CN1569802A - Production method with reclaimed waste nylon as material - Google Patents
Production method with reclaimed waste nylon as material Download PDFInfo
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- CN1569802A CN1569802A CN 200410020535 CN200410020535A CN1569802A CN 1569802 A CN1569802 A CN 1569802A CN 200410020535 CN200410020535 CN 200410020535 CN 200410020535 A CN200410020535 A CN 200410020535A CN 1569802 A CN1569802 A CN 1569802A
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Abstract
The invention discloses a production method with reclaimed waste nylon as material which consists of, charging waste nylon, acidic catalyst, and tap water into hydrolysis reactor, heating, stirring and reacting, cooling down and filtering, isolating solid body from liquid substance, obtaining solid crude adipic acid, charging tap water, industrial activated carbon, heating, agitating, filtering the activated carbon, cooling to separate the solid adipic acid.
Description
One, technical field: the present invention relates to a kind of production method that is applicable to waste and old nylon 66 for main material production hexanodioic acid, hexanediamine.
Two, background technology: nylon formal name used at school polymeric amide, principal item has nylon 66.The physical strength of nylon 66 is good, and the tensile strength height has good wear resistance and self lubricity, and thermotolerance, chemical proofing, resistance to fatigue, oil-proofness are good.Be widely used in the engineering plastics of daily fiber, automotive industry and electronic industry in people's life, fishery is used for net cage and fishnet, and agricultural is used for nylon rope or the like.China's nylon consumption in 2004 is at 170,000 tons, and 2010 annual requirements will reach 300,000 tons.Nylon is the macromolecular material of difficult degradation under field conditions (factors), and its waste is more and more.The nylon waste that China in 2004 can collect in batch reaches 40,000 tons, and these wastes have caused the serious environmental pollution, brings hidden danger for the Sustainable development of national economy.Eliminate the pollution that the nylon waste causes to environment, become the problem of current social common concern and research.
Adopt acid hydrolyzation, alkaline hydrolysis method to reclaim hexanodioic acid and hexanediamine to the recycling of waste and old nylon 66 at present, but in acidolysis and alkaline hydrolysis process, produce a large amount of liquid debris and solid waste, cause secondary pollution to environment.
Three, summary of the invention:
1, goal of the invention: the invention provides the production method that a kind of useless nylon is recycled, its purpose is not produce environmental pollution, extracting hexanodioic acid and hexanediamine from discarded nylon 66, is the preparation method of raw material production hexanodioic acid and hexanediamine thereby provide a kind of with discarded nylon 66.
2, technical scheme: main technical schemes of the present invention is achieved in that
The production method that a kind of useless nylon is recycled, it is characterized in that adopting following processing condition: waste nylon 66, an acidic catalyst, tap water are added in the hydrolysis reactor by weight 1: 0.001～1.2: 0.8～1 ratio, heating makes the hydrolysis reaction actuator temperature reach 95～110 ℃, stirring reaction 5～8 hours, be cooled to 20～30 ℃ of filtrations, solids is separated with liquids, get the thick hexanodioic acid of solids, get liquids A and retain; By weight the thick hexanodioic acid of 0.3～1: 0.5～1: 0.01～0.1 adding solids, tap water, industrial gac, this mixture is heated 80～100 ℃, stirred 2～3 hours, filter, filtering gac, filtrate are cooled to 20～30 ℃, separate out the solids hexanodioic acid.
Solid-liquid separation obtains liquids A, ratio by weight 0.2～1: 0.02～0.6: 0.4～0.6 adds liquids A, alkaline neutraliser, tap water, be neutralized to neutrality, stir liquid mixture B, liquid mixture B is added rotary kiln, under 133Pa～3990Pa pressure, distill under 150～220 ℃ of conditions of temperature, overhead product liquid C, liquid C gets liquid D through 133Pa/150 ℃～2660Pa/220 of a rectifying intercepting ℃ cut, and liquid D is a hexanediamine.
An acidic catalyst of above-mentioned indication is one or more following mixtures: sulfuric acid, phosphoric acid, hydrochloric acid, nitric acid, carbonic acid, 12-phospho-wolframic acid, 12-silicotungstic acid, 12-germanotungstic acid, 12-arsenowolframic acid.
The alkaline neutraliser of above-mentioned indication is one or more following mixtures: unslaked lime, yellow soda ash, sodium bicarbonate, salt of wormwood, saleratus, sodium phosphate, Sodium phosphate dibasic, sodium hydroxide, potassium hydroxide.
3, advantage and effect:
(1). prepared adipic acid product quality index meets SH/T1499 industry first grade standard, hexanediamine product quality indicator accord with Q/CNPC-CHX-04-05-1999 industry first grade standard;
(2). technology is simple, be applicable to the industrialization continuous production;
(3). cost is low, economic benefit is high.
Four, description of drawings: Fig. 1 is a process flow sheet of the present invention;
Five, embodiment: following the present invention is further described combined process schema and embodiment, but not only comprises following examples:
Embodiment one:
The production technique of hexanodioic acid is as follows:
With 1000Kg waste nylon 66, the 2Kg12-phospho-wolframic acid, the 1000Kg tap water adds in the hydrolysis reactor, heating makes the hydrolysis reaction actuator temperature reach 100 ℃, stirring reaction 6.5 hours, be cooled to 25 ℃ of filtrations, solids is separated with liquids, get the thick hexanodioic acid of solids, get liquids A, the thick hexanodioic acid of solids adds tap water 1000Kg, add industrial gac 25Kg, heat 90 ℃, stirred 2.5 hours, and filtered the filtering gac, filtrate is cooled to 25 ℃, separate out the hexanodioic acid of 594kg, solids B detects by adipic acid product quality standard SH/T1499 industry first grade quality index, and it is qualified that product detects, and packs, warehouse-in, sell by industrial first grade hexanodioic acid.
The production technique of hexanediamine is as follows:
Solid-liquid separation obtains liquids A, add ammonium phosphate 5Kg, tap water 500Kg, neutralization, stir liquid mixture B, liquid mixture B is added rotary kiln, under 2660Pa pressure, distill under 160 ℃ of conditions of temperature, cat head slips out thing liquid C, liquid C gets the 493Kg liquid D through 1330Pa/150 ℃ of cut of rectifying intercepting, liquid D is pressed hexanediamine target level of product quality Q/CNPC-CHX-04-05-1999 industry first grade quality index and is detected, and it is qualified that product detects, and packs, puts in storage, sells by industrial first grade hexanediamine.
Embodiment two:
The production technique of hexanodioic acid is as follows:
With 1000Kg waste nylon 66,200Kg98% sulfuric acid, the 1000Kg tap water adds in the hydrolysis reactor, heating makes the hydrolysis reaction actuator temperature reach 100 ℃, stirring reaction 6.5 hours, be cooled to 25 ℃ of filtrations, solids is separated with liquids, get the thick hexanodioic acid of solids, get liquids A, the thick hexanodioic acid of solids adds tap water 1000Kg, add industrial gac 25Kg, heat 90 ℃, stirred 2.5 hours, and filtered the filtering gac, filtrate is cooled to 25 ℃, separate out the 591kg adipic acid, detect by adipic acid product quality standard SH/T1499 industry first grade quality index, it is qualified that product detects, and packs, warehouse-in, sell by industrial first grade hexanodioic acid.
The production technique of hexanediamine is as follows:
Solid-liquid separation obtains liquids A, add unslaked lime 300Kg, tap water 500Kg, neutralization, stir liquid mixture B, liquid mixture B is added rotary kiln, under 2660Pa pressure, distill under 160 ℃ of conditions of temperature, cat head slips out thing liquid C, liquid C gets the 490Kg liquid D through 1330Pa/150 ℃ of cut of rectifying intercepting, liquid D is pressed hexanediamine target level of product quality Q/CNPC-CHX-04-05-1999 industry first grade quality index and is detected, and it is qualified that product detects, and packs, puts in storage, sells by industrial first grade hexanediamine.
In like manner, conclusion through the experiment gained, above-mentioned an acidic catalyst adopts sulfuric acid, phosphoric acid, hydrochloric acid, nitric acid, carbonic acid, 12-phospho-wolframic acid, 12-silicotungstic acid, 12-germanotungstic acid, 12-arsenowolframic acid, and above-mentioned alkaline neutraliser adopts mixture: unslaked lime, yellow soda ash, sodium bicarbonate, salt of wormwood, saleratus, sodium phosphate, Sodium phosphate dibasic, sodium hydroxide, potassium hydroxide, also can realize purpose of the present invention fully.
Claims (4)
1, a kind of production method of useless nylon recycling, it is characterized in that adopting following processing condition: waste nylon 66, an acidic catalyst, tap water are added in the hydrolysis reactor by weight 1: 0.001～1.2: 0.8～1 ratio, heating makes the hydrolysis reaction actuator temperature reach 95～110 ℃, stirring reaction 5～8 hours, be cooled to 20～30 ℃ of filtrations, solids is separated with liquids, get the thick hexanodioic acid of solids, get liquids A and retain; By weight the thick hexanodioic acid of 0.3～1: 0.5～1: 0.01～0.1 adding solids, tap water, industrial gac, this mixture is heated 80～100 ℃, stirred 2～3 hours, filter, filtering gac, filtrate are cooled to 20～30 ℃, separate out the solids hexanodioic acid.
2, production method according to a kind of useless nylon recycling described in the claim 1, it is characterized in that adopting following processing condition: solid-liquid separation obtains liquids A, ratio by weight 0.2～1: 0.02～0.6: 0.4～0.6 adds liquids A, alkaline neutraliser, tap water, be neutralized to neutrality, stir liquid mixture B, liquid mixture B is added rotary kiln, under 133Pa～3990Pa pressure, distill under 150～220 ℃ of conditions of temperature, overhead product liquid C, liquid C gets liquid D through 133Pa/150 ℃～2660Pa/220 of a rectifying intercepting ℃ cut, and liquid D is a hexanediamine.
3, the production method of recycling according to a kind of useless nylon described in the claim 1 is characterized in that an acidic catalyst that adds is one or more following mixtures: sulfuric acid, phosphoric acid, hydrochloric acid, nitric acid, carbonic acid, 12-phospho-wolframic acid, 12-silicotungstic acid, 12-germanotungstic acid, 12-arsenowolframic acid.
4, the production method of recycling according to a kind of useless nylon described in the claim 2 is characterized in that the alkaline neutraliser that adds is one or more following mixtures: unslaked lime, yellow soda ash, sodium bicarbonate, salt of wormwood, saleratus, sodium phosphate, Sodium phosphate dibasic, sodium hydroxide, potassium hydroxide.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200410020535 CN1273434C (en) | 2004-05-13 | 2004-05-13 | Production method with reclaimed waste nylon as material |
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| CN 200410020535 CN1273434C (en) | 2004-05-13 | 2004-05-13 | Production method with reclaimed waste nylon as material |
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| CN1569802A true CN1569802A (en) | 2005-01-26 |
| CN1273434C CN1273434C (en) | 2006-09-06 |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101856120A (en) * | 2010-03-23 | 2010-10-13 | 无锡市天赐康生物科技有限公司 | Health food for improving immunity of human body and preparation method thereof |
| CN101423623B (en) * | 2007-11-02 | 2011-05-11 | 宁波大学 | Depolymerization and recovery method of high temperature resistant nylon poly-para-phenylene diformyl hexane diamine |
| CN101857540B (en) * | 2009-04-09 | 2013-04-17 | 宁波大学 | Method for producing adipic acid, hexamethylenediamine hydrochloride and polyhexamethylene (di)guanidine chloride from nylon-66 through depolymerization |
| CN107056625A (en) * | 2017-06-07 | 2017-08-18 | 巢湖市鼎盛渔具有限公司 | A kind of recovery method of polyamide 66 fishing net waste material |
| CN107056624A (en) * | 2017-04-19 | 2017-08-18 | 青岛科技大学 | A kind of alcoholysis recovery method of nylon 66 material |
| CN110563570A (en) * | 2019-09-24 | 2019-12-13 | 中国科学院山西煤炭化学研究所 | Method for preparing terephthalic acid and p-phenylenediamine by degrading p-aramid |
| CN115246692A (en) * | 2021-04-25 | 2022-10-28 | 中国石油化工股份有限公司 | Method for treating wastewater of adipic acid production process |
| CN116272794A (en) * | 2023-03-13 | 2023-06-23 | 江苏长海复合材料股份有限公司 | Chopped fiber process for nylon pellets |
-
2004
- 2004-05-13 CN CN 200410020535 patent/CN1273434C/en not_active Expired - Fee Related
Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101423623B (en) * | 2007-11-02 | 2011-05-11 | 宁波大学 | Depolymerization and recovery method of high temperature resistant nylon poly-para-phenylene diformyl hexane diamine |
| CN101857540B (en) * | 2009-04-09 | 2013-04-17 | 宁波大学 | Method for producing adipic acid, hexamethylenediamine hydrochloride and polyhexamethylene (di)guanidine chloride from nylon-66 through depolymerization |
| CN101856120A (en) * | 2010-03-23 | 2010-10-13 | 无锡市天赐康生物科技有限公司 | Health food for improving immunity of human body and preparation method thereof |
| CN107056624A (en) * | 2017-04-19 | 2017-08-18 | 青岛科技大学 | A kind of alcoholysis recovery method of nylon 66 material |
| CN107056625A (en) * | 2017-06-07 | 2017-08-18 | 巢湖市鼎盛渔具有限公司 | A kind of recovery method of polyamide 66 fishing net waste material |
| CN107056625B (en) * | 2017-06-07 | 2019-04-23 | 巢湖市鼎盛渔具有限公司 | A kind of recovery method of -66 fishing net waste material of polyamide |
| CN110563570A (en) * | 2019-09-24 | 2019-12-13 | 中国科学院山西煤炭化学研究所 | Method for preparing terephthalic acid and p-phenylenediamine by degrading p-aramid |
| CN115246692A (en) * | 2021-04-25 | 2022-10-28 | 中国石油化工股份有限公司 | Method for treating wastewater of adipic acid production process |
| CN115246692B (en) * | 2021-04-25 | 2023-08-08 | 中国石油化工股份有限公司 | Treatment method of adipic acid production process wastewater |
| CN116272794A (en) * | 2023-03-13 | 2023-06-23 | 江苏长海复合材料股份有限公司 | Chopped fiber process for nylon pellets |
| CN116272794B (en) * | 2023-03-13 | 2023-11-07 | 江苏长海复合材料股份有限公司 | Chopped fiber process for nylon pellets |
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| CN1273434C (en) | 2006-09-06 |
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