CN110817840B - Method for carbonizing polyolefin - Google Patents
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Abstract
The invention belongs to the technical field of waste polymer carbonization, and particularly relates to a method for carbonizing polyolefin, and more particularly relates to a method for promoting low-temperature and green carbonization of waste polyolefin by using biomass. Heating a mixture of polyolefin and biomass in an oxygen-containing atmosphere to perform carbonization reaction; wherein the polyolefin reacts with oxygen under the heating condition to form an oxygen-containing intermediate cross-linked structure, and the oxygen-containing intermediate cross-linked structure is subjected to condensation and/or polymerization reaction with an intermediate product containing hydroxyl and/or oxygen free radicals formed in the carbonization process of the biomass to form a cross-linked structure, so that the breakage of a polymer main chain is inhibited, the carbonization of the polyolefin is promoted, and an amorphous carbonization product is formed. Compared with the traditional carbonization process, the method not only greatly reduces the energy loss, but also innovatively solves the problem that the polyolefin is difficult to form carbon under the condition of no catalyst, and provides a feasible new technology for large-scale recycling of waste polyolefin in the future.
Description
Technical Field
The invention belongs to the technical field of waste polymer carbonization, and particularly relates to a method for carbonizing polyolefin, and more particularly relates to a method for promoting low-temperature and green carbonization of waste polyolefin by using biomass.
Background
In recent years, with the rapid development of petrochemical industry and polymer synthesis technology, the yield of organic polymer materials is greatly improved, and the organic polymer materials are widely applied to various industries. Plastics are widely used as main polymer materials in the fields of chemical industry, building industry, electronics, medicine and the like. According to statistics, the worldwide plastic yield is only 150 million tons in 1950, but 3.6 million tons in 2018, and the plastic yield in China is also dramatically increased from less than 1 kiloton to 8000 million tons at that time, so that the plastic yield is the first country for world plastic production and consumption.
However, the widespread use of plastic products inevitably produces a large amount of waste plastic while facilitating our lives. The plastic has good chemical stability, is difficult to degrade under natural conditions, and often needs tens of years or even hundreds of years, thereby causing serious environmental problems, such as pollution of waste agricultural mulching films. Therefore, the problems of recycling, disposal and reuse of waste plastics have been imminent. Common methods for treating waste plastics include landfill, incineration and chemical recovery. These conventional methods have certain advantages, but the disadvantages are also obvious. Although the landfill method is simple, a large amount of land is occupied, the environment is polluted, the economic investment is large, and the like. Although the incineration method can achieve the purpose of recycling the waste plastics, a large amount of harmful gas is generated in the incineration process, so that the serious pollution to the atmosphere is easily caused, and the human health is harmed. Although the chemical recovery method can play a role in recovery and simultaneously generate certain economic benefits, the obtained product has a plurality of byproducts and low added value.
Among the waste plastics, the waste polyolefins (mainly polyethylene PE and polypropylene PP) account for a considerable proportion (more than 70%). For example, the main component of the agricultural mulching film commonly used in agricultural production is PE, and in addition, the recycling value is high, the aging resistance is good, and the like, so that the recycling of polyolefin is particularly emphasized in recent years. The carbon element content in the polyolefin reaches 85.7 percent, so that the preparation of the carbon material with high added value by using the polyolefin as a carbon source is a new waste polyolefin recovery way with great potential. The subject group of the Tangtao researchers at the Changchun institute of China has proposed a "catalyst-combination" (i.e., a combination of a degradation catalyst and a carbon-forming catalyst) strategy to catalyze the carbonization of polyolefins to prepare carbon materials with high added values, including Carbon Nanotubes (CNTs) and Carbon Nanofibers (CNFs) (Synthesis of multiwalled carbon nanotubes by catalytic Synthesis of polypropylene, and chemical International Edition 2005,44, 1517-section 1520); the method has the disadvantages that a large amount of metallic nickel and organically modified montmorillonite are used as catalysts, the catalysts cannot be recycled, and the carbon material purification process is complex, so the cost is high, and the mass preparation is difficult. Pol group of university of Universal university of United states utilizes a high temperature high pressure reactor to convert waste polyolefins into solid Carbon Spheres (CSs) and CNTs (upper: Converting waste plastics into continuous, solid, pure carbon microspheres. environmental Science Technology 2010,44, 4753-4759); the method has the disadvantages of high pressure and high temperature, harsh reaction conditions and high equipment requirement. Recently, the Sungho Lee project group in Korea proposed a strategy for preheat oxygen crosslinking for Linear Low Density Polyethylene (LLDPE), which after pre-crosslinking successfully converts to highly ordered graphitic carbon at High temperatures (High performance graphical carbon from polyethylene: Thermal oxidation as a stabilization path accessed. chemistry of Materials2017,29, 9518-9527); the method has the advantages of no need of catalyst and the disadvantages of complex pretreatment means and low universality, thereby limiting the large-scale application of the method in polyolefin recovery. Therefore, a polyolefin recovery carbonization technology which is free of catalyst, low in energy consumption, green and suitable for industrialization still needs to be proposed urgently so as to have important economic and social benefits for recycling large-scale waste polyolefin.
Disclosure of Invention
In view of the above-identified deficiencies in the art or needs for improvement, the present invention provides a process for the carbonization of polyolefins, which is prepared by mixing polyolefin which is cracked under high temperature and cannot be carbonized and biomass containing oxygen-containing functional groups, heating the mixture to carbonization temperature, because the polyolefin reacts with oxygen in the heating process to form an oxygen-containing intermediate cross-linked structure, while the biomass containing oxygen-containing functional groups can generate a large amount of intermediate products containing hydroxyl and/or oxygen free radicals in the low-temperature carbonization process, the oxygen-containing intermediate cross-linked structure formed by the polyolefin and the intermediate products formed by the biomass are subjected to condensation and/or polymerization reaction to form a cross-linked structure, the fracture of a polyolefin main chain is inhibited, the carbonization of the polyolefin is promoted, and an amorphous carbonization product is formed, therefore, the technical problems of large amount of catalysts, high energy consumption, complex process and the like in the polyolefin recovery carbonization method in the prior art are solved.
To achieve the above object, according to one aspect of the present invention, there is provided a method for carbonizing a polyolefin, comprising the steps of:
(1) fully mixing polyolefin and biomass to obtain a mixture of the polyolefin and the biomass; wherein the polyolefin is a thermoplastic polyolefin capable of undergoing pyrolysis upon heating; the biomass is biomass containing oxygen-containing functional groups;
(2) heating the mixture of the polyolefin and the biomass in an oxygen-containing atmosphere to perform carbonization reaction; the polyolefin reacts with oxygen under the heating condition to form an oxygen-containing intermediate cross-linked structure, and the intermediate cross-linked structure and an intermediate product containing hydroxyl and/or oxygen free radicals formed in the carbonization process of the biomass undergo condensation and/or polymerization reaction to form a cross-linked structure, so that the fracture of a polyolefin main chain is inhibited, the carbonization of the polyolefin is promoted, and an amorphous carbonization product is formed.
Preferably, the mixing in step (1) is ball milling.
Preferably, the polyolefin is one or more of polyethylene, polypropylene, poly-1-butene, poly-1-pentene, poly-1-hexene, poly-1-octene and poly-4-methyl-1-pentene.
Preferably, the biomass is hydroxyl-containing biomass.
Preferably, the biomass is selected from one or more of sodium lignosulfonate, starch, glucose, sucrose, straw, cellulose, hemicellulose and sawdust.
Preferably, the mass ratio of the polyolefin to the biomass in the mixture in the step (1) is 1: 9-9: 1.
Preferably, the heating temperature in the step (2) is 200-550 ℃.
Preferably, the heating temperature in the step (2) is 250-450 ℃.
Preferably, the heating rate in the step (2) is 1-50 ℃/min, and the heat preservation time is 5-90 min after the temperature is raised to the carbonization reaction temperature.
Preferably, the heating rate in the step (2) is 5-20 ℃/min, and the heat preservation time is 10-30 min after the temperature is raised to the carbonization reaction temperature.
In general, compared with the prior art, the above technical solution contemplated by the present invention can achieve the following beneficial effects:
(1) the invention provides a method for carbonizing polyolefin, which comprises the following steps of mixing and heating thermoplastic polyolefin which is difficult to form carbon under pyrolysis with biomass containing oxygen-containing functional groups to a carbonization temperature, and finally carbonizing the polyolefin through an intermediate product formed in the biomass carbonization process, wherein the method comprises the following steps: the polyolefin reacts with oxygen in the heating process to form an oxygen-containing intermediate cross-linked structure, while biomass containing oxygen-containing functional groups can generate a large amount of intermediate products containing hydroxyl and/or oxygen free radicals in the low-temperature carbonization process, and the oxygen-containing cross-linked structure formed by the polyolefin and the intermediate products formed by the biomass are subjected to condensation and/or polymerization reaction to form a cross-linked structure, so that the fracture of a polyolefin main chain is inhibited, the carbonization of the polyolefin is promoted, and an amorphous carbonization product is formed. The method for carbonizing the polyolefin provided by the invention is a simple and effective carbonization method for promoting waste polyolefin to be carbonized at low temperature and in green by using biomass, and can realize efficient carbonization of the polyolefin at low temperature without a catalyst.
(2) According to the invention, the biomass material and the polyolefin are subjected to co-carbonization to obtain the carbon material with high added value. Meanwhile, the biomass is introduced, so that the catalyst-free carbonization of the polyolefin is realized, and the carbonization reaction temperature is obviously reduced. The method is green and sustainable, has simple process, provides a practical and feasible way for large-scale recovery of the waste polyolefin, and has great industrialization potential.
(3) The carbon material obtained by the method is amorphous carbon, further purification treatment is not needed, and the preparation process is greatly simplified.
Drawings
In FIG. 1, (a) is a graph showing the co-carbonization product of LLDPE and starch at 340 deg.C, (b) is a graph showing the co-carbonization product of LLDPE and sodium lignosulfonate at 340 deg.C, (c) is a graph showing the co-carbonization product of LLDPE and cellulose at 320 deg.C, (d) is a graph showing the co-carbonization product of LLDPE and sucrose at 300 deg.C, and (e) is a graph showing the co-carbonization product of LLDPE and glucose at 320 deg.C.
FIG. 2 is an X-ray diffraction pattern of the product of the co-carbonization of LLDPE with starch at 340 ℃.
FIG. 3 is a scanning electron micrograph of the product of the co-carbonization of LLDPE with starch at 340 ℃.
FIG. 4 is a comparison of the IR spectra of LLDPE, sodium lignosulfonate and the material obtained after co-carbonization of the two.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is described in further detail below with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention. In addition, the technical features involved in the embodiments of the present invention described below may be combined with each other as long as they do not conflict with each other.
The invention provides a polyolefin carbonization method, which comprises the following steps:
(1) fully mixing polyolefin and biomass to obtain a mixture of the polyolefin and the biomass; wherein the polyolefin is a thermoplastic polyolefin capable of undergoing pyrolysis upon heating; the biomass is biomass containing oxygen-containing functional groups;
(2) heating the mixture of the polyolefin and the biomass in an oxygen-containing atmosphere to perform carbonization reaction; wherein the polyolefin reacts with oxygen under the heating condition to form an oxygen-containing intermediate cross-linked structure, and the oxygen-containing intermediate cross-linked structure is subjected to condensation and/or polymerization reaction with an intermediate product containing hydroxyl and/or oxygen free radicals formed in the carbonization process of the biomass to form a cross-linked structure, so that the fracture of a polyolefin main chain is inhibited, the carbonization of the polyolefin is promoted, and an amorphous carbonization product is formed.
The polyolefin suitable for the carbonization method is thermoplastic polyolefin which is difficult to form carbon under high temperature cracking, the polyolefin can be directly degraded into micromolecular carbon-containing compounds in the high temperature cracking process and can not be crosslinked into carbon, however, the low temperature carbonization of the polyolefin can be realized by introducing oxygen-containing biomass.
The polyolefins to which the carbonization process according to the invention can be applied can in principle be any polyolefins which are not themselves crosslinked, including branched or unbranched polyolefins, such as high-density polyethylene (HDPE) which may be unbranched, linear low-density polyethylene (LDPE) which may also be branched, linear low-density polyethylene (LLDPE), etc.
In some embodiments, the polyolefin is one or more of polyethylene, polypropylene, poly-1-butene, poly-1-pentene, poly-1-hexene, poly-1-octene, and poly-4-methyl-1-pentene.
The invention utilizes the reaction of polyolefin and oxygen in the air in the temperature rising process to form an oxygen-containing intermediate crosslinking structure; in addition, a large amount of intermediate products containing hydroxyl and/or oxygen free radicals are generated in the low-temperature carbonization of the biomass, and the intermediate products can further react with the oxygen-containing cross-linked structure of the polyolefin through an acetal reaction, a free radical reaction and the like, so that the cross-linked structure is stabilized, the fracture of the polyolefin main chain is inhibited, and the further carbonization of the polyolefin is promoted. Thus, the carbonization of the polyolefin can be realized, and the carbon conversion rate of the polyolefin is improved.
To achieve adequate mixing of the polyolefin and biomass, in some embodiments, the mixing of step (1) is ball milling. The ball milling speed is 20-400 r/min, preferably 50-200 r/min, and the stirring and mixing time is 2-30 min, preferably 10-20 min.
The invention utilizes the intermediate product containing hydroxyl formed by the biomass in the process of heating and low-temperature carbonization to perform an acetal reaction, a free radical polymerization reaction and the like with the polyolefin forming an oxygen-containing cross-linked structure, so as to form a relatively stable cross-linked structure, inhibit the fracture of the polyolefin main chain and promote the carbonization. Therefore, the biomass of the present invention may be a biomass which forms an intermediate product containing hydroxyl groups during low-temperature carbonization, or may be a biomass which itself contains hydroxyl groups, and in some embodiments, the biomass of the present invention is selected from one or more of sodium lignosulfonate, starch, glucose, sucrose, straw, cellulose, hemicellulose, and sawdust.
Mixing polyolefin and biomass according to a certain mass ratio, wherein the mass ratio of the polyolefin to the biomass in the mixture in the step (1) is 1: 9-9: 1; preferably 1:5 to 5:1, and more preferably 1:2 to 2: 1.
The method adopts low-temperature carbonization, and the heating temperature in the step (2) is 200-550 ℃, preferably 250-450 ℃.
In the experimental process, it is found that when the heating rate is too fast, for example, more than 50 ℃/min, polyolefin can be directly cracked and can not react with oxygen in the air to form an oxygen-containing intermediate crosslinking structure. In some embodiments of the invention, the heating rate in the heating process is 1-50 ℃/min, preferably 5-20 ℃/min, and the heat preservation time after the temperature is raised to the carbonization reaction temperature is 5-90 min, preferably 10-30 min.
The biomass used in the invention has extremely low price and extremely rich sources, and can realize the carbonization of polyolefin at lower temperature. Compared with the traditional carbonization process, the method not only greatly reduces the energy loss, but also innovatively solves the problem that the polyolefin is difficult to form carbon under the condition of no catalyst, and provides a feasible new technology for large-scale recycling of waste polyolefin in the future.
The following are examples:
example 1
A method for carbonizing a polyolefin, comprising the steps of:
(1) 0.5g of LLDPE (produced by Michelson petrochemical company, Inc., China petrochemical group, with a molecular weight of 141000g/mol) and 1g of starch (produced by chemical reagent, Inc., China pharmaceutical group) are weighed and placed into a ball mill, and stirred and mixed for 5min at a rotating speed of 70r/min to obtain a uniform mixture of the two.
(2) The mixture was transferred to a crucible, which was placed in a muffle furnace set to a carbonization temperature of 340 ℃ at a heating rate of 5 ℃/min and held at that temperature for 30 min.
(3) And after the muffle furnace is naturally cooled, obtaining a carbonized product, weighing the mass, wherein the yield is 35 wt%.
The carbonized product was prepared as shown in the content (a) of FIG. 1. The product completely presents a carbon black color, which indicates that the mixture of LLDPE and starch is carbonized at 340 ℃, the X-ray diffraction pattern of figure 2 indicates that the carbon material has (002) crystal planes and (101) crystal planes, and the scanning electron microscope pattern of figure 3 indicates that the carbon material is an amorphous porous carbon material.
Example 2
The biomass used in example 1 was changed from starch to sodium lignosulfonate (produced by Shandong Haobo chemical Co., Ltd., molecular weight of 52000g/mol), and the other steps were not changed to obtain a co-carbonized product of LLDPE and sodium lignosulfonate with a yield of 56 wt%.
The carbonized product was prepared as shown in the content (b) of FIG. 1. The product appeared completely dark to carbon, indicating that the mixture of LLDPE and sodium lignosulfonate had carbonized at 340 ℃.
The infrared comparison spectrum of figure 4 shows that at 340 ℃, LLDPE generates a large number of oxygen-containing functional groups such as aldehyde groups when heated, sodium lignosulfonate also generates a large number of oxygen-containing functional groups such as hydroxyl groups, and after the two are co-carbonized, the obtained carbon material has a large number of C-O functional groups, which indicates that the aldehyde groups of the LLDPE and the hydroxyl groups of the sodium lignosulfonate are likely to have an acetal reaction.
Example 3
The biomass used in example 1 was changed from starch to cellulose (manufactured by Shanghai Michelin Biochemical technology Co., Ltd.) and the other steps were not changed to obtain a co-carbonized product of LLDPE and cellulose at a yield of 45 wt%.
The carbonized product was prepared as shown in the content (c) of FIG. 1. The product appeared completely black with carbon indicating that the mixture of LLDPE and cellulose had carbonized at 320 ℃.
Example 4
The biomass used in example 1 was changed from starch to sucrose (produced by national pharmaceutical group chemical Co., Ltd.) and the other steps were not changed to obtain a co-carbonized product of LLDPE and sucrose at a yield of 48 wt%.
The carbonized product was prepared as shown in the content (d) of FIG. 1. The product appeared completely dark to carbon, indicating that the mixture of LLDPE and sucrose had carbonized at 300 ℃.
Example 5
The biomass used in example 1 was changed from starch to glucose (manufactured by Sahn chemical technology Co., Ltd.) without changing the other steps, to obtain a co-carbonized product of LLDPE and glucose at a yield of 47 wt%.
The carbonized product was prepared as shown in the content (e) of FIG. 1. The product appeared completely dark with charcoal indicating that the mixture of LLDPE and glucose had carbonized at 320 ℃.
Example 6
The polyolefin used in example 1 above was changed from LLDPE to low density polyethylene (LDPE, produced by national chemical group Co., Ltd.), and the other steps were not changed to obtain a co-carbonized product of LDPE and starch at a yield of 50 wt% (the mass of the carbonized product is the percentage of the mass of the initial polyolefin and biomass mixture).
Example 7
The polyolefin used in example 1 was changed from LLDPE to PP (produced by national pharmaceutical group chemical Co., Ltd.) without changing the other steps, to obtain a co-carbonized product of PP and starch at a yield of 46 wt%.
Example 8
The amount of sodium lignosulfonate used in example 2 above was changed to 0.5g, and the other steps were unchanged to give a co-carbonized product of LLDPE and sodium lignosulfonate with a yield of 55 wt%.
Example 9
The amount of sodium lignosulfonate used in example 2 above was changed to 0.25g, and the other steps were unchanged to give a co-carbonized product of LLDPE and sodium lignosulfonate with a yield of 73 wt%.
Comparative example 1
(1) 2g of LLDPE (manufactured by Shandong Yousio chemical Co., Ltd.) was weighed into a crucible.
(2) The crucible with the sample is placed in a muffle furnace, the muffle furnace is set to raise the temperature to 340 ℃ at a rate of 5 ℃/min, and the temperature is maintained at that temperature for 30 min.
(3) And after the crucible is naturally cooled, taking out the carbonized product, and weighing the mass.
The carbonized product obtained appeared tan, indicating that the LLDPE itself could not be completely carbonized at 340 ℃.
Comparative example 2
The polyolefin used in comparative example 1 above was changed from LLDPE (linear low density polyethylene) to LDPE (low density polyethylene), and the other steps were not changed.
The resulting carbonized product appeared tan indicating that the LDPE itself could not be carbonized at 340 ℃.
Comparative example 3
The polyolefin used in comparative example 1 was changed from LLDPE to PP, and the other steps were unchanged.
The carbonized product obtained appeared tan, indicating that PP itself could not be carbonized at 340 ℃.
It will be understood by those skilled in the art that the foregoing is only a preferred embodiment of the present invention, and is not intended to limit the invention, and that any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the scope of the present invention.
Claims (9)
1. A method for carbonizing a polyolefin, comprising the steps of:
(1) fully mixing polyolefin and biomass to obtain a mixture of the polyolefin and the biomass; wherein the polyolefin is a thermoplastic polyolefin capable of undergoing pyrolysis upon heating; the biomass is biomass containing oxygen-containing functional groups;
(2) heating the mixture of the polyolefin and the biomass in an oxygen-containing atmosphere to perform carbonization reaction; the polyolefin reacts with oxygen under the heating condition to form an oxygen-containing intermediate cross-linked structure, and the intermediate cross-linked structure and an intermediate product containing hydroxyl and/or oxygen free radicals formed in the carbonization process of the biomass undergo condensation and/or polymerization reaction to form a cross-linked structure, so that the fracture of a polyolefin main chain is inhibited, the carbonization of the polyolefin is promoted, and an amorphous carbonization product is formed.
2. The carbonization method according to claim 1, wherein the mixing in step (1) is ball milling.
3. The carbonization method according to claim 1, wherein the polyolefin is one or more of polyethylene, polypropylene, poly-1-butene, poly-1-pentene, poly-1-hexene, poly-1-octene and poly-4-methyl-1-pentene.
4. The carbonization method according to claim 1, wherein the biomass is a biomass containing hydroxyl groups.
5. Carbonization process according to claim 4, characterized in that the biomass is selected from one or more of sodium lignosulfonate, starch, glucose, sucrose, straw, cellulose, hemicellulose and sawdust.
6. The carbonization method according to claim 1, wherein the mass ratio of the polyolefin to the biomass in the mixture of step (1) is 1:9 to 9: 1.
7. The carbonization method according to claim 1, wherein the heating temperature in the step (2) is 200 to 550 ℃.
8. The carbonization method according to claim 7, wherein the temperature rise rate in the heating in the step (2) is 1 to 50 ℃/min, and the holding time after the temperature rise to the carbonization reaction temperature is 5 to 90 min.
9. The carbonization method according to claim 7, wherein the temperature rise rate in the heating in the step (2) is 5 to 20 ℃/min, and the holding time after the temperature rise to the carbonization reaction temperature is 10 to 30 min.
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