standard)], trichlorethylene was dehydrated and the ion exchange resin was regenerated in the same manner as in Examples 1 to 3 and Comparative Examples 1 to 4, except that the heating temperature and cooling temperature were as shown in Table 2. .
連続７時間再生後の、装置の状態または凝縮タンクの水
のＰＨを第３表に示す。Table 3 shows the condition of the device or the pH of the water in the condensing tank after 7 hours of continuous regeneration.
また再生が終わった後のイオン交換樹脂の脱水能力を調
べる為に、２４０ｐｐｍの水分を含有したトリクロロエ
チレンの脱水を流速１２０１ ／ｈｒテ行い、脱水後の
トリクロロエチレン中の水分量の経時変化を測定した。In addition, in order to examine the dehydration ability of the ion exchange resin after regeneration, trichlorethylene containing 240 ppm of water was dehydrated at a flow rate of 1201/hr, and the change in water content in trichlorethylene after dehydration was measured over time.
その結果を第４表に示す。The results are shown in Table 4.
ハ）発明の効果
本発明によれば２水分を含有した１、１．１−トリクロ
ロエタンまたはトリクロロエチレンの脱水後のイオン交
換樹脂の再生において、ｌ、１゜１−トリクロロエタン
またはトリクロロエチレンの分解による塩酸の発生を防
止し、装置等を腐食することなく再生を行うことを可能
とし、またイオン交換樹脂と接触させた後の再生用循環
ガスを簡単な処置により再循環させることにより、再生
の連続操業を可能とし、さらに脱水と再生との連続操業
が可能であり、しかも再生後のイオン交換樹脂は長時間
にわたって高い脱水能力を有するものであり、工業的に
も経済的にも、また環境的見地からも見ても非常に優れ
た方法である。c) Effects of the invention According to the present invention, in the regeneration of an ion exchange resin after dehydration of 1,1.1-trichloroethane or trichloroethylene containing 2 water, hydrochloric acid is generated by decomposition of 1,1.1-trichloroethane or trichloroethylene. This makes it possible to perform regeneration without corroding equipment, etc., and allows continuous regeneration operation by recirculating the regeneration gas after contact with the ion exchange resin with a simple procedure. Furthermore, continuous operation of dehydration and regeneration is possible, and the regenerated ion exchange resin has a high dehydration ability over a long period of time. This is a very good method to look at.
第１図は、本発明によるイオン交換樹脂の再生方法にお
ける一実施態様のフローシートである。
ｌ、吸着塔
２、イオン交換樹脂
５、再生用循環ガス供給管
ヒーター
および１２．温度計
および１１． 冷却器
凝縮タンクFIG. 1 is a flow sheet of one embodiment of the method for regenerating ion exchange resin according to the present invention. l, adsorption tower 2, ion exchange resin 5, regeneration circulating gas supply pipe heater, and 12. Thermometer and 11. cooler condensing tank
Claims (1)
はトリクロロエチレンの脱水に使用されたイオン交換樹
脂を、再生用循環ガスにより再生するに際し、１，１，
１−トリクロロエタンの脱水に使用されたイオン交換樹
脂を再生する場合は５０℃〜７０℃の再生用循環ガスを
、またトリクロロエチレンの脱水に使用されたイオン交
換樹脂を再生する場合は７０℃〜９０℃の再生用循環ガ
スを、それぞれイオン交換樹脂と接触させ、次いで再生
用循環ガスを０℃〜１２℃に冷却して凝縮液を分離した
後、再生用循環ガスを再度循環し、イオン交換樹脂と接
触させることを特徴とするイオン交換樹脂の再生方法。1. When regenerating an ion exchange resin used for dehydrating 1,1,1-trichloroethane or trichloroethylene containing water using a regeneration circulating gas, 1,1,
When regenerating the ion exchange resin used for dehydrating 1-trichloroethane, use a regeneration circulating gas at 50°C to 70°C, and when regenerating the ion exchange resin used for dehydrating trichlorethylene, use 70°C to 90°C. The regeneration circulating gas is brought into contact with the ion exchange resin, and then the regeneration circulating gas is cooled to 0°C to 12°C to separate the condensate, and then the regeneration circulating gas is circulated again and the ion exchange resin and A method for regenerating an ion exchange resin, which comprises bringing it into contact.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP29827188A JP2625993B2 (en) | 1988-11-28 | 1988-11-28 | Regeneration method of ion exchange resin |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP29827188A JP2625993B2 (en) | 1988-11-28 | 1988-11-28 | Regeneration method of ion exchange resin |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH02144144A true JPH02144144A (en) | 1990-06-01 |
| JP2625993B2 JP2625993B2 (en) | 1997-07-02 |
Family
ID=17857478
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP29827188A Expired - Lifetime JP2625993B2 (en) | 1988-11-28 | 1988-11-28 | Regeneration method of ion exchange resin |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP2625993B2 (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0539490U (en) * | 1991-11-01 | 1993-05-28 | 共立工業株式会社 | Dehydrating cassette for dry cleaning solvent |
| JP2009291676A (en) * | 2008-06-03 | 2009-12-17 | Toyobo Co Ltd | Solvent refining apparatus |
| CN115155249A (en) * | 2022-09-05 | 2022-10-11 | 济南德洋低温科技有限公司 | Method and device for recovering special gas adsorbed by molecular sieve |
-
1988
- 1988-11-28 JP JP29827188A patent/JP2625993B2/en not_active Expired - Lifetime
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0539490U (en) * | 1991-11-01 | 1993-05-28 | 共立工業株式会社 | Dehydrating cassette for dry cleaning solvent |
| JP2009291676A (en) * | 2008-06-03 | 2009-12-17 | Toyobo Co Ltd | Solvent refining apparatus |
| CN115155249A (en) * | 2022-09-05 | 2022-10-11 | 济南德洋低温科技有限公司 | Method and device for recovering special gas adsorbed by molecular sieve |
Also Published As
| Publication number | Publication date |
|---|---|
| JP2625993B2 (en) | 1997-07-02 |
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