CN1453271A - Method of eleminating miniature amount of impurities in epsilon-caprolactam water solution - Google Patents
Method of eleminating miniature amount of impurities in epsilon-caprolactam water solution Download PDFInfo
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- CN1453271A CN1453271A CN 02114079 CN02114079A CN1453271A CN 1453271 A CN1453271 A CN 1453271A CN 02114079 CN02114079 CN 02114079 CN 02114079 A CN02114079 A CN 02114079A CN 1453271 A CN1453271 A CN 1453271A
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- water solution
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- caprolactam
- caprolactam water
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Abstract
The present invention features that electric dialysis membrane is used to eliminate the inorganic impurities and miniature amount of organic impurities in water solution of epsilon-caprolactam, that is, water solution of epsilon-caprolactam of 5-90 wt% concentration is made to pass through electric dialysis membrane at 0-150 deg.c. The said method is used to replace ion exchange process for refining caprolactam and can reduce greatly the conductivity and extinction value of water solution of epsilon-caprolactam and eliminate ammonium radical, acid radical and other ions and miniature amount of organic impurities in water solution of epsilon-caprolactam. s
Description
Technical field
The present invention relates to a kind of method of removing trace impurity in the epsilon-caprolactam water solution, particularly adopt the removal method of electrodialytic membranes inorganic impurity in the caprolactam water solution and micro organic impurity.
Background technology
ε-Ji Neixianan is a main raw material of producing nylon-6.Industrial, in its refining purification process, inorganic impurity and micro organic impurity are to adopt the method for ion exchange resin absorption to remove in the epsilon-caprolactam water solution.The limitation of this technology is: ion exchange resin needs regular regeneration, and regeneration expense costliness; Need bronsted lowry acids and bases bronsted lowry during regeneration, have equipment corrosion; Exist hexanolactam to run off during back flushing and produce the problems such as waste water of a large amount of high COD content.So for a long time, people are seeking the novel method of substitutional ion exchange always, but do not appear in the newspapers.
Carrying out the concentration that the caprolactam water solution of ion exchange resin absorption requires has certain requirement, the too high ion-exchange effect that influences of concentration, and concentration is too low can to increase working cost.The specific conductivity that enters the caprolactam water solution of ion exchange resin is about 20～25 μ s/cm, and after ion-exchange, the specific conductivity of caprolactam water solution requires to reduce to≤and 5 μ s/cm, 290nm place extinction value reduce to about 0.3.
Summary of the invention
The object of the present invention is to provide a kind of method of removing trace impurity in the epsilon-caprolactam water solution, particularly adopt the removal method of electrodialytic membranes inorganic impurity in the caprolactam water solution and micro organic impurity.
The present invention is achieved in that promptly under 10 ℃～80 ℃, 5%wt～90%wt caprolactam water solution is passed through electrodialytic membranes, because the existence of electric field, the most inorganic impurities and the part organic impurity that have electric charge after the ionization move under effect of electric field, arrive the concubine (this partial material is carried out cycling and reutilization generally speaking) of packed-bed electrodialysis film; Thereby the content of impurity in the main discharge chamber solution is reduced greatly, reach the purpose of removing impurity, the specific conductivity of this partial material and extinction value reduce significantly, can directly enter the subsequent processing of caprolactam refining.
1, the device that uses in the present invention is an electrodialytic membranes;
2, caprolactam concentration in the present invention is 5%wt～90%wt, is generally 10%wt～80%wt;
3, the inorganic impurity of removing in the present invention is mainly ammonium class inorganic salt, mainly shows as the reduction of specific conductivity;
4, can remove the part organic impurity in the present invention, mainly show as the reduction of 290nm place extinction value;
5, the caprolactam water solution temperature should be controlled at 10 ℃～80 ℃.
Positively effect of the present invention is: ion exchange resin does not need regular regeneration, and the regeneration expense is low; Do not need bronsted lowry acids and bases bronsted lowry during regeneration, do not have equipment corrosion; Do not have hexanolactam to run off during back flushing, and produce the problems such as waste water of a large amount of high COD content.
Concrete embodiment
Embodiment 1: with concentration be the epsilon-caprolactam water solution of 30%wt under 50 ℃ by the electrodialytic membranes device, residence time of material is 15 minutes, experimental result sees Table 1.
Embodiment 1 experimental result
| Analysis project | Raw material | The main chamber | Concubine |
| Specific conductivity (μ s/cm) | ??19.0 | ???2.05 | ??28 |
| 290nm place extinction value | ??0.55 | ???0.320 | ??0.563 |
Embodiment 2: use with concentration as the epsilon-caprolactam water solution of 40%wt under 50 ℃ by the electrodialytic membranes device.Residence time of material is 30 minutes.Experimental result sees Table 2.
Embodiment 2 experimental results
| Analysis project | Raw material | The main chamber | Concubine |
| Specific conductivity (μ s/cm) | ??17.5 | ??2.00 | ??32 |
| 290nm place extinction value | ??0.52 | ??0.290 | ??0.57 |
Claims (4)
1, a kind of method of removing trace impurity in the epsilon-caprolactam water solution, it is characterized in that adopting the removal method of electrodialytic membranes with inorganic impurity in the caprolactam water solution and micro organic impurity, be about to 5%wt～90%wt epsilon-caprolactam water solution and under 0 ℃～150 ℃, pass through electrodialytic membranes, replace the ion-exchange process in the caprolactam refining operation, reduce the specific conductivity and the extinction value of epsilon-caprolactam water solution significantly.
2, a kind of method of removing trace impurity in the epsilon-caprolactam water solution according to claim 1 is characterized in that ε-Ji Neixianan concentration is 5%wt～90%wt, is generally 10%wt～80%wt.
3, a kind of method of removing trace impurity in the epsilon-caprolactam water solution according to claim 1 is characterized in that service temperature is 0 ℃～150 ℃, is preferably 20 ℃～100 ℃.
4, a kind of method of removing trace impurity in the epsilon-caprolactam water solution according to claim 1 is characterized in that the residence time of material is 5～60 minutes, is preferably 10～40 minutes.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 02114079 CN1247545C (en) | 2002-04-23 | 2002-04-23 | Method of eleminating miniature amount of impurities in epsilon-caprolactam water solution |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 02114079 CN1247545C (en) | 2002-04-23 | 2002-04-23 | Method of eleminating miniature amount of impurities in epsilon-caprolactam water solution |
Publications (2)
| Publication Number | Publication Date |
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| CN1453271A true CN1453271A (en) | 2003-11-05 |
| CN1247545C CN1247545C (en) | 2006-03-29 |
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| CN 02114079 Expired - Lifetime CN1247545C (en) | 2002-04-23 | 2002-04-23 | Method of eleminating miniature amount of impurities in epsilon-caprolactam water solution |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101190893B (en) * | 2006-11-20 | 2010-04-14 | 中国石油化学工业开发股份有限公司 | System and method for purifying crude caprolactam water solution |
| CN104098495A (en) * | 2014-07-28 | 2014-10-15 | 湘潭大学 | Method for improving caprolactam refining process |
| CN106554309A (en) * | 2015-09-24 | 2017-04-05 | 中国石油化工股份有限公司 | The method of remaining salt impurity in a kind of deep removal benzene-own solution |
| CN108623523A (en) * | 2018-04-24 | 2018-10-09 | 河北美邦工程科技股份有限公司 | Ion-exchange adds the polishing purification technique of triple effect evaporation distillation kettle base solution after hydrogen in a kind of caprolactam production process |
| CN110694479A (en) * | 2019-10-31 | 2020-01-17 | 山东益丰生化环保股份有限公司 | Purification method of cyanamide solution |
-
2002
- 2002-04-23 CN CN 02114079 patent/CN1247545C/en not_active Expired - Lifetime
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101190893B (en) * | 2006-11-20 | 2010-04-14 | 中国石油化学工业开发股份有限公司 | System and method for purifying crude caprolactam water solution |
| CN104098495A (en) * | 2014-07-28 | 2014-10-15 | 湘潭大学 | Method for improving caprolactam refining process |
| CN106554309A (en) * | 2015-09-24 | 2017-04-05 | 中国石油化工股份有限公司 | The method of remaining salt impurity in a kind of deep removal benzene-own solution |
| CN108623523A (en) * | 2018-04-24 | 2018-10-09 | 河北美邦工程科技股份有限公司 | Ion-exchange adds the polishing purification technique of triple effect evaporation distillation kettle base solution after hydrogen in a kind of caprolactam production process |
| CN108623523B (en) * | 2018-04-24 | 2020-07-28 | 河北美邦工程科技股份有限公司 | Refining and purifying process of bottom liquid of triple-effect evaporation distillation still after ion exchange hydrogenation in caprolactam production process |
| CN110694479A (en) * | 2019-10-31 | 2020-01-17 | 山东益丰生化环保股份有限公司 | Purification method of cyanamide solution |
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|---|---|
| CN1247545C (en) | 2006-03-29 |
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| ASS | Succession or assignment of patent right |
Owner name: CHINA PETROLEUM & CHEMICAL CORPORATION Free format text: FORMER OWNER: BALIN BRANCH CORP. SINOPEC Effective date: 20050107 |
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| C41 | Transfer of patent application or patent right or utility model | ||
| TA01 | Transfer of patent application right |
Effective date of registration: 20050107 Address after: 100029, No. 6, Xin Xin Street East, Beijing, Chaoyang District Applicant after: Sinopec Corp. Address before: 414003 No. 1 Dongting Road, Hunan, Yueyang Applicant before: Baling Branch, China Petro-Chemical Co., Ltd. |
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Granted publication date: 20060329 |