CN106220758A - A kind of waste PE plastic agricultural film produces the preparation method of OPE - Google Patents
A kind of waste PE plastic agricultural film produces the preparation method of OPE Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F8/00—Chemical modification by after-treatment
- C08F8/06—Oxidation
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- Separation, Recovery Or Treatment Of Waste Materials Containing Plastics (AREA)
Abstract
A kind of waste PE plastic agricultural film produces the preparation method of OPE, by waste PE plastic agricultural film by screening, wash, be dried, pulverize, screen, wash, be dried, low temperature release under condition of nitrogen gas, Pintsch process, oxidation, material spray, technology of the package process are prepared from, the properties of product that properties of product of the present invention are prepared with PE resin pyrolysis oxidization are consistent, and indivedual indexs have exceeded product index prepared by PE resin pyrolysis oxidization.
Description
Technical field
The invention belongs to organic material technical field, relate to the regeneration of waste plastics, particularly to a kind of waste PE plastic
Agricultural film produces the preparation method of OPE.
Background technology
China is that agricultural plastic film produces and uses most countries.Agricultural plastic film be mainly canopy film and mulch film,
The modern agricultural covering material such as forage grass film, sunshade net, fly net.The thin film used is common polyvinyl chloride film, polychlorostyrene second
Alkene Anti-fogging Film, Plain PE film, polyethylene dripless film, polyethylene multifunctional composite film and EVA multifunctional composite film etc..
At present China's various canopy film year usage amount about 1,500,000 tons, year the amount of upgrading demand about 700,000 tons, wherein polyethylene film be maximum use
Amount, needs to update 450,000 tons in year.
China starts late in terms of reclaiming useless agricultural film, the most perfect.China mainly uses still at present
Landfill method, burning method, melted method of reproduction and chemical recycling etc..Landfill and burning can not fundamentally solve pollution problem, again
Cause the wasting of resources.Owing to PE Agricultural Films uses in natural environment, produced catabiosis by sun exposure, point
Son fracture, material is hardening.Macromolecular material once decomposes, by irrecoverable.The polyvinyl resin that melted recovery technology reclaims
Can reduce, simple, the unwarranted product of quality can only be done.
Summary of the invention
It is an object of the invention to overcome problem described above, it is provided that a kind of use screen, wash, be dried, condition of nitrogen gas
Lower low temperature release, Pintsch process, oxidation, material spray, technology of the package, formed and particularly relate to waste PE plastic agricultural film production oxygen
Change the preparation method of Tissuemat E.
In order to realize above-mentioned purpose, this invention takes following technical solution: a kind of waste PE plastic is agricultural thin
Film produces the preparation method of OPE, it is characterised in that: include following operating procedure:
A), waste PE plastic process, including screening, wash, be dried, disintegrating process, detailed process is, is sieved by waste PE plastic
Choosing, selects after pure white waste PE plastic carries out washing, is dried, pulverizes, uses as raw material；
B), cracking process, cracking process be high temperature degradation reaction, belong to chemical reaction, including suction, low temperature release, Pintsch process
Technique；For ensureing that cracking process is smoothed out, depolymerization still uses heated by natural gas mode, is divided into little fire and big fire, is equipped with air blast
Chiller, vacuum equipment and nitrogen enter device, and stirring vane uses special helical design；
The detailed process of the most 1. suction technique is, closes the nitrogen valve on depolymerization still, inlet valve, outlet valve, closes receptor
On big atmospheric valve and little atmospheric valve, start vacuum pump, open the vacuum valve on receptor, treat in depolymerization still vacuum pressure-
0.06MPa, opens inlet valve, is sucked in depolymerization still by polyethylene material；
2. the detailed process of low temperature release process is,
A), in polyethylene is fully entrained depolymerization still, close vacuum valve, open big atmospheric valve, little atmospheric valve, close inlet valve,
Open nitrogen valve, control nitrogen flow 2～5L/min, stop vacuum pump, start combustion furnace big fire, little fire heating；
B), when being warming up to 3 and being little, temperature reaches 160～170 DEG C, opens the stirring of depolymerization still, after normally stirring 5 minutes, closes
Big atmospheric valve, keeps constant temperature, until the amount that oligomer is released is close to zero, continues to heat up；
C), occurring boiling phenomenon in thermostatic process, stop heating immediately, the air blast opening burner carries out the cold of the interior material of still
But, reduce the temperature to plateau, after keeping a period of time, be warmed up to 160～170 DEG C again；
3. the detailed process of Pintsch process technique is,
When raw material is warming up to 300 DEG C, stop big fire heating, with little fire heating heat up, nitrogen flow be adjusted to 5～
10L/min, when the amount that oligomer is released exceedes the 20% of waste PE plastic amount, terminates for depolymerization；
C), cooling down operation,
When thing amount the most to be oligomerized is to the weight specified, the little fire of brennschluss burner, the air blast opening burner carries out the cold of the interior material of still
But；
2. when in still material temperature degree be down to less than 300 DEG C, the air blast of brennschluss burner, stop the stirring on depolymerization still, carry out the standard of binder
Standby；
D), oxidizing process, including binder, oxidation, blowing technique,
The most 1. the detailed process of binder technique is,
A), when in depolymerization still, material temperature is at 240 DEG C, and stopping depolymerization still stirs, and closes bottom discharge valve and the bottom discharge of stills for air blowing
Valve, inserts depolymerization still discharge nozzle in stills for air blowing；
B), all valves closed on depolymerization still, the little atmospheric valve on receptor, open nitrogen depolymerization still is forced into 0.06～
During 0.08MPa, unwind the outlet valve of poly-still, PE wax is pressed into stills for air blowing；
2. the detailed process of oxidation technology is,
A), after PE wax is completely forced into stills for air blowing, when material temperature is to 180～190 DEG C in stills for air blowing, the hard of PE wax amount 10% is put into
Fat acid；
B), open stirring, control to adjust frequency conversion, i.e. control speed of agitator；
C), when in stills for air blowing material temperature degree be down to 180～190 DEG C, open compressed air inlet valve, be passed through 60～80L/ml flows
Compressed gas, starts stills for air blowing are led to oxygen；
D), operation in, when oxidation temperature in the kettle rise to 150～160 DEG C, open cooling water, when temperature in the kettle drops to 150
DEG C, close cooling water, so go round and begin again and carry out logical oxygen operation control；
E), reacting 1～1.5 hour, stop stirring, close oxygen intake valve, oxidation reaction terminates；
The detailed process of blowing technique is,
A), close the vacuum valve on still, nitrogen valve, bottom discharge valve, drain valve in the middle of oxidation, open putting on still in the middle of oxidation
Empty valve and inlet valve；
B), install filter screen, hopper is inserted still in the middle of oxidation, open stills for air blowing bottom discharge valve, expect to put into by the OPE of stills for air blowing
Still in the middle of oxidation；
E), material spray, all put in the middle of oxidation after still until OPE, close still upper feeding valve in the middle of oxidation, close atmospheric valve, open
Nitrogen valve is forced into 0.1MPa to still in the middle of oxidation, opens air compressor machine, and air enters still in the middle of oxidation, opens in the middle of oxidation
The bottom discharge valve of still carries out material spray；The device that material spray uses can guarantee that granule is uniform, fine and smooth；
F), packing, after pelletize to be sprayed terminates, packaging personnel must wear protective garment, uses specific purpose tool, by the product of pelletize
Product carry out mesh screen, and the product being sieved is loaded in packaging bag.
Advantages of the present invention:
(1), the present invention be chemical recycling, itself need macromolecule PE material is cracked, polyethylene film use process
In degree of decomposition on the final mass of product without impact；
(2), for ensureing that cracking process is smoothed out, depolymerization still uses heated by natural gas mode, is divided into little fire and big fire, is equipped with drum
Air-cooling device, vacuum equipment and nitrogen enter device；
(3), the antioxidant of little molecule that adds when mainly producing polyethylene film of the waste materials that produces of the present invention, the present invention is straight
Connecing and be added in Tissuemat E or in OPE, on product quality without impact. OPE is as macromolecule material
The processing aid of material, the basis of macromolecular material adds antioxidant to increase the aging-resistant of material itself in raw being also required to
Energy；
(4), the present invention uses first low temperature (160-170 DEG C) stirring to discharge the materials such as low molecular antioxidant, it is ensured that high anneal crack
Solution can be normally carried out, and agitating device uses special stirring vane and shaft, plays maximized purpose；
(5), the present invention use stearic acid as catalyst poly-second wax aoxidize, both ensured stability and the quickening of oxidizing process
Oxidizing process, decreases again the rear road processing procedure of product, and stearic acid itself is also lubrication prescription, and oxidic polyethylene has complementation
Effect；
(6), no waste of the present invention discharge, production process produce side-product directly add in the final product；
(7), material spray use special device, use the rotating speed of up to 10,000 revs/min to carry out cyclonic separation, container volume exceedes
800 cubic metres, it is ensured that granule is uniform, fine and smooth, popularization and application have good economic and social benefit.
Accompanying drawing explanation
Fig. 1 is the process chart of the present invention.
Fig. 2 is the cracking process equipment connection diagram of the present invention.
Fig. 3 is the oxidizing process equipment connection diagram of the present invention.
In figure: 1. outlet valve；2. inlet valve；3. nitrogen valve；4. big atmospheric valve；5. vacuum valve；The least atmospheric valve；7. water
Groove；8. drain valve；9.PE wax；10. catalyst inlet；11. oxygen intakes；12. emptying outlets；13. discharge sour water mouths；14. is empty
Gas；15. products.
Detailed description of the invention
The invention will be further described below in conjunction with the accompanying drawings, but not as limitation of the present invention:
A kind of waste PE plastic agricultural film produces the preparation method of OPE, including following operating procedure:
A), waste PE plastic process, including screening, wash, be dried, disintegrating process, detailed process is, is sieved by waste PE plastic
Choosing, selects after pure white waste PE plastic carries out washing, is dried, pulverizes, uses as raw material；
B), cracking process, cracking process be high temperature degradation reaction, belong to chemical reaction,
Reaction equation: [CH2-CH2]n1 High temperature, no oxygen[CH2-CH2]n2 ,
N1: molecular weight, n2: ≈ 1800 molecular weight；
Including suction, low temperature release, Pintsch process technique；For ensureing that cracking process is smoothed out, depolymerization still uses natural gas to add
Hot mode, is divided into little fire and big fire, is equipped with blast cooling device, vacuum equipment and nitrogen and enters device, and stirring vane uses spy
Different helical design；
The detailed process of the most 1. suction technique is, closes the nitrogen valve 3 on depolymerization still, inlet valve 2, outlet valve 1, closes and receives
Big atmospheric valve 4 on device and little atmospheric valve 6, start vacuum pump, open the vacuum valve 5 on receptor, treat Vacuum Pressure in depolymerization still
Power, at-0.06MPa, opens inlet valve 2, is sucked in depolymerization still by polyethylene material；Receptor is by little atmospheric valve 6 with tank 7 even
Connect, below receptor, be provided with drain valve 8；
2. the detailed process of low temperature release process is,
A), in polyethylene is fully entrained depolymerization still, close vacuum valve 5, open big atmospheric valve 4, little atmospheric valve 6, close charging
Valve 2, opens nitrogen valve 3, controls nitrogen flow 2～5L/min, stops vacuum pump, starts combustion furnace big fire, little fire heating；
B), when being warming up to 3 and being little, temperature reaches 160～170 DEG C, opens the stirring of depolymerization still, after normally stirring 5 minutes, closes
Big atmospheric valve 4, keeps constant temperature, until the amount that oligomer is released is close to zero, continues to heat up；
C), occurring boiling phenomenon in thermostatic process, stop heating immediately, the air blast opening burner carries out the cold of the interior material of still
But, reduce the temperature to plateau, after keeping a period of time, be warmed up to 160～170 DEG C again；
3. the detailed process of Pintsch process technique is,
When raw material is warming up to 300 DEG C, stop big fire heating, with little fire heating heat up, nitrogen flow be adjusted to 5～
10L/min, when the amount that oligomer is released exceedes the 20% of waste PE plastic amount, terminates for depolymerization；
C), cooling down operation,
When thing amount the most to be oligomerized is to the weight specified, the little fire of brennschluss burner, the air blast opening burner carries out the cold of the interior material of still
But；
2. when in still material temperature degree be down to less than 300 DEG C, the air blast of brennschluss burner, stop the stirring on depolymerization still, carry out the standard of binder
Standby；
D), oxidizing process, including binder, oxidation, blowing technique,
Oxidizing process reaction principle is, PE wax is through catalysis oxidation, and it is oxygen-containing oligomeric that strand occurs fracture to generate
Thing, makes to carry on strand, reaction equation :-[-CH2-CH2-]n-oxygen-[-CH2-CHOH-CO-CHCOOH-CH2-]n1-
(OPE) wherein n ≈ 1800 molecular weight；
The most 1. the detailed process of binder technique is,
A), when in depolymerization still, material temperature is at 240 DEG C, and stopping depolymerization still stirs, and closes bottom discharge valve and the bottom discharge of stills for air blowing
Valve, inserts depolymerization still discharge nozzle in stills for air blowing；
B), all valves closed on depolymerization still, the little atmospheric valve 6 on receptor, open nitrogen and depolymerization still be forced into 0.06
～during 0.08MPa, unwind the outlet valve 1 of poly-still, PE wax 9 is pressed into stills for air blowing；Stills for air blowing be provided above catalyst inlet
10 and oxygen intake 11, stills for air blowing are connected with accepter, and accepter is provided above being vented outlet 12, the row of being provided with on accepter
Put sour water mouth 13；
2. the detailed process of oxidation technology is,
A), after PE wax 9 is completely forced into stills for air blowing, when material temperature is to 180～190 DEG C in stills for air blowing, PE wax 9 amount 10% is put into
Stearic acid；
B), open stirring, control to adjust frequency conversion, i.e. control speed of agitator；
C), when in stills for air blowing material temperature degree be down to 180～190 DEG C, open compressed air inlet valve, be passed through 60～80L/ml flows
Compressed gas, starts stills for air blowing are led to oxygen；
D), operation in, when oxidation temperature in the kettle rise to 150～160 DEG C, open cooling water, when temperature in the kettle drops to 150
DEG C, close cooling water, so go round and begin again and carry out logical oxygen operation control；
E), reacting 1～1.5 hour, stop stirring, close oxygen intake valve, oxidation reaction terminates；
The detailed process of blowing technique is,
A), close the vacuum valve on still, nitrogen valve, bottom discharge valve, drain valve in the middle of oxidation, open putting on still in the middle of oxidation
Empty valve and inlet valve；
B), install filter screen, hopper is inserted still in the middle of oxidation, open stills for air blowing bottom discharge valve, expect to put into by the OPE of stills for air blowing
Still in the middle of oxidation；
E), material spray, all put in the middle of oxidation after still until OPE, close still upper feeding valve in the middle of oxidation, close atmospheric valve, open
Nitrogen valve is forced into 0.1MPa to still in the middle of oxidation, opens air compressor machine, and air 14 enters still in the middle of oxidation, opens in oxidation
Between the bottom discharge valve of still carry out material spray；The device that material spray uses can guarantee that granule is uniform, fine and smooth；
F), packing, after pelletize to be sprayed terminates, packaging personnel must wear protective garment, uses specific purpose tool, by the product of pelletize
Product carry out mesh screen, and the product 15 being sieved is loaded in packaging bag.
Obviously, above-described embodiment is only for clearly demonstrating example of the present invention, and not to embodiment
Limit.For those of ordinary skill in the field, other multi-form can also be made on the basis of the above description
Change or variation, here without also cannot all of embodiment be given exhaustive, and thus amplified out apparent
Change or variation still in protection scope of the present invention among.
Claims (1)
1. the preparation method of a waste PE plastic agricultural film production OPE, it is characterised in that: include following operation
Step:
A), waste PE plastic process, including screening, wash, be dried, disintegrating process, detailed process is, is sieved by waste PE plastic
Choosing, selects after pure white waste PE plastic carries out washing, is dried, pulverizes, uses as raw material；
B), cracking process, cracking process be high temperature degradation reaction, belong to chemical reaction, including suction, low temperature release, Pintsch process
Technique；For ensureing that cracking process is smoothed out, depolymerization still uses heated by natural gas mode, is divided into little fire and big fire, is equipped with air blast
Chiller, vacuum equipment and nitrogen enter device, and stirring vane uses special helical design；
The detailed process of the most 1. suction technique is, closes the nitrogen valve (3) on depolymerization still, inlet valve (2), outlet valve (1), closes
Close the big atmospheric valve (4) on receptor and little atmospheric valve (6), start vacuum pump, open the vacuum valve (5) on receptor, wait to solve
In poly-still, vacuum pressure is at-0.06MPa, opens inlet valve (2), is sucked in depolymerization still by polyethylene material；
2. the detailed process of low temperature release process is,
A), in polyethylene is fully entrained depolymerization still, closes vacuum valve (5), open big atmospheric valve (4), little atmospheric valve (6), close
Close inlet valve (2), open nitrogen valve (3), control nitrogen flow 2～5L/min, stop vacuum pump, start combustion furnace big fire, little fire
Heating；
B), when being warming up to 3 and being little, temperature reaches 160～170 DEG C, opens the stirring of depolymerization still, after normally stirring 5 minutes, closes
Big atmospheric valve (4), keeps constant temperature, until the amount that oligomer is released is close to zero, continues to heat up；
C), occurring boiling phenomenon in thermostatic process, stop heating immediately, the air blast opening burner carries out the cold of the interior material of still
But, reduce the temperature to plateau, after keeping a period of time, be warmed up to 160～170 DEG C again；
3. the detailed process of Pintsch process technique is,
When raw material is warming up to 300 DEG C, stop big fire heating, with little fire heating heat up, nitrogen flow be adjusted to 5～
10L/min, when the amount that oligomer is released exceedes the 20% of waste PE plastic amount, terminates for depolymerization；
C), cooling down operation,
When thing amount the most to be oligomerized is to the weight specified, the little fire of brennschluss burner, the air blast opening burner carries out the cold of the interior material of still
But；
2. when in still material temperature degree be down to less than 300 DEG C, the air blast of brennschluss burner, stop the stirring on depolymerization still, carry out the standard of binder
Standby；
D), oxidizing process, including binder, oxidation, blowing technique,
The most 1. the detailed process of binder technique is,
A), when in depolymerization still, material temperature is at 240 DEG C, and stopping depolymerization still stirs, and closes bottom discharge valve and the bottom discharge of stills for air blowing
Valve, inserts depolymerization still discharge nozzle in stills for air blowing；
B), all valves closed on depolymerization still, the little atmospheric valve (6) on receptor, open nitrogen and depolymerization still be forced into
When 0.06～0.08MPa, unwind the outlet valve (1) of poly-still, PE wax (9) is pressed into stills for air blowing；
2. the detailed process of oxidation technology is,
A), after PE wax (9) is completely forced into stills for air blowing, when material temperature is to 180～190 DEG C in stills for air blowing, PE wax (9) amount is put into
The stearic acid of 10%；
B), open stirring, control to adjust frequency conversion, i.e. control speed of agitator；
C), when in stills for air blowing material temperature degree be down to 180～190 DEG C, open compressed air inlet valve, be passed through 60～80L/ml flows
Compressed gas, starts stills for air blowing are led to oxygen；
D), operation in, when oxidation temperature in the kettle rise to 150～160 DEG C, open cooling water, when temperature in the kettle drops to 150
DEG C, close cooling water, so go round and begin again and carry out logical oxygen operation control；
E), reacting 1～1.5 hour, stop stirring, close oxygen intake valve, oxidation reaction terminates；
The detailed process of blowing technique is,
A), close the vacuum valve on still, nitrogen valve, bottom discharge valve, drain valve in the middle of oxidation, open putting on still in the middle of oxidation
Empty valve and inlet valve；
B), install filter screen, hopper is inserted still in the middle of oxidation, open stills for air blowing bottom discharge valve, expect to put into by the OPE of stills for air blowing
Still in the middle of oxidation；
E), material spray, all put in the middle of oxidation after still until OPE, close still upper feeding valve in the middle of oxidation, close atmospheric valve, open
Nitrogen valve is forced into 0.1MPa to still in the middle of oxidation, opens air compressor machine, and air (14) enters still in the middle of oxidation, opens oxidation
The bottom discharge valve of middle still carries out material spray；The device that material spray uses can guarantee that granule is uniform, fine and smooth；
F), packing, after pelletize to be sprayed terminates, packaging personnel must wear protective garment, uses specific purpose tool, by the product of pelletize
Product carry out mesh screen, and the product (15) being sieved is loaded in packaging bag.
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| CN201610661248.1A CN106220758B (en) | 2016-08-13 | 2016-08-13 | A kind of preparation method of waste PE plastic agricultural film production oxidized polyethylene wax |
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|---|---|---|---|
| CN201610661248.1A CN106220758B (en) | 2016-08-13 | 2016-08-13 | A kind of preparation method of waste PE plastic agricultural film production oxidized polyethylene wax |
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| CN106220758B CN106220758B (en) | 2018-08-17 |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107286274A (en) * | 2017-06-24 | 2017-10-24 | 衡水毅美新材料科技有限公司 | The preparation facilities and method of a kind of high density OPE |
| CN107286277A (en) * | 2017-07-14 | 2017-10-24 | 成都新柯力化工科技有限公司 | A kind of method that screw extruder low temperature pyrolyzer regenerated plastics prepare Tissuemat E |
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| CN104277167A (en) * | 2013-07-10 | 2015-01-14 | 胡永生 | Preparation method of high-density oxidized polyethylene wax |
| CN105315391A (en) * | 2015-10-14 | 2016-02-10 | 封开县粤华塑料色母有限责任公司 | Method for preparing polyethylene wax through waste polyethylene |
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|---|---|---|---|---|
| EP0243190A1 (en) * | 1986-04-23 | 1987-10-28 | Nippon Oil Co. Ltd. | Catalysts for polymerization of olefins |
| CN1206719A (en) * | 1997-07-11 | 1999-02-03 | 科莱恩有限公司 | Process for oxidizing polyvinyl wax |
| US20030130438A1 (en) * | 2001-06-28 | 2003-07-10 | Akikazu Amagai | Bifunctional phenylene ether oligomer, its derivatives its use and process for the production thereof |
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| CN104277229A (en) * | 2013-07-10 | 2015-01-14 | 胡永生 | Preparation method of high-density oxidized polyethylene wax emulsion |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107286274A (en) * | 2017-06-24 | 2017-10-24 | 衡水毅美新材料科技有限公司 | The preparation facilities and method of a kind of high density OPE |
| CN107286277A (en) * | 2017-07-14 | 2017-10-24 | 成都新柯力化工科技有限公司 | A kind of method that screw extruder low temperature pyrolyzer regenerated plastics prepare Tissuemat E |
| CN107286277B (en) * | 2017-07-14 | 2019-12-24 | 泗阳金拓驰环保科技有限公司 | Method for preparing polyethylene wax by low-temperature cracking of recycled plastic through screw extruder |
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|---|---|
| CN106220758B (en) | 2018-08-17 |
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