CN107337585A - A kind of method that lignin microwave depolymerization prepares single phenolic compound - Google Patents
A kind of method that lignin microwave depolymerization prepares single phenolic compound Download PDFInfo
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- CN107337585A CN107337585A CN201710602146.7A CN201710602146A CN107337585A CN 107337585 A CN107337585 A CN 107337585A CN 201710602146 A CN201710602146 A CN 201710602146A CN 107337585 A CN107337585 A CN 107337585A
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- lignin
- phenolic compound
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- single phenolic
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- 229920005610 lignin Polymers 0.000 title claims abstract description 70
- 150000002989 phenols Chemical class 0.000 title claims abstract description 44
- 238000000034 method Methods 0.000 title claims abstract description 26
- 238000012691 depolymerization reaction Methods 0.000 claims abstract description 27
- 239000002245 particle Substances 0.000 claims abstract description 26
- 238000004227 thermal cracking Methods 0.000 claims abstract description 21
- 239000012495 reaction gas Substances 0.000 claims abstract description 18
- 239000007788 liquid Substances 0.000 claims abstract description 16
- 239000012159 carrier gas Substances 0.000 claims abstract description 15
- 238000006243 chemical reaction Methods 0.000 claims abstract description 14
- 239000002904 solvent Substances 0.000 claims abstract description 14
- 229910010271 silicon carbide Inorganic materials 0.000 claims abstract description 13
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 claims abstract description 12
- 238000005292 vacuum distillation Methods 0.000 claims abstract description 12
- 239000008246 gaseous mixture Substances 0.000 claims abstract description 11
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 18
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical group OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 15
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 12
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 12
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 12
- 239000001257 hydrogen Substances 0.000 claims description 12
- 229910052739 hydrogen Inorganic materials 0.000 claims description 12
- 229910052757 nitrogen Inorganic materials 0.000 claims description 9
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 8
- 238000009833 condensation Methods 0.000 claims description 8
- 230000005494 condensation Effects 0.000 claims description 8
- 239000007789 gas Substances 0.000 claims description 8
- LEQAOMBKQFMDFZ-UHFFFAOYSA-N glyoxal Chemical compound O=CC=O LEQAOMBKQFMDFZ-UHFFFAOYSA-N 0.000 claims description 8
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 claims description 8
- 230000035484 reaction time Effects 0.000 claims description 6
- 229920001732 Lignosulfonate Polymers 0.000 claims description 5
- 239000003513 alkali Substances 0.000 claims description 5
- 238000000197 pyrolysis Methods 0.000 claims description 5
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 claims description 4
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 4
- IKHGUXGNUITLKF-XPULMUKRSA-N acetaldehyde Chemical compound [14CH]([14CH3])=O IKHGUXGNUITLKF-XPULMUKRSA-N 0.000 claims description 4
- 235000019253 formic acid Nutrition 0.000 claims description 4
- 229940015043 glyoxal Drugs 0.000 claims description 4
- TZIHFWKZFHZASV-UHFFFAOYSA-N methyl formate Chemical compound COC=O TZIHFWKZFHZASV-UHFFFAOYSA-N 0.000 claims description 4
- 239000010703 silicon Substances 0.000 claims description 4
- 229910052710 silicon Inorganic materials 0.000 claims description 4
- 229910021431 alpha silicon carbide Inorganic materials 0.000 claims description 3
- 239000008187 granular material Substances 0.000 claims description 3
- 230000003301 hydrolyzing effect Effects 0.000 claims description 3
- 239000005543 nano-size silicon particle Substances 0.000 claims description 3
- 238000005516 engineering process Methods 0.000 abstract description 5
- 230000008569 process Effects 0.000 description 6
- 238000006068 polycondensation reaction Methods 0.000 description 4
- 238000010504 bond cleavage reaction Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 230000007017 scission Effects 0.000 description 3
- 239000002028 Biomass Substances 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 239000011203 carbon fibre reinforced carbon Substances 0.000 description 2
- 239000012141 concentrate Substances 0.000 description 2
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- LCGLNKUTAGEVQW-UHFFFAOYSA-N Dimethyl ether Chemical group COC LCGLNKUTAGEVQW-UHFFFAOYSA-N 0.000 description 1
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 1
- 229910003978 SiClx Inorganic materials 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000004913 activation Effects 0.000 description 1
- 150000004945 aromatic hydrocarbons Chemical class 0.000 description 1
- 125000003118 aryl group Chemical group 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 229920002678 cellulose Polymers 0.000 description 1
- 239000001913 cellulose Substances 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000006837 decompression Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- 239000012847 fine chemical Substances 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- 238000002309 gasification Methods 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 230000001533 ligninolytic effect Effects 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- -1 methoxyl group Chemical group 0.000 description 1
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 1
- 150000003384 small molecules Chemical class 0.000 description 1
- 238000010025 steaming Methods 0.000 description 1
- 230000010512 thermal transition Effects 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- 239000002023 wood Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C37/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom of a six-membered aromatic ring
- C07C37/50—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom of a six-membered aromatic ring by reactions decreasing the number of carbon atoms
- C07C37/52—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom of a six-membered aromatic ring by reactions decreasing the number of carbon atoms by splitting polyaromatic compounds, e.g. polyphenolalkanes
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a kind of method that lignin microwave depolymerization prepares single phenolic compound, first in terms of mass fraction, 10 parts of lignin is well mixed with 5~10 parts of silicon-carbide particles, are placed in microwave depolymerization reaction environment；Secondly the gaseous mixture of carrier gas and reaction gas is continuously passed through into microwave depolymerization reaction environment, proceeds by microwave depolymerization reaction；Then thermal cracking steam that microwave depolymerization is reacted to generation cools down, and obtains solvent-based thermal cracking liquid；Finally solvent-based thermal cracking liquid is evaporated under reduced pressure, when being distillated without distillate, vacuum distillation terminates, and the component not distilled out now is single phenolic compound.The present invention increases substantially single phenolic compound yield and yield by changing reaction atmosphere, and important technology support is provided for single phenolic compound for lignin Efficient Conversion.
Description
Technical field
The invention belongs to biomass energy technology field, and in particular to a kind of lignin microwave depolymerization prepares single phenols chemical combination
The method of thing.
Background technology
Lignin is one of important component of biomass, is to enrich degree on the earth to be only second to the renewable of cellulose
Carbon source.Lignin source is mainly industrial lignin at present, is the accessory substance of pulp and paper industry, the whole world comes from papermaking every year
For the lignin amount of industry up to more than 50,000,000 tons, Land use systems main at present utilize added value still by its direct combustion heat supplying
It is very low, it is badly in need of seeking the new way of lignin higher value application.
Lignin due in structure existing carbochain have aromatic rings again, and be connected with methoxyl group (- OCH3), hydroxyl (- OH), carboxylic
The various active structure of functional groups such as base (- CO), it is the ideal original for producing the high value fine chemicals such as aromatic hydrocarbons, phenolic compound
Material.The a certain degree of degraded of lignin can be realized by the means of thermochemical study, however, lignin heat chemistry turns at this stage
Change degraded and the problems such as degradation efficiency is low, charing phenomenon is serious, converted product yield is low, collection of products is difficult be present, it is serious to restrict
The Efficient Conversion of lignin utilizes.Most research under high pressure, high temperature, a large amount of hydrogen atmospheres by realizing lignin at present
Degraded, but the undesirable development that govern technology of too high cost input and product qualities.
The content of the invention
It is an object of the invention to provide a kind of method that lignin microwave depolymerization prepares single phenolic compound, on overcoming
The defects of prior art is present is stated, the present invention increases substantially single phenolic compound yield and receipts by changing reaction atmosphere
Rate, important technology support is provided for single phenolic compound for lignin Efficient Conversion.
To reach above-mentioned purpose, the present invention adopts the following technical scheme that：
A kind of method that lignin microwave depolymerization prepares single phenolic compound, comprises the following steps：
Step 1：In terms of mass fraction, 10 parts of lignin are well mixed with 5~10 parts of silicon-carbide particles, are placed in microwave
In depolymerization reaction environment；
Step 2：The gaseous mixture of carrier gas and reaction gas is continuously passed through into microwave depolymerization reaction environment, proceeds by microwave
Depolymerization reaction；
Step 3：The thermal cracking steam of microwave depolymerization reaction generation is cooled down, obtains solvent-based thermal cracking liquid；
Step 4：Solvent-based thermal cracking liquid is evaporated under reduced pressure, when being distillated without distillate, vacuum distillation terminates,
The component not distilled out now is single phenolic compound.
Further, described lignin be lignosulfonates, sulfate-reducing conditions, alkali lignin, dealkalize lignin,
Hydrolytic lignin or pyrolysis lignin, and the particle diameter of lignin is 0.05~0.5mm, moisture content≤10%.
Further, described silicon-carbide particle is nano silicon carbide granulate, alpha-silicon carbide particle or silicon B-carbide particle,
The particle diameter of silicon-carbide particle is 0.1~1.0mm.
Further, the flow of the gaseous mixture described in step 2 is：Mixed corresponding to lignin in every gram of step 1
Throughput is 10~50mL/min.
Further, described carrier gas is nitrogen, and described reaction gas is hydrogen and the mixed gas of organic vapor, hydrogen
The volume ratio of gas and organic vapor is 1:(10~50), and the volume ratio of carrier gas and reaction gas is 10:(1~5).
Further, described organic vapor is methanol, ethanol, acetone, acetaldehyde, glyoxal, formic acid, ether or formic acid first
Ester.
Further, microwave depolymerization reaction condition in step 2：Microwave frequency is 2.45GHz, microwave power be 600~
1200W, heating-up temperature are 500~650 DEG C, the reaction time is 5~8 minutes.
Further, the thermal cracking steam that microwave depolymerization is reacted to generation in step 3 is carried out under 1~5 DEG C of condensation temperature
Cooling.
Further, in step 4 vacuum distillation temperature be 20~35 DEG C, relative degree of vacuum be -0.085~-
0.095Mpa。
Further, it is evaporated under reduced pressure in step 4 after the distillate distillated vaporizes again and is circulated as organic vapor for walking
In rapid two.
Compared with prior art, the present invention has technique effect beneficial below：
The method that lignin microwave depolymerization proposed by the present invention prepares single phenolic compound, realize the quick height of lignin
Imitate depolymerization so that lignin depolymerization prepares the yield that single phenolic compound has reached theoretical, and the profit of lignin is greatly improved
It is as follows with rate and value, specific advantage：
(1) traditional depolymerization reaction generally only adds carrier gas such as nitrogen and carried out, and causes the thermal transition efficiency of lignin very low, and
And easily secondary polycondensation generates tarry to the single phenolic compound intermediate generated during lignin conversion in condensation process
Material can not use, in addition, tradition using nitrogen be carrier gas reaction generation product liquid due to viscosity large fluidity difference often
Adhesion can not be collected into well on the reactor wall.Innovative proposing of the invention is mixed carrier gas with reaction gas,
On the one hand reaction gas prevents the secondary polycondensation of single phenols intermediate of depolymerization generation well, on the other hand will be anti-as solvent
The single phenolic compound that should be generated carries out reaction system, and collection efficiency increases substantially.
(2) present invention proposes the gaseous mixture that carrier gas and reaction gas are passed through during microwave depolymerization, to improve lignin
Depolymerization is the yield of single phenolic compound；Wherein, nitrogen as carrier gas primarily serve protection gas effect, reaction gas be hydrogen and
The mixed gas of organic vapor, the volume ratio of hydrogen is smaller in reaction gas, and main function is to reduce the ether in lignin
Key and the activation energy of carbon-carbon bond fracture, aid in scission of link；Organic vapor is the relatively low small organic molecule of boiling point in reaction gas, mainly
Effect is that these small molecule organic vapors can be grafted onto the two of scission of link rapidly when the ehter bond in lignin, carbon-carbon bond fracture
End, as the methyl in methanol and hydroxyl are grafted onto the both ends of scission of link respectively, to prevent the key of fracture from carrying out secondary polycondensation, so as to big
Amplitude improves the efficiency and conversion ratio that lignin microwave depolymerization generates single phenolic compound.
(3) after the present invention collects the organic vapor in reaction gas again in condensation process, reclaimed by being evaporated under reduced pressure,
Again gasification cycle is by the use of the efficiency for organic vapor as the organic vapor in reaction gas, is greatly improved participating in reaction, and
And without discharging of waste liquid, technique clean environment firendly.
Embodiment
Embodiments of the present invention are described in further detail below：
For single secondary polycondensation phenomenon of phenolic compound intermediate in current lignin thermal conversion processes it is serious, be converted into list
Phenolic compound efficiency and low yield, single phenolic compound viscosity great Yi of generation cause collection difficulty etc. to be asked in tube wall deposition
Topic, the present invention propose a kind of method that lignin microwave depolymerization prepares single phenolic compound, comprised the following steps：
(1) lignin of 10 mass parts is well mixed with the silicon-carbide particle of (5~10) mass parts, is placed in microwave depolymerization
In reaction environment.Described lignin is lignosulfonates, sulfate-reducing conditions, alkali lignin, dealkalize lignin, hydrolysis wood
Quality or pyrolysis lignin, particle diameter are 0.05~0.5mm, moisture content≤10%；Described carborundum is nanometer silicon carbide, α-carbon
SiClx or silicon B-carbide, particle diameter are 0.1~1.0mm.
(2) gaseous mixture of carrier gas and reaction gas is continuously passed through in microwave reaction environment, proceeds by microwave depolymerization reaction.Institute
The flow for the gaseous mixture stated is：Mixed gas flow corresponding to every gram of lignin is 10~50mL/min；Described carrier gas is nitrogen,
The volume ratio of carrier gas and reaction gas is 10:(1~5)；Described reaction gas is hydrogen and the mixed gas of organic vapor, hydrogen
Volume ratio with organic vapor is 1:(10~50), wherein, organic vapor is methanol, ethanol, acetone, acetaldehyde, glyoxal, first
One kind in acid, ether, methyl formate.Described microwave depolymerization reaction condition is microwave frequency 2.45GHz, microwave power 600
~1200W, 500~650 DEG C of heating-up temperature, 5~8 minutes reaction time.
(3) the thermal cracking steam of microwave depolymerization generation is cooled down under 1~5 DEG C of condensation temperature, obtains solvent-borne type hot tearing
Solve liquid.
(4) solvent-based thermal cracking liquid is evaporated under reduced pressure, 20~35 DEG C of vacuum distillation temperature, relative degree of vacuum-
0.085~-0.095Mpa, when being distillated without distillate, vacuum distillation terminates, and the component not distilled out now is single phenol generalization
Compound.
(5) the above-mentioned distillate distilled out vaporizes the organic vapor that Posterior circle is used in step (2) again.
The present invention is described in further detail with reference to embodiment：
Embodiment 1
The implementation process that the present invention is introduced by taking alkali lignin raw material as an example is as follows：
By 10g alkali lignins (0.2~0.5mm of particle diameter, moisture content 8%) and 5g nano silicon carbide granulate (particle diameter 0.1~
0.45mm) it is well mixed, carries out microwave depolymerization reaction.100mL/min nitrogen, 1mL/min are continuously passed through in microwave depolymerization reaction
The gaseous mixture of hydrogen and 10mL/min methanol, microwave depolymerization reaction is proceeded by, microwave depolymerization reaction condition is microwave frequency
2.45GHz, microwave power 600W, 500 DEG C of heating-up temperature, 8 minutes reaction time.The thermal cracking steam of microwave depolymerization generation is 1
Cooled down under DEG C condensation temperature, obtain solvent-based thermal cracking liquid.Solvent-based thermal cracking liquid is evaporated under reduced pressure, depressurized
20 DEG C of vapo(u)rizing temperature, relative degree of vacuum -0.085Mpa, when being distillated without distillate, vacuum distillation terminates, and does not distill out now
Component is single phenolic compound.Weighed, single phenolic compound is 7.6g, and yield reaches 76%；Molecular weight determination range set
In in 95~179Da, it is mainly single phenolic compound to illustrate product.
Embodiment 2
The implementation process that the present invention is introduced by taking pyrolysis lignin raw material as an example is as follows：
By 10g pyrolysis lignins (0.05~0.1mm of particle diameter, moisture content 3%) and 10g alpha-silicon carbide particle (particle diameter
0.45~1.0mm) it is well mixed, carry out microwave depolymerization reaction.Microwave depolymerization reaction in be continuously passed through 300mL/min nitrogen,
The gaseous mixture of 3mL/min hydrogen and 150mL/min acetaldehyde, proceeds by microwave depolymerization reaction, and microwave depolymerization reaction condition is micro-
Wave frequency rate 2.45GHz, microwave power 1200W, 650 DEG C of heating-up temperature, 5 minutes reaction time.The thermal cracking of microwave depolymerization generation
Steam is cooled down under 5 DEG C of condensation temperatures, obtains solvent-based thermal cracking liquid.Solvent-based thermal cracking liquid is subjected to decompression steaming
Evaporate, 35 DEG C of vacuum distillation temperature, relative degree of vacuum -0.095Mpa, when being distillated without distillate, vacuum distillation terminates, now not
The component distilled out is single phenolic compound.Weighed, single phenolic compound is 6.8g, and yield reaches 68%；Molecule measuring
Determine scope and concentrate on 95~131Da, it is mainly single phenolic compound to illustrate product.
Embodiment 3
The implementation process that the present invention is introduced by taking lignosulfonates raw material as an example is as follows：
By 10g lignosulfonates (0.1~0.3mm of particle diameter, moisture content 5%) and 8g silicon B-carbide particle (particle diameter
0.45~0.6mm) it is well mixed, carry out microwave depolymerization reaction.Microwave depolymerization reaction in be continuously passed through 200mL/min nitrogen,
The gaseous mixture of 2mL/min hydrogen and 50mL/min methyl formates, proceeds by microwave depolymerization reaction, and microwave depolymerization reaction condition is
Microwave frequency 2.45GHz, microwave power 1000W, 550 DEG C of heating-up temperature, 6 minutes reaction time.The hot tearing of microwave depolymerization generation
Solution steam is cooled down under 3 DEG C of condensation temperatures, obtains solvent-based thermal cracking liquid.Solvent-based thermal cracking liquid is depressurized
Distillation, 30 DEG C of vacuum distillation temperature, relative degree of vacuum -0.090Mpa, when being distillated without distillate, vacuum distillation terminates, now
The component not distilled out is single phenolic compound.Weighed, single phenolic compound is 7.3g, and yield reaches 73%；Molecular weight
Measurement range concentrates on 110~184Da, and it is mainly single phenolic compound to illustrate product.
Lignin in above-described embodiment can also be sulfate-reducing conditions, dealkalize lignin or hydrolytic lignin；It is organic
Steam can also be ethanol, acetone, glyoxal, formic acid or ether.
Claims (10)
1. a kind of method that lignin microwave depolymerization prepares single phenolic compound, it is characterised in that comprise the following steps：
Step 1：In terms of mass fraction, 10 parts of lignin are well mixed with 5~10 parts of silicon-carbide particles, are placed in microwave depolymerization
In reaction environment；
Step 2：The gaseous mixture of carrier gas and reaction gas is continuously passed through into microwave depolymerization reaction environment, proceeds by microwave depolymerization
Reaction；
Step 3：The thermal cracking steam of microwave depolymerization reaction generation is cooled down, obtains solvent-based thermal cracking liquid；
Step 4：Solvent-based thermal cracking liquid is evaporated under reduced pressure, when being distillated without distillate, vacuum distillation terminates, now
The component not distilled out is single phenolic compound.
2. the method that a kind of lignin microwave depolymerization according to claim 1 prepares single phenolic compound, it is characterised in that
Described lignin is lignosulfonates, sulfate-reducing conditions, alkali lignin, dealkalize lignin, hydrolytic lignin or pyrolysis
Lignin, and the particle diameter of lignin is 0.05~0.5mm, moisture content≤10%.
3. the method that a kind of lignin microwave depolymerization according to claim 1 prepares single phenolic compound, it is characterised in that
Described silicon-carbide particle is nano silicon carbide granulate, alpha-silicon carbide particle or silicon B-carbide particle, the particle diameter of silicon-carbide particle
For 0.1~1.0mm.
4. the method that a kind of lignin microwave depolymerization according to claim 1 prepares single phenolic compound, it is characterised in that
The flow of gaseous mixture described in step 2 is：Mixed gas flow corresponding to lignin in every gram of step 1 is 10~50mL/
min。
5. the method that a kind of lignin microwave depolymerization according to claim 1 prepares single phenolic compound, it is characterised in that
Described carrier gas is nitrogen, and described reaction gas is the body of hydrogen and the mixed gas of organic vapor, hydrogen and organic vapor
Product is than being 1:(10~50), and the volume ratio of carrier gas and reaction gas is 10:(1~5).
6. the method that a kind of lignin microwave depolymerization according to claim 5 prepares single phenolic compound, it is characterised in that
Described organic vapor is methanol, ethanol, acetone, acetaldehyde, glyoxal, formic acid, ether or methyl formate.
7. the method that a kind of lignin microwave depolymerization according to claim 1 prepares single phenolic compound, it is characterised in that
Microwave depolymerization reaction condition in step 2：Microwave frequency is 2.45GHz, microwave power is 600~1200W, heating-up temperature 500
~650 DEG C, the reaction time be 5~8 minutes.
8. the method that a kind of lignin microwave depolymerization according to claim 1 prepares single phenolic compound, it is characterised in that
The thermal cracking steam that microwave depolymerization is reacted to generation in step 3 is cooled down under 1~5 DEG C of condensation temperature.
9. the method that a kind of lignin microwave depolymerization according to claim 1 prepares single phenolic compound, it is characterised in that
Vacuum distillation temperature is 20~35 DEG C in step 4, and relative degree of vacuum is -0.085~-0.095Mpa.
10. the method that a kind of lignin microwave depolymerization according to claim 1 prepares single phenolic compound, its feature exist
In being evaporated under reduced pressure in step 4 after the distillate distillated vaporizes again and circulated as organic vapor in step 2.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107987866A (en) * | 2018-01-15 | 2018-05-04 | 陕西科技大学 | A kind of device and method of the efficient depolymerization co-producing bio-oil of solid waste microwave and charcoal |
| CN110407888A (en) * | 2019-08-09 | 2019-11-05 | 陕西科技大学 | A method of promoting sulfate-reducing conditions depolymerization using discarded cigarette filter |
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| CN110407888B (en) * | 2019-08-09 | 2020-11-06 | 陕西科技大学 | Method for promoting depolymerization of sulfate lignin by using waste cigarette filter tip |
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