CN115651268A - Method for preparing polyethylene wax by continuously cracking waste polyethylene - Google Patents
Method for preparing polyethylene wax by continuously cracking waste polyethylene Download PDFInfo
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- CN115651268A CN115651268A CN202211225404.1A CN202211225404A CN115651268A CN 115651268 A CN115651268 A CN 115651268A CN 202211225404 A CN202211225404 A CN 202211225404A CN 115651268 A CN115651268 A CN 115651268A
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- waste polyethylene
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- -1 polyethylene Polymers 0.000 title claims abstract description 152
- 239000004698 Polyethylene Substances 0.000 title claims abstract description 150
- 229920000573 polyethylene Polymers 0.000 title claims abstract description 150
- 239000002699 waste material Substances 0.000 title claims abstract description 85
- 238000005336 cracking Methods 0.000 title claims abstract description 79
- 238000000034 method Methods 0.000 title claims abstract description 68
- 239000012071 phase Substances 0.000 claims description 36
- 230000008569 process Effects 0.000 claims description 29
- 239000007789 gas Substances 0.000 claims description 23
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 20
- 238000007670 refining Methods 0.000 claims description 19
- 239000012535 impurity Substances 0.000 claims description 18
- 239000002994 raw material Substances 0.000 claims description 16
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 claims description 15
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- 239000001257 hydrogen Substances 0.000 claims description 12
- 229910052739 hydrogen Inorganic materials 0.000 claims description 12
- 239000011261 inert gas Substances 0.000 claims description 11
- 229920001684 low density polyethylene Polymers 0.000 claims description 11
- 239000004702 low-density polyethylene Substances 0.000 claims description 11
- 229920000092 linear low density polyethylene Polymers 0.000 claims description 10
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- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 description 4
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Abstract
The invention provides a method for preparing polyethylene wax by continuously cracking waste polyethylene, which comprises the following steps: the waste polyethylene is cracked continuously at 300-500 deg.c to obtain gas phase product and non-gas phase product, and the non-gas phase product is separated and refined to obtain polyethylene wax. By adopting the technical scheme, the polyethylene wax, the micro-powder polyethylene wax and the oxidized polyethylene wax with the number average molecular weights of 1000-2000, 2000-3000, 3000-4000 and 4000-5000 can be obtained with low cost and high yield.
Description
Technical Field
The invention relates to the field of recycling of high molecular waste, in particular to a method for preparing polyethylene wax by continuously cracking waste polyethylene.
Background
The polyethylene wax is low-molar-mass polyethylene with the number-average molecular weight of 1000-5000 and has a high melting pointAt 90 ℃, the relative density is between 0.91 and 0.96g/cm 3 And the color is mostly white or yellowish. Because of its high melting point, low melt viscosity, excellent wear resistance, thermal stability and lubricity, it can be used as lubricant and dispersant in various fields. The polyethylene wax product is of a polymerization type and a cracking type, and the performance and the application of the polyethylene wax product mainly depend on the molar mass, the molecular weight distribution, the molecular structure and the like. The performance indexes of the method are not uniformly specified so far, and only corresponding indexes are selected according to different purposes. At present, most of domestic high-performance polyethylene wax products come from foreign imports, and mainly comprise polymeric polyethylene wax of Honeywell corporation and Clariant corporation in Germany in the United states and cracking polyethylene wax of Korea and Thailand.
The polyethylene wax product with controllable molar mass and narrow distribution can be obtained by polymerizing ethylene monomer, but the method has large processing equipment and high production cost. The cracking production process is that the raw material is subjected to high-temperature thermal cracking or catalytic cracking at the temperature of more than 300 ℃ under an anaerobic condition to generate a polyethylene wax product, and the property of the produced polyethylene wax is greatly influenced by the source of the cracking raw material. The polyethylene wax produced by using the polyethylene waste plastics has rich and cheap raw material sources, but the product quality is not well controlled. Because the plastic has poor thermal conductivity and high viscosity during heating, a melt which is easy to convey is difficult to form; secondly, the waste plastics can generate carbon deposition during pyrolysis, which not only affects the wax yield, but also adheres to equipment and pipelines to cause blockage, and is difficult to clean.
Patent CN201810569475.0 discloses a method for producing polyethylene wax from waste polyethylene: classifying waste polyethylene, cleaning, drying, pretreating, and feeding into a cracking device, adding an AL-MCM-48 catalyst accounting for 0.1% of the weight of the waste polyethylene, and heating while stirring; after the reaction is finished, the wax product is filtered and granulated, and the gas-liquid phase product enters a condensing system for cooling and recovery. The practical production of the process has the following problems: the waste polyethylene sorting, cleaning and drying processes are time-consuming and labor-consuming, and a large amount of water and energy are consumed; the added AL-MCM-48 solid acid catalyst not only can abrade stirring equipment at high temperature, but also can accelerate the coking and carbon deposition process of polyethylene, cause serious equipment coking, and reduce the wax yield; after the reaction is finished, the wax product filtering process is faced with the problems of high viscosity wax product and catalyst powder and difficult separation.
CN201210132597.6 discloses a method for preparing segment phenoxy group-containing polyethylene wax by thermal degradation, which comprises the following steps of: 100, uniformly mixing hydroquinone and polyethylene granules, adding the mixture into a high-pressure stirring reaction kettle, introducing nitrogen, reacting for 0.5 to 5 hours at 330 to 380 ℃, taking out wax blocks after the reaction is finished, and crushing to obtain a product. The polyethylene used by the method is fresh polyethylene granules, so the cost is higher; the hydroquinone is also higher in price, and aromatic hydrocarbon groups are introduced into the system, so that the color and the stability of the product are influenced; the reaction time is long, the polyethylene can generate coke-forming and carbon-depositing processes at the high temperature of 330-380 ℃, equipment coking is serious, and the yield of the polyethylene wax can be reduced.
CN201510665356.1 discloses a method for producing polyethylene wax from waste polyethylene: firstly, cleaning waste polyethylene, then putting the waste polyethylene into a cracking furnace, adding a petroleum ether solution, and dissolving for 2-3 h at room temperature; then introducing steam into the furnace, and continuously cracking for 1-2 h; adding 2, 6-tetramethyl-N-piperidine oxide into the solution after cracking, continuously stirring, and reacting for 30-50 min; cooling the cracked solution to room temperature, and discharging; and detecting the product quality after crushing. The practical production of the process has the following problems: the waste polyethylene cleaning process is time-consuming and labor-consuming, and consumes a large amount of water; adding petroleum ether solution to dissolve for 2-3 h at room temperature, which wastes time and labor and consumes a large amount of petroleum ether; introducing steam into the furnace, continuously cracking for 1-2 h, adding 2, 6-tetramethyl-N-piperidine oxide into the solution after cracking, and continuously stirring to react for 30-50 min, which is a time-consuming and labor-consuming process; and subsequent cooling, discharging and crushing processes are adopted, so that the whole process is too complex, the energy consumption and material consumption are high, and the technical economy is difficult to guarantee.
Disclosure of Invention
In view of the defects of the prior art, the invention aims to provide a method for preparing polyethylene wax by continuously cracking waste polyethylene, which is used for solving the problems of easy coking, low wax yield, poor product quality, incapability of continuous production, high safety risk, high labor intensity and high energy and material consumption in the cracking process of waste polyethylene in the prior art, thereby providing a method for producing polyethylene wax which can be continuously operated, is safe and stable, has low energy consumption, high wax yield and good product quality and is not easy to deposit carbon.
To achieve the above objects and other related objects, the present invention is achieved by the following technical solutions.
The invention provides a method for preparing polyethylene wax by continuously cracking waste polyethylene, which comprises the following steps: the waste polyethylene is cracked continuously at 300-500 deg.c to obtain gas phase product and non-gas phase product, and the non-gas phase product is separated and refined to obtain polyethylene wax.
Preferably, the waste polyethylene is subjected to cracking after pretreatment.
More preferably, the pre-treatment comprises one or more selected from cleaning, granulating, milling.
The cleaning technique is selected according to the raw material condition and local conditions. More preferably, the cleaning is selected from one or more of water cleaning, organic solvent cleaning, dry cleaning, and ultrasonic cleaning.
The waste polyethylene raw material is waste, preferably, the material of the waste polyethylene is one or more selected from LLDPE, LDPE and HDPE.
From the viewpoint of raw material and product stability, it is preferable that one material is mainly subjected to classification pretreatment, and the content of other elements except carbon and hydrogen should not exceed 10wt%. Preferably, the waste polyethylene raw material contains more than 50wt% of any one selected from LLDPE, LDPE and HDPE, and the content of other elements except hydrocarbon is not more than 10wt%. More preferably, the waste polyethylene feedstock has a content of any one selected from LLDPE, LDPE and HDPE of more than 90wt%.
Preferably, the waste polyethylene is uniformly and continuously fed to the cracking process for cracking.
Preferably, in the cracking step, the cracking time of the waste polyethylene is 1 to 60 minutes. More preferably, the lysis time is 2 to 30 minutes.
Preferably, nitrogen or inert gas is used as the protective gas for cracking. The inert gas is helium or argon.
Preferably, in the cracking, the heating mode may be one or more selected from electric heating, steam heating, molten salt heating, microwave or infrared. More preferably, the heating means is electric heating or infrared heating. The electric heating or infrared heating is adopted, so that the temperature rise is fast, the heating is uniform, and the energy utilization rate is high.
Preferably, the waste polyethylene is fed to the splitting process via a feeder. More preferably, the feeder is a screw feeder, a conveyor belt or a feed pump.
Preferably, the cracking temperature is 350 to 450 ℃.
Preferably, the gas phase product comprises one or more of hydrogen, methane, ethane, ethylene, propane, propylene, butane and butene.
Preferably, the non-gas phase product comprises a liquid phase and a solid phase. More preferably, the solid phase comprises polyethylene wax and impurities. The impurities comprise one or more of waste polyethylene modified filler or entrained impurities, solid-phase products or auxiliary agents with high carbon-hydrogen ratio in the reaction process. High hydrocarbon ratio in this application means a hydrocarbon ratio higher than 1. 1.
Preferably, the separation is selected from one or more of hydrocyclone separation, centrifugation, filtration, sedimentation.
And refining to obtain a higher-quality polyethylene wax product. Preferably, the refining is selected from one or more of filtration, oxidative modification, hydrofinishing, solvent refining, adsorption refining and spray drying. The refining process can also select whether to carry out oxidation and grafting modification according to the characteristics of the product and market requirements.
More preferably, the solvent in the solvent refining is one or more selected from the group consisting of n-hexane, petroleum ether, n-dodecane, methylcyclohexane, decalin, toluene, xylene, ethanol, acetone, methyl ethyl ketone, and methyl isobutyl ketone.
More preferably, the material of the filter screen used for filtering is metal or ceramic. Preferably, the filtration is performed using a melt filter. More preferably, the precision of the filtration is 0.01 to 100 μm, and more preferably, the precision of the filtration is 0.1 to 50 μm.
More preferably, the cracking process also adopts a cracking catalyst, and the cracking catalyst is selected from MCM-41, MCM-48, SAPO molecular sieve, ZSM molecular sieve and CaCO 3 MgO, znO and aluminosilicate.
Compared with the prior art, the invention has the following advantages:
1. the method has simple and continuous flow: the whole process comprises three steps of raw material pretreatment, continuous cracking and product separation and refining, avoids complex operation processes of repeated heating and cooling, feeding and discharging and the like in an intermittent production process, and has the advantages of high automation degree, safe and reliable process, stable product property, time and labor saving, energy saving and environmental protection.
2. The product scheme is flexible: the method can adjust the operation conditions such as the types of the auxiliary agents, the reaction temperature, the reaction duration and the like according to the target product to obtain polyethylene wax and other products with different molecular structures and molecular weight distributions, and has strong market adaptability.
3. The special design improves the uniformity of heat transfer, mass transfer, momentum transfer and chemical reaction in the reactor, avoids product distribution disorder and coke formation caused by local overheating or inhomogeneous material, and has high yield of target products, simple and convenient operation and high efficiency.
By the technical scheme, the polyethylene wax, the micro-powder polyethylene wax and the oxidized polyethylene wax with the number average molecular weights of 1000-2000, 2000-3000, 3000-4000 and 4000-5000 can be obtained with low cost and high benefit.
Detailed Description
The embodiments of the present invention are described below with reference to specific embodiments, and other advantages and effects of the present invention will be easily understood by those skilled in the art from the disclosure of the present specification. The invention is capable of other and different embodiments and of being practiced or of being carried out in various ways, and its several details are capable of modification in various respects, all without departing from the spirit and scope of the present invention.
It is to be understood that the process equipment or devices not specifically mentioned in the following examples are conventional in the art.
Furthermore, it is to be understood that one or more method steps mentioned in the present invention does not exclude that other method steps may also be present before or after the combined steps or that other method steps may also be inserted between these explicitly mentioned steps, unless otherwise indicated. Moreover, unless otherwise indicated, the numbering of the various method steps is merely a convenient tool for identifying the various method steps, and is not intended to limit the order in which the method steps are arranged or the scope of the invention in which the invention may be practiced, and changes or modifications in the relative relationship may be made without substantially changing the technical content.
The embodiment of the application provides a specific embodiment, which is a method for preparing polyethylene wax by continuously cracking waste polyethylene, and the method comprises the following steps: continuously cracking waste polyethylene raw materials at 300-500 ℃ to obtain gas-phase products and non-gas-phase products, and separating and refining the non-gas-phase products to obtain the polyethylene wax. The waste polyethylene raw material is waste. In particular to a method for continuously processing waste polyethylene into polyethylene wax with practical use value in large scale.
In one embodiment, the waste polyethylene feedstock is pretreated and then cracked. In a more preferred embodiment, the pre-treatment comprises one or more selected from the group consisting of washing, granulating, milling. The cleaning technique is selected according to the raw material condition and local conditions. More preferably, the cleaning is selected from one or more of water cleaning, organic solvent cleaning, dry cleaning, and ultrasonic cleaning.
In a preferred embodiment, the waste polyethylene is one or more selected from LLDPE, LDPE and HDPE.
From the viewpoint of raw material preparation and product stability, it is preferable that one material is mainly subjected to classification pretreatment, and the content of other elements except carbon and hydrogen should not exceed 10wt%. In a preferred embodiment, the waste polyethylene contains more than 50wt% of any one selected from LLDPE, LDPE and HDPE, and no more than 10wt% of other elements than hydrocarbons. In a more preferred embodiment, said waste polyethylene contains no more than 5 wt.% of elements other than carbon and hydrogen. In a more preferred embodiment, said waste polyethylene contains no elements other than carbon and hydrogen.
In a more preferred embodiment, the waste polyethylene is present in an amount of more than 60wt% of any one selected from LLDPE, LDPE and HDPE. In a more preferred embodiment, the waste polyethylene is present in an amount of more than 90wt% of any one selected from LLDPE, LDPE and HDPE. Thus, the processing process can be more stable and easily controlled, and the molecular weight distribution of the formed polyethylene wax with the final target number average molecular weight is narrower.
In a preferred embodiment, the waste polyethylene is fed homogeneously and continuously to the cracking process for cracking.
In a preferred embodiment, the cracking time of the waste polyethylene raw material in the cracking step is 1 to 60 minutes. More preferably, the lysis time is 2 to 30 minutes. The lysis time is 5min, 10min, 15min, 20min, 25min or 30min.
In a preferred embodiment, nitrogen or inert gas is used as the protective gas for the cracking. The inert gas is helium or argon.
In a preferred embodiment, the heating means may be one or more selected from electric heating, steam heating, molten salt heating, microwave or infrared when cracking. More preferably, the heating means is electric heating or infrared heating. The electric heating or infrared heating is adopted, so that the temperature rise is fast, the heating is uniform, and the energy utilization rate is high.
In a preferred embodiment, the waste polyethylene is fed to the splitting process via a feeder. More preferably, the feeder is a screw feeder, a conveyor belt or a feed pump.
The cracking temperature and the residence time of the cracking process influence the molecular weight and the molecular weight distribution of the polyethylene wax finally obtained. In a preferred embodiment, the temperature of the cleavage is 350 to 450 ℃, such as 350 ℃, 360 ℃, 370 ℃, 380 ℃, 390 ℃, 400 ℃, 410 ℃, 420 ℃, 430 ℃, 440 ℃ or 450 ℃.
In a preferred embodiment, the gas phase product comprises one or more of hydrogen, methane, ethane, ethylene, propane, propylene, butane and butene.
In a preferred embodiment, the non-gaseous phase product comprises a liquid phase and a solid phase. In a more preferred embodiment, the solid phase comprises polyethylene wax and impurities. The impurities comprise one or more of waste polyethylene modified filler or entrained impurities, solid-phase products or auxiliary agents with high carbon-hydrogen ratio in the reaction process. High hydrocarbon ratio in this application means a hydrocarbon ratio higher than 1. 1.
In a preferred embodiment, the separation is selected from one or more of hydrocyclone separation, centrifugation, filtration, sedimentation.
When the impurities are larger solids, the impurities can be separated by adopting filtration and sedimentation separation means so as to remove the larger solid impurities. The larger solid can be straw, leaves, mud blocks, and stones. And thus the cost can be low. These impurities are often present in recycled waste polyethylene mulch.
When the impurities are smaller solids, centrifugation and hydrocyclone separation can be used to remove the smaller solids. The smaller solid may be nano or micro calcium carbonate.
And refining to obtain a polyethylene wax product with higher quality. In a preferred embodiment, the refining is selected from one or more of filtration, oxidative modification, hydrofinishing, solvent refining, adsorptive refining and spray drying. The refining process can also select whether to carry out oxidation and grafting modification according to the characteristics of the product and market requirements.
In a preferred embodiment, the filter screen used for filtering is made of metal or ceramic. Preferably, the filtration is performed using a melt filter. In a preferred embodiment, the precision of the filtration is 0.01 to 100 μm, in a more preferred embodiment, the precision of the filtration is 0.1 to 50 μm. For example, it may be 5 μm, 7 μm, 10 μm, 13 μm, 15 μm, 17 μm, 20 μm, 23 μm, 25 μm, 28 μm, 30 μm, 32 μm, 35 μm, 37 μm, 40 μm, 43 μm, 45 μm, 47 μm or 50 μm.
In a preferred embodiment, the oxidative modification is carried out by soaking in a solution of hydrogen peroxide at 75 to 95 deg.C, such as 75 deg.C, 76 deg.C, 77 deg.C, 78 deg.C, 79 deg.C, 80 deg.C, 81 deg.C, 82 deg.C, 83 deg.C, 84 deg.C, 85 deg.C, 86 deg.C, 87 deg.C, 88 deg.C, 89 deg.C, 90 deg.C, 91 deg.C, 92 deg.C, 93 deg.C, 94 deg.C or 95 deg.C. In a preferred embodiment, the concentration of the aqueous hydrogen peroxide solution is from 25 to 35wt%. Such as 25wt%, 26wt%, 27wt%, 28wt%, 29wt%, 30wt%, 31wt%, 32wt%, 33wt%, 34wt%, or 35wt%.
In a preferred embodiment, oxidative modification means graft modification with maleic anhydride and/or acrylic acid monomers at 120 to 180 ℃. For example, the temperature may be 120 ℃, 125 ℃, 130 ℃, 135 ℃, 140 ℃, 145 ℃, 150 ℃, 155 ℃, 160 ℃, 165 ℃, 170 ℃, 175 ℃ or 180 ℃.
In a preferred embodiment, the hydrofinishing refers to hydrofinishing with hydrogen at 250 to 350 ℃. For example, the temperature may be 250 ℃, 255 ℃, 260 ℃, 265 ℃, 270 ℃, 275 ℃, 280 ℃, 285 ℃, 290 ℃, 295 ℃, 300 ℃, 305 ℃, 310 ℃, 315 ℃, 320 ℃, 325 ℃, 330 ℃, 335 ℃, 340 ℃, 345 ℃ or 350 ℃.
In a preferred embodiment, the solvent refining refers to a solvent soaking treatment.
In a preferred embodiment, the adsorption purification means an adsorption treatment using an adsorbent. The adsorbent is activated carbon. In a preferred embodiment, the solvent in the solvent refining is one or more selected from n-hexane, petroleum ether, n-dodecane, methylcyclohexane, decalin, toluene, xylene, ethanol, acetone, butanone, and methyl isobutyl ketone.
In a preferred embodiment, the cracking is further carried out using a cracking catalyst selected from the group consisting of MCM-41, MCM-48, SAPO molecular sieve, ZSM molecular sieve, caCO 3 MgO, znO and aluminosilicate. The catalysts are used in the present application for lowering the reaction temperature and for improving the product distribution, i.e. for narrowing the molecular weight distribution.
In a specific embodiment, a spray dryer is used for granulation, specifically, a polyethylene wax solution is treated by the spray dryer, polyethylene wax serving as a heavy component is precipitated and collected after passing through the spray dryer, and light components such as solvent or fine impurity powder and the like are taken away in gas along with atomization and then treated.
The technical solution and technical effects of the present application are further explained and illustrated by specific examples below.
In embodiments 1 to 6 of the present application, a specific method for continuously preparing polyethylene wax is adopted, in which pretreated waste polyethylene is used as a raw material, and is continuously fed into a continuous cracking reactor, and then enters a melt filter for filtration, and a gas-phase product and a non-gas-phase product are obtained by separation, the non-gas-phase product can be further mixed with an auxiliary agent for refining, and the refined polyethylene wax is granulated to obtain a final product.
The pretreatment is to clean the waste polyethylene to remove impurities attached to the surface or the interior of the waste polyethylene, and can also further enable the appearance of the waste polyethylene to meet the feeding requirement of a device by means of grinding and the like, wherein the impurities include soil, straws, calcium carbonate and the like.
The wax formation rate in this application is the ratio of the finally obtained polyethylene wax to the polyethylene content in the raw material. The polyethylene content in the waste polyethylene is obtained by adopting an infrared test.
Example 1
The embodiment provides a specific method for preparing polyethylene wax by continuously cracking waste polyethylene, which comprises the following steps:
in the cracking process, inert gas nitrogen is adopted to provide a protective gas environment, waste polyethylene powder purchased in the market and a powdery cracking catalyst MCM-41 are uniformly mixed and sent into a continuous cracking reactor through a feeder, the cracking reactor is a tubular reactor, the mixture is primarily cracked for 30min at 350 ℃, then enters a melt filter for filtration, the filtration precision is 10 microns, and a gas-phase product is separated from a non-gas-phase product in the melt filter and then enters a gas recovery tank; mixing the non-gaseous phase product with an auxiliary agent hydrogen according to the volume ratio of 100; 1, adopting ethanol as a precipitator to precipitate polyethylene wax, and drying and grinding the precipitated polyethylene wax to obtain the refined polyethylene wax.
In the embodiment, the waste polyethylene powder purchased in the market is waste polyethylene grinding powder with HDPE content of more than 90wt%.
The obtained polyethylene wax has snow white appearance and no peculiar smell, the number average molecular weight is 4950, the melting point is 123.80 ℃, and the molecular weight distribution index is 2.68.
Comparative example 1
The difference from the example 1 is that the purchased waste polyethylene powder in the example contains HDPE, PET and PVC, and the mass ratio of the HDPE to the PET to the PVC is 1: (0.8-1.2): (0.8-1.2). The rest is the same as in example 1.
The physical and chemical properties of the obtained polyethylene wax are as follows: the obtained polyethylene wax has yellow brown appearance, pungent smell, number average molecular weight of 4730, melting point of 120.50 deg.C, and molecular weight distribution index of 5.68.
Comparative example 2
The difference from example 1 is that the initial cleavage is carried out at 550 ℃.
The rest is the same as in example 1.
The physical and chemical properties of the obtained polyethylene wax are as follows: the polyethylene wax obtained has a deep yellow appearance, a diesel-like taste, a number-average molecular weight of 730, a melting point of 60.50 ℃ and a molecular weight distribution index of 7.14.
Example 2
The embodiment provides a specific method for preparing polyethylene wax by continuously cracking waste polyethylene, which comprises the following steps:
in the cracking process, inert gas nitrogen is adopted to provide a protective gas environment, the pretreated waste polyethylene film fragments and a powdery cracking catalyst MCM-48 are uniformly mixed and are fed into a continuous cracking reactor through a feeder, the cracking reactor is a reaction kettle with a stirrer, the temperature of the cracking reactor is 370 ℃, and the average retention time of materials is 60min; discharging the material from the reaction kettle, feeding the material into a melt filter, wherein the filtering precision is 100 microns, and separating a gas-phase product from a non-gas-phase product in the melt filter, and feeding the gas-phase product into a gas recovery tank; mixing the hot non-gas-phase product with an auxiliary agent, and then feeding the mixture into a product solvent refining tank to obtain a hot mixed solution, wherein the solvent is p-xylene-ethylene glycol according to a mass ratio of 1:1, mixing; refining at 90 deg.C for 10min to obtain polyethylene wax granules or powder.
In this example, the waste polyethylene film fragments are waste films with LLDPE content of more than 95 wt%. Pretreating the waste mulching film, wherein the pretreatment is to separate and remove impurities such as straws, leaves, mud blocks, stones and the like by using an anhydrous cleaning technology; then a high-temperature horizontal centrifuge is adopted to centrifugally separate and remove the cracked nano or micron-sized solid impurities (such as micron or nano calcium carbonate).
The polyethylene wax obtained has a number average molecular weight of 4280, a melting point of 116.50 ℃ and a molecular weight distribution index of 3.92.
Example 3
The embodiment provides a specific method for preparing polyethylene wax by continuously cracking waste polyethylene, which comprises the following steps:
in the cracking process, inert gas nitrogen is adopted to provide a protective gas environment, after purging is finished, the pretreated waste polyethylene granules are fed into a continuous cracking reactor through a feeder, the cracking reactor is formed by combining a tubular reactor and a fixed bed reactor filled with a cracking catalyst MCM-48, materials are firstly subjected to primary cracking at 350 ℃ in the tubular reactor and then are conveyed to the fixed bed reactor filled with the cracking catalyst MCM-48, the average temperature of a bed layer is 370 ℃, and the average residence time of the materials is 20min; the material at the outlet of the reactor enters a melt filter, the filtering precision is 3 microns, and a gas-phase product and a non-gas-phase product are separated and then enter a gas recovery tank; mixing the non-gas-phase product with petroleum ether according to a mass ratio of 1.
In the embodiment, the content of LDPE in the waste polyethylene granules is more than 95 wt%. Impurities are removed by washing.
The obtained polyethylene wax has the number average molecular weight of 2820, the melting point of 108.70 ℃ and the molecular weight distribution index of 3.26.
Example 4
The embodiment provides a specific method for preparing polyethylene wax by continuously cracking waste polyethylene, which comprises the following steps:
in the cracking process, inert gas nitrogen is adopted to provide a protective gas environment, pretreated waste polyethylene powder and a powdery cracking catalyst MCM-41 are uniformly mixed, the mixture is fed into a continuous cracking reactor and a reactor tubular reactor through a feeder, the mixture is subjected to primary cracking for 10min at 400 ℃, then the mixture enters a melt filter, the filtering precision is 20 microns, and a gas-phase product and a non-gas-phase product are separated and then enter a gas recovery tank; mixing the non-gas-phase product with 30wt% of hydrogen peroxide solution according to the mass ratio of 1.
In the embodiment, the content of LDPE in the waste polyethylene powder is more than 95 wt%.
The obtained oxidized polyethylene wax had a number average molecular weight of 2360, a melting point of 105.50 ℃, a molecular weight distribution index of 3.39 and an acid value of 26mgKOH/g.
Example 5
The embodiment provides a specific method for preparing polyethylene wax by continuously cracking waste polyethylene, which comprises the following steps:
firstly, purging with inert gas nitrogen to provide a protective gas environment, after purging is finished, feeding the pretreated waste polyethylene powder into a continuous cracking reactor through a feeder, wherein the reactor is a slurry bed reactor, primarily cracking for 15min at 450 ℃, then feeding the waste polyethylene powder into a ceramic membrane melt filter, the filtering precision is 0.1 micron, and separating gas-phase products from non-gas-phase products and then feeding the gas-phase products into a gas recovery tank; mixing the non-gas-phase product with an auxiliary agent maleic anhydride according to a mass ratio of 1.
In the embodiment, the HDPE content in the waste polyethylene powder is more than 90wt%.
The obtained graft-modified polyethylene wax has a number average molecular weight of 1130, a melting point of 97.20 ℃, a molecular weight distribution index of 4.71 and an acid value of 37mgKOH/g.
Example 6
The embodiment provides a specific method for preparing polyethylene wax by continuously cracking waste polyethylene, which comprises the following steps:
firstly, purging with inert gas nitrogen to provide a protective gas environment, feeding the pretreated waste polyethylene powder into a continuous cracking reactor through a feeder after purging is finished, wherein the reactor is a tubular reactor, primarily cracking at 500 ℃ for 2min, then feeding the waste polyethylene powder into a ceramic membrane melt filter, the filtering precision is 0.5 micron, and separating gas-phase products from non-gas-phase products and then feeding the gas-phase products into a gas recovery tank; mixing the non-gas-phase product and auxiliary agent hydrogen in a volume ratio of 1.
In the embodiment, the HDPE content in the waste polyethylene powder is more than 90wt%.
The polyethylene wax obtained had a number average molecular weight of 1510, a melting point of 103.40 ℃ and a molecular weight distribution index of 3.96.
The wax formation rate in examples 1 to 6 of the present application was higher than 95%.
The foregoing embodiments are merely illustrative of the principles and utilities of the present invention and are not intended to limit the invention. Those skilled in the art can modify or change the above-described embodiments without departing from the spirit and scope of the present invention. Accordingly, it is intended that all equivalent modifications or changes which may be made by those skilled in the art without departing from the spirit and scope of the present invention as defined in the appended claims.
Claims (10)
1. A method for preparing polyethylene wax by continuously cracking waste polyethylene comprises the following steps: continuously cracking waste polyethylene at 300-500 ℃ to obtain a gas-phase product and a non-gas-phase product, and separating and refining the non-gas-phase product to obtain the polyethylene wax.
2. The process of claim 1, wherein the waste polyethylene is cracked after being subjected to a pretreatment selected from one or more of washing, pelletizing, and grinding.
3. The method of claim 1, wherein the waste polyethylene is one or more selected from LLDPE, LDPE and HDPE.
4. The method as claimed in claim 1, wherein the waste polyethylene contains more than 50wt% of any one of LLDPE, LDPE and HDPE, and the waste polyethylene contains no more than 10wt% of other elements except hydrocarbon.
5. The method of claim 1, wherein the waste polyethylene is continuously and uniformly fed to the cracking process for cracking, and the cracking time of the waste polyethylene raw material in the cracking process is 1-60 minutes.
6. The method of claim 1, wherein nitrogen or an inert gas is used as a protective gas for the cracking.
7. The method of claim 1, wherein the pyrolysis temperature is 350 to 450 ℃.
8. The method of claim 1, wherein the gas phase product comprises one or more of hydrogen, methane, ethane, ethylene, propane, propylene, butane, and butene.
9. The method of claim 1, wherein the non-vapor phase product comprises a liquid phase and a solid phase, the solid phase comprising polyethylene wax and impurities.
10. The method of claim 1, further comprising a cracking catalyst selected from the group consisting of MCM-41, MCM-48, SAPO, ZSM, caCO, and mixtures thereof 3 One or more of MgO, znO and aluminosilicate.
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| CN102504330A (en) * | 2011-10-25 | 2012-06-20 | 中国科学院广州能源研究所 | Method for preparing polyolefin wax |
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| CN102504330A (en) * | 2011-10-25 | 2012-06-20 | 中国科学院广州能源研究所 | Method for preparing polyolefin wax |
| CN104861096A (en) * | 2014-02-21 | 2015-08-26 | 胡浩斌 | Method for preparing polyethylene wax by using waste polyethylene plastic |
| US20190002664A1 (en) * | 2015-12-18 | 2019-01-03 | Solvay Sa | Process for producing waxes and liquid fuels from waste plastic |
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