CN102504330B - Method for preparing polyolefin wax - Google Patents
Method for preparing polyolefin wax Download PDFInfo
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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
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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 wax-like, therefore is commonly called as polyolefin-wax, mainly refers to polyethylene wax and Poly Propylene Wax, is widely used in the 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 larger 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.
The present domestic method of producing polyolefin-wax by the waste plastic pyrolysis generally adopts conventional equipment or Novel hot cracker cheaply.As, patent (CN 101885857 A) adopts 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, electrified heating and stirring, jaw crusher, vacuum pump, produces polyethylene wax with the conventional equipment pyrolysis of waste plastics of the stainless cracked gas recovery still of cooling jacket, stainless cracked oil hold tank, stainless tail gas emulsion tank.Another patent (CN 2680664Y) discloses the device that a kind of Novel hot cracking polyethylene is produced wax, and this device comprises the equipment such as pyrolysis oven, pyrolysis still, heat exchanger, burner, agitator.
In above-mentioned prior art, waste plastic is produced method required equipment and the processing condition simple and feasible of polyethylene wax, has satisfied the requirement of medium and small sized enterprises' suitability for industrialized production, 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 is also different, and the randomness of cracking stock also further affects the quality of polyethylene wax; Waste plastic has than high viscosity and low conductive characteristics, and this will have a significant impact 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 for above-mentioned prior art existence, the invention provides a kind of method for preparing high-quality polyolefin-wax, be intended to by conventional equipment, intermittently cracking technology solves the randomness of waste plastic or resin raw material and low conductivity etc. self deficiency, and improves the quality of the polyolefin-wax that cracking generates.
The technical solution adopted in the present invention is:
A kind of method for preparing polyolefin-wax comprises the steps:
1) reaction raw materials is placed in reactor, carries out heat scission reaction under vacuum condition;
2) split product cools to 260～335 ℃, the Exhaust Gas mixture;
3) material in reactor continues to be down to room temperature, adds solvent to extract, and liquid-solid separation obtains solid product and product liquid;
4) product liquid obtains solvent and target product through distillation.
Preferably, described reaction raw materials is at least a in vinyon, acrylic plastering, polyvinyl resin, acrylic resin.
Preferably, described reaction raw materials is at least a in the discarded vinyon that contains the following polyester of 10wt%, acrylic plastering, polyvinyl resin, 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 ℃, after 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 ℃, after 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, tetrahydrofuran (THF) and naphthane etc., and solvent and quality of material are than greater than 2.
Step 2) the expellant gas mixture carries out condensation by water cooler, obtains liquid oil and uncooled gas, reclaims respectively; The temperature of water cooler is less than 45 ℃.
Step 3) gained solid product mixes with raw material through after simply removing the gred, and enters the next round cracking.
In 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 refers to that raw material maintains and carries out cracking under temperature of reaction, the two-part thermo-cracking refers in cracking process to use two kinds of cracking temperatures (to comprise first after the lesser temps cracking again in higher temperature cracking, or first 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 prepares high-quality polyolefin-wax product take discarded vinyon, acrylic plastering, polyvinyl resin, acrylic resin as raw material, and production cost is low, to equipment require low; The intermediate product that preparation technology produces can be collected respectively, carries out recycle, and energy-conserving and environment-protective are suitable for applying.
Figure of description
Fig. 1 is 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: reactor vacuum pump valve, valve 2: reactor 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 in reactor, carries out heat scission reaction under vacuum condition;
2) split product cools to 260～335 ℃, the Exhaust Gas mixture;
3) material in reactor continues to be down to room temperature, adds solvent to extract, and liquid-solid separation obtains solid product and product liquid;
4) product liquid obtains solvent and target product through distillation.
Preferably, described reaction raw materials is at least a in vinyon, acrylic plastering, polyvinyl resin, acrylic resin.
Preferably, described reaction raw materials is at least a in the discarded vinyon that contains the following polyester of 10wt%, acrylic plastering, polyvinyl resin, 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 ℃, after 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 ℃, after 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, tetrahydrofuran (THF) and naphthane etc., and solvent and quality of material are than greater than 2.
Step 2) the expellant gas mixture carries out condensation by water cooler, obtains liquid oil and uncooled gas, reclaims respectively; The temperature of water cooler is less than 45 ℃.
Step 3) gained solid product mixes with raw material through after simply removing the gred, and enters the next round cracking.
The present invention is further illustrated below in conjunction with embodiment, but be not limited to this.Below in each embodiment reaction raw materials used be discarded vinyon, acrylic plastering, polyvinyl resin, the acrylic resin that reclaims.Can contain not the polyester higher than 10wt% in raw material.
Embodiment 1
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) add a certain amount of above-mentioned high-density polyethylene resin in reactor, sealed reactor, the beginning heat temperature raising, the question response temperature in the kettle rises to 100 ℃, open reactor vacuum pump valve 1, open vacuum pump and vacuumize, when vacuum tightness is 0.095Mpa, close vacuum pump, continuation is heated reactor, when the question response temperature in the kettle rises to 200 ℃, and turn on agitator, stirring velocity is 90rpm, then, rise to 400 ℃, keep constant temperature, stopped reaction after reaction 60min uses the cooling jacket of reactor that reactor is cooled;
When 2) the question response temperature in the kettle is cooled to 280 ℃, open reactor vent valve 2, the low molecular carbon hydrogen molecule that cracking produces enters into water cooler by pipeline, the cooler outlet temperature is controlled at below 45 ℃, low molecular carbon hydrogen is condensed into liquid oil and enters into storage recovery in fuel oil tank, and uncooled low molecular carbon hydrogen enters in the splitting gas storage tank by pipeline and stores;
3) material in reactor is cooled to room temperature, add solvent to extract, the solvent of extraction use is normal hexane, solvent is 4:1 with the quality of material ratio, after adding, fully mixes with material by solvent, entering tripping device by pipeline separates, after separating the simple slagging-off of solid product process that obtains, mix with raw material, enter the next round cracking, separate the product liquid that obtains and obtain solvent and target product through air distillation, wherein solvent cycle is used, after the solvent distillation, the solid of gained is polyethylene wax, its productive rate is 61.2 wt%, molecular weight is about 3372, melt drop temperature is 115 ℃, take out, packing, obtain the polyethylene wax finished product.
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 steps:
1) add a certain amount of above-mentioned acrylic resin in reactor, sealed reactor, the beginning heat temperature raising, the question response temperature in the kettle rises to 100 ℃, open reactor vacuum pump valve 1, the unlatching vacuum pump vacuumizes, when vacuum tightness is 0.05Mpa, close vacuum pump, continue reactor is heated, when the question response temperature in the kettle rises to 200 ℃, turn on agitator, stirring velocity is 90rpm, continues to be warming up to 340 ℃, after isothermal reaction 210min, use the cooling jacket of reactor that reactor is cooled;
When 2) the question response temperature in the kettle is cooled to 335 ℃, open reactor vent valve 2, the low molecular carbon hydrogen molecule that cracking produces enters into water cooler by pipeline, the temperature out of water cooler is controlled at below 40 ℃, low molecular carbon hydrogen is condensed into liquid oil and enters into storage recovery in fuel oil tank, and uncooled low molecular carbon hydrogen enters in the splitting gas storage tank by pipeline and stores;
3) material in reactor continues to be cooled to room temperature, add solvent to extract, the solvent of extraction use is tetrahydrofuran (THF), solvent is 2.1:1 with the quality of material ratio, fully mix with material after solvent adds, enter tripping device by pipeline and separate, after separating the simple slagging-off of solid product process that obtains, mix with raw material, enter 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 steps:
1) add a certain amount of acrylic resin and polyvinyl resin in reactor, its mass ratio is 1:1, sealed reactor, the beginning heat temperature raising, in the question response still, medium temperature rises to 100 ℃, open reactor vacuum pump valve 1, the unlatching vacuum pump vacuumizes, when vacuum tightness is 0.005Mpa, close vacuum pump, continuation is heated reactor, subsequently, when the question response temperature in the kettle rises to 200 ℃, turn on agitator, stirring velocity 90rpm, continue to be warmed up to 450 ℃, after isothermal reaction 10 minutes, pass into cooling water temperature to 340 ℃ in the cooling jacket of reactor, isothermal reaction 150 minutes,
2) question response is complete, cool to 300 ℃, open reactor vent valve 2, the low molecular carbon hydrogen molecule that cracking produces enters into water cooler by pipeline, the cooler outlet temperature is controlled at below 40 ℃, low molecular carbon hydrogen is condensed into liquid oil and enters into storage recovery in fuel oil tank, and uncooled low molecular carbon hydrogen enters in the splitting gas storage tank by pipeline and stores;
3) reactor continues to be cooled to room temperature, open reactor and add mass ratio 1:1 tetrahydrofuran (THF) and hexanaphthene mixed solvent, solvent is 5:1 with the quality of material ratio, after adding, fully mixes with material by solvent, entering tripping device by pipeline separates, do not dissolve part through after simply removing the gred, mix with raw material, enter the next round cracking, obtain product liquid after extracting and separating and obtain solvent and target product through air distillation, wherein solvent cycle is used, target product is polyolefin-wax, its productive rate is 51.2 wt%, molecular weight is about 5120, melt drop temperature is 124 ℃, take out, packing, obtain the polyolefin-wax finished product.
Embodiment 4
Product: polyolefin-wax
Raw material: discarded 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 steps:
1) add a certain amount of discarded acrylic plastering and vinyon in reactor, mass ratio 1:1, amount of polyester 10%, sealed reactor, the beginning heat temperature raising, in the question response still, medium temperature rises to 100 ℃, open reactor vacuum pump valve 1, the unlatching vacuum pump vacuumizes, when vacuum tightness is 0.025Mpa, close vacuum pump, continuation is heated reactor, subsequently, when the question response temperature in the kettle rises to 200 ℃, turn on agitator, stirring velocity 90rpm, continue to be warmed up to 340 ℃, after isothermal reaction 150 minutes, continue to be heated to 450 ℃, isothermal reaction 10min.
2) question response is complete, cool to 290 ℃, open reactor vent valve 2, the low molecular carbon hydrogen molecule that cracking produces enters into water cooler by pipeline, the cooler outlet temperature is controlled at below 40 ℃, low molecular carbon hydrogen is condensed into liquid oil and enters into storage recovery in fuel oil tank, and uncooled low molecular carbon hydrogen enters in the splitting gas storage tank by pipeline and stores;
3) reactor continues to be cooled to room temperature, open tetrahydrofuran (THF) and hexanaphthene mixed solvent that reactor adds mass ratio 1:2, solvent is 6:1 with the quality of material ratio, after adding, fully mixes with material by solvent, entering tripping device by pipeline separates, do not dissolve part through after simply removing the gred, mix with raw material, enter the next round cracking, obtain product liquid after extracting and separating and obtain solvent and target product through air distillation, wherein solvent cycle is used, target product is polyolefin-wax, its productive rate is 43.3wt%, molecular weight is about 4877, melt drop temperature is 121 ℃, take out, packing, obtain the polyolefin-wax finished product.
Above embodiment is only for introducing preferred case of the present invention, preparation in accordance with the present invention, except available polyethylene resin, acrylic resin or its mixture as reaction raw materials, also discarded vinyon, acrylic plastering or its mixture of available utilization is prepared as reaction raw materials, all can obtain high-quality polyolefin-wax.What obtain take polyethylene as raw material is polyethylene wax, and what obtain take polypropylene as raw material is Poly Propylene Wax, and what mixing raw material obtained is polyolefin-wax.
Therefore, to those skilled in the art, any apparent changes and improvements of carrying out in the scope that does not deviate from spirit of the present invention all should be regarded as a part of the present invention.
Claims (6)
1. a method for preparing polyolefin-wax, comprise the steps:
1) reaction raw materials is placed in reactor, carries out heat scission reaction under vacuum condition;
2) split product cools to 260～335 ℃, the Exhaust Gas mixture;
3) material in reactor continues to be down to room temperature, adds solvent to extract, and liquid-solid separation obtains solid product and product liquid;
4) product liquid obtains solvent and target product through distillation;
It is characterized in that:
The described reaction raw materials of step 1) is at least a in vinyon, acrylic plastering, polyvinyl resin, acrylic resin;
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;
Step 3) extraction solvent for use is at least a in normal hexane, tetrahydrofuran (THF) and naphthane.
2. a kind of method for preparing polyolefin-wax according to claim 1, is characterized in that, the condition of step 1) heat scission reaction is: begin to react vacuum tightness 0.005～0.095Mpa, 340～380 ℃, after reaction 10～180min, be warming up to 380～450 ℃, continue reaction 10～180min.
3. a kind of method for preparing polyolefin-wax according to claim 1, is characterized in that, the condition of step 1) heat scission reaction is: begin to react vacuum tightness 0.005～0.095Mpa, 380～450 ℃, after reaction 10～180min, be cooled to 340～380 ℃, continue reaction 10～180min.
4. a kind of method for preparing polyolefin-wax according to claim 1, is characterized in that, step 3) extraction solvent for use is at least a in normal hexane, tetrahydrofuran (THF) and naphthane, and solvent and quality of material are than greater than 2.
5. a kind of method for preparing polyolefin-wax according to claim 1, is characterized in that step 2) the expellant gas mixture carries out condensation by water cooler, obtains liquid oil and uncooled gas, reclaim respectively; The temperature of water cooler is less than 45 ℃.
6. a kind of method for preparing polyolefin-wax according to claim 1, is characterized in that, step 3) gained solid product through simple slagging-off after, mix with raw material, enter the next round cracking.
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| US11845900B2 (en) | 2016-03-31 | 2023-12-19 | H&R Internationale Beteiligung Gmbh | Process for the preparation of a C20 to C60 wax from the selective thermal decomposition of plastic polyolefin polymer |
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