CN102731760B - Method for carrying out alcoholysis and then polymerization on recycled polyester bottle chip melts - Google Patents
Method for carrying out alcoholysis and then polymerization on recycled polyester bottle chip melts Download PDFInfo
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- CN102731760B CN102731760B CN201210246569.7A CN201210246569A CN102731760B CN 102731760 B CN102731760 B CN 102731760B CN 201210246569 A CN201210246569 A CN 201210246569A CN 102731760 B CN102731760 B CN 102731760B
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Abstract
The invention provides a method for carrying out alcoholysis and then polymerization on recycled polyester bottle chip melts. The method comprises the following steps: putting the recycled dry polyester bottles into a screw extruder to be extruded and melted and carrying out alcoholysis reaction; and then feeding the obtained melts into a polycondensation and homogenization reaction kettle for reaction to finally obtain the pure polyester melts with uniform viscosity. The method has the following beneficial effects that the method is simple and convenient to operate; and the pure polyester melts with uniform viscosity can be obtained and have stable quality.
Description
Technical field
The invention provides a kind of method by repolymerization after polyester fondant alcoholysis, especially a kind of method by repolymerization after the alcoholysis of recovery polyester bottle sheet material melt.
Background technology
The method of traditional mode of production polyester filament is to take primary polyester slice as raw material, and this material characteristic is that purity is high, stable viscosity, moisture few.The technological process of production is short, and idiographic flow is dry-screw rod melt extruded-single filter-spinning.Shortcoming is that cost is high, the resource that consumes petroleum in a large number.By recovery polyester bottle sheet material, carrying out the production POLYESTER YARNS technological process of production is that crystallization-dry-screw rod melt extruded-coarse filtration-force (forcing) pump-essence is filtered the reactor-spinning of (cascade filtration)-ol solution-homogenizing.In order to save petroleum resources, having developed with recovery polyester bottle slice is that raw material is produced polyester filament.Owing to reclaiming, polyester bottle sheet material limiting viscosity is large, quality is unstable, moisture many, impure many, volume density is little (0.35g/c ㎡), again owing to reclaiming the source difference of polyester bottles, the polymerization degree that reclaims polyester bottle slice is different, so polyester bottle slice by screw extruder extrusion molten after the range of molecular weight distributions of melt large, thereby the viscosity fluctuation of melt is large, unstable, main manifestations is that the distribution of bottle sheet molecular melt amount is wide, and melt viscosity declines, and causing spinning polyester filament can not normally carry out.
Summary of the invention
Technical problem to be solved by this invention is, provides a kind of and take by reclaiming the method for repolymerization after the alcoholysis of polyester bottle sheet material melt, realizing that to reclaim polyester bottle sheet material melt be raw material, carries out repolymerization after alcoholysis, produces stable viscosity melt.
The present invention is achieved in that and a kind ofly by reclaiming the method for repolymerization after the alcoholysis of polyester bottle sheet material melt, it is characterized in that, it comprises the steps:
The first step, puts into screw extruder and carries out extrusion molten and obtain melt reclaiming dry polyester bottle slice, and the melt of gained is entered to alcoholysis reaction still after filtering, at 250-300 ℃, ethylene glycol is joined in melt, and alcoholysis reaction 20-30min, obtains molten mass;
Second step, delivers to polycondensation homogenizing reactor by the resulting molten mass of the first step and reacts, and in vacuum tightness, is to stir under 300-400Pa condition, and temperature of reaction is 200-300 ℃, and the reaction times is 1-4 hour, finally obtains the polyester fondant that viscosity homogeneous is pure.
Preferably, the polycondensation homogenizing reactor in described second step is mouse cage stirring-type, and built-in stirring ring configures three grades of vacuum pumps, viscosity numerical value on-line monitorings and vacuumizes simulation conversion system.
In second step, oligopolymer is easily separated out from film, removes oligopolymer, and reaction is carried out towards the direction of producing polyester, can finally obtain the polyester fondant that viscosity homogeneous is pure.
Preferably, the temperature of reaction in described second step is 280 ℃, and the reaction times is 1.5 hours.
A kind of method by repolymerization after the alcoholysis of recovery polyester bottle sheet material melt that the present invention adopts, easy and simple to handle, can obtain the polyester fondant that viscosity homogeneous is pure, steady quality.
Embodiment
By specific embodiment, further describe the present invention below, but the present invention is not limited only to following examples.Within the scope of the invention or within not departing from content of the present invention, spirit and scope, within method of the present invention is suitably improved and be will become apparent to those skilled in the art that they are all deemed to be included in the scope of the invention.
embodiment 1
By reclaiming dry polyester bottle slice, enter screw extruder (JHM3950-16, Mechanology Inc. of Zhoushan Of Zhejiang Province Hisense) carry out melt extruded, the melt of gained is entered to reactor (THPC0.7M3 after filtering, Yangzhou Tian Hao pressurized vessel company limited), the polycondensation that utilizes polyester is a reversible reaction, at 280 ℃, agitator speed is 2-3r/min, ethylene glycol is added in polyester bottles material melt, reaction is carried out towards alcoholysis direction, reactor capacity is 100Kg, alcoholysis 20-30min at 280 ℃, realize partial alcoholysis, make the molecular weight of melt basically identical.Again the melt product of alcoholysis is delivered in polycondensation homogenizing reactor (THJC4.8M3 Yangzhou Tian Hao pressurized vessel company limited) subsequently, this polycondensation homogenizing reactor is mouse cage stirring-type, built-in stirring ring, capacity is 1500Kg, configure the on-line monitoring of three grades of vacuum pumps and viscosity numerical value and vacuumize simulation conversion system, stirring velocity is 2-3r/min, because stirring has swept melt film, under vacuum 300-400Pa condition, oligopolymer is easily separated out from film, remove oligopolymer, reaction is carried out towards the direction of producing polyester, finally obtain the polyester fondant that viscosity homogeneous is pure.
Vacuumizing (vacuum tightness is 300-400Pa, according to bottle sheet melt viscosity size, regulates vacuum tightness), reacting 1.5 hours at 280 ℃.Melt viscosity 0.815 ± 0.001 dl/g after homogenizing.
embodiment 2
Working method, repeats embodiment 1, and embodiment 1 is different,
Vacuumizing (vacuum tightness is 300-400Pa, according to bottle sheet melt viscosity size, regulates vacuum tightness), reacting 1.5 hours at 200 ℃.Melt viscosity 0.720 ± 0.001 dl/g after homogenizing.
embodiment 3
Working method, repeats embodiment 1, and embodiment 1 is different,
Vacuumizing (vacuum tightness is 300-400Pa, according to bottle sheet melt viscosity size, regulates vacuum tightness), reacting 1.5 hours at 300 ℃.Melt viscosity 0.780 ± 0.001 dl/g after homogenizing.
Claims (2)
1. by a method for repolymerization after the alcoholysis of recovery polyester bottle sheet material melt, it is characterized in that, it comprises the steps:
The first step, puts into screw extruder and carries out extrusion molten and obtain melt reclaiming dry polyester bottle slice, by gained
Melt enter after filtering alcoholysis reaction still, at 280 ℃, agitator speed 2-3r/min, joins ethylene glycol in melt, alcoholysis reaction 20-30min, obtains molten mass;
Second step, delivers to polycondensation homogenizing reactor by the resulting molten mass of the first step and reacts, and in vacuum tightness, is
Under 300-400Pa condition, stir, temperature of reaction is 200-300 ℃, and the reaction times is 1-4 hour, finally obtains the polyester fondant that viscosity homogeneous is pure;
Polycondensation homogenizing reactor in described second step is mouse cage stirring-type, and built-in stirring ring configures three grades of vacuum pumps, viscosity numerical value on-line monitorings and vacuumizes simulation conversion system.
2. as claimed in claim 1 a kind ofly it is characterized in that reclaiming the method for repolymerization after the alcoholysis of polyester bottle sheet material melt, the temperature of reaction in described second step is 280 ℃, and the reaction times is 1.5 hours.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201210246569.7A CN102731760B (en) | 2012-07-17 | 2012-07-17 | Method for carrying out alcoholysis and then polymerization on recycled polyester bottle chip melts |
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| CN201210246569.7A CN102731760B (en) | 2012-07-17 | 2012-07-17 | Method for carrying out alcoholysis and then polymerization on recycled polyester bottle chip melts |
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| CN102731760A CN102731760A (en) | 2012-10-17 |
| CN102731760B true CN102731760B (en) | 2014-03-26 |
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| CN103357605B (en) * | 2013-07-13 | 2015-04-15 | 福建锦兴环保科技有限公司 | Cleaning device and process for waste polyester bottle chip |
| CN103614785A (en) * | 2013-10-31 | 2014-03-05 | 安徽东锦化纤科技有限公司 | Technology for preparing recycled polyester |
| CN103627028A (en) * | 2013-10-31 | 2014-03-12 | 安徽东锦化纤科技有限公司 | Granulating process for impurity removal, homogenization and viscosification of foaming materials of waste and old terylene clothes and terylene cloth leftovers |
| CN103911681B (en) * | 2014-04-14 | 2015-12-02 | 杭州华尔利化纤有限公司 | A kind of method utilizing the PET bottle manufacture weaving long filament of recovery |
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| CN106283226A (en) * | 2016-08-15 | 2017-01-04 | 宁波大发化纤有限公司 | A kind of method joining quality melt for raw material preparation height with Waste Polyester textile |
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| CN106279756A (en) * | 2016-08-15 | 2017-01-04 | 宁波大发化纤有限公司 | The polyurethane contained in diethylene glycol alcoholysis removal Waste Polyester textile is for the method for polyester spinning melts |
| CN106279759A (en) * | 2016-08-15 | 2017-01-04 | 宁波大发化纤有限公司 | The polyurethane contained in glycolysis alcoholysis removal Waste Polyester textile is for the method for polyester spinning melts |
| CN106283227A (en) * | 2016-08-15 | 2017-01-04 | 宁波大发化纤有限公司 | A kind of method that micro-alcoholysis Waste Polyester textile raw material carries out Direct-spinning of PET Fiber |
| CN106758276B (en) * | 2017-01-18 | 2019-05-14 | 龙福环能科技股份有限公司 | A kind of production method regenerating full polyester filament carpet |
| CN110229378B (en) * | 2019-05-20 | 2021-11-19 | 安徽东锦资源再生科技有限公司 | Crystallization drying process for recycling polyester bottle flakes |
| CN114211719A (en) * | 2021-12-10 | 2022-03-22 | 浙江海利环保科技股份有限公司 | Device and method for melt depolymerization and tackifying of recycled polyester bottle flakes |
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Denomination of invention: Method for carrying out alcoholysis and then polymerization on recycled polyester bottle chip melts Effective date of registration: 20180903 Granted publication date: 20140326 Pledgee: Qi Shang bank, Limited by Share Ltd, Binzhou, Yangxin branch Pledgor: Longfu Recycling Energy Scientech Co., Ltd. Registration number: 2018370000157 |
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