CN109046349A - The method that monatomic palladium catalyst and preparation method and catalysis oxidation 5-HMF prepare 2,5-FDCA - Google Patents
The method that monatomic palladium catalyst and preparation method and catalysis oxidation 5-HMF prepare 2,5-FDCA Download PDFInfo
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Abstract
The present invention relates to the methods that monatomic palladium catalyst and preparation method thereof and catalysis oxidation 5-HMF prepare 2,5-FDCA, belong to the 5-HMF selective oxidation preparation field 2,5-FDCA.The monatomic palladium catalyst structure of the present invention are as follows: active component palladium is in high degree of dispersion and manganese dioxide surface is evenly distributed in a manner of monoatomic；Wherein, the content of palladium is 0.2~3wt%, and the content of manganese dioxide is 97~99.8wt%.Method for preparing catalyst of the invention is simple, and for catalysis oxidation 5-HMF preparation 2,5-FDCA, application method is simple, and when catalysis oxidation, selects performance good, reusability is good.
Description
Technical field
The present invention relates to the sides that monatomic palladium catalyst and preparation method and catalysis oxidation 5-HMF prepare 2,5-FDCA
Method belongs to the 5-HMF selective oxidation preparation field 2,5-FDCA.
Background technique
Energy problem is a worldwide problem, and now, demand of the society to fossil energy increasingly increases, many in life
Organic material both is from fossil energy, in addition, due to coal, petroleum, natural gas these fossil energies non-renewable and
Caused environmental problem is largely used, the substitute for finding these energy will necessarily become the coke that countries in the world are paid close attention to jointly
Point.Biomass energy is from a wealth of sources and can regenerate, and has good potential value in terms of substituting fossil energy, in recent years
As studied hot spot.
By glucose sugar or it is fructose converting come 5 hydroxymethyl furfural, it is considered to be the widely used platform chemical combination of one kind
Object can prepare a series of furan compound, such as 2,5-furandicarboxylic acid, 2- Fonnyl-furan -2- by catalysis oxidation
Formic acid, 2,5-Diformyl furans etc..
2,5-furandicarboxylic acid can be used as a kind of high added value product obtained by 5 hydroxymethyl furfural selective oxidation
Raw material synthesize some polyester materials haveing excellent performance, and then can be widely applied to the fields such as packaging material engineering plastics.With stone
The fossil resources such as oil are that many organic materials of Material synthesis are not only difficult to degrade, but also the exhaust gas generated in the synthesis process is useless
Slag can largely cause environmental pollution, and FDCA synthesizes poly- from biomass and using 2,5-furandicarboxylic acid as monomer
Ester material can be degraded, and meet sustainable development and protect the requirement of environment.
The organic anti-of 2,5- furandicarboxylic acid (i.e. 2,5-FDCA) is prepared in catalysis oxidation 5 hydroxymethyl furfural (i.e. 5-HMF)
Ying Zhong is frequently accompanied by the generation of some by-products, is that one kind has using noble metal catalyst catalysis oxidation 5 hydroxymethyl furfural
The method that effect ground improves reaction-ure conversion-age and target product yield.
Patent publication No. is that CN106749130A discloses a kind of Pt catalyst oxidation 5 hydroxymethyl furfural preparation
The method of 2,5-furandicarboxylic acid.But the preparation method of the catalyst is complicated, needs to prepare under 280 DEG C of hot conditions, and
And it needs with ozone to be presoma.The catalyst is during catalysis oxidation 5 hydroxymethyl furfural prepares 2,5-furandicarboxylic acid
Required oxygen pressure is 0.4Mpa, higher than synthesis under normal pressure condition of the invention.
Patent publication No. is that CN104277020A is disclosed using Pd/Bi2O3Catalysis oxidation 5 hydroxymethyl furfural preparation 2,5-
The method of furandicarboxylic acid, and disclose Pd/Bi2O3The preparation method of catalyst is deposition-precipitation method.But the Pd/Bi2O3
The application method of catalyst is complicated, is needed by catalyst in hydrogen atmosphere before use, restore 1 under the conditions of 150~250 DEG C~
5h increases cumbersome degree, and due to needing to handle in the hydrogen atmosphere of high temperature, increases security risk.
Summary of the invention
The invention solves first technical problem be to provide a kind of monatomic palladium catalyst.Monatomic palladium of the invention
When catalyst is for catalysis oxidation 5-HMF preparation 2,5-FDCA, it is anti-to solve traditional catalyst catalysis 5 hydroxymethyl furfural oxidation
Problem of environmental pollution caused by highly basic (sodium hydroxide, potassium hydroxide etc.) should be needed to use in the process, and improve 5-HMF
Conversion ratio and 2,5-FDCA yield.
Monatomic palladium catalyst, the catalyst structure are as follows: active component palladium is in high degree of dispersion and in a manner of monoatomic
It is evenly distributed on manganese dioxide surface；Wherein, the content of palladium is 0.2~3wt%, the content of manganese dioxide is 97~
99.8wt%.Monatomic palladium catalyst produced by the present invention can use Pd/MnO2To indicate.
The invention solves second technical problem be to provide the preparation method of monatomic palladium catalyst a kind of, the preparation
Method is simple, cost is relatively low, and the preparation method can make active component palladium high degree of dispersion and uniformly be divided in a manner of monoatomic
Cloth is on manganese dioxide surface, without agglomeration.
The preparation method of monatomic palladium catalyst: being 5 by the weight ratio of ammonium sulfate, ammonium persulfate, palladium nitrate and manganese sulfate
~7:2~3:0.05~0.08:1~2 take raw material, add water and stir to obtain mixture, then mixture is placed at 120~160 DEG C
9~14h is reacted, it is then cooling, be filtered, washed to neutrality, black precipitate is obtained, by black precipitate drying, is crushed up to single former
Sub- palladium catalyst.
It is preferred: ammonium sulfate, ammonium persulfate, palladium nitrate and manganese sulfate weight ratio be 5.24~6.24:2.36~2.86:
0.066~0.077:1.56~1.81；It is furthermore preferred that ammonium sulfate, ammonium persulfate, palladium nitrate and manganese sulfate weight ratio be 5.24
~6.08:2.36~2.74:0.066~0.077:1.56~1.81；It is further preferred that ammonium sulfate, ammonium persulfate, palladium nitrate
Weight ratio with manganese sulfate is 6.08:2.74:0.077:1.81.
It is preferred: mixture being placed at 140 DEG C and reacts 12h.
Preferred: black precipitate drying temperature is 120 DEG C, drying time 12h.
The invention solves third technical problem be monatomic palladium catalyst application, will be produced by the present invention single former
For sub- palladium catalyst for catalysis oxidation 5-HMF preparation 2,5-FDCA, method is simple, easy to operate.This method does not need that highly basic is added
(sodium hydroxide, potassium hydroxide etc.).
The method that monatomic palladium catalyst catalysis oxidation 5-HMF prepares 2,5-FDCA: by the monatomic palladium catalyst of preparation,
The mixing of the aqueous solution of Anhydrous potassium carbonate and 5-HMF, in oxygen atmosphere, temperature is reacted under the conditions of being 80~110 DEG C, is made 2,5-
FDCA。
It is preferred: the weight ratio of monatomic palladium catalyst, Anhydrous potassium carbonate and 5-HMF be 0.9~1.1:3~4:0.7~
0.9；Preferably, the weight ratio of monatomic palladium catalyst, potassium carbonate and 5-HMF are 1~1.1:3.35~3.5:0.77~0.8；
It is furthermore preferred that the weight ratio of monatomic palladium catalyst, potassium carbonate and 5-HMF is 1.1:3.5:0.8.
It is preferred: oxygen gas flow rate 25ml/min.
Preferred: reaction temperature is 90~110 DEG C；Further preferred reaction temperature is 110 DEG C.
It is preferred: reaction time at least 3h；Preferred reaction time is 5h.
Beneficial effects of the present invention:
1, monatomic palladium catalyst Pd/MnO of the invention2Unique structure, active component palladium is in high degree of dispersion and with single original
The mode of son is evenly distributed on manganese dioxide surface, solves precious metal atom and is agglomerated into the atomic group of different-grain diameter size and leads
The poor problem of the catalytic performance of cause.
2, Pd/MnO of the invention2Middle Pd and carrier MnO2Between active force it is strong, solve traditional loaded catalyst
With the active force of carrier bad disadvantage of repeat performance caused by weak.Using palladium catalyst catalysis oxidation 5- of the present invention
HMF preparation 2,5-FDCA, within a short period of time, so that it may aoxidize 5-HMF, and conversion ratio reaches 98% or more, 2,5-FDCA
Yield reaches 90% or more, and catalyst reusability of the invention is good, reuses 5 times, the conversion of 5-HMF oxidation reaction
Rate remains unchanged substantially, and 2,5-FDCA yield only reduces 2%.
3, it using in palladium catalyst catalysis 5 hydroxymethyl furfural oxidation reaction process of the invention, does not need using highly basic
(sodium hydroxide, potassium hydroxide etc.) can make 5 hydroxymethyl furfural high conversion rate, and 2,5-furandicarboxylic acid yield is high, solves
Traditional catalyst catalysis needs to use equipment corrosion and problem of environmental pollution caused by highly basic.
4, palladium catalyst preparation method of the invention is simple, any processing is not needed yet using preceding, using simplicity, in normal pressure
It is lower to can be used, it is with a wide range of applications.
Detailed description of the invention
Fig. 1 becomes for 5 hydroxymethyl furfural conversion rate of oxidation in embodiment 1 and at any time the yield of 2,5-furandicarboxylic acid
The curve graph of change.
Fig. 2 is the repeat performance figure of catalyst A1 in embodiment 1.
Fig. 3 is the Electron microscope figure of catalyst A1 in embodiment 1.
Specific embodiment
The invention solves first technical problem be to provide a kind of monatomic palladium catalyst.Monatomic palladium of the invention
When catalyst is for catalysis oxidation 5-HMF preparation 2,5-FDCA, it is anti-to solve traditional catalyst catalysis 5 hydroxymethyl furfural oxidation
Problem of environmental pollution caused by highly basic (sodium hydroxide, potassium hydroxide etc.) should be needed to use in the process, and improve 5-HMF
Conversion ratio and 2,5-FDCA yield.
The calculation formula of conversion ratio and yield of the present invention is as follows:
Wherein, 5-HMF is 5 hydroxymethyl furfural；2,5-FDCA be 2,5-furandicarboxylic acid.
The monatomic palladium catalyst of the present invention, the catalyst structure are as follows: active component palladium is in high degree of dispersion and with monatomic
Mode be evenly distributed on manganese dioxide surface；Wherein, the content of palladium is 0.2~3wt%, the content of manganese dioxide is 97~
99.8wt%.Monatomic palladium catalyst of the invention can use Pd/MnO2To indicate.
The invention solves second technical problem be to provide the preparation method of monatomic palladium catalyst a kind of, the preparation
Method is simple, cost is relatively low, and the preparation method can make active component palladium high degree of dispersion and uniformly be divided in a manner of monoatomic
Cloth is on manganese dioxide surface, without agglomeration.
The preparation method of monatomic palladium catalyst: being 5 by the weight ratio of ammonium sulfate, ammonium persulfate, palladium nitrate and manganese sulfate
~7:2~3:0.05~0.08:1~2 take raw material, add hydromagnetic power to stir to get mixture, then mixture is placed in 120~160
9~14h is reacted at DEG C, is then taken out after its natural cooling, is filtered, washed filtrate to neutrality, black precipitate is obtained, by black
Precipitating drying crushes up to monatomic palladium catalyst Pd/MnO2。
It is preferred in order to improve the performance of catalyst: ammonium sulfate, ammonium persulfate, palladium nitrate and manganese sulfate weight ratio be
5.24~6.24:2.36~2.86:0.066~0.077:1.56~1.81；It is furthermore preferred that ammonium sulfate, ammonium persulfate, palladium nitrate
Weight ratio with manganese sulfate is 5.24~6.08:2.36~2.74:0.066~0.077:1.56~1.81；When ammonium sulfate, over cure
The weight ratio of sour ammonium, palladium nitrate and manganese sulfate is 6.08:2.74:0.077:1.81, at this time monatomic palladium catalyst obtained
Can preferably, when for catalysis oxidation 5-HMF preparation 2,5-FDCA, 5-HMF high conversion rate, the yield of 2,5-FDCA are high, and should
It is best that catalyst carries out repeat performance.
It is preferred: mixture being placed at 140 DEG C and reacts 12h in order to improve monatomic performance of Pd catalyst.
Preferred: black precipitate drying temperature is 120 DEG C, drying time 12h.
The invention solves third technical problem be monatomic palladium catalyst application, will be produced by the present invention single former
For sub- palladium catalyst for catalysis oxidation 5-HMF preparation 2,5-FDCA, method is simple, easy to operate.This method does not need that highly basic is added
(sodium hydroxide, potassium hydroxide etc.).
The method that monatomic palladium catalyst catalysis oxidation 5-HMF prepares 2,5-FDCA, it is characterised in that: by the single former of preparation
The aqueous solution of sub- palladium catalyst, Anhydrous potassium carbonate and 5-HMF mixes, and in oxygen atmosphere, temperature is anti-under the conditions of being 80~110 DEG C
It answers, is made 2,5-FDCA.
Need to use highly basic (sodium hydroxide, potassium hydroxide etc.) during 5-HMF catalytic oxidation in the prior art
Come reduce catalyst active component loss, this method replaces highly basic to provide one for the conversion of 5-HMF with basic salt potassium carbonate
A alkaline environment, due to using highly basic, not avoiding equipment corrosion and problem of environmental pollution caused by using highly basic.
It is preferred in order to improve monatomic performance of Pd catalyst: monatomic palladium catalyst, Anhydrous potassium carbonate and 5-HMF
Weight ratio is 0.9~1.1:3~4:0.7~0.9；It is furthermore preferred that the weight ratio of monatomic palladium catalyst, potassium carbonate and 5-HMF
For 1~1.1:3.35~3.5:0.77~0.8；It is further preferred that the weight of monatomic palladium catalyst, potassium carbonate and 5-HMF
Than for 1.1:3.5:0.8.
It is preferred: oxygen gas flow rate 25ml/min.
Preferred: reaction temperature is 90~110 DEG C；Further preferred reaction temperature is 110 DEG C.
It is preferred: reaction time at least 3h；Preferred reaction time is 5h.
A specific embodiment of the invention is further described below with reference to embodiment, is not therefore limited the present invention
System is among the embodiment described range.
Embodiment 1
The preparation of step 1, catalyst: ammonium sulfate 6.08g, ammonium persulfate 2.74g, palladium nitrate 77mg, manganese sulfate are weighed
Deionized water 43ml is added in reaction kettle in 1.81g.It is put into magneton stirring 10min, is put into reaction kettle after taking out magneton
12h is reacted in 140 DEG C of baking ovens.It is taken out after its natural cooling, filtration washing filtrate to neutrality.Obtained black precipitate is placed in
Dry 12h in 120 DEG C of baking ovens.Blocks of solid is ground into powdery in drying process, it is standby to finally obtain black powder catalyst A1
With.In the catalyst, the content of palladium is 1.5wt%, and manganese dioxide content is 98.5wt%.The scanning electron microscope (SEM) photograph of A1 such as Fig. 3 institute
Show.From figure 3, it can be seen that palladium atom high is dispersed in manganese dioxide surface, and there is no agglomeration.
Step 2, monatomic palladium catalyst prepare 2,5-FDCA for catalysis oxidation 5-HMF: weigh it is above-mentioned prepare urge
In agent 110mg, 5-HMF80mg, Anhydrous potassium carbonate 350mg addition there-necked flask, deionized water 40ml is added, then be passed through flow velocity
It for the oxygen of 25ml/min, and reacts, tests under the different reaction time, the conversion ratio of 5-HMF and 2 under conditions of 110 DEG C,
The yield of 5-FDCA.Reaction result is shown in Table 1 and Fig. 1.
Table 1
| The catalysis oxidation time/h | Conversion ratio/% of 5-HMF | Yield/% of 2,5-FDCA |
| 1 | 38.2 | 17.1 |
| 2 | 64.0 | 42.5 |
| 3 | 98.1 | 85.3 |
| 4 | 100 | 89.2 |
| 5 | 100 | 94.2 |
It will react later catalyst filtration recycling in 5 hours, and re-use 4 times by the method for above-mentioned steps 2, every time
5h is reacted, as a result as shown in Figure 2.4 conversion ratios for measuring 5-HMF are 100%, and 2,5-FDCA yield is respectively
93.8%, 93.2%, 93.0%, 92.2%.
Embodiment 2
The preparation of step 1, catalyst: ammonium sulfate 5.24g, ammonium persulfate 2.36g, palladium nitrate 66mg, manganese sulfate are weighed
Deionized water 37ml is added in reaction kettle in 1.56g.It is put into magneton stirring 10min, is put into reaction kettle after taking out magneton
12h is reacted in 140 DEG C of baking ovens.It is taken out after its natural cooling, filtration washing filtrate to neutrality.By obtained black precipitate as
Dry 12h in 120 DEG C of baking ovens.Blocks of solid is ground into powdery in drying process, it is spare to finally obtain black powder catalyst.
In the catalyst, the content of palladium is 1.42wt%, and the content of manganese dioxide is 98.58wt%.
Step 2, monatomic palladium catalyst prepare 2,5-FDCA for catalysis oxidation 5-HMF: weigh it is above-mentioned prepare urge
In agent 110mg, 5-HMF80mg, Anhydrous potassium carbonate 350mg addition there-necked flask, deionized water 40ml is added.It is passed through flow velocity again
For the oxygen of 25ml/min, and 5h being reacted under conditions of 110 DEG C, the conversion ratio for measuring 5-HMF is 100%, 2,5-FDCA
Yield is 95.1%.Catalyst filtration is recycled, and is re-used according to the above method 4 times, each reaction 5h.Measure 5-HMF
4 conversion ratios be 100%, 2,5-FDCA yield is respectively 94.2%, 94.0%, 93.5%, 90.7%.
Embodiment 3
The preparation of step 1, catalyst: ammonium sulfate 6.24g, ammonium persulfate 2.86g, palladium nitrate 77mg, manganese sulfate are weighed
Deionized water 45ml is added in reaction kettle in 1.67g.It is put into magneton stirring 10min, is put into reaction kettle after taking out magneton
12h is reacted in 140 DEG C of baking ovens.It is taken out after its natural cooling, filtration washing filtrate to neutrality.By obtained black precipitate as
Dry 12h in 120 DEG C of baking ovens.Blocks of solid is ground into powdery in drying process, it is spare to finally obtain black powder catalyst.
In the catalyst, the content of palladium is 1.03wt%, and the content of manganese dioxide is 98.97wt%.
Step 2, monatomic palladium catalyst prepare 2,5-FDCA for catalysis oxidation 5-HMF: weigh it is above-mentioned prepare urge
In agent 100mg, 5-HMF77mg, Anhydrous potassium carbonate 335mg addition there-necked flask, deionized water 39ml is added.It is passed through flow velocity again
For the oxygen of 25ml/min, and 5h is reacted under conditions of 110 DEG C.The conversion ratio for measuring 5-HMF is 98%, 2,5-FDCA production
Rate is 90.1%.
Catalyst filtration is recycled, and is re-used according to the above method 4 times, each reaction 5h.Measure 4 times of 5-HMF
Conversion ratio be respectively 98%, 98.3%, 97.5%, 97.2%, 97.6%, 2,5-FDCA yield is respectively 90.1%,
89.5%, 89.4%, 88.9%.
Embodiment 4
The preparation of step 1, catalyst: ammonium sulfate 5.24g, ammonium persulfate 2.36g, palladium nitrate 66mg, manganese sulfate are weighed
Deionized water 37ml is added in reaction kettle in 1.56g.It is put into magneton stirring 10min, is put into reaction kettle after taking out magneton
14h is reacted in 130 DEG C of baking ovens.It is taken out after its natural cooling, filtration washing filtrate to neutrality.By obtained black precipitate as
Dry 12h in 120 DEG C of baking ovens.Blocks of solid is ground into powdery in drying process, it is spare to finally obtain black powder catalyst.
In the catalyst, the content of palladium is 0.92wt%, and the content of manganese dioxide is 99.08wt%.
Step 2, monatomic palladium catalyst prepare 2,5-FDCA for catalysis oxidation 5-HMF: weigh it is above-mentioned prepare urge
In agent 90mg, 5-HMF 90mg, Anhydrous potassium carbonate 400mg addition there-necked flask, deionized water 40ml is added.It is passed through flow velocity again
For the oxygen of 25ml/min, and 5h is reacted under conditions of 110 DEG C.The conversion ratio of HMF, which is measured, as the yield of 95.8%, FDCA is
86.1%.
Embodiment 5
The preparation of step 1, catalyst: ammonium sulfate 5.24g, ammonium persulfate 2.36g, palladium nitrate 66mg, manganese sulfate are weighed
Deionized water 37ml is added in reaction kettle in 1.56g.It is put into magneton stirring 10min, is put into reaction kettle after taking out magneton
10h is reacted in 150 DEG C of baking ovens.It is taken out after its natural cooling, filtration washing filtrate to neutrality.By obtained black precipitate as
Dry 12h in 120 DEG C of baking ovens.Blocks of solid is ground into powdery in drying process, it is spare to finally obtain black powder catalyst.
In the catalyst, the content of palladium is 1.38wt%, and the content of manganese dioxide is 98.62wt%.
Step 2, monatomic palladium catalyst prepare 2,5-FDCA for catalysis oxidation 5-HMF: weigh it is above-mentioned prepare urge
In agent 110mg, 5-HMF90mg, Anhydrous potassium carbonate 300mg addition there-necked flask, deionized water 40ml is added.It is passed through flow velocity again
For the oxygen of 25ml/min, and 5h is reacted under conditions of 90 DEG C.The conversion ratio for measuring 5-HMF is the yield of 98.6%, FDCA
It is 88.4%.
Claims (10)
1. monatomic palladium catalyst, which is characterized in that the catalyst structure are as follows: active component palladium is in high degree of dispersion and with single original
The mode of son is evenly distributed on manganese dioxide surface；Wherein, the content of palladium is 0.2~3wt%, the content of manganese dioxide is 97~
99.8wt%.
2. the preparation method of monatomic palladium catalyst described in claim 1, it is characterised in that: press ammonium sulfate, ammonium persulfate, nitre
The weight ratio of sour palladium and manganese sulfate is that 5~7:2~3:0.05~0.08:1~2 take raw material, adds water and stirs to obtain mixture, then will
Mixture is placed in 9~14h of reaction at 120~160 DEG C, then cools down, is filtered, washed to neutrality, black precipitate is obtained, by black
Precipitating drying crushes up to monatomic palladium catalyst.
3. the preparation method of monatomic palladium catalyst according to claim 2, it is characterised in that: ammonium sulfate, ammonium persulfate,
The weight ratio of palladium nitrate and manganese sulfate is 5.24~6.24:2.36~2.86:0.066~0.077:1.56~1.81；Preferably,
Ammonium sulfate, ammonium persulfate, palladium nitrate and manganese sulfate weight ratio be 5.24~6.08:2.36~2.74:0.066~0.077:
1.56~1.81；It is furthermore preferred that ammonium sulfate, ammonium persulfate, palladium nitrate and manganese sulfate weight ratio be 6.08:2.74:0.077:
1.81。
4. the preparation method of monatomic palladium catalyst according to claim 2, it is characterised in that: mixture is placed in 140
12h is reacted at DEG C.
5. the preparation method of monatomic palladium catalyst according to claim 2, it is characterised in that: black precipitate drying temperature
It is 120 DEG C, drying time 12h.
6. the method that monatomic palladium catalyst catalysis oxidation 5-HMF prepares 2,5-FDCA, it is characterised in that: by claim 2~5
The aqueous solution mixing of the monatomic palladium catalyst, Anhydrous potassium carbonate and 5-HMF of any one preparation, in oxygen atmosphere, temperature is
It is reacted under the conditions of 80~110 DEG C, is made 2,5-FDCA.
7. the method that monatomic palladium catalyst catalysis oxidation 5-HMF according to claim 6 prepares 2,5-FDCA, feature
Be: the weight ratio of monatomic palladium catalyst, Anhydrous potassium carbonate and 5-HMF is 0.9~1.1:3~4:0.7~0.9；Preferably,
The weight ratio of monatomic palladium catalyst, potassium carbonate and 5-HMF is 1~1.1:3.35~3.5:0.77~0.8；It is furthermore preferred that single
The weight ratio of atom palladium catalyst, potassium carbonate and 5-HMF is 1.1:3.5:0.8.
8. the method that monatomic palladium catalyst catalysis oxidation 5-HMF according to claim 6 prepares 2,5-FDCA, feature
It is: oxygen gas flow rate 25ml/min.
9. the method that monatomic palladium catalyst catalysis oxidation 5-HMF according to claim 6 prepares 2,5-FDCA, feature
Be: reaction temperature is 90~110 DEG C；Preferable reaction temperature is 110 DEG C.
10. the method that monatomic palladium catalyst catalysis oxidation 5-HMF according to claim 6 prepares 2,5-FDCA, special
Sign is: reaction time at least 3h；Preferred reaction time is 5h.
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| Publication number | Priority date | Publication date | Assignee | Title |
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