CN105749946B - A kind of solid base catalyst NH4Al(OH)2CO3, preparation method and its catalyzed conversion glucose method - Google Patents
A kind of solid base catalyst NH4Al(OH)2CO3, preparation method and its catalyzed conversion glucose method Download PDFInfo
- Publication number
- CN105749946B CN105749946B CN201610237172.XA CN201610237172A CN105749946B CN 105749946 B CN105749946 B CN 105749946B CN 201610237172 A CN201610237172 A CN 201610237172A CN 105749946 B CN105749946 B CN 105749946B
- Authority
- CN
- China
- Prior art keywords
- solid base
- base catalyst
- glucose
- mixture
- catalyst
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Classifications
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/584—Recycling of catalysts
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Furan Compounds (AREA)
- Catalysts (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Low-Molecular Organic Synthesis Reactions Using Catalysts (AREA)
Abstract
The invention discloses a kind of solid base catalyst NH4Al(OH)2CO3, preparation method and its catalyzed conversion glucose method.NH4Al(OH)2CO3By using inorganic salt containing aluminium and/or aluminium isopropoxide as silicon source, urea CO (NH2)2Directly synthesized for precipitating reagent without calcining and activating by hydrothermal solution.The preparation method of the solid base catalyst is simple, economic and environment-friendly and recyclable regenerative.When it is applied to catalysis glucose conversion, with solid base NH4Al(OH)2CO3Carry out transforming glucose as solvent for catalyst, the methylimidazole villaumite of 1 butyl of ionic liquid 3 and dimethyl sulfoxide (DMSO) and prepare 5 hydroxymethylfurfurals.The yield that solid base catalyst catalysis glucose conversion prepares 5 hydroxymethylfurfurals is high, and catalyst it is easily separated, it is repeatable utilize, expend low, have a good application prospect.
Description
Technical field
The invention belongs to catalyst preparation and applied technical field, and in particular to a kind of solid base catalyst NH4Al(OH)2CO3, the application process of preparation method and this catalyst in catalysis glucose conversion prepares 5 hydroxymethyl furfural.
Background technology
Warmed as the worsening shortages of fossil energy, global climate are hurried, environmental pollution constantly aggravates, increasing people
Seek a kind of renewable green energy resource.
Among numerous regenerative resources, biomass energy is only reproducible green energy of one kind in addition to fossil energy
Source, the whole world pass through biomass caused by photosynthesis nearly 1.0 × 10 every year11Ton.By biorefinery, biomass energy can be by
Liquid fuel and high negative value chemicals.And as long as the carbohydrate of biomass derived is biomass part, therefore largely
The conversion of biomass derived carbohydrate is devoted in research.
The carbohydrate of biomass derived can obtain a kind of important platform chemicals -5 hydroxymethyl furfural by conversion.It is logical
Various high valuable chemicals can further be prepared by crossing 5 hydroxymethyl furfural, such as:Pass through rehydration, 5-
Hydroxymethylfurfural can be converted into levulic acid;By selective oxidation, 5 hydroxymethyl furfural can be converted into 2,5- furans two
Methanol, 2,5- furans dicarbaldehyde and 2,5- furandicarboxylic acids etc..
The catalyst of catalysis glucose conversion has at present:Traditional inorganic or organic acid, salt, ionic liquid, solid acid are urged
Agent, solid base catalyst.Although traditional inorganic or organic acid can effectively transforming glucose, the corruption to equipment
Erosion is very serious, increases industrial cost, and be also to have very big pollution to environment., caused spent acid is not easy to reclaim, also
It can not recycle.Saline catalyst can also transforming glucose prepare 5 hydroxymethyl furfural, but these catalyst are poisonous not
It is recyclable.Such as CrCl3、AlCl3、ZrCl4Deng.Ionic liquid expensive, it is impossible to it is raw to carry out large-scale industry
Production.Compared to some homogeneous catalysts, the advantage of heterogeneous catalysis is clearly.It is that the hot one kind of the comparison studied recently is urged
Agent, it is easily separated, recyclable, corrosion-free, nontoxic.But there is also some shortcomings, solid catalyst system for homogeneous catalyst
Preparation Method is complicated, and cost is high, and catalytic efficiency does not have the height of homogeneous catalyst.
In catalysis glucose conversion prepares the heterogeneous catalysis of 5 hydroxymethyl furfural, solid acid catalyst account for mainly
Part, because numerous studies prove, acid catalyst is advantageous to glucose and is converted into 5 hydroxymethyl furfural.And solid base is urged
It is also seldom that agent catalysis glucose conversion prepares 5 hydroxymethyl furfural.With solid base NH4Al(OH)2CO3For catalyst, Portugal is catalyzed
Grape sugar prepares 5 hydroxymethyl furfural, is not yet reported that.
The content of the invention
Goal of the invention:In order to overcome the deficiencies in the prior art, the present invention provides a kind of solid base catalyst
NH4Al(OH)2CO3And preparation method thereof, with the aluminum carbonate basic ammonium of simple, economic and environment-friendly acquisition high catalytic efficiency.The present invention
Purpose also reside in and propose the catalyst efficient catalytic glucose conversion method for preparing 5 hydroxymethyl furfural.
Technical scheme:To achieve the above object, the present invention uses following technical scheme:
A kind of solid base catalyst NH4Al(OH)2CO3, solid base catalyst NH4Al(OH)2CO3It is with inorganic salt containing aluminium
And/or aluminium isopropoxide is silicon source, urea CO (NH2)2Directly synthesized for precipitating reagent without calcining and activating by hydrothermal solution.
Preferably, the inorganic salt containing aluminium is selected from AlCl3、Al(NO3)3、Al2(SO4)3、AlCl3·6H2O、 Al
(NO3)3·9H2O、Al2(SO4)3·16H2One or more in O, wherein AlCl3、AlCl3·6H2O is as inorganic salt containing aluminium
Best results.
Above-mentioned solid base catalyst NH4Al(OH)2CO3Preparation method, comprise the following steps:
(1) using as the inorganic salt containing aluminium of silicon source and/or aluminium isopropoxide and CO (NH2)2It is added in deionized water, then
Constantly agitating solution, until becoming homogeneous phase solution;
(2) after the homogeneous phase solution that step (1) obtains becomes clarification, solution is transferred to 100~200mL liners poly- four at once
Reacted among the reactor of PVF, then reactor react into 5~60h at 100~300 DEG C, when reacted between reach and set
Time when, take out reactor, naturally cool to room temperature;
(3) reacted product is collected by filtering, washing after cooling down, 3~48h is finally dried at 60~150 DEG C, i.e.,
Obtain solid base catalyst NH4Al(OH)2CO3。
Preferably, silicon source and CO (NH in the step (1)2)2The ratio between the amount of material be 1-10:1-200.
Invention further provides above-mentioned solid base catalyst NH4Al(OH)2CO3The method of catalyzed conversion glucose, institute
The method of stating comprises the following steps:
(1) first by glucose and the solid base catalyst NH4Al(OH)2CO3It is added in solvent, obtains mixture A;
(2) the mixture A and then by step (1) obtained is quickly transferred in oil bath stirring reaction energetically, after obtaining reaction
Mixture B;
(3) mixture B that step (2) obtains is added into deionized water to be quenched, then with centrifuge with 5000~
20000rpm speed separates 3~15min, collects upper strata hydrolyzate, both obtains 5 hydroxymethyl furfural, product uv-spectrophotometric
Meter is analyzed.
Preferably, reaction dissolvent is 1- butyl -3- methylimidazole villaumites, the one of dimethyl sulfoxide (DMSO) in the step (1)
Kind or the two mixing, the mixed solution effect of wherein 1- butyl -3- methylimidazole villaumites and dimethyl sulfoxide (DMSO) are more excellent.
Preferably, the mass ratio of solid base catalyst and glucose is 3 in the step (1):1.
Preferably, the temperature of oil bath is 60~180 DEG C in the step (2), the time of the stirring reaction is 2~12
h。
Preferably, above-mentioned solid base catalyst NH4Al(OH)2CO3The method of catalyzed conversion glucose, specific steps are such as
Under
(1) first by 0.01~1g glucose and 0.01~5g solid base catalyst NH4Al(OH)2CO3It is added to 0~10
In the solvent of g1- butyl -3- methylimidazole villaumites and 0~10g dimethyl sulfoxide (DMSO)s, mixture A, wherein 1- butyl -3- first are obtained
It is 0 when base imidazoles villaumite and dimethyl sulfoxide (DMSO) difference;
(2) the mixture A and then by step (1) obtained is quickly transferred in 60~180 DEG C of oil baths stirring reaction 2 energetically
~12h, obtain reacted mixture B;
(3) deionized water is added in the liquid for obtaining step (2) to be quenched, then with centrifuge with 5000~
20000rpm speed separates 3~15min, collects upper strata hydrolyzate, both obtains 5 hydroxymethyl furfural, product ultraviolet spectrometry light
Degree meter is analyzed.
Beneficial effect:Compared with prior art, the invention has the advantages that:
(1) the solid base catalyst NH that the present invention is synthesized using hydrothermal method4Al(OH)2CO3Preparation method raw material and technique pole
It is simple, cheap, easily separated, can be recycled, green, there is preferable market application foreground.
(2) this solid base catalyst NH4Al(OH)2CO3When being converted applied to glucose, the production of product 5 hydroxymethyl furfural
Rate is higher and catalyst is easily separated, it is repeatable utilize, expend it is low.
Brief description of the drawings
Fig. 1 is the XRD spectrum of catalyst aluminum carbonate basic ammonium prepared by embodiment 1.
Embodiment
The present invention is further explained with reference to embodiment.Percentage composition in following embodiments is such as without special theory
Bright is weight/mass percentage composition.
Embodiment 1
By 2mmolAlCl3·6H2O and 36mmol CO (NH2)2Be added among 50mL deionized water, then constantly
Ground agitating solution, until becoming homogeneous phase solution.After solution becomes clarification, solution is transferred to 100mL liners at once and gathered
Among the reactor of tetrafluoroethene, then reactor reacted into 36h at 140 DEG C.When the time of setting is reached between when reacted, take
Go out reactor, naturally cool to room temperature.After cooling reacted product is collected by filtering, washing.Finally again by the production of collection
Product dry 24h, i.e. resulting solid base catalyst NH at 100 DEG C4Al(OH)2CO3.The product is subjected to XRD analysis, XRD
Collection of illustrative plates at 2 θ=10~80 ° as shown in figure 1, it can be seen that there is very strong diffraction maximum, all diffraction maximums and alkali formula
The standard card figure of aluminium carbonate ammonium is consistent (JCPDS Card 042-0250), and the composition for illustrating the product is NH4Al(OH)2CO3。
First by 0.1g glucose and 0.3g solid base catalyst NH4Al(OH)2CO3It is added to 1g1- butyl -3- methyl miaows
In the mixed solution of azoles villaumite and 1g dimethyl sulfoxide (DMSO)s, then said mixture is quickly transferred to stir energetically in 120 DEG C of oil baths
Reaction 4h is mixed, obtains reacted mixture.By in resulting liquid add deionized water quenched, then with centrifuge with
10000rpm speed separation 10min, collects upper strata hydrolyzate, both obtains 5 hydroxymethyl furfural, product ultraviolet specrophotometer
Analyzed, the yield of 5 hydroxymethyl furfural is 42.17wt%.
Embodiment 2
By 2mmolAlCl3·6H2O and 54mmolCO (NH2)2Be added among 50mL deionized water, then constantly
Ground agitating solution, until becoming homogeneous phase solution.After solution becomes clarification, solution is transferred to 100mL liners at once and gathered
Among the reactor of tetrafluoroethene, then reactor reacted into 36h at 140 DEG C.When the time of setting is reached between when reacted, take
Go out reactor, naturally cool to room temperature.After cooling reacted product is collected by filtering, washing.Finally again by the production of collection
Product dry 24h, i.e. resulting solid base catalyst NH at 100 DEG C4Al(OH)2CO3。
First by 0.1g glucose and 0.3g solid base catalyst NH4Al(OH)2CO3It is added to 1g1- butyl -3- methyl miaows
In the mixed solution of azoles villaumite and 1g dimethyl sulfoxide (DMSO)s.Then said mixture is quickly transferred to stir energetically in 120 DEG C of oil baths
Reaction 4h is mixed, obtains reacted mixture.By in resulting liquid add deionized water quenched, then with centrifuge with
10000rpm speed separation 10min, collects upper strata hydrolyzate, both obtains 5 hydroxymethyl furfural, product ultraviolet specrophotometer
Analyzed, the yield of 5 hydroxymethyl furfural is 39.31wt%.
Embodiment 3
By 2mmolAlCl3·6H2O and 72mmolCO (NH2)2Be added among 50mL deionized water, then constantly
Ground agitating solution, until becoming homogeneous phase solution.After solution becomes clarification, solution is transferred to 100mL liners at once and gathered
Among the reactor of tetrafluoroethene, then reactor reacted into 36h at 140 DEG C.When the time of setting is reached between when reacted, take
Go out reactor, naturally cool to room temperature.After cooling reacted product is collected by filtering, washing.Finally again by the production of collection
Product dry 24h, i.e. resulting solid base catalyst NH at 100 DEG C4Al(OH)2CO3。
First by 0.1g glucose and 0.3g solid base catalyst NH4Al(OH)2CO3It is added to 1g1- butyl -3- methyl miaows
In the mixed solution of azoles villaumite and 1g dimethyl sulfoxide (DMSO)s.Then said mixture is quickly transferred to stir energetically in 120 DEG C of oil baths
Reaction 4h is mixed, obtains reacted mixture.By in resulting liquid add deionized water quenched, then with centrifuge with
10000rpm speed separation 10min, upper collection upper strata hydrolyzate, both obtains 5 hydroxymethyl furfural, product uv-spectrophotometric
Meter is analyzed, and the yield of 5 hydroxymethyl furfural is 33.51wt%.
Embodiment 4
By 2mmol aluminium isopropoxides C9H21AlO3With 36mmol NH4HCO3Be added among 50mL deionized water, then
Constantly agitating solution, until becoming homogeneous phase solution.After solution becomes clarification, solution is transferred in 100mL at once
Among the reactor of lining teflon, then reactor reacted into 36h at 140 DEG C.The time of setting is reached between when reacted
When, reactor is taken out, naturally cools to room temperature.After cooling reacted product is collected by filtering, washing.It will finally collect again
Product 24h, i.e., resulting solid base catalyst NH are dried at 100 DEG C4Al(OH)2CO3。
First by 0.1g glucose and 0.3g solid base catalyst NH4Al(OH)2CO3It is added to 1g1- butyl -3- methyl miaows
In the mixed solution of azoles villaumite and 1g dimethyl sulfoxide (DMSO)s.Then said mixture is quickly transferred to stir energetically in 120 DEG C of oil baths
Reaction 4h is mixed, obtains reacted mixture.By in resulting liquid add deionized water quenched, then with centrifuge with
10000rpm speed separation 10min, upper collection upper strata hydrolyzate, both obtains 5 hydroxymethyl furfural, product uv-spectrophotometric
Meter is analyzed, and the yield of 5 hydroxymethyl furfural is 35.23wt%.
Embodiment 5
By 2mmol aluminium isopropoxides C9H21AlO3With 36mmol (NH4)2CO3Be added among 50mL deionized water, so
Constantly agitating solution afterwards, until becoming homogeneous phase solution.After solution becomes clarification, solution is transferred to 100mL at once
Among the reactor of inner liner polytetrafluoroethylene, then reactor reacted into 36h at 140 DEG C.Reached between when reacted setting when
Between when, take out reactor, naturally cool to room temperature.After cooling reacted product is collected by filtering, washing.It will finally receive again
The product of collection dries 24h, i.e. resulting solid base catalyst NH at 100 DEG C4Al(OH)2CO3。
First by 0.1g glucose and 0.3g solid base catalyst NH4Al(OH)2CO3It is added to 1g1- butyl -3- methyl miaows
In the mixed solution of azoles villaumite and 1g dimethyl sulfoxide (DMSO)s.Then said mixture is quickly transferred to stir energetically in 120 DEG C of oil baths
Reaction 4h is mixed, obtains reacted mixture.By in resulting liquid add deionized water quenched, then with centrifuge with
10000rpm speed separation 10min, upper collection upper strata hydrolyzate, both obtains 5 hydroxymethyl furfural, product uv-spectrophotometric
Meter is analyzed, and the yield of 5 hydroxymethyl furfural is 32.19wt%.
Embodiment 6
Solid base catalyst NH4Al(OH)2CO3Preparation method with embodiment 1, simply by silicon source AlCl3·6H2O is changed into
C9H21AlO3.Prepared with the catalyst that will be prepared applied to glucose conversion in 5 hydroxymethyl furfural experiment.By 0.1 g grapes
The solid base catalyst NH of sugar and 0.3g4Al(OH)2CO3It is added to 1g1- butyl -3- methylimidazole villaumites and 1 g dimethyl is sub-
In the mixed solution of sulfone.Then said mixture is quickly transferred in 120 DEG C of oil baths stirring reaction 4h energetically, reacted
Mixture afterwards.Quenched deionized water is added in resulting liquid, then with centrifuge with 10000rpm speed point
From 10min, upper collection upper strata hydrolyzate, 5 hydroxymethyl furfural is both obtained, product is analyzed with ultraviolet specrophotometer, 5- hydroxyl first
The yield of base furfural is 37.25wt%.From experimental result as can be seen that using C9H21AlO3It can be and compare as silicon source yield
Considerable, and C9H21AlO3It is using Al atoms as the octahedral structure of hexa-coordinate, potentially contributes to form catalyst n H4Al
(OH)2CO3。
Embodiment 7
Solid base catalyst NH4Al(OH)2CO3Preparation method with embodiment 1.By 0.1g glucose and 0.1g solid
Base catalyst NH4Al(OH)2CO3It is added in the mixed solution of 1g1- butyl -3- methylimidazole villaumites and 1g dimethyl sulfoxide (DMSO)s.
Then said mixture is quickly transferred in 120 DEG C of oil baths stirring reaction 4h energetically, obtains reacted mixture.By gained
To liquid in add deionized water and quenched, then 10min is separated with 10000rpm speed with centrifuge, collects upper strata
Hydrolyzate, 5 hydroxymethyl furfural is both obtained, product is analyzed with ultraviolet specrophotometer, and the yield of 5 hydroxymethyl furfural is
29.04wt%.
Embodiment 8
Solid base catalyst NH4Al(OH)2CO3Preparation method with embodiment 1.By 0.1g glucose and 0.2g solid
Base catalyst NH4Al(OH)2CO3It is added in the mixed solution of 1g1- butyl -3- methylimidazole villaumites and 1g dimethyl sulfoxide (DMSO)s.
Then said mixture is quickly transferred in 120 DEG C of oil baths stirring reaction 4h energetically, obtains reacted mixture.By gained
To liquid in add deionized water and quenched, then 10min is separated with 10000rpm speed with centrifuge, collects upper strata
Hydrolyzate, 5 hydroxymethyl furfural is both obtained, product is analyzed with ultraviolet specrophotometer, and the yield of 5 hydroxymethyl furfural is
39.60wt%.
Embodiment 9
Solid base catalyst NH4Al(OH)2CO3Preparation method with embodiment 1.By 0.1g glucose and 0.4g solid
Base catalyst NH4Al(OH)2CO3It is added in the mixed solution of 1g1- butyl -3- methylimidazole villaumites and 1g dimethyl sulfoxide (DMSO)s.
Then said mixture is quickly transferred in 120 DEG C of oil baths stirring reaction 4h energetically, obtains reacted mixture.By gained
To liquid in add deionized water and quenched, then 10min is separated with 10000rpm speed with centrifuge, collects upper strata
Hydrolyzate, 5 hydroxymethyl furfural is both obtained, product is analyzed with ultraviolet specrophotometer, and the yield of 5 hydroxymethyl furfural is
35.45wt%.
Embodiment 10
Solid base catalyst NH4Al(OH)2CO3Preparation method with embodiment 1.By 0.1g glucose and 0.5g solid
Base catalyst NH4Al(OH)2CO3It is added in the mixed solution of 1g1- butyl -3- methylimidazole villaumites and 1g dimethyl sulfoxide (DMSO)s.
Then said mixture is quickly transferred in 120 DEG C of oil baths stirring reaction 4h energetically, obtains reacted mixture.By gained
To liquid in add deionized water and quenched, then 10min is separated with 10000rpm speed with centrifuge, collects upper strata
Hydrolyzate, 5 hydroxymethyl furfural is both obtained, product is analyzed with ultraviolet specrophotometer, and the yield of 5 hydroxymethyl furfural is
28.81wt%.
Embodiment 11
Solid base catalyst NH4Al(OH)2CO3Preparation method with embodiment 1.By 0.1g glucose and 0.3g solid
Base catalyst NH4Al(OH)2CO3It is added in the mixed solution of 1g1- butyl -3- methylimidazole villaumites and 1g dimethyl sulfoxide (DMSO)s.
Then said mixture is quickly transferred in 140 DEG C of oil baths stirring reaction 4h energetically, obtains reacted mixture.By gained
To liquid in add deionized water and quenched, then 10min is separated with 10000rpm speed with centrifuge, collects upper strata
Hydrolyzate, 5 hydroxymethyl furfural is both obtained, product is analyzed with ultraviolet specrophotometer, and the yield of 5 hydroxymethyl furfural is
25.66wt%.
Embodiment 12
Solid base catalyst NH prepared by embodiment 14Al(OH)2CO3Recycling.
Solid base catalyst NH4Al(OH)2CO3NH4 +Easily it is lost in, therefore catalyst needs after separation, washing are dried
Again could be recycled by ammonia treatment.Concretely comprise the following steps:By the solid base catalyst NH after separation4Al(OH)2CO3Immersion
In 25wt% concentrated ammonia liquors, 24h is stirred energetically.Then refilter, wash 10 times, it is left back that 24h is dried at 100 DEG C.Finally use
The catalyst of this circulation is catalyzed glucose conversion under the conditions of same as Example 1, and the yield for obtaining 5 hydroxymethyl furfural is
44.22wt%.The circulate operation of same catalyst, the yield results of 5 hydroxymethyl furfural are as shown in table 1.Can from table 1
Go out, the catalyst all remains the yield of the high 5- hydroxymethylfurfurals of comparison in 5 circulations.
NH prepared by the embodiment 1 of table 14Al(OH)2CO3Influence of the access times to 5 hydroxymethyl furfural yield
Catalyst access times | 5 hydroxymethyl furfural yield (wt%) |
1 | 42.17 |
2 | 44.22 |
3 | 42.05 |
4 | 41.23 |
5 | 40.37 |
Above description is some optimal modes and other embodiment for implementing the present invention, simply to the skill of the present invention
Explanation example effect is played in art design, and it is not intended to limit the scope of the present invention, and those skilled in the art are not departing from
In the spirit and scope of technical solution of the present invention, modify and equivalent substitution, all should fall within the scope and spirit of the invention.
Claims (6)
- A kind of 1. solid base catalyst NH4Al(OH)2CO3The method of catalyzed conversion glucose, it is characterised in that:Including following step Suddenly:(1) first by glucose and solid base catalyst NH4Al(OH)2CO3It is added in solvent, obtains mixture A;The solid Base catalyst NH4Al(OH)2CO3It is using inorganic salt containing aluminium and/or aluminium isopropoxide as silicon source, urea CO (NH2)2Need not for precipitating reagent Calcining and activating is directly synthesized by hydrothermal solution;(2) the mixture A and then by step (1) obtained is quickly transferred in oil bath stirring reaction energetically, obtains reacted mixed Compound B;(3) the mixture B that step (2) obtains is added into deionized water to be quenched, then with centrifuge with 5000~20000rpm Speed separate 3~15min, collect upper strata hydrolyzate, both 5 hydroxymethyl furfural, product divided with ultraviolet specrophotometer Analysis.
- 2. solid base catalyst NH according to claim 14Al(OH)2CO3The method of catalyzed conversion glucose, its feature It is:Solvent is 1- butyl -3- methylimidazole villaumites, the mixing of the one or both of dimethyl sulfoxide (DMSO) in the step (1).
- 3. solid base catalyst NH according to claim 14Al(OH)2CO3The method of catalyzed conversion glucose, its feature It is:The mass ratio of solid base catalyst and glucose is 3: 1 in the step (1).
- 4. solid base catalyst NH according to claim 14Al(OH)2CO3The method of catalyzed conversion glucose, its feature It is:The temperature of oil bath is 60~180 DEG C in the step (2), and the time of the stirring reaction is 2~12h.
- 5. according to the solid base catalyst NH described in claim any one of 1-44Al(OH)2CO3The side of catalyzed conversion glucose Method, it is characterised in that:(1) first by 0.01~1g glucose and 0.01~5g solid base catalyst NH4Al(OH)2CO3It is added to 0~10g1- fourths In the solvent of base -3- methylimidazole villaumites and 0~10g dimethyl sulfoxide (DMSO)s, mixture A, wherein 1- butyl -3- methylimidazoles are obtained It is 0 when villaumite and dimethyl sulfoxide (DMSO) difference;(2) the mixture A and then by step (1) obtained is quickly transferred in 60~180 DEG C of oil baths 2~12h of stirring reaction energetically, Obtain reacted mixture B;(3) deionized water is added in the liquid for obtaining step (2) to be quenched, then with centrifuge with 5000~20000rpm's Speed separates 3~15min, collects upper strata hydrolyzate, both obtains 5 hydroxymethyl furfural, and product is divided with ultraviolet specrophotometer Analysis.
- 6. solid base catalyst NH according to claim 14Al(OH)2CO3The method of catalyzed conversion glucose, its feature It is:The inorganic salt containing aluminium is selected from AlCl3、Al(NO3)3、Al2(SO4)3、AlCl3·6H2O、Al(NO3)3·9H2O、Al2 (SO4)3·16H2One or more in O.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN201610237172.XA CN105749946B (en) | 2016-04-15 | 2016-04-15 | A kind of solid base catalyst NH4Al(OH)2CO3, preparation method and its catalyzed conversion glucose method |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN201610237172.XA CN105749946B (en) | 2016-04-15 | 2016-04-15 | A kind of solid base catalyst NH4Al(OH)2CO3, preparation method and its catalyzed conversion glucose method |
Publications (2)
Publication Number | Publication Date |
---|---|
CN105749946A CN105749946A (en) | 2016-07-13 |
CN105749946B true CN105749946B (en) | 2018-02-13 |
Family
ID=56333971
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
CN201610237172.XA Active CN105749946B (en) | 2016-04-15 | 2016-04-15 | A kind of solid base catalyst NH4Al(OH)2CO3, preparation method and its catalyzed conversion glucose method |
Country Status (1)
Country | Link |
---|---|
CN (1) | CN105749946B (en) |
Families Citing this family (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN108610311B (en) * | 2018-05-30 | 2021-12-10 | 盐城工学院 | Method for preparing 5-hydroxymethylfurfural by using boehmite to catalyze glucose at low temperature |
CN113845552B (en) * | 2020-11-06 | 2024-01-05 | 南开大学 | Method for catalyzing glucose to isomerise into fructose by using solid base |
Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN102618932A (en) * | 2012-03-31 | 2012-08-01 | 合肥工业大学 | Method for preparing basic ammonium aluminum carbonate hydroxide whisker and aluminum oxide whisker co-production liquid sodium silicate from bentonite |
CN103303949A (en) * | 2013-05-23 | 2013-09-18 | 北京化工大学 | Vegetable-sponge-shaped hydrotalcite-like compound and preparation method thereof |
Family Cites Families (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US7880049B2 (en) * | 2006-06-06 | 2011-02-01 | Wisconsin Alumni Research Foundation | Production of liquid alkanes in the jet fuel range (C8-C15) from biomass-derived carbohydrates |
-
2016
- 2016-04-15 CN CN201610237172.XA patent/CN105749946B/en active Active
Patent Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN102618932A (en) * | 2012-03-31 | 2012-08-01 | 合肥工业大学 | Method for preparing basic ammonium aluminum carbonate hydroxide whisker and aluminum oxide whisker co-production liquid sodium silicate from bentonite |
CN103303949A (en) * | 2013-05-23 | 2013-09-18 | 北京化工大学 | Vegetable-sponge-shaped hydrotalcite-like compound and preparation method thereof |
Non-Patent Citations (2)
Title |
---|
An overview of dehydration, aldol-condensation and hydrogenation processes for production of liquid alkanes from biomass-derived carbohydrates;Juben N.Chheda, James A.Dumesic;《Catalysis Today》;20070107;第127卷;59-70 * |
固体酸碱催化葡萄糖制备5-羟甲基糠醛;陈文文,李春喜;《中国科技论文》;20130630;第8卷(第6期);549-552 * |
Also Published As
Publication number | Publication date |
---|---|
CN105749946A (en) | 2016-07-13 |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
CN106215951B (en) | A kind of core-shell structure magnetic carbon-based solid acid catalyst and preparation method thereof and application during lignocellulosic hydrolysis and saccharification | |
CN104117367B (en) | A kind of BiOBr/RGO composite aerogel and its preparation method and application | |
CN102923791A (en) | Method for preparing multi-tunnel cobaltosic oxide flower-like microspheres by solvothermal method | |
CN108940313A (en) | A kind of biomass carbon based solid acid catalyst and its preparation method and application | |
CN103694203B (en) | Method of catalyzing fructose by cellulose base sulfonic acid catalyst to prepare 5-hydroxymethyl furfural | |
CN105879902A (en) | Preparation method for molecular sieve catalyst of sugar conversion preparation of lactic acid and lactate | |
CN105749946B (en) | A kind of solid base catalyst NH4Al(OH)2CO3, preparation method and its catalyzed conversion glucose method | |
CN100551903C (en) | Utilize the ion liquid abstraction method from waste water, to reclaim the method for dimethyl formamide | |
CN109261202A (en) | A kind of catalyst and its preparation method and application preparing isobide for sorb dehydration of alcohols | |
CN110004756B (en) | Method for separating components of wood fiber biomass | |
CN101773840A (en) | Method for hydrothermal synthesis of carbon-silicon composite solid acid catalyst | |
CN105820052B (en) | Utilize the method for Supported on Zeolite catalyst preparation butyl acetate | |
CN104383904A (en) | Method for preparing 5-hydroxymethylfurfural from mesoporous self-assembly sulfonated nano-zirconia catalytic fructose | |
CN108610311B (en) | Method for preparing 5-hydroxymethylfurfural by using boehmite to catalyze glucose at low temperature | |
CN109675550A (en) | A kind of molybdenum-boron/sepiolite catalyst and its preparation method and application | |
CN106166499A (en) | A kind of method that in green solvent system, catalysis fibre element converts preparation 5 Hydroxymethylfurfural | |
CN110092795A (en) | A kind of preparation method of isobide | |
CN102671712A (en) | Preparation method of novel solid superacid catalyst and application thereof in catalysis of microcrystalline cellulose for synthesis of levulinic acid | |
CN102850303B (en) | New application and using method of mesoporous solid acid catalyst | |
CN104624242B (en) | A kind of biodiesel synthesis acidic ion liquid immobilized AlCl_3 catalyst and preparation method thereof | |
CN106831391A (en) | The method that chemicals is prepared by microalgae Direct Hydrothermal oxidation | |
CN102993131B (en) | Method for preparing cyclohexene oxide by cyclization of o-chlorocyclohexanol | |
CN110483678A (en) | A kind of catalyst and its preparation method and application preparing isobide for sorb dehydration of alcohols | |
CN103130755B (en) | Method for preparing furfural through catalytic conversion of xylose by acid photocatalyst under ultraviolet light | |
CN108864030A (en) | A method of carbon dioxide synthesizing annular carbonate is catalyzed with new catalyst |
Legal Events
Date | Code | Title | Description |
---|---|---|---|
C06 | Publication | ||
PB01 | Publication | ||
C10 | Entry into substantive examination | ||
SE01 | Entry into force of request for substantive examination | ||
GR01 | Patent grant | ||
GR01 | Patent grant |