CN103467378A - Process method for producing caprolactam by using recovered waste chinlon silks and leftovers and application of phosphoric acid serving as catalyst in process method - Google Patents
Process method for producing caprolactam by using recovered waste chinlon silks and leftovers and application of phosphoric acid serving as catalyst in process method Download PDFInfo
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- CN103467378A CN103467378A CN2013104340722A CN201310434072A CN103467378A CN 103467378 A CN103467378 A CN 103467378A CN 2013104340722 A CN2013104340722 A CN 2013104340722A CN 201310434072 A CN201310434072 A CN 201310434072A CN 103467378 A CN103467378 A CN 103467378A
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- phosphoric acid
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- catalyst
- polyamide fibre
- waste silk
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/52—Improvements relating to the production of bulk chemicals using catalysts, e.g. selective catalysts
Abstract
The invention discloses a process method for producing caprolactam by using recovered waste chinlon silks and leftovers. The process method comprises the following steps of: (1) heating to melt the waste chinlon silks and the leftovers; (2) depolymerizing the molten waste chinlon silks and leftovers, wherein phosphoric acid is used as a catalyst during depolymerization; (3) oxidizing the system by using potassium permanganate serving as an oxidant; (4) alkalifying the system by using sodium hydroxide; (5) filtering to obtain crude caprolactam; (6) performing concentration, water removal, rectification and crystallization on the obtained crude caprolactam to obtain pure caprolactam. The invention discloses an application of the phosphoric acid serving as the catalyst in the method. Aiming at the fact that too many byproducts are generated when a strong base is used as a depolymerization catalyst, the phosphoric acid catalyst is singly used, and further the following advantages are achieved: the process is simple, few byproducts are generated, the equipment corrosion is small, the production process is safe, the cost is reduced, and waste materials are recycled to favor environmental protection.
Description
Technical field
The present invention relates to the recovery process of caprolactam monomer, relate in particular to a kind of processing method of utilizing polyamide fibre waste silk, tankage remanufacture hexanolactam.
Background technology
At present, because general polyamide fibre factory is not recycled into the technique of raw material to tankage, producing the waste material produced in the polyamide fibre process is directly to sell other factory, causes therefore the waste material price is cheap and easily produce problem of environmental pollution.
Along with the development of economy and society, the world today useless more and more payes attention to energy-conservation subtracting, and the recycling of polymer waste is also become to one of study hotspot of polymer arts.The industrial applications example of getting hexanolactam by the chemical depolymerization legal system comprises: domestic Jinan synthon station-service chemical depolymerization legal system is got hexanolactam [Jinan chemical fibre mill.Hexanolactam is produced in polyamide fibre 6 waste silk depolymerization, synthetic fiber industry, 1978, (1): 85-87], but there is following problem: still produce coking in the depolymerization still, impact is conducted heat, and reduces the depolymerization yield, and plant factor is not high, the by product of depolymerization is many, yield poorly, the yield of crude caprolactam reaches 85%, and refining rear total recovery reaches 75%.The existing method of utilizing waste and old nylon 6 to produce caprolactams, existing patent report, for example, patent (CN1374296) has been reported the method that the waste and old nylon 6 of a kind of use is produced caprolactams, employing be sodium hydroxide catalyst.Patent (CN101157646) has been reported a kind of method of utilizing the intimate lactan of nylon 6 waste and scrap manufacture orders, employing be alkali or the salt catalyst of basic metal, alkaline-earth metal, and what obtain is caprolactam water solution.Patent (CN101423487) has been reported a kind of method of recovering epsilon-caprolactam by catalysis waste nylon 6 degradation, employing be phosphorus heteropoly tungstic acid catalyzer, what obtain is micro-yellow solid ε-caprolactam.Patent (CN102382052) has been reported the method for waste nylon 6 degradation recovery ε-caprolactam in a kind of ionic liquid/water binary mixture, but the imidazolium halide class ionic-liquid catalyst adopted is expensive, and the yield of hexanolactam is not high.Patent (CN102503890) has reported that a kind of presence of acidic ionic liquid catalyst that utilizes is hydrolyzed the method that waste and old nylon 6 reclaims ε-caprolactam, employing be acidic ionic liquid catalysts, expensive, and what obtain is the hydrolysis crude product.
Summary of the invention
The objective of the invention is in order to overcome above-mentioned the deficiencies in the prior art, the processing method of utilizing polyamide fibre waste silk, tankage remanufacture hexanolactam that a kind of price is low, the rate of recovery is high is provided.
In order to realize the foregoing invention purpose, the technical solution used in the present invention is:
A kind of processing method of utilizing polyamide fibre waste silk, tankage remanufacture hexanolactam comprises the following steps:
1) polyamide fibre waste silk, tankage are carried out to heating and melting;
2) the polyamide fibre waste silk after melting, tankage are carried out to depolymerization, separate in collecting process and use phosphoric acid as catalyzer;
3) add potassium permanganate as oxygenant, system is carried out to oxidation;
4) add sodium hydroxide to be alkalized to system;
5) filter and obtain crude caprolactam;
6) to the crude caprolactam obtained concentrated, dewatered, rectifying and crystallization obtain pure hexanolactam.
Wherein, in step 2) pass into superheated vapour simultaneously in reaction system in the solution collecting process.
In order to realize the foregoing invention purpose, another technical solution used in the present invention is:
A kind of phosphoric acid is the application in polyamide fibre waste silk, tankage remanufacture hexanolactam as catalyzer, and it uses phosphoric acid as catalyzer in polyamide fibre waste silk, tankage are separated to collecting process.
Wherein, pass into superheated vapour simultaneously in separating collecting process in reaction system.
Beneficial effect of the present invention is: due to the without putrefaction under field conditions (factors) of useless nylon, difficult degradation, cause serious environmental problem, the method by chemical degradation reclaims monomer and has economic benefit and social benefit.Too much for using highly basic to make the depolymerization catalyst byproducts, and use separately phosphoric acid catalyst, technique is simple, and by product is few, and equipment corrosion is little, production process safety, Cost reduction, the waste recovery utilization, be conducive to environment protection.
Embodiment
By describing technology contents of the present invention, structural attitude in detail, being realized purpose and effect, below in conjunction with embodiment, be explained in detail.
The present invention utilizes the processing method of polyamide fibre waste silk, tankage remanufacture hexanolactam, comprises the following steps:
1) polyamide fibre waste silk, tankage are carried out to heating and melting;
2) too much for using highly basic to make the depolymerization catalyst byproducts, select to use separately the H3PO4 catalyzer, the polyamide fibre waste silk after melting, tankage are carried out to depolymerization; In order to solve the useless slow problem of polyamide fibre hydrolysis rate, can also pass into superheated vapour simultaneously in separating collecting process in reaction system simultaneously, accelerate hydrolysis rate, and reduce by product quantity.
3) add potassium permanganate as oxygenant, system is carried out to oxidation, remove reducing impurity;
4) add sodium hydroxide to be alkalized to system;
5) filter and obtain crude caprolactam;
6) to the crude caprolactam obtained concentrated, dewatered, rectifying and crystallization obtain pure hexanolactam, improves the purity of hexanolactam by rectifying, crystallization.
Due to the without putrefaction under field conditions (factors) of useless nylon, difficult degradation, cause serious environmental problem, the method by chemical degradation reclaims monomer and has economic benefit and social benefit.Too much for using highly basic to make the depolymerization catalyst byproducts, and use separately phosphoric acid catalyst, technique is simple, and by product is few, and equipment corrosion is little, production process safety, Cost reduction, the waste recovery utilization, be conducive to environment protection.
The foregoing is only embodiments of the invention; not thereby limit the scope of the claims of the present invention; every equivalent structure or conversion of equivalent flow process that utilizes description of the present invention to do; or directly or indirectly be used in other relevant technical fields, all in like manner be included in scope of patent protection of the present invention.
Claims (4)
1. a processing method of utilizing polyamide fibre waste silk, tankage remanufacture hexanolactam, is characterized in that, comprises the following steps:
1) polyamide fibre waste silk, tankage are carried out to heating and melting;
2) the polyamide fibre waste silk after melting, tankage are carried out to depolymerization, separate in collecting process and use phosphoric acid as catalyzer;
3) add potassium permanganate as oxygenant, system is carried out to oxidation;
4) add sodium hydroxide to be alkalized to system;
5) filter and obtain crude caprolactam;
6) to the crude caprolactam obtained concentrated, dewatered, rectifying and crystallization obtain pure hexanolactam.
2. the processing method of utilizing polyamide fibre waste silk, tankage remanufacture hexanolactam according to claim 1, is characterized in that, in step 2) pass into superheated vapour simultaneously in reaction system in the solution collecting process.
3. phosphoric acid application in polyamide fibre waste silk, tankage remanufacture hexanolactam as catalyzer, is characterized in that, in polyamide fibre waste silk, tankage are separated to collecting process, uses phosphoric acid as catalyzer.
4. phosphoric acid according to claim 3 application in polyamide fibre waste silk, tankage remanufacture hexanolactam as catalyzer, is characterized in that, passes into superheated vapour in separating collecting process simultaneously in reaction system.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2013104340722A CN103467378A (en) | 2013-09-23 | 2013-09-23 | Process method for producing caprolactam by using recovered waste chinlon silks and leftovers and application of phosphoric acid serving as catalyst in process method |
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| Application Number | Priority Date | Filing Date | Title |
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| CN2013104340722A CN103467378A (en) | 2013-09-23 | 2013-09-23 | Process method for producing caprolactam by using recovered waste chinlon silks and leftovers and application of phosphoric acid serving as catalyst in process method |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108250144A (en) * | 2017-12-19 | 2018-07-06 | 浙江恒逸锦纶有限公司 | A kind of method for recycling nylon 6/poly and closing caprolactam in MONOMER RECOVERY device efflux wastewater |
| CN109233271A (en) * | 2018-09-25 | 2019-01-18 | 福建锦江科技有限公司 | Utilize the short glass fiber reinforced nylon 6 material and preparation method thereof of 6 waste silk of polyamide fibre production |
| CN109553561A (en) * | 2018-11-28 | 2019-04-02 | 四川塑金科技有限公司 | Regenerate the preparation method and fabric of cloth textile |
| CN114057621A (en) * | 2021-11-29 | 2022-02-18 | 东华大学 | Method for efficiently depolymerizing waste polyamide 6 and application thereof |
| WO2023144337A1 (en) | 2022-01-28 | 2023-08-03 | Cap Iii B.V. | Process for the recovery of epsilon-caprolactam from nylon 6-containing multi-component material |
| EP4306510A1 (en) | 2022-07-11 | 2024-01-17 | Cap Iii B.V. | Process for the recovery of epsilon-caprolactam from nylon 6-containing multi-component material |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5241066A (en) * | 1992-06-25 | 1993-08-31 | Basf Corporation | Method of recovering caprolactam from mixed waste |
| CN1239744A (en) * | 1998-06-18 | 1999-12-29 | 济南八方锦纶集团有限公司 | Caprolactum recovering process from nylon-6 fiber washing water |
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2013
- 2013-09-23 CN CN2013104340722A patent/CN103467378A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5241066A (en) * | 1992-06-25 | 1993-08-31 | Basf Corporation | Method of recovering caprolactam from mixed waste |
| CN1239744A (en) * | 1998-06-18 | 1999-12-29 | 济南八方锦纶集团有限公司 | Caprolactum recovering process from nylon-6 fiber washing water |
Non-Patent Citations (1)
| Title |
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| 黄南薰: "回收锦纶6废料和废渣工艺技术的探讨", 《合成纤维》 * |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108250144A (en) * | 2017-12-19 | 2018-07-06 | 浙江恒逸锦纶有限公司 | A kind of method for recycling nylon 6/poly and closing caprolactam in MONOMER RECOVERY device efflux wastewater |
| CN109233271A (en) * | 2018-09-25 | 2019-01-18 | 福建锦江科技有限公司 | Utilize the short glass fiber reinforced nylon 6 material and preparation method thereof of 6 waste silk of polyamide fibre production |
| CN109553561A (en) * | 2018-11-28 | 2019-04-02 | 四川塑金科技有限公司 | Regenerate the preparation method and fabric of cloth textile |
| CN114057621A (en) * | 2021-11-29 | 2022-02-18 | 东华大学 | Method for efficiently depolymerizing waste polyamide 6 and application thereof |
| WO2023144337A1 (en) | 2022-01-28 | 2023-08-03 | Cap Iii B.V. | Process for the recovery of epsilon-caprolactam from nylon 6-containing multi-component material |
| EP4306510A1 (en) | 2022-07-11 | 2024-01-17 | Cap Iii B.V. | Process for the recovery of epsilon-caprolactam from nylon 6-containing multi-component material |
| WO2024013196A1 (en) | 2022-07-11 | 2024-01-18 | Cap Iii B.V. | Process for the recovery of epsilon-caprolactam from nylon 6-containing multi-component material |
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Application publication date: 20131225 |