CN102504330A - Method for preparing polyolefin wax - Google Patents
Method for preparing polyolefin wax Download PDFInfo
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- CN102504330A CN102504330A CN2011103273793A CN201110327379A CN102504330A CN 102504330 A CN102504330 A CN 102504330A CN 2011103273793 A CN2011103273793 A CN 2011103273793A CN 201110327379 A CN201110327379 A CN 201110327379A CN 102504330 A CN102504330 A CN 102504330A
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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 invention discloses a method for preparing a polyolefin wax. The method comprises the following steps: (1) placing raw materials for reaction in a reaction kettle, and carrying out thermal cracking reaction in a vacuum condition; (2) cooling the pyrolysis product to 260-335 DEG C, and discharging air mixture; (3) continuously cooling the materials in the reaction kettle to room temperature, adding a solvent for extracting, and carrying out liquid-solid separation to obtain a solid product and a liquid product; and (4) distilling the liquid product to obtain the solvent and a target product. According to the method, high-quality polyolefin wax product is prepared by taking polyethylene plastic, polypropylene plastic, polyethylene resin and polypropylene resin as raw materials, and has the advantages of low production cost and low equipment requirement; and intermediate products prepared in the preparation process can be separately collected for cyclic utilization, so that the method is energy-saving and environment-friendly and is suitable for generalization and use.
Description
Technical field
The present invention relates to a kind of method for preparing high-quality polyolefin-wax.
Background technology
Low molecular weight polycaprolactone alkene at room temperature becomes the wax shape, therefore is commonly called as polyolefin-wax, mainly refers to polyethylene wax and Poly Propylene Wax, is widely used in industries such as chemical industry, light industry, food.The polyolefin-wax year consumption in the whole world is about 33.63 ten thousand t, and is still continuing growth.China's polyolefin-wax industrial scale can not be met the need of market, and the basic dependence on import of especially high-grade polyolefin-wax has the bigger market space.Utilize waste plastic produce high-quality polyolefin-wax for the recycling of waste resource, eliminate environmental pollution etc. and have important economy and social effect.
At present domesticly produce the method for polyolefin-wax, generally adopt conventional equipment or novel cheaply thermal cracker through the waste plastic pyrolysis.As, patent (CN 101885857 A) adopts the stainless cracked gas of the unlimited stainless material box in stainless cooling reactor, the top of stainless cracking still, belt stirrer and the cooling jacket of screw extrusion press, charged heating and stirring, jaw crusher, vacuum pump, band cooling jacket to reclaim the conventional equipment pyrolysis preparing polyethylene wax from waste plastic of still, stainless cracked oil hold tank, stainless tail gas emulsion tank.Another patent (CN 2680664Y) discloses the device that a kind of novel thermo-cracking Vilaterm is produced wax, and this device comprises equipment such as pyrolysis oven, pyrolysis still, heat exchanger, burner, whisking appliance.
Waste plastic is produced the method required equipment and the processing condition simple and feasible of polyethylene wax in the above-mentioned prior art, has satisfied medium and small sized enterprises' industrial production requirement, but the quality of resulting polyethylene wax is not high; Because the recovery of waste plastic involves a wide range of knowledge, the composition of every batch of recovery also has nothing in common with each other, and the randomness of cracking stock also further influences the quality of polyethylene wax; Waste plastic has than high viscosity and low conductive characteristics, and this will have very big influence to heat transfer and mass transfer in the pyrolytic reaction process; Therefore, art methods exists the not high problems and shortcomings of polyethylene wax quality that adopt low cost simple equipment pyrolysis waste plastic to produce.
Summary of the invention
Problems and shortcomings to above-mentioned prior art existence; The invention provides a kind of method for preparing high-quality polyolefin-wax; Be intended to through conventional equipment, intermittently cracking technology solves randomness and low conductivity etc. self deficiency of waste plastic or resin raw material, and improves the quality of the polyolefin-wax that cracking generates.
The technical scheme that the present invention adopted is:
A kind of method for preparing polyolefin-wax comprises the steps:
1) reaction raw materials is placed reaction kettle, under vacuum condition, carry out heat scission reaction;
2) split product cools to 260～335 ℃, discharges gaseous mixture;
3) material in reactor continues to reduce to room temperature, adds solvent and extracts, and liquid-solid separation obtains solid product and product liquid;
4) product liquid obtains solvent and title product through distillation.
Preferably, said reaction raw materials is at least a in vinyon, acrylic plastering, polyvinyl resin, the acrylic resin.
Preferably, said reaction raw materials is at least a in the discarded vinyon that contains the polyester below the 10wt%, acrylic plastering, polyvinyl resin, the acrylic resin.
Preferably, the condition of step 1) heat scission reaction is: begin to react vacuum tightness 0.005～0.095Mpa, 340～450 ℃ of temperature of reaction, reaction 10～210min.
Preferably, the condition of step 1) heat scission reaction is: begin to react vacuum tightness 0.005～0.095Mpa, and 340～380 ℃, behind reaction 10～180min, be warming up to 380～450 ℃, continue reaction 10～180min.
Preferably, the condition of step 1) heat scission reaction is: begin to react vacuum tightness 0.005～0.095Mpa, and 380～450 ℃, behind reaction 10～180min, be cooled to 340～380 ℃, continue reaction 10～180min.
Preferably, step 3) extraction solvent for use is at least a in normal hexane, THF and the naphthane etc., and solvent and quality of material are than greater than 2.
Step 2) the expellant gas mixture carries out condensation through water cooler, obtains liquid oil and uncooled gas, reclaims respectively; The temperature of water cooler is less than 45 ℃.
Step 3) gained solid product with raw materials mix, gets into the next round cracking through after simply removing the gred.
Among the above-mentioned preparation method; Heat scission reaction both can adopt the one-part form reaction also can adopt the two-part reaction; The one-part form thermo-cracking is meant that raw material maintains and carries out cracking under the temperature of reaction; The two-part thermo-cracking be meant in cracking process use two kinds of cracking temperatures (comprise earlier after the lesser temps cracking again in higher temperature cracking, or earlier after higher temperature cracking again in lower temperature cracking), can be according to actual needs; Take different heat scission reaction modes, obtain the product of different output, different molecular weight, different melt drop temperature.
Beneficial effect of the present invention is: the present invention is a raw material with discarded vinyon, acrylic plastering, polyvinyl resin, acrylic resin, prepares high-quality polyolefin-wax product, and production cost is low, to equipment require low; The intermediate product that preparation technology produced can be collected respectively, carries out recycle, and energy-conserving and environment-protective are suitable for applying.
Figure of description
Fig. 1 is the position annexation and the process flow sheet of each equipment of a kind of method of producing high-quality polyolefin-wax of the present invention, valve 1: reaction kettle vacuum pump valve, valve 2: reaction kettle vent valve, valve 3: discharging valve of reaction kettle, valve 4: tripping device baiting valve.
Embodiment
A kind of method for preparing polyolefin-wax comprises the steps:
1) reaction raw materials is placed reaction kettle, under vacuum condition, carry out heat scission reaction;
2) split product cools to 260～335 ℃, discharges gaseous mixture;
3) material in reactor continues to reduce to room temperature, adds solvent and extracts, and liquid-solid separation obtains solid product and product liquid;
4) product liquid obtains solvent and title product through distillation.
Preferably, said reaction raw materials is at least a in vinyon, acrylic plastering, polyvinyl resin, the acrylic resin.
Preferably, said reaction raw materials is at least a in the discarded vinyon that contains the polyester below the 10wt%, acrylic plastering, polyvinyl resin, the acrylic resin.
Preferably, the condition of step 1) heat scission reaction is: begin to react vacuum tightness 0.005～0.095Mpa, 340～450 ℃ of temperature of reaction, reaction 10～210min.
Preferably, the condition of step 1) heat scission reaction is: begin to react vacuum tightness 0.005～0.095Mpa, and 340～380 ℃, behind reaction 10～180min, be warming up to 380～450 ℃, continue reaction 10～180min.
Preferably, the condition of step 1) heat scission reaction is: begin to react vacuum tightness 0.005～0.095Mpa, and 380～450 ℃, behind reaction 10～180min, be cooled to 340～380 ℃, continue reaction 10～180min.
Preferably, step 3) extraction solvent for use is at least a in normal hexane, THF and the naphthane etc., and solvent and quality of material are than greater than 2.
Step 2) the expellant gas mixture carries out condensation through water cooler, obtains liquid oil and uncooled gas, reclaims respectively; The temperature of water cooler is less than 45 ℃.
Step 3) gained solid product with raw materials mix, gets into the next round cracking through after simply removing the gred.
Below in conjunction with embodiment the present invention is further described, but is not limited thereto.Below among each embodiment used reaction raw materials be discarded vinyon, acrylic plastering, polyvinyl resin, the acrylic resin that reclaims.Can contain the polyester that is not higher than 10wt% in the raw material.
Product: polyethylene wax
Raw material: high-density polyethylene resin
Equipment: the electric heating reacting kettle of belt stirrer and cooling jacket, vacuum pump, water cooler, fuel oil tank, tripping device, water distilling apparatus, each device location and annexation are consulted Fig. 1
Preparation process:
1) in reaction kettle, add a certain amount of above-mentioned high-density polyethylene resin, sealed reactor, the beginning heat temperature raising, the question response temperature in the kettle rises to 100 ℃; Open reaction kettle vacuum pump valve 1, the open vacuum pump vacuumizes, and when vacuum tightness is 0.095Mpa, closes vacuum pump; Continuation is heated reaction kettle, when the question response temperature in the kettle rises to 200 ℃, and turn on agitator; Stirring velocity is 90rpm, then, rises to 400 ℃; Keep constant temperature, stopped reaction behind the reaction 60min uses the cooling jacket of reaction kettle that reaction kettle is cooled;
When 2) the question response temperature in the kettle is cooled to 280 ℃; Open reaction kettle vent valve 2; The low molecular carbon hydrogen molecule that cracking produces enters into water cooler through pipeline; The cooler outlet temperature is controlled at below 45 ℃, and low molecular carbon hydrogen is condensed into liquid oil and enters into storage recovery in the fuel oil tank, and uncooled low molecular carbon hydrogen enters in the splitting gas storage tank through pipeline and stores;
3) material in reactor is cooled to room temperature, adds solvent and extracts, and the solvent that extraction is used is normal hexane, and solvent is 4:1 with the quality of material ratio; Solvent adding back and material thorough mixing get into tripping device through pipeline and separate, after the simple slagging-off of solid product process that separation obtains, with raw materials mix; Get into the next round cracking, separate the product liquid that obtains and obtain solvent and target product through air distillation, wherein solvent cycle is used, and the solid of solvent distillation back gained is polyethylene wax; Its productive rate is 61.2 wt%, and molecular weight is about 3372, and melt drop temperature is 115 ℃; Take out, packing obtains the polyethylene wax finished product.
Embodiment 2
Product: Poly Propylene Wax
Raw material: acrylic resin
Equipment: the electric heating reacting kettle of belt stirrer and cooling jacket, vacuum pump, water cooler, fuel oil tank, tripping device, water distilling apparatus, each device location and annexation are consulted Fig. 1;
Reactions step:
1) in reaction kettle, adds a certain amount of above-mentioned acrylic resin, sealed reactor, beginning heat temperature raising; The question response temperature in the kettle rises to 100 ℃, opens reaction kettle vacuum pump valve 1, and the open vacuum pump vacuumizes; When vacuum tightness is 0.05Mpa, close vacuum pump, continue reaction kettle is heated; When the question response temperature in the kettle rose to 200 ℃, turn on agitator, stirring velocity were 90rpm; Continue to be warming up to 340 ℃, behind the isothermal reaction 210min, use the cooling jacket of reaction kettle that reaction kettle is cooled;
When 2) the question response temperature in the kettle is cooled to 335 ℃; Open reaction kettle vent valve 2; The low molecular carbon hydrogen molecule that cracking produces enters into water cooler through pipeline; The temperature out of water cooler is controlled at below 40 ℃, and low molecular carbon hydrogen is condensed into liquid oil and enters into storage recovery in the fuel oil tank, and uncooled low molecular carbon hydrogen enters in the splitting gas storage tank through pipeline and stores;
3) material in reactor continues to be cooled to room temperature, adds solvent and extracts, and the solvent that extraction is used is THF; Solvent is 2.1:1 with the quality of material ratio; Solvent adding back and material thorough mixing get into tripping device through pipeline and separate, after the simple slagging-off of solid product process that separation obtains; With raw materials mix, get into the next round cracking; Separate the product liquid that obtains and obtain solvent and target product through underpressure distillation, wherein solvent cycle is used, and target product is Poly Propylene Wax; Its productive rate is 49.4 wt%, and the main scope of molecular weight is 6549, and melt drop temperature is 135 ℃; Take out, packing obtains the Poly Propylene Wax finished product.
Embodiment 3
Product: polyolefin-wax
Raw material: acrylic resin and polyvinyl resin
Equipment: the electric heating reacting kettle of belt stirrer and cooling jacket, vacuum pump, water cooler, fuel oil tank, tripping device, water distilling apparatus, each device location and annexation are consulted Fig. 1;
Reactions step:
1) in reaction kettle, add a certain amount of acrylic resin and polyvinyl resin, its mass ratio is 1:1, sealed reactor, beginning heat temperature raising; Medium temperature rises to 100 ℃ in the question response still, opens reaction kettle vacuum pump valve 1, and the open vacuum pump vacuumizes, when vacuum tightness is 0.005Mpa; Close vacuum pump, continue reaction kettle is heated, subsequently, when the question response temperature in the kettle rises to 200 ℃; Turn on agitator, stirring velocity 90rpm continues to be warmed up to 450 ℃; After the isothermal reaction 10 minutes, feed cooling water temperature to 340 ℃, isothermal reaction 150 minutes in the cooling jacket of reaction kettle;
2) question response finishes; Cool to 300 ℃; Open reaction kettle vent valve 2, the low molecular carbon hydrogen molecule that cracking produces enters into water cooler through pipeline, and the cooler outlet temperature is controlled at below 40 ℃; Low molecular carbon hydrogen is condensed into liquid oil and enters into storage recovery in the fuel oil tank, and uncooled low molecular carbon hydrogen enters in the splitting gas storage tank through pipeline and stores;
3) reaction kettle continues to be cooled to room temperature; Open reaction kettle and add mass ratio 1:1 THF and hexanaphthene mixed solvent, solvent is 5:1 with the quality of material ratio, and solvent adds back and material thorough mixing, separates through pipeline entering tripping device; Do not dissolve part through after simply removing the gred,, get into the next round cracking with raw materials mix; Obtain product liquid after the extracting and separating and obtain solvent and target product through air distillation, wherein solvent cycle is used, and target product is polyolefin-wax; Its productive rate is 51.2 wt%, and molecular weight is about 5120, and melt drop temperature is 124 ℃; Take out, packing obtains the polyolefin-wax finished product.
Product: polyolefin-wax
Raw material: depleted acrylic plastering and vinyon, mass ratio 1:1, amount of polyester 10%
Equipment: the electric heating reacting kettle of belt stirrer and cooling jacket, vacuum pump, water cooler, fuel oil tank, tripping device, water distilling apparatus, each device location and annexation are consulted Fig. 1;
Reactions step:
1) in reaction kettle, adds a certain amount of depleted acrylic plastering and vinyon, mass ratio 1:1, amount of polyester 10%, sealed reactor; The beginning heat temperature raising, medium temperature rises to 100 ℃ in the question response still, opens reaction kettle vacuum pump valve 1, and the open vacuum pump vacuumizes; When vacuum tightness is 0.025Mpa, close vacuum pump, continue reaction kettle is heated, subsequently; When the question response temperature in the kettle rises to 200 ℃, turn on agitator, stirring velocity 90rpm continues to be warmed up to 340 ℃; After the isothermal reaction 150 minutes, continue to be heated to 450 ℃, isothermal reaction 10min.
2) question response finishes; Cool to 290 ℃; Open reaction kettle vent valve 2, the low molecular carbon hydrogen molecule that cracking produces enters into water cooler through pipeline, and the cooler outlet temperature is controlled at below 40 ℃; Low molecular carbon hydrogen is condensed into liquid oil and enters into storage recovery in the fuel oil tank, and uncooled low molecular carbon hydrogen enters in the splitting gas storage tank through pipeline and stores;
3) reaction kettle continues to be cooled to room temperature; Open THF and hexanaphthene mixed solvent that reaction kettle adds mass ratio 1:2, solvent is 6:1 with the quality of material ratio, and solvent adds back and material thorough mixing, separates through pipeline entering tripping device; Do not dissolve part through after simply removing the gred,, get into the next round cracking with raw materials mix; Obtain product liquid after the extracting and separating and obtain solvent and target product through air distillation, wherein solvent cycle is used, and target product is polyolefin-wax; Its productive rate is 43.3wt%, and molecular weight is about 4877, and melt drop temperature is 121 ℃; Take out, packing obtains the polyolefin-wax finished product.
Above embodiment is merely and introduces preferred case of the present invention; Preparation in accordance with the present invention; Except available polyethylene resin, acrylic resin or its mixture as the reaction raw materials; Also available depleted vinyon, acrylic plastering or its mixture of utilizing prepares as reaction raw materials, all can obtain high-quality polyolefin-wax.What with the Vilaterm be that raw material obtains is polyethylene wax, and what with the Vestolen PP 7052 be that raw material obtains is Poly Propylene Wax, and what mixing raw material obtained is polyolefin-wax.
Therefore, to those skilled in the art, any conspicuous variation and the improvement in the scope that does not deviate from spirit of the present invention, carried out all should be regarded as a part of the present invention.
Claims (8)
1. a method for preparing polyolefin-wax comprises the steps:
1) reaction raw materials is placed reaction kettle, under vacuum condition, carry out heat scission reaction;
2) split product cools to 260～335 ℃, discharges gaseous mixture;
3) material in reactor continues to reduce to room temperature, adds solvent and extracts, and liquid-solid separation obtains solid product and product liquid;
4) product liquid obtains solvent and title product through distillation.
2. a kind of method for preparing polyolefin-wax according to claim 1 is characterized in that, the said reaction raw materials of step 1) is at least a in vinyon, acrylic plastering, polyvinyl resin, the acrylic resin.
3. according to the said a kind of method for preparing polyolefin-wax of claim 1, it is characterized in that the condition of step 1) heat scission reaction is: begin to react vacuum tightness 0.005～0.095Mpa, 340～450 ℃ of temperature of reaction, reaction 10～210min.
4. according to the said a kind of method for preparing polyolefin-wax of claim 1, it is characterized in that the condition of step 1) heat scission reaction is: begin to react vacuum tightness 0.005～0.095Mpa; 340～380 ℃; Behind reaction 10～180min, be warming up to 380～450 ℃, continue reaction 10～180min.
5. according to the said a kind of method for preparing polyolefin-wax of claim 1, it is characterized in that the condition of step 1) heat scission reaction is: begin to react vacuum tightness 0.005～0.095Mpa; 380～450 ℃; Behind reaction 10～180min, be cooled to 340～380 ℃, continue reaction 10～180min.
6. according to the said a kind of method for preparing polyolefin-wax of claim 1, it is characterized in that step 3) extraction solvent for use is at least a in normal hexane, THF and the naphthane etc., solvent and quality of material are than greater than 2.
7. according to the said a kind of method for preparing polyolefin-wax of claim 1, it is characterized in that step 2) the expellant gas mixture carries out condensation through water cooler, obtains liquid oil and uncooled gas, reclaim respectively; The temperature of water cooler is less than 45 ℃.
8. according to the said a kind of method for preparing polyolefin-wax of claim 1, it is characterized in that step 3) gained solid product with raw materials mix, gets into the next round cracking through after simply removing the gred.
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Cited By (17)
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|---|---|---|---|---|
| CN103484146A (en) * | 2013-06-06 | 2014-01-01 | 河南科技大学 | Method used for preparing liquid hydrocarbon from polydicyclopentadiene by cracking reaction |
| CN103628184A (en) * | 2012-08-23 | 2014-03-12 | 中国石油化工股份有限公司 | Recovery processing method of ultrahigh molecular weight polyethylene dry spinning jelly and waste fiber solvent |
| CN105542489A (en) * | 2016-01-30 | 2016-05-04 | 扬州金橡塑化工材料厂 | Method for preparing polyethylene wax by virtue of splitting decomposition of polypropylene |
| WO2017168163A1 (en) * | 2016-03-31 | 2017-10-05 | Trifol Resources Limited | PROCESS FOR THE PREPARATION OF A C20 to C60 WAX FROM THE SELECTIVE THERMAL DECOMPOSITION OF PLASTIC POLYOLEFIN POLYMER |
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| CN107266612A (en) * | 2017-06-13 | 2017-10-20 | 扬州罗兰新材料有限公司 | A kind of two-step method produces the manufacture method of chemical fibre masterbatch composite polypropylene wax |
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| CN103484146A (en) * | 2013-06-06 | 2014-01-01 | 河南科技大学 | Method used for preparing liquid hydrocarbon from polydicyclopentadiene by cracking reaction |
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| CN105542489A (en) * | 2016-01-30 | 2016-05-04 | 扬州金橡塑化工材料厂 | Method for preparing polyethylene wax by virtue of splitting decomposition of polypropylene |
| CN105542489B (en) * | 2016-01-30 | 2019-03-29 | 扬州金橡塑化工材料厂 | A method of macromolecule wax is prepared with polypropylene pyrolysis |
| CN108884265A (en) * | 2016-03-31 | 2018-11-23 | 霍尼韦尔国际公司 | The method for producing polyolefin-wax product |
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