CN100400575C - Two-stage vacuum hot chemical treating and recovering process and apparatus for halogen-containing waste plastic - Google Patents
Two-stage vacuum hot chemical treating and recovering process and apparatus for halogen-containing waste plastic Download PDFInfo
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- CN100400575C CN100400575C CNB2006100326618A CN200610032661A CN100400575C CN 100400575 C CN100400575 C CN 100400575C CN B2006100326618 A CNB2006100326618 A CN B2006100326618A CN 200610032661 A CN200610032661 A CN 200610032661A CN 100400575 C CN100400575 C CN 100400575C
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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
- Y02P20/141—Feedstock
- Y02P20/143—Feedstock the feedstock being recycled material, e.g. plastics
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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
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W30/00—Technologies for solid waste management
- Y02W30/50—Reuse, recycling or recovery technologies
- Y02W30/62—Plastics recycling; Rubber recycling
Abstract
The present invention discloses a two-stage vacuum hot chemical treating and recovering process and an apparatus thereof for halogen containing waste plastics. The present invention aims to provide a process and an apparatus thereof treating and recovering halogen containing waste plastics in a harmless mode for the recovery field of the halogen containing waste plastics. The process comprises the steps of the melting of the halogen containing waste plastics, fire retardant separation, fire retardant gas condensation, no gas condensation treatment, the fusant pyrolysis of the halogen containing waste plastics of which fire retardant is removed, pyrogenation gas condensation, pyrolysis residue treatment, etc. The apparatuses which are used by the method comprise a feeding hopper, a feeding screw rod of a vacuum melting separation tank, the vacuum melting separation tank, a stirrer, a feeding screw rod of a vacuum pyrolysis reactor, the vacuum pyrolysis reactor, a gas condenser of the fire retardant, a pyrolysis oil condenser, a gas washing tower, a non-condensation gas treating system, a vacuum pump, a collecting tank of halogen containing fire retardant, a collecting tank of low halogen pyrolysis oil, a discharge screw rod of pyrolysis residue, a vacuum seal valve, a pyrolysis residue storage device and an electric heating system.
Description
Technical field
The present invention relates to a kind of recovery method of halogen-containing waste plastic, particularly a kind of halogen-containing waste thermoplastics two-stage vacuum hot chemical treating and recovering process that contains the addition type halogenated flame retardant.
The invention still further relates to a kind of halogen-containing waste plastic two-stage vacuum hot chemical and handle retrieving arrangement.
Background technology
Along with the develop rapidly of plastics industry and electric industry in recent ten years, waste or used plastics particularly in the waste and old electric electric installation handling problem of a large amount of Halogen plastics very outstanding.In electronic electric equipment, for the reason of safety, a lot of plastic components have all added halogenated flame retardant.Handle recovered energy if adopt the burning mode, halogen in the fire retardant may form hypertoxic carcinogenic substances such as Dioxins, furans in burning, if adopt common plastics method for pyrolysis to reclaim oil fuel, then halogenated flame retardant can generate various halo organic micromolecule compounds simultaneously at the plastics pyrolytic and is blended in the pyrolysis oil, causes the further utilization difficulty of pyrolysis oil.Structure from halogenated flame retardant, chlorine atom in the halogenated flame retardant molecule mainly links to each other with the aromatic carbon atom of flame retardant molecule with bromine atoms, its bond energy is bigger than the carbon in the polyvinyl chloride (PVC)-chlorine bond energy, carbon-halogen bond fracture temperature is more near the carbon-to-carbon rupture temperature, therefore the Halogen pyrolysis product of fire retardant mainly is various organic halogens, do not resemble the PVC based on hydrogen halide, these halides can not resemble can come out from the plastic melt separate easily the hydrogenchloride, so existing P VC two levels of thermal is separated the pyrolysis dehalogenation that dehydrochlorination technology is not suitable for the Halogen flame retardant plastics.
113 to 124 pages of catalyse pyrolysis technologies that disclose a kind of halogen-containing waste plastic of " Journal of Material Cycles and Waste Management " the 5th phase in 2003, its method are to adopt Fe (Fe
3O
4)-C and Ca (CaCO
3)-C adsorptive catalyst carries out high-temperature catalytic absorption dehalogenation to the pyrolysis gas of Halogen plastics, and the halogen concentration of pyrolysis oil is reduced to ppm level level, and weak point is that the catalyst consumption amount is big and can't regenerates to cause the cost height, also produces a large amount of catalyzer wastes.
U.S. Patent Publication No. 2005142057 discloses with polyolefine (as polypropylene, polyethylene etc.) and Halogen flame retardant plastics copyrolysis under nitrogen, the hydrogen that utilizes the polyolefine pyrolysis to produce transforms hydrogen halide with organic halogen, reach and separate halogen and obtain the Halogen pyrolysis oil, weak point is the higher polyolefin plastics of price that must provide a large amount of in addition.
European Patent Publication No 1354172 discloses a kind of two-stage converter pyrolysis installation, at first waste or used plastics under nitrogen atmosphere about 330 ℃ decompose brominated flame retardant in first step converter, enter second stage converter then and carry out the low halogen pyrolysis oil product of pyrolysis acquisition at about 400 ℃, weak point is the isolating high Halogen organic liquid of the first step, must handle through special methods, the content of halogen of second stage pyrolysis oil product is still too high, must handle and could use through dehalogenation once more.
Summary of the invention
The objective of the invention is at deficiency of the prior art, a kind of halogen-containing waste plastic two-stage vacuum hot chemical treating and recovering process is provided,, realize reclaiming extremely low pyrolysis oil and the halogen containing flame-retardant of halogen-containing concentration by harmless art breading halogen-containing waste plastic.
Another object of the present invention is to provide a kind of halogen-containing waste plastic two-stage vacuum hot chemical to handle retrieving arrangement.
Halogen-containing waste plastic two-stage vacuum hot chemical treating and recovering process of the present invention comprises the steps:
(1) the broken also melting treatment of halogen-containing waste plastic is got melt;
(2) fire retardant separates: the halogen-containing waste plastic melt after step (1) is handled is that 250～350 ℃, pressure are under 1～10kpa in temperature, vacuum separation 1～3 hour, fire retardant gas in the halogen-containing waste plastic melt and the volatilization of other micro-molecular gas;
(3) fire retardant condensation of gas:, collect phlegma with fire retardant gas and other micro-molecular gas condensations that step (2) evaporates;
(4) non-condensable gas is handled: the noncondensable gas that step (2) is produced passes through with behind the alkali liquid washing, sends into gas treating system and handles;
(5) take off waste or used plastics melt pyrolysis behind the fire retardant: the waste or used plastics melt behind the separation fire retardant that step (2) is obtained is that 500～600 ℃, pressure are under 5～15Kpa in temperature, pyrolysis 30～60 minutes, most of plastic melt is decomposed into pyrolysis gas and evaporates, and produces the small part solid residue simultaneously and collects;
(6) pyrolysis air cooling is coagulated: the pyrolysis gas that step (5) is produced is isolated pyrolysis oil by condensation;
(7) noncondensable gas that step (5) is produced is sent into gas treating system and is handled by with behind the alkali liquid washing.
The preferred version of the solid residue collection and treatment described in the step (10) is after charging into the nitrogen protection vacuum pyrolysis reactor, opens vacuum seal valve, starts residue discharging screw rod the pyrolysis residue is drained into the residue holder from the vacuum pyrolysis pot bottom.
The halogen-containing waste plastic two-stage vacuum hot chemical that the present invention proposes is handled retrieving arrangement, comprise feed hopper, vacuum fusion separating tank feed worm, vacuum fusion separating tank, agitator, vacuum pyrolysis reactor feed worm, vacuum pyrolysis reactor, fire retardant gas condenser, vacuum pump, pyrolysis oil condenser, gas wash tower, non-condensable gas treatment system, halogen containing flame-retardant holding tank, low halogen pyrolysis oil holding tank, pyrolysis residue discharging screw rod, vacuum seal valve, pyrolysis residue holder, electro-thermal heating system, wherein:
One end of vacuum fusion separating tank feed worm connects feed hopper, the other end connects the vacuum fusion separating tank, one end of vacuum pyrolysis reactor feed worm is connected with the lower end of vacuum fusion separating tank, the other end is connected with the vacuum pyrolysis reactor upper end, the fire retardant gas condenser is connected by the upper end of pipeline with the vacuum fusion separating tank, agitator places vacuum fusion separating tank and vacuum pyrolysis reactor respectively, vacuum pump respectively with the vacuum fusion separating tank, vacuum pyrolysis reactor connects, electric heating system respectively with the vacuum fusion separating tank, vacuum pyrolysis reactor connects, the upper end of vacuum pyrolysis reactor is connected with the pyrolysis oil condenser, the lower end is connected with pyrolysis residue discharging screw rod, the condensate discharge mouth of fire retardant gas condenser is connected with the halogen containing flame-retardant holding tank, the non-condensable gas outlet of fire retardant gas condenser is connected with gas wash tower by vacuum pump, the condensate discharge mouth of pyrolysis oil condenser is connected with low halogen pyrolysis oil holding tank, the non-condensable gas outlet of pyrolysis oil condenser is connected with gas wash tower by vacuum pump, gas wash tower is connected with the noncondensable gas treatment system, and pyrolysis residue discharging screw rod is connected with pyrolysis residue holder by vacuum seal valve.
Compared with prior art, the present invention has following advantage:
(1) the halogen-containing waste plastic two-stage vacuum hot chemical treating and recovering process that proposes of the present invention has reduced the speed that the viscosity of melt, the fire retardant that increased melt inside are sent to bath surface by the method that adopts vacuum separation and high-speed stirring, improved the volatility of flame retardant molecule, thereby it is more complete that halogen is separated.
(2) separation temperature of halogen-containing waste plastic two-stage vacuum hot chemical treating and recovering process of the present invention is reduced under the decomposition temperature of fire retardant, can reclaim most of fire retardant, need to have reduced the quantity of the small molecules Organohalogen compounds of processing greatly.
(3) the productive rate height of the pyrolysis liquid that obtains of halogen-containing waste plastic two-stage vacuum hot chemical treating and recovering process of the present invention, the purity height of pyrolysis gas.
Description of drawings
Fig. 1 is that halogen-containing waste plastic two-stage vacuum hot chemical of the present invention is handled the retrieving arrangement structural representation.
Embodiment
Below in conjunction with accompanying drawing and embodiment the present invention is described in further detail:
As shown in Figure 1, one end of vacuum fusion separating tank feed worm 2 connects feed hopper 1, the other end connects vacuum fusion separating tank 3, one end of vacuum pyrolysis reactor feed worm 5 is connected with the lower end of vacuum fusion separating tank 3, the other end is connected with the upper end of vacuum pyrolysis reactor 6, fire retardant gas condenser 7 is connected by the upper end of pipeline with vacuum fusion separating tank 3, agitator 4,8 place vacuum fusion separating tank 3 and vacuum pyrolysis reactor 6 inside respectively, electric heating system 19,20 are installed in vacuum fusion separating tank 3 respectively, the outside surface of vacuum pyrolysis reactor 6, the upper end of vacuum pyrolysis reactor 6 is connected with the high-temperature gas inlet of pyrolysis oil condenser 10, and the lower end is connected with pyrolysis residue discharging screw rod 16.The condensate discharge mouth of fire retardant gas condenser 7 bottoms is connected with the inlet of halogen containing flame-retardant holding tank 14, and the non-condensable gas outlet of fire retardant gas condenser is connected with gas wash tower 11 by vacuum pump 9.The condensate discharge mouth of pyrolysis oil condenser 10 bottoms is connected with low halogen pyrolysis oil holding tank 15, the non-condensable gas outlet of pyrolysis oil condenser 10 is connected with the inlet mouth of gas wash tower 11 by vacuum pump 13, the clean air outlet at gas wash tower 11 tops is connected with noncondensable gas treatment system 12, and pyrolysis residue discharging screw rod 16 is connected with pyrolysis residue holder 18 by vacuum seal valve 17.
Embodiment 1
With main plastic components is the appliance shell mixed plastic broken material analysis of HIPS, ABS, PP and PS, finds that main fire retardant agent is decabromodiphynly oxide, octabromodiphenyl ether, tetrabromo-bisphenol etc., brominated about 10%.
The broken also melting treatment of above-mentioned halogen-containing waste plastic is got melt;
Melt is that 250 ℃, pressure are that fusion separated fire retardant gas in the halogen-containing waste plastic melt and the volatilization of other micro-molecular gas 1 hour in the vacuum fusion separating tank of 10kpa in temperature; Phlegma is collected in the fire retardant gas that evaporates and other micro-molecular gas condensations; The noncondensable gas that produces is sent into gas treating system and is handled by with behind the alkali liquid washing; The waste or used plastics melt that separates behind the fire retardant is that 500 ℃, pressure are pyrolysis 30 minutes in the vacuum pyrolysis jar of 15Kpa in temperature.
The productive rate that obtains fire-retardant agent liquid is 12.3%, the pyrolysis oil productive rate is 67%, the pyrolysis residue is 11%, obtained flame-retardant agent liquid contains decabromodiphynly oxide, octabromodiphenyl ether, tetrabromo-bisphenol total 16%, other are various small molecules organic bromide machines, moisture content etc., and the organic bromine content of pyrolysis oil is 1.67%.
With main plastic components is the appliance shell mixed plastic fragmentation of HIPS, ABS, PP and PS, analyzes and finds that main fire retardant is decabromodiphynly oxide, octabromodiphenyl ether, tetrabromo-bisphenol etc., brominated about 10%.
The broken also melting treatment of above-mentioned halogen-containing waste plastic is got melt;
Melt is 350 ℃ in temperature, charge into that fusion separated 3 hours in the vacuum fusion separating tank of nitrogen atmosphere under normal pressure, fire retardant gas in the halogen-containing waste plastic melt and the volatilization of other micro-molecular gas; Phlegma is collected in the fire retardant gas that evaporates and other micro-molecular gas condensations; The noncondensable gas that produces is sent into gas treating system and is handled by with behind the alkali liquid washing; The waste or used plastics melt that separates behind the fire retardant is that 600 ℃, pressure are pyrolysis 60 minutes in the vacuum pyrolysis jar of 5Kpa in temperature.
The productive rate that obtains fire-retardant agent liquid is 18.9%, and the pyrolysis oil productive rate is 69%, and residue is 8%.The concentration of the decabromodiphynly oxide in the obtained flame-retardant agent liquid, octabromodiphenyl ether, tetrabromo-bisphenol reaches 40%, and the organic bromine content of pyrolysis oil is 0.03%.
Embodiment 3
With main plastic components is the appliance shell mixed plastic broken material analysis of HIPS, ABS, PP and PS, finds that main fire retardant agent is decabromodiphynly oxide, octabromodiphenyl ether, tetrabromo-bisphenol etc., brominated about 10%.
The broken also melting treatment of above-mentioned halogen-containing waste plastic is got melt;
Melt is that 300 ℃, pressure are that fusion separated fire retardant gas in the halogen-containing waste plastic melt and the volatilization of other micro-molecular gas 2 hours in the vacuum fusion separating tank of 5kpa in temperature; Phlegma is collected in the fire retardant gas that evaporates and other micro-molecular gas condensations; The noncondensable gas that produces is sent into gas treating system and is handled by with behind the alkali liquid washing; The waste or used plastics melt that separates behind the fire retardant is that 550 ℃, pressure are pyrolysis 50 minutes in the vacuum pyrolysis jar of 10Kpa in temperature.
The productive rate that obtains fire-retardant agent liquid is 13.1%, the pyrolysis oil productive rate is 76%, the pyrolysis residue is 9%, obtained flame-retardant agent liquid contains decabromodiphynly oxide, octabromodiphenyl ether, tetrabromo-bisphenol total 17%, other are various small molecules organic bromide machines, moisture content etc., and the organic bromine content of pyrolysis oil is 1.35%.
Claims (3)
1. a halogen-containing waste plastic two-stage vacuum hot chemical treating and recovering process is characterized in that comprising the steps:
(1) the broken also melting treatment of halogen-containing waste plastic is got melt;
(2) fire retardant separates: the halogen-containing waste plastic melt after step (1) is handled is that 250～350 ℃, pressure are under 1～10kpa in temperature, vacuum separation 1～3 hour, fire retardant gas in the halogen-containing waste plastic melt and the volatilization of other micro-molecular gas;
(3) fire retardant condensation of gas:, collect phlegma with fire retardant gas and other micro-molecular gas condensations that step (2) evaporates;
(4) non-condensable gas is handled: the noncondensable gas that step (2) is produced passes through with behind the alkali liquid washing, sends into gas treating system and handles;
(5) take off waste or used plastics melt pyrolysis behind the fire retardant: the waste or used plastics melt behind the separation fire retardant that step (2) is obtained is that 500～600 ℃, pressure are under 5～15Kpa in temperature, pyrolysis 30～60 minutes, most of plastic melt is decomposed into pyrolysis gas and evaporates, and produces the small part solid residue simultaneously and collects;
(6) pyrolysis air cooling is coagulated: the pyrolysis gas that step (5) is produced is isolated pyrolysis oil by condensation;
(7) noncondensable gas that step (5) is produced is sent into gas treating system and is handled by with behind the alkali liquid washing.
2. method according to claim 1 is characterized in that the solid residue collection and treatment that described step (5) produces is to charge under the nitrogen protection, the pyrolysis residue is drained into the residue holder.
3. a halogen-containing waste plastic two-stage vacuum hot chemical is handled retrieving arrangement, it is characterized in that comprising feed hopper, vacuum fusion separating tank feed worm, vacuum fusion separating tank, agitator, vacuum pyrolysis reactor feed worm, vacuum pyrolysis reactor, fire retardant gas condenser, pyrolysis oil condenser, gas wash tower, non-condensable gas treatment system, vacuum pump, halogen containing flame-retardant holding tank, low halogen pyrolysis oil holding tank, pyrolysis residue discharging screw rod, vacuum seal valve, pyrolysis residue holder, electro-thermal heating system, wherein:
One end of vacuum fusion separating tank feed worm connects feed hopper, the other end connects the vacuum fusion separating tank, one end of vacuum pyrolysis reactor feed worm is connected with the lower end of vacuum fusion separating tank, the other end is connected with the vacuum pyrolysis reactor upper end, the fire retardant gas condenser is connected by the upper end of pipeline with the vacuum fusion separating tank, agitator places vacuum fusion separating tank and vacuum pyrolysis reactor respectively, electric heating system respectively with the vacuum fusion separating tank, vacuum pyrolysis reactor connects, the upper end of vacuum pyrolysis reactor is connected with the high-temperature gas inlet of pyrolysis oil condenser, the lower end is connected with pyrolysis residue discharging screw rod, the condensate discharge mouth of fire retardant gas condenser is connected with the inlet of halogen containing flame-retardant holding tank, the non-condensable gas outlet of fire retardant gas condenser is connected with gas wash tower by vacuum pump, the condensate discharge mouth of pyrolysis oil condenser is connected with low halogen pyrolysis oil holding tank, the non-condensable gas outlet of pyrolysis oil condenser is connected with gas wash tower by vacuum pump, gas wash tower is connected with the noncondensable gas treatment system, and pyrolysis residue discharging screw rod is connected with pyrolysis residue holder by vacuum seal valve.
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| CNB2006100326618A CN100400575C (en) | 2006-01-06 | 2006-01-06 | Two-stage vacuum hot chemical treating and recovering process and apparatus for halogen-containing waste plastic |
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| CNB2006100326618A CN100400575C (en) | 2006-01-06 | 2006-01-06 | Two-stage vacuum hot chemical treating and recovering process and apparatus for halogen-containing waste plastic |
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| CN100400575C true CN100400575C (en) | 2008-07-09 |
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| CN101220173B (en) * | 2007-12-14 | 2010-08-11 | 华南理工大学 | Apparatus and method for dehalogenation regeneration of waste and old electric plastics |
| TWI755726B (en) | 2014-10-30 | 2022-02-21 | 美商艾科詹瑟斯有限公司 | System for forming a solid fuel composition from mixed solid waste |
| CN107109273A (en) | 2014-10-30 | 2017-08-29 | 埃科金苏斯有限责任公司 | The technique that solid fuel composition is formed by hybrid solid discarded object |
| US9771536B2 (en) | 2014-10-30 | 2017-09-26 | EcoGensus LLC | Solid fuel composition formed from mixed solid waste |
| CN105001896B (en) * | 2015-07-28 | 2016-08-24 | 安徽奥生资源利用科技有限公司 | A kind of waste plastics recovery purifier |
| CN107151561B (en) * | 2017-07-19 | 2019-03-15 | 北京科技大学 | A kind of polystyrene foam plastics pyrolysis oil preparation device |
| CN107573957A (en) * | 2017-10-16 | 2018-01-12 | 江苏绿尚环保科技有限公司 | A kind of solid waste thermal decomposition processing unit |
| US10618025B2 (en) | 2018-04-04 | 2020-04-14 | EcoGensus LLC | Process vessel for forming fuel compositions and related systems and methods |
| KR102228583B1 (en) * | 2019-04-30 | 2021-03-16 | 한국에너지기술연구원 | Pyrolysis oil production system from plastic waste and use thereof |
| CN116064064A (en) * | 2021-10-29 | 2023-05-05 | 中国石油化工股份有限公司 | Method and system for recycling waste plastics through pyrolysis |
| CN115368627B (en) * | 2022-10-26 | 2023-01-24 | 国高材高分子材料产业创新中心有限公司 | Method for recovering flame-retardant polyester |
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