CN108751278B - Method and equipment for refining phenol-containing wastewater - Google Patents
Method and equipment for refining phenol-containing wastewater Download PDFInfo
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- CN108751278B CN108751278B CN201810538438.3A CN201810538438A CN108751278B CN 108751278 B CN108751278 B CN 108751278B CN 201810538438 A CN201810538438 A CN 201810538438A CN 108751278 B CN108751278 B CN 108751278B
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Abstract
The invention belongs to the field of biomass energy conversion and utilization and environmental protection, and relates to a refining method and equipment of phenolic wastewater, which comprises the following steps: step one, crushing waste plastics by adopting a crusher, wherein 3-10kg of waste plastics is needed for treating each 1L of water phase of bio-oil or industrial wastewater; performing vacuum pyrolysis treatment in a vacuum pyrolysis reactor to obtain pyrolyzed steam; the pressure of vacuum pyrolysis is 5-15kPa, the heating rate is 10-50 ℃/min, and the heating temperature is 500-; thirdly, activating the steam by adopting a low-temperature plasma discharge reactor to obtain a high-activity substance; the discharge voltage of the low-temperature plasma discharge reactor is 15-20kV during activation, and the discharge frequency is 8-12 kHz; and step four, introducing the high-activity substances into the water phase of the biological oil or the industrial wastewater, and reacting the high-activity substances with phenols. It can use plastic waste to refine phenols in industrial waste water.
Description
Technical Field
The invention belongs to the field of biomass energy conversion and utilization and environmental protection, and relates to a refining method of industrial wastewater, in particular to a refining method of a water phase after refining and separating bio-oil, and particularly relates to a refining method and equipment of phenol-containing wastewater.
Background
Biomass energy, as the only renewable energy source directly convertible into carbon-containing liquid fuels, is becoming increasingly important today as fossil fuels become increasingly depleted and the environment becomes increasingly more severe. Biomass pyrolysis oil (hereinafter referred to as bio-oil) as a primary fuel has obvious defects in physical and chemical properties, and must be modified and refined to improve the quality of the bio-oil. At present, the refining and modification methods mainly comprise catalytic cracking, catalytic hydrogenation, catalytic esterification and other methods, wherein the catalytic cracking refining method has high safety and relatively mild reaction conditions, and is widely concerned by scholars at home and abroad. After the primary bio-oil is subjected to catalytic cracking and upgrading by a molecular sieve, the obtained liquid-phase product can be obviously layered, the upper layer is an oil-phase product mainly comprising hydrocarbon substances, the lower layer is a water phase, and the water phase contains more kinds of organic matters. Most of organic matters in the oil-phase product and the water-phase product can be extracted and separated through extraction separation, and the separated organic matters can be directly or indirectly used as fuel.
However, after extraction and separation, the water phase still contains residual organic matters mainly comprising phenols, and phenolic compounds belong to organic pollutants with high toxicity (carcinogenicity), but the phenols contain a large amount of hydroxyl groups which have strong hydrophilicity, so that the phenols in the water phase are difficult to be effectively separated.
However, in industrial production, phenols exist not only in the water phase of bio-oil, but also in industrial wastewater generated in the industries of petrifaction, printing and dyeing, pesticides and the like, and surface water is extremely easy to be polluted because effective phenols cannot be obtained from phenols in the industrial wastewater.
In the prior art, few researches on conversion and utilization of phenols in a water phase of biological oil are focused, and a small amount of researches are mostly focused on: firstly, water phase esterification separation, for example, an ultrasonic-assisted esterification coupling extraction method for recovering organic acid in a biological oil hydrogenation water phase disclosed in Chinese patent CN104628558A, is characterized by comprising the following specific steps: taking a mixture of an organic solvent and a biological oil hydrogenation water phase in a mass ratio of 1: 2-4: 1, heating the mixture to 60 ℃, adding absolute ethanol in a molar ratio of 1: 1-1: 3 to organic acid, adding an inorganic acid catalyst or a solid acid esterification reaction catalyst in a molar ratio of 10% of organic acid, and uniformly mixing; under the ultrasonic wave condition with the ultrasonic frequency of 40kHz, keeping the temperature of 60 ℃ for reacting for 2-3 h until the reaction is finished; separating to obtain an organic layer after reaction, and separating and recovering the ester substances from the organic layer by a rectification method. Secondly, chemical extraction and the like, for example, Chinese patent CN102976906B discloses a method for separating phenols from bio-oil, which relates to a method for separating phenols from biomass pyrolysis oil. The method comprises the following steps: distilling bio-oil, intercepting fractions below 160 ℃, adding an alkali solution to alkalize until the pH value is more than 10; extracting the alkalized solution with extractant, acidifying the water phase left after extraction with acid, adding salt solution, re-extracting with back extractant, and removing organic phase by reduced pressure distillation to obtain phenol mixture. The treatment of phenol-containing waste water by using low-temperature plasma technology has been reported and researched at present, but the prior technical method mainly uses the low-temperature plasma technology to generate active substances with strong oxidizing property, and directly introduces the waste water or uses an aeration mode to forcedly oxidize and decompose phenol substances.
Meanwhile, the industrial treatment method of the wastewater containing phenols is generally divided into three major types, namely a physical chemical method, a chemical method and a biochemical method, wherein the physical chemical method mainly removes the phenols by means of adsorption, extraction, electroosmosis, ultrafiltration and the like, and the chemical method mainly removes the phenols directly by means of precipitation, neutralization, oxidation, electrolysis, photocatalysis and the like. These methods basically involve the use of chemical materials such as oxygen, solvents or catalysts, and have problems in reprocessing these materials, with a high risk of secondary contamination during reprocessing. Therefore, there is a need to develop a new method that avoids the use of oxygen, solvents and catalysts.
Disclosure of Invention
The invention provides a method and equipment for refining phenolic wastewater, which can refine phenolic substances in industrial wastewater by utilizing plastic wastes.
In order to achieve the technical purpose, the invention adopts the technical scheme that the method for refining the phenol-containing wastewater comprises the following steps:
step one, crushing waste plastics by adopting a crusher, wherein 3-10kg of waste plastics is needed for treating each 1L of water phase of bio-oil or industrial wastewater;
performing vacuum pyrolysis treatment in a vacuum pyrolysis reactor to obtain pyrolyzed steam; the pressure of vacuum pyrolysis is 5-15kPa, the heating rate is 10-50 ℃/min, and the heating temperature is 500-;
thirdly, activating the steam by adopting a low-temperature plasma discharge reactor to obtain a high-activity substance; the discharge voltage of the low-temperature plasma discharge reactor is 15-20kV during activation, and the discharge frequency is 8-12 kHz;
and step four, introducing the high-activity substances into the water phase of the biological oil or the industrial wastewater, and reacting the high-activity substances with phenols.
As an improved technical scheme of the invention, the waste plastic is made of polyethylene or polypropylene.
As an improved technical scheme of the invention, the particle size of the crushed waste plastic is 0.1-0.3 mm.
Another object of the present invention is to provide an apparatus for the refining method of the present application, comprising a pulverizer for pulverizing waste plastics, a vacuum pyrolysis reactor, a vacuum pump, a low-temperature plasma discharge reactor, and a wastewater treatment tank;
the inlet of the vacuum pyrolysis reactor is communicated with the outlet of the pulverizer; the outlet of the vacuum pyrolysis reactor is communicated with the inlet of a vacuum pump, the outlet of the vacuum pump is communicated with the inlet of the low-temperature plasma discharge reactor, and the outlet of the low-temperature plasma discharge reactor is communicated with the inlet of the wastewater treatment box.
As the improved technical scheme of the application, the vacuum pump is a jet type vacuum pump.
As the improved technical scheme of the application, the vacuum pump is a mechanical vacuum pump.
As an improved technical scheme of the application, the low-temperature plasma discharge reactor adopts dielectric barrier discharge.
Advantageous effects
The method adopts waste plastic pyrolysis gas activated by low-temperature plasma discharge to realize conversion and utilization of phenolic substances. The method does not use any solvent and catalyst, realizes the synchronous conversion and utilization of waste plastics and phenols, separates the converted floating oil layer, and can be added into the refined bio-oil phase to be used as fuel, thereby further increasing the yield of hydrocarbon substances; the unreacted gaseous product is still rich in C2H4Or C3H6It can also be used as gas fuel or chemical raw material.
In summary, the present application has the following advantages: 1. the use of chemical reagents is avoided, namely, no solvent consumption, no loss and no secondary pollution exist; 2. the catalyst is avoided, namely, the problems of catalyst consumption, inactivation loss, regeneration and the like do not exist; 3. the recycling way of the waste plastics is widened, and the joint conversion of solid waste and liquid waste is realized; 4. the conversion of phenolic substances is close to 100%.
Drawings
FIG. 1 is a schematic flow diagram of a refining process of the present application;
FIG. 2 is a schematic view of the structure of an apparatus for refining of the present application;
in the figure: 1. a pulverizer; 2. a vacuum pyrolysis reactor; 3. a low temperature plasma discharge reactor; 4. a wastewater treatment tank.
Detailed Description
In order to make the purpose and technical solution of the embodiments of the present invention clearer, the technical solution of the embodiments of the present invention will be clearly and completely described below with reference to the drawings of the embodiments of the present invention. It is to be understood that the embodiments described are only a few embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the described embodiments of the invention without any inventive step, are within the scope of protection of the invention.
It will be understood by those skilled in the art that, unless otherwise defined, all terms (including technical and scientific terms) used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. It will be further understood that terms, such as those defined in commonly used dictionaries, should be interpreted as having a meaning that is consistent with their meaning in the context of the prior art and will not be interpreted in an idealized or overly formal sense unless expressly so defined herein.
The term "connected" as used herein may mean either a direct connection between the components or an indirect connection between the components via other components.
A method for refining water phase of biological oil and phenolic wastewater is characterized by comprising the following steps:
s1: crushing waste plastics made of polyethylene or polypropylene, wherein the crushed waste plastics have a particle size of 0.1-0.3mm, preferably 0.2 mm; the crushed waste plastics are filled into a vacuum pyrolysis reactor,
the ratio of the amount of the charged waste water to the waste water to be treated is about (3 to 10) kg of waste plastic to 1L of waste water to be treated, and it is preferable to use 3kg of waste plastic per 1L of aqueous phase of industrial waste water or bio-oil to be treated.
S2: the pressure in the vacuum pyrolysis reactor is kept at 5-15kPa by utilizing the suction of a vacuum pump, and then the temperature is raised to 500-600 ℃ at the temperature rise rate of 10-50 ℃/min, and the waste plastic heat is generatedThe waste plastics are made of polyethylene or polypropylene, so the steam formed after pyrolysis mainly comprises ethylene (C)2H4) Or propylene (C)3H6). In this embodiment, 10kPa is selected as the pressure, 30 ℃/min is selected as the temperature rise rate, and 550 ℃ is selected as the temperature.
S3: the pyrolysis gas passes through a low-temperature plasma discharge reactor (in the embodiment, a dielectric barrier discharge type low-temperature plasma discharge reactor is adopted) under the suction of a vacuum pump, and the reaction conditions are as follows: the discharge voltage is 15-20kV, the discharge frequency is 8-12kHz, the pyrolysis gas is activated and dissociated to generate high-activity substances, and the high-activity substances are mainly [ CH ]3]、[CH2]、[CH]、[H]And the like.
S4: and (3) introducing pyrolysis gas rich in high-activity substances into the water phase or wastewater of the biological oil, wherein the high-activity substances and phenols are subjected to contact reaction, hydroxyl is removed in the form of water, and meanwhile, a product mainly containing hydrocarbons is generated, a surface oil-bearing layer appears, and the conversion reaction is finished when the oil-bearing layer is not increased any more. Because the activated waste water is directly introduced into the waste water treatment tank, the treatment time is shortened, the activity of high-activity substances is kept, and the whole device can be in a closed state.
The reaction principle of the reaction of the high-activity substances and phenols is as follows:
in the formula: r, R1、R2And R3Each represents a different branched group, predominantly a hydrocarbon group; the product is not limited to the examples in formula; and one product may be formed from the reaction of phenols with one or more types of particle fragments.
The phenols in this application are all phenols with one or more hydroxyl groups on the benzene ring.
In the above method, the vacuum pump may be a jet vacuum pump or a mechanical vacuum pump.
In order to realize the above refining method, any existing apparatus and equipment for realizing the method can be adopted, and the present embodiment is preferably equipment for the refining method, comprising a crusher 1 for crushing waste plastics, a vacuum pyrolysis reactor 2, a vacuum pump 3, a low-temperature plasma discharge reactor 4 and a wastewater treatment tank 5; the pulverizer, the vacuum pyrolysis reactor, the vacuum pump, the low-temperature plasma discharge reactor and the wastewater treatment tank are sequentially communicated in a closed manner.
The inlet of the vacuum pyrolysis reactor is communicated with the outlet of the pulverizer; the outlet of the vacuum pyrolysis reactor is communicated with the inlet of a vacuum pump, the outlet of the vacuum pump is communicated with the inlet of the low-temperature plasma discharge reactor, and the outlet of the low-temperature plasma discharge reactor is communicated with the inlet of the wastewater treatment box.
As the improved technical scheme of the application, the vacuum pump is a jet type vacuum pump.
As the improved technical scheme of the application, the vacuum pump is a mechanical vacuum pump.
As an improved technical scheme of the application, the low-temperature plasma discharge reactor adopts dielectric barrier discharge.
The concrete application is as follows:
example 1
Crushing 300g of Polyethylene (PE) waste plastics to 0.1mm, filling the crushed plastic into a vacuum pyrolysis reactor, pumping by using a vacuum pump to keep the pressure in the vacuum pyrolysis reactor at 5kPa, starting to heat the waste plastics at the heating rate of 10 ℃/min, keeping the final temperature at 500 ℃, pyrolyzing the waste plastics to form steam, passing pyrolysis gas through a dielectric barrier discharge type low-temperature plasma discharge reactor under the suction of the vacuum pump, discharging the pyrolysis gas by using the low-temperature plasma discharge reactor at the high voltage of 15kV and the high frequency of 8kHz, activating and dissociating part of ethylene molecules in the pyrolysis gas to generate CH3、CH2And high-activity particle fragments such as CH and H, then introducing pyrolysis gas rich in high-activity substances into 100mL of water phase refined from the bio-oil, carrying out contact reaction with phenolic substances, removing hydroxyl groups of the pyrolysis gas, generating a small amount of surface oil-bearing layer at the same time, and stopping discharging when the oil-bearing layer is not increased any more, namely the conversion reaction is finished. When the gas collected at last is not increased any more, the whole reaction is completed, the vacuum pump is closed, the pyrolysis is stopped, and the whole system is recovered to normal temperatureSeparating floating oil layer and gas product at normal pressure.
The gaseous products were analyzed for organics using an Agilent model 7890A Gas Chromatograph (GC): it was found that C was contained in the obtained gas2H456% of CH412% of CO, 13% of CO215% of the total weight of the composition, and a small amount of H2、C2H6、H2O, etc., and the total content is 4 percent.
The types of organic substances before and after aqueous phase purification were analyzed by an Agilent 7890A/5975 gas chromatography/mass spectrometry (GC/MS) analyzer, and the results of the detection and analysis are shown in Table 1. The main organic compounds detected before and after the refining are listed in table 1, and 7 main substances detected in the water phase obtained after the bio-oil refining and separation are phenolic organic substances. After the refining conversion of the method, 9 organic compounds are detected in the surface oil slick layer, and 8 organic compounds are hydrocarbon substances. In the reacted water, 2 kinds of alcohol compounds which are less harmful to the environment and are easier to handle are detected. Experiments show that the conversion rate of phenolic substances in a water phase after refining and separating bio-oil is higher and is 100 percent; the converted product (floating oil layer) can be directly or indirectly used as fuel, and the yield of hydrocarbon oil phase products prepared from biomass is further increased; meanwhile, a small amount of organic matters remained in water are less harmful and easy to treat.
TABLE 1 types of organic substances before and after aqueous phase purification
Example 2
Pulverizing 1000g polypropylene (PP) waste plastic to 0.1mm, filling into a vacuum pyrolysis reactor, pumping with a vacuum pump to maintain the pressure in the vacuum pyrolysis reactor at 15kPa, heating the waste plastic at a temperature rise rate of 50 ℃/min to a final temperature of 600 ℃, pyrolyzing the waste plastic to form vapor, passing pyrolysis gas through a dielectric barrier discharge type low-temperature reactor under the suction of the vacuum pumpThe low-temperature plasma discharge reactor discharges pyrolysis gas at 20kV high voltage and 12kHz high frequency, partial ethylene molecules in the pyrolysis gas are activated and dissociated to generate CH3、CH2And high-activity particle fragments such as CH and H, and then introducing pyrolysis gas rich in high-energy active substances into 300mL of water phase refined from the bio-oil, carrying out contact reaction with phenolic substances, removing hydroxyl groups of the phenolic substances, generating a small amount of surface oil-bearing layer at the same time, and stopping discharging when the oil-bearing layer is not increased any more, namely the conversion reaction is finished. And when the finally collected gas is not increased any more, finishing all reactions, closing the vacuum pump, stopping pyrolysis, and separating the floating oil layer and the gas product when the whole system is recovered to normal temperature and normal pressure.
The gaseous products were analyzed for organics using an Agilent model 7890A Gas Chromatograph (GC): it was found that C was contained in the obtained gas3H658% by weight, C2H48% of CH47% of CO, 9% of CO213% by weight, and small amount of H2、C2H6、C3H8、H2O, etc., accounting for 5 percent of the total.
The types of organic substances before and after aqueous phase purification were analyzed by an Agilent 7890A/5975 gas chromatography/mass spectrometry (GC/MS) analyzer, and the results of the detection and analysis are shown in Table 2. The main organic compounds detected before and after the refining, 10 main compounds detected in the water phase obtained after the bio-oil refining and separation, 8 of which are phenolic organic compounds, are listed in table 2. After the refining conversion of the method, 11 organic compounds are detected in the surface oil slick layer, and 9 of the organic compounds are hydrocarbon substances. In the reacted water, 3 kinds of alcohol compounds which are less harmful to the environment and are easier to handle are detected. Experiments show that the conversion rate of phenolic substances in a water phase after refining and separating bio-oil is higher and is 100 percent; the converted product (floating oil layer) can be directly or indirectly used as fuel, and the yield of hydrocarbon oil phase products prepared from biomass is further increased; meanwhile, a small amount of organic matters remained in water are less harmful and easy to treat.
TABLE 2 types of organic substances before and after aqueous phase purification
Example 3
Adding a phenol reagent into pure water to prepare a phenol-containing aqueous solution with moderate concentration as a treatment object of an experiment.
Crushing 300g of Polyethylene (PE) and 300g of polypropylene (PP) waste plastic into 0.1mm, mixing, filling the mixture into a vacuum pyrolysis reactor, pumping by using a vacuum pump to keep the pressure in the vacuum pyrolysis reactor at 10kPa, starting to heat the waste plastic at the temperature rise rate of 30 ℃/min, keeping the final temperature at 550 ℃, pyrolyzing the waste plastic to form steam, passing pyrolysis gas through a dielectric barrier discharge type low-temperature plasma discharge reactor under the suction of the vacuum pump, discharging the pyrolysis gas by using the low-temperature plasma discharge reactor at the high voltage of 18kV and the high frequency of 10kHz, activating and dissociating part of ethylene and propylene molecules in the pyrolysis gas to generate CH3、CH2And (3) introducing pyrolysis gas rich in high-activity substances into 200mL of phenol-containing aqueous solution, carrying out contact reaction with the phenol substances to remove hydroxyl groups of the phenol-containing aqueous solution, generating a small amount of surface oil-bearing layer at the same time, and stopping discharging when the oil-bearing layer is not increased any more, namely the conversion reaction is finished. And when the finally collected gas is not increased any more, finishing all reactions, closing the vacuum pump, stopping pyrolysis, and separating the floating oil layer and the gas product when the whole system is recovered to normal temperature and normal pressure.
The gaseous products were analyzed for organics using an Agilent model 7890A Gas Chromatograph (GC): it was found that C was contained in the obtained gas3H631% of C2H428% of CH410% of CO, 7% of CO and216% by weight, and small amount of H2、C2H6、C3H8、H2O, etc. accounting for 8 percent of the total weight.
Organic species before and after the reaction of the phenol-containing aqueous solution were analyzed by an Agilent 7890A/5975 gas chromatography/mass spectrometry (GC/MS) analyzer, and the detection analysis results are shown in table 3. Experiments show that phenol in the aqueous solution can be completely converted into various hydrocarbon compounds and separated from the aqueous solution, and meanwhile, few alcohol substances remain in the water.
TABLE 3 types of organic substances before and after reaction of phenol-containing aqueous solution
In conclusion, the scheme of the embodiment overcomes the defects in the conversion and utilization of the water phase of the existing bio-oil and the phenol-containing industrial wastewater, and further widens the recycling and reusing way of the waste plastics.
The technical scheme of the application can synchronously convert the waste plastics of polyethylene and polypropylene materials and phenolic wastewater to prepare available fuels or chemicals, and has important significance for realizing sustainable development of energy and environment.
The above are merely embodiments of the present invention, which are described in detail and with particularity, and therefore should not be construed as limiting the scope of the invention. It should be noted that, for those skilled in the art, various changes and modifications can be made without departing from the spirit of the present invention, and these changes and modifications are within the scope of the present invention.
Claims (7)
1. A refining method of phenol-containing wastewater is characterized by comprising the following steps:
step one, crushing waste plastics by adopting a crusher, wherein 3-10kg of waste plastics is needed for treating each 1L of water phase of bio-oil or industrial wastewater;
performing vacuum pyrolysis treatment in a vacuum pyrolysis reactor to obtain pyrolyzed steam; the pressure of vacuum pyrolysis is 5-15kPa, the heating rate is 10-50 ℃/min, and the heating temperature is 500-;
thirdly, activating the steam by adopting a low-temperature plasma discharge reactor to obtain a high-activity substance; the discharge voltage of the low-temperature plasma discharge reactor is 15-20kV during activation, and the discharge frequency is 8-12 kHz;
and step four, introducing the high-activity substances into the water phase of the biological oil or the industrial wastewater, and reacting the high-activity substances with phenols.
2. The method of claim 1, wherein the waste plastics is polyethylene or polypropylene.
3. The method of claim 1, wherein the pulverized waste plastic has a particle size of 0.1 to 0.3 mm.
4. An apparatus for a refining method of phenol-containing wastewater according to any one of claims 1 to 3, comprising a pulverizer for pulverizing waste plastics, a vacuum pyrolysis reactor, a vacuum pump, a low-temperature plasma discharge reactor, and a wastewater treatment tank;
the inlet of the vacuum pyrolysis reactor is communicated with the outlet of the pulverizer; the outlet of the vacuum pyrolysis reactor is communicated with the inlet of a vacuum pump, the outlet of the vacuum pump is communicated with the inlet of the low-temperature plasma discharge reactor, and the outlet of the low-temperature plasma discharge reactor is communicated with the inlet of the wastewater treatment box.
5. The apparatus for the purification process of phenol-containing wastewater according to claim 4, wherein the vacuum pump is a jet vacuum pump.
6. The apparatus for a method of purifying phenol-containing wastewater according to claim 4, wherein the vacuum pump is a mechanical vacuum pump.
7. The apparatus for a refining process of phenol-containing wastewater according to claim 4, wherein the low-temperature plasma discharge reactor employs dielectric barrier discharge.
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