CN113528185A - Method for extracting paraffin from wax residue - Google Patents
Method for extracting paraffin from wax residue Download PDFInfo
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- CN113528185A CN113528185A CN202110874901.3A CN202110874901A CN113528185A CN 113528185 A CN113528185 A CN 113528185A CN 202110874901 A CN202110874901 A CN 202110874901A CN 113528185 A CN113528185 A CN 113528185A
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- 239000001993 wax Substances 0.000 title claims abstract description 110
- 239000012188 paraffin wax Substances 0.000 title claims abstract description 67
- 238000000034 method Methods 0.000 title claims abstract description 44
- 239000011259 mixed solution Substances 0.000 claims abstract description 44
- 239000003960 organic solvent Substances 0.000 claims abstract description 21
- 238000001035 drying Methods 0.000 claims abstract description 20
- 238000010438 heat treatment Methods 0.000 claims abstract description 20
- 239000007788 liquid Substances 0.000 claims abstract description 11
- 238000002156 mixing Methods 0.000 claims abstract description 8
- 238000004090 dissolution Methods 0.000 claims abstract description 3
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 40
- 239000003208 petroleum Substances 0.000 claims description 20
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 claims description 16
- 238000007873 sieving Methods 0.000 claims description 5
- 241000779819 Syncarpia glomulifera Species 0.000 claims description 2
- 239000001739 pinus spp. Substances 0.000 claims description 2
- 239000003495 polar organic solvent Substances 0.000 claims description 2
- 229940036248 turpentine Drugs 0.000 claims description 2
- 238000011084 recovery Methods 0.000 abstract description 17
- 238000004821 distillation Methods 0.000 abstract description 8
- 238000000605 extraction Methods 0.000 abstract description 7
- 238000000926 separation method Methods 0.000 abstract description 4
- 238000001914 filtration Methods 0.000 abstract description 3
- 238000002386 leaching Methods 0.000 abstract description 3
- 125000004122 cyclic group Chemical group 0.000 abstract 1
- 230000015572 biosynthetic process Effects 0.000 description 19
- 239000002893 slag Substances 0.000 description 19
- 238000003786 synthesis reaction Methods 0.000 description 19
- 239000007787 solid Substances 0.000 description 13
- 238000005303 weighing Methods 0.000 description 10
- 239000002699 waste material Substances 0.000 description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 5
- 239000003054 catalyst Substances 0.000 description 4
- 239000002994 raw material Substances 0.000 description 4
- 238000004846 x-ray emission Methods 0.000 description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 3
- 229910052799 carbon Inorganic materials 0.000 description 3
- -1 ester compounds Chemical class 0.000 description 3
- 229930195733 hydrocarbon Natural products 0.000 description 3
- 150000002430 hydrocarbons Chemical class 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 239000003245 coal Substances 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 239000002537 cosmetic Substances 0.000 description 2
- 239000002283 diesel fuel Substances 0.000 description 2
- 238000005265 energy consumption Methods 0.000 description 2
- 235000013305 food Nutrition 0.000 description 2
- 239000000314 lubricant Substances 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 239000005022 packaging material Substances 0.000 description 2
- 238000004513 sizing Methods 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 239000002023 wood Substances 0.000 description 2
- 239000004215 Carbon black (E152) Substances 0.000 description 1
- 150000001298 alcohols Chemical class 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000002149 energy-dispersive X-ray emission spectroscopy Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 239000000295 fuel oil Substances 0.000 description 1
- 238000002290 gas chromatography-mass spectrometry Methods 0.000 description 1
- 238000002309 gasification Methods 0.000 description 1
- 229910001385 heavy metal Inorganic materials 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
- 238000012797 qualification Methods 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 238000012216 screening Methods 0.000 description 1
- 239000013049 sediment Substances 0.000 description 1
- 238000007711 solidification Methods 0.000 description 1
- 230000008023 solidification Effects 0.000 description 1
- 230000002269 spontaneous effect Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
- C10G73/00—Recovery or refining of mineral waxes, e.g. montan wax
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
- C10G73/00—Recovery or refining of mineral waxes, e.g. montan wax
- C10G73/42—Refining of petroleum waxes
Landscapes
- Chemical & Material Sciences (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Fats And Perfumes (AREA)
Abstract
The invention relates to a method for extracting paraffin from wax residue, which comprises the following specific steps: wrapping the pretreated wax residue with filter paper to form a wax residue bag; mixing the wax residue bag with an organic solvent to form a mixed liquid bag; carrying out ultrasonic heating dissolution on paraffin in the mixed liquid bag to obtain a mixed solution of the paraffin and an organic solvent; and distilling the mixed solution, and drying the residual mixed solution to obtain the paraffin. The invention adopts a mode of wrapping filter paper with filter residue, avoids filter residue leakage in the extraction process, and can effectively solve the problems of difficult solid-liquid separation and high-temperature filtration in the common leaching method. In addition, the method adopts ultrasonic assisted wax residue extraction, reduces the time required by extraction and the amount of added organic solvent, enables the paraffin to be dissolved in the organic solvent as much as possible, and further improves the recovery rate and quality of the paraffin. The invention recycles the organic solvent through distillation, realizes the repeated cyclic utilization of the organic solvent and provides a resource utilization method for wax residue treatment.
Description
Technical Field
The invention belongs to the technical field of Fischer-Tropsch synthesis wax residue treatment, and particularly relates to a method for extracting paraffin from wax residue.
Background
Fischer-Tropsch synthesis technology (Fischer-Tropsch synthesis) is a main reaction process for preparing oil from coal, wherein synthesis gas produced by coal gasification efficiently synthesizes liquid fuels such as light hydrocarbon, heavy oil, heavy wax and the like and other chemical products under Fischer-Tropsch catalyst and proper reaction conditions. After Fischer-Tropsch synthesis, the catalyst is usually discharged out of a Fischer-Tropsch synthesis device in the form of wax residue, and because the wax residue contains 20-75% of wax, most of liquid wax is filtered and recycled by a wax discharge system in a Fischer-Tropsch reactor to obtain filtered wax residue, and the filtered wax residue still contains 40-60% of wax and a large amount of waste catalyst. Due to the characteristics of easy spontaneous combustion of the wax residue, high content of heavy metals in the waste catalyst and the like, the filtered wax residue is listed in the name list of dangerous wastes, belongs to the dangerous wastes and needs to be disposed by a unit with the treatment qualification of the dangerous wastes. At present, the common disposal methods for wax slag in China are incineration, solidification and landfill, and the like, so that the disposal cost is high, economic burden is brought to enterprises, and serious resource waste is caused. Therefore, the method for extracting the paraffin based on the Fischer-Tropsch synthesis wax residue has urgent demand.
CN105542855A discloses a method and a system for treating wax residue, the method comprises: the wax residue is separated after being melted at high temperature to obtain molten wax and solid residue, and the solid residue is distilled to recover the residual wax and then is incinerated. However, this method does not disclose a method of separation after melting at high temperature, and the difficulty of evaporating the residual wax by distillation is high and the recovery rate is not high. The process does not address the quality of the recovered finished wax.
CN213172211U discloses a processing system of ft sediment wax, and the method includes: the wax residue is treated at high temperature to reach a molten state, then repeatedly extracted by a solvent and filtered, the product wax is recovered by distillation, and finally the solid residue is incinerated. However, the method firstly needs to convert the solid wax residue into a molten state at high temperature, so that the energy consumption is high and the economical efficiency is poor. And the process does not detail the recovery rate and the quality of the product wax recovery.
Disclosure of Invention
The invention aims to provide a method for extracting paraffin from wax residue, which directly utilizes a solvent for extraction without converting solid wax residue into a molten state at high temperature, has simple operation and low investment cost, does not bring economic burden to enterprises, has high recovery rate and high quality of paraffin, and can be used as a paraffin raw material.
The technical scheme of the invention is as follows: a method for extracting paraffin from wax residue comprises the following specific steps:
A. wrapping the pretreated wax residue with filter paper to form a wax residue bag;
B. mixing the wax residue bag with an organic solvent to form a mixed liquid bag;
C. carrying out ultrasonic heating dissolution on paraffin in the mixed liquid bag to obtain a mixed solution of the paraffin and an organic solvent;
D. and distilling the mixed solution, and drying the residual mixed solution to obtain the paraffin.
Preferably, the pretreatment is to crush the wax residue and screen the crushed wax residue through a screen.
Preferably, the mesh number of the screen is 90-150 meshes.
Preferably, the wax residue is Fischer-Tropsch synthesis wax residue.
Preferably, the organic solvent is a non-polar organic solvent. More preferably, the organic solvent is at least one of petroleum ether, n-hexane, naphtha or turpentine.
Preferably, the volume ratio of the mass of the wax residue to the organic solvent is 30-50 g/L.
Preferably, the ultrasonic heating temperature is 70-90 ℃, and the time is 3-4 h; the ultrasonic power is 20-30 KHz.
Preferably, the drying temperature is 40-60 ℃, and the drying time is 8-12 h.
According to the invention, the filter paper is adopted to wrap the filter residue, so that the wax residue leakage in the extraction process is avoided, the problems of difficult solid-liquid separation and high-temperature filtration in a common leaching method can be effectively solved, and the recovery rate and quality of paraffin are further improved. In addition, the method adopts ultrasonic-assisted wax residue extraction, reduces the time required by extraction and the amount of added organic solvent, and enables the paraffin to be dissolved in the organic solvent as much as possible, so that the paraffin has high recovery rate and high quality. The recovery rate of the paraffin in the wax residue by the method provided by the invention is up to 98%. Moreover, the paraffin recovered by the process of the present application is of high quality.
In addition, the organic solvent in the method can be repeatedly recycled, the requirement of clean production is met, and the equipment investment is low.
Further, the solid residue in the filter paper bag can be continuously recycled after high-temperature roasting, and the solid residue in the filter paper bag obtained in the step D can be placed in a muffle furnace to be heated to 400-600 ℃ at a speed of 5-10 ℃/min and kept for 2-4 h.
Has the advantages that:
(1) the method has the advantages that the recovery rate of the paraffin in the paraffin residue reaches more than 98 percent, and the obtained paraffin has better quality.
(2) The organic solvent in the method can be repeatedly recycled, the requirement of clean production is met, and the equipment investment is low.
(3) According to the method, the wax residue is wrapped by the filter paper, so that the problems of difficult solid-liquid separation and high-temperature filtration in the common leaching method can be effectively solved.
(4) The solid residue in the method can be continuously recycled after high-temperature roasting.
Drawings
FIG. 1 is a flow chart of a method for extracting paraffin from wax residue.
Detailed Description
In order to further illustrate the present invention, the method for extracting paraffin from wax residue provided by the present invention is described in detail with reference to fig. 1 and examples, but they should not be construed as limiting the scope of the present invention.
The present invention adopts a gravimetric method to determine the recovery rate of paraffin. See formula (1) for a specific calculation.
Wherein, W1 and W2 respectively represent the mass (g) of the wax slag ladle before and after treatment, W represents the mass (g) of the wax slag, and a represents the mass percentage content of the carbon-containing compound in the wax slag obtained by XRF analysis.
The present invention utilizes X-ray fluorescence spectroscopy (XRF, Eagle III, EDAX inc., usa) to analyze the composition of fischer-tropsch wax residues, as shown in table 1.
TABLE 1 Fischer-Tropsch wax residue composition Table
Example 1
Crushing Fischer-Tropsch synthesis wax residue (weighed and recorded as W) by using a crusher, and then sieving the crushed Fischer-Tropsch synthesis wax residue by using a 90-mesh sieve; wrapping 2g of wax slag by using filter paper to obtain a wax slag bag, and weighing the wax slag bag as W1; mixing the wax residue bag with 60ml of petroleum ether to obtain a mixed solution, wherein the mass ratio of the wax residue to the petroleum ether is 1: 30; placing the mixed solution in an ultrasonic heating device, heating the mixed solution to 90 ℃ in an ultrasonic water bath, keeping the ultrasonic power at 20KHz, preserving the heat for 4 hours to gradually dissolve the paraffin in the petroleum ether, and taking out a paraffin residue bag when the mixed solution is hot to obtain the mixed solution of the paraffin and the petroleum ether; transferring the mixed solution of paraffin and petroleum ether to a rotary evaporator for distillation, recovering the petroleum ether, and drying the rest mixed solution in a drying oven at 60 ℃ for 11h to obtain paraffin; putting the taken wax residue bag in an oven for drying for 12h at the temperature of 60 ℃, weighing and marking as W2; putting the dried solid residue in the filter paper bag into a muffle furnace, heating to 400 ℃ at a speed of 5 ℃/min, and keeping for 2 hours; the mass percent of carbon-containing compounds in the wax residue before treatment was analyzed by XRF and the paraffin recovery was calculated to be 95.04% using equation (1).
Example 2
Crushing Fischer-Tropsch synthesis wax residue (weighed and recorded as W) by using a crusher, and sieving the crushed Fischer-Tropsch synthesis wax residue by using a 120-mesh sieve; wrapping 2g of wax slag by using filter paper to obtain a wax slag bag, and weighing the wax slag bag as W1; mixing the wax residue bag with 60ml of petroleum ether to obtain a mixed solution, wherein the mass ratio of the wax residue to the petroleum ether is 1: 30; placing the mixed solution in an ultrasonic heating device, heating the mixed solution to 90 ℃ in an ultrasonic water bath, keeping the ultrasonic power at 30KHz, preserving the heat for 4 hours to gradually dissolve the paraffin in the petroleum ether, and taking out a paraffin residue bag when the mixed solution is hot to obtain the mixed solution of the paraffin and the petroleum ether; transferring the mixed solution of paraffin and petroleum ether to a rotary evaporator for distillation, recovering the petroleum ether, and drying the rest mixed solution in an oven at 50 ℃ for 12h to obtain paraffin; putting the taken wax residue bag in an oven for drying for 12h at the temperature of 60 ℃, weighing and marking as W2; and (3) putting the dried solid residue in the filter paper bag into a muffle furnace, heating to 550 ℃ at a speed of 10 ℃/min, and keeping for 4 h. The recovery of paraffin in this example was 98.93% by weight.
Example 3
Crushing Fischer-Tropsch synthesis wax residue (weighed and recorded as W) by using a crusher, and screening by using a 150-mesh screen; wrapping 2g of wax slag by using filter paper to obtain a wax slag bag, and weighing the wax slag bag as W1; mixing the wax residue bag with 40ml of petroleum ether to obtain a mixed solution, wherein the mass ratio of the wax residue to the petroleum ether is 1: 20; placing the mixed solution in an ultrasonic heating device, heating the mixed solution to 90 ℃ in an ultrasonic water bath, keeping the ultrasonic power at 20KHz, preserving the heat for 4 hours to gradually dissolve the paraffin in the petroleum ether, and taking out a paraffin residue bag when the mixed solution is hot to obtain the mixed solution of the paraffin and the petroleum ether; transferring the mixed solution of paraffin and petroleum ether to a rotary evaporator for distillation, recovering the petroleum ether, and drying the rest mixed solution in a drying oven at 60 ℃ for 10h to obtain paraffin; putting the taken wax residue bag in an oven for drying for 11h at 50 ℃, weighing and marking as W2; and (3) putting the dried solid residue in the filter paper bag into a muffle furnace, heating to 600 ℃ at the speed of 5 ℃/min, and keeping for 3 h. The recovery of paraffin in this example was 90.57% by weight.
Example 4
Crushing Fischer-Tropsch synthesis wax residue (weighed and recorded as W) by using a crusher, and sieving the crushed Fischer-Tropsch synthesis wax residue by using a 120-mesh sieve; wrapping 2g of wax slag by using filter paper to obtain a wax slag bag, and weighing the wax slag bag as W1; mixing the wax residue bag with 50ml of n-hexane to obtain a mixed solution, wherein the mass ratio of the wax residue to the n-hexane is 1: 25; placing the mixed solution in an ultrasonic heating device, heating the mixed solution to 70 ℃ in an ultrasonic water bath, keeping the ultrasonic power at 20KHz, preserving the heat for 4 hours to gradually dissolve the paraffin in the n-hexane, and taking out a wax residue bag when the mixed solution is hot to obtain the mixed solution of the paraffin and the n-hexane; transferring the mixed solution of paraffin and n-hexane to a rotary evaporator for distillation, recovering n-hexane, and drying the remaining mixed solution in a drying oven at 60 ℃ for 12h to obtain paraffin; putting the taken wax residue bag in an oven for drying for 10h at 50 ℃, weighing and marking as W2; and (3) putting the dried solid residue in the filter paper bag into a muffle furnace, heating to 550 ℃ at a speed of 10 ℃/min, and keeping for 4 h. The recovery of paraffin in this example was determined by gravimetric method to be 96.86%.
Example 5
Crushing Fischer-Tropsch synthesis wax residue (weighed and recorded as W) by using a crusher, and sieving the crushed Fischer-Tropsch synthesis wax residue by using a 120-mesh sieve; wrapping 2g of wax slag by using filter paper to obtain a wax slag bag, and weighing the wax slag bag as W1; mixing a wax residue bag with 60ml of naphtha to obtain a mixed solution, wherein the mass ratio of the wax residue to the naphtha is 1: 30; placing the mixed solution in an ultrasonic heating device, heating the mixed solution to 90 ℃ in an ultrasonic water bath, keeping the ultrasonic power at 30KHz, preserving the heat for 3 hours to gradually dissolve the paraffin into the naphtha, and taking out a wax residue bag when the mixed solution is hot to obtain the mixed solution of the paraffin and the naphtha; transferring the mixed solution of paraffin and naphtha to a rotary evaporator for distillation, recovering naphtha, and placing the residual mixed solution in an oven for drying for 12 hours at 60 ℃ to obtain paraffin; putting the taken wax residue bag in an oven for drying for 12h at the temperature of 60 ℃, weighing and marking as W2; and (3) putting the dried solid residue in the filter paper bag into a muffle furnace, heating to 400 ℃ at the speed of 5 ℃/min, and keeping for 2 h. The recovery of paraffin in this example was 98.69% by weight.
GC-MS analysis of the paraffins recovered in examples 1 to 5 is shown in the following Table. The paraffin hydrocarbons obtained in each example are mainly straight-chain paraffin hydrocarbons of C8 to C29 and isomers thereof, and are important raw materials for producing diesel oil, and alcohols and ester compounds are important raw materials for producing candles, wood sizing agents, lubricants, coatings, packaging materials, foods and cosmetics.
TABLE 1 distribution of the contents of the components
According to the embodiments 1 to 5, the recovery rate of the paraffin wax in the Fischer-Tropsch synthesis wax residue is 90.57 to 98.93 percent by extracting the paraffin wax in the Fischer-Tropsch synthesis wax residue. Furthermore, the recovered paraffin of the present invention is an important raw material for producing diesel oil, candles, wood board sizing agents, lubricants, paints, packaging materials, foods and cosmetics. Therefore, the method has the advantages that the paraffin can be extracted at a high recovery rate, high-quality paraffin can be obtained, the organic solvent can be recycled, the requirement of clean production is met, the equipment investment is low, the energy consumption is low, the adaptability is strong, the low carbon and the environment are protected, and a recycling method is provided for the treatment of the wax residue.
Although the present invention has been described in detail with reference to the above embodiments, it is only a part of the embodiments of the present invention, not all of the embodiments, and other embodiments can be obtained without inventive step according to the embodiments, and the embodiments are included in the scope of the present invention.
Claims (9)
1. A method for extracting paraffin from wax residue comprises the following specific steps:
A. wrapping the pretreated wax residue with filter paper to form a wax residue bag;
B. mixing the wax residue bag with an organic solvent to form a mixed liquid bag;
C. carrying out ultrasonic heating dissolution on paraffin in the mixed liquid bag to obtain a mixed solution of the paraffin and an organic solvent;
D. and distilling the mixed solution, and drying the residual mixed solution to obtain the paraffin.
2. The method according to claim 1, wherein the pretreatment comprises crushing the wax residue and sieving the crushed wax residue through a sieve.
3. The method according to claim 2, wherein the mesh number of the screen is 90 to 150 mesh.
4. The method of claim 1, wherein the wax residue is a fischer-tropsch wax residue.
5. The method according to claim 1, characterized in that the organic solvent is a non-polar organic solvent.
6. The method according to claim 1 or 5, characterized in that the organic solvent is at least one of petroleum ether, n-hexane, naphtha or turpentine.
7. The method according to claim 1, wherein the ratio of the mass of the wax residue to the volume of the organic solvent is 30 to 50 g/L.
8. The method according to claim 1, wherein the ultrasonic heating is carried out at a temperature of 70-90 ℃ for 3-4 h; the ultrasonic power is 20-30 KHz.
9. The method according to claim 1, wherein the drying temperature is 40-60 ℃ and the drying time is 8-12 h.
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2021
- 2021-07-30 CN CN202110874901.3A patent/CN113528185A/en active Pending
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CN102701959A (en) * | 2012-06-05 | 2012-10-03 | 山东大学 | Novel method for extracting benzoic acid from TA (Terephthalic Acid) residues |
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Application publication date: 20211022 |
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