CN108863995A - The high-efficiency environment friendly preparation method of 2- methylfuran - Google Patents
The high-efficiency environment friendly preparation method of 2- methylfuran Download PDFInfo
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- CN108863995A CN108863995A CN201810625660.7A CN201810625660A CN108863995A CN 108863995 A CN108863995 A CN 108863995A CN 201810625660 A CN201810625660 A CN 201810625660A CN 108863995 A CN108863995 A CN 108863995A
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D307/00—Heterocyclic compounds containing five-membered rings having one oxygen atom as the only ring hetero atom
- C07D307/02—Heterocyclic compounds containing five-membered rings having one oxygen atom as the only ring hetero atom not condensed with other rings
- C07D307/34—Heterocyclic compounds containing five-membered rings having one oxygen atom as the only ring hetero atom not condensed with other rings having two or three double bonds between ring members or between ring members and non-ring members
- C07D307/36—Heterocyclic compounds containing five-membered rings having one oxygen atom as the only ring hetero atom not condensed with other rings having two or three double bonds between ring members or between ring members and non-ring members with only hydrogen atoms or radicals containing only hydrogen and carbon atoms, directly attached to ring carbon atoms
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- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/72—Copper
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Abstract
The invention discloses the high-efficiency environment friendly preparation methods of 2- methylfuran, specifically include following steps：Copper nitrate, aluminum nitrate are dissolved in deionized water first, citric acid solution obtained solution A is added, is then made using sol-gal process and contains silica solution, then solution A is added to containing in silica solution, and ammonia precipitation process is added, catalyst is made；Catalyst obtained is placed in autoclave by highest, and furfural and isopropanol are added in autoclave, it is passed through hydrogen 5min in advance into autoclave, it then proceedes to be passed through hydrogen, be reacted at 2-3MPa, 200-280 DEG C, it is cooled to room temperature after reaction, filtering removes catalyst, and 2- methylfuran is made.This method is easy to operate, at low cost, and target product yield is high.
Description
Technical field：
The present invention relates to organic synthesis fields, are specifically related to the high-efficiency environment friendly preparation method of 2- methylfuran.
Background technique：
Furfural is as a kind of reproducible biomass energy, the carbohydrate dehydration preparation extracted by various crops.Currently,
The furfural amount that China extracts from biomass every year is about 2.8 × 105T, is mainly used for plus hydrogen prepares furfuryl alcohol (FOL), 2- methyl
A series of derivatives such as furans (2-MF), 2- methyltetrahydrofuran (MTHF), tetrahydrofurfuryl alcohol (THFA), 1- amylalcohol (1-pentanol)
Object.2- methylfuran is widely used in medical synthesis as one of most important product of furfural hydrogenation, in addition, due to its Gaoxin
Alkane value is considered as the substitute of gasoline.
2- methylfuran is important the intermediate of organic matter, medicine synthesis, is widely used in medicine, pesticide and macromolecule
Field, 2- methylfuran add the 2- methyltetrahydrofuran obtained after hydrogen to be even more the important organic solvent of chemical industry.With the country
The development in the fields such as outer medicine and pesticide, the demand of 2- methylfuran product sharply increase, and the market prospects of the product are opened
It is wealthy, but market competition is growing more intense, and energy-saving and emission-reduction and reduction unit consumption are imperative.
Chinese patent (CN201110435732.X) discloses a kind of preparation method of 2- methylfuran, and this method includes：
Under the conditions of selective hydrogenation, in the presence of hydrogenation catalyst, gas phase furfural and hydrogen are connect in hydrogenator
Touching carries out hydrogenation reaction, and reaction product is condensed to and carried out the separation of organic phase and water phase, obtained organic phase is sent to essence
It evaporates progress rectifying in tower and obtains 2- methylfuran, wherein will be by being released at least partly in hydrogenation process by heat exchange
Heat takes out the heat source as tower bottom of rectifying tower.Low energy consumption for this method, energy conservation and environmental protection.
Summary of the invention：
The object of the present invention is to provide the high-efficiency environment friendly preparation methods of 2- methylfuran, and this method is easy to operate, and target produces
Object high income.
To achieve the above object, the present invention uses following technical scheme：
The high-efficiency environment friendly preparation method of 2- methylfuran, includes the following steps：
(1) copper nitrate, aluminum nitrate are dissolved in stirring to solid in deionized water to dissolve, mixed liquor is made；Into mixed liquor
Citric acid solution is added, is stirred, obtained solution A；
(2) ethyl alcohol and hexamethylene are mixed evenly, oleic acid, triethylamine is then added, after being stirred, is finally added dropwise
Ethyl orthosilicate is transferred in reaction kettle after being stirred and reacts 20h at 150 DEG C, after reaction, siliceous hexamethylene is made
Alkane colloidal sol；
(3) solution A made from step (1) is added drop-wise to hexamethylene colloidal sol siliceous made from step (2), is stirred when being added dropwise
It mixes, ammonia precipitation process is then added dropwise after being added dropwise, is filtered after precipitating, and is successively washed and is sunk with deionized water, dehydrated alcohol
It forms sediment, it is dry, catalyst is made；
(4) catalyst obtained above is placed in autoclave, and furfural and isopropanol is added to reaction under high pressure
In kettle, it is passed through hydrogen 5min in advance into autoclave, then proceedes to be passed through hydrogen, it is anti-at 2-3MPa, 200-280 DEG C
It answers, is cooled to room temperature after reaction, filter, remove catalyst, 2- methylfuran is made.
As a preferred embodiment of the above solution, in step (1), in mixed liquor, aluminum ions concentration is 3-5mol/L, copper ion
Concentration is 2-6mol/L.
As a preferred embodiment of the above solution, in step (1), the mass concentration of the citric acid solution is 10-20%.
As a preferred embodiment of the above solution, in step (1), the molar ratio of the citric acid and copper nitrate is 1：(3-7).
As a preferred embodiment of the above solution, in step (2), the ethyl alcohol, hexamethylene, oleic acid, triethylamine, ethyl orthosilicate
Volume ratio is 1:50:0.5:1:1.
As a preferred embodiment of the above solution, in step (2), the rate of addition of the ethyl orthosilicate is 1-3mL/min.
As a preferred embodiment of the above solution, in step (3), the rate of addition of solution A is 2-5ml/L.
As a preferred embodiment of the above solution, in step (3), the catalyst, the mass ratio of copper oxide and silica is (2-
6)：1.
As a preferred embodiment of the above solution, in step (4), the catalyst：The mass ratio of furfural is (0.01-0.03)：4.
As a preferred embodiment of the above solution, in step (4), the time of the reaction is 2-10h.
The invention has the advantages that：
Catalyst produced by the present invention is using copper oxide and aluminium oxide as active component, using silica as carrier, and in order to mention
The activity of high catalyst is soluble in water first using copper nitrate, aluminum nitrate as raw material during preparation, and lemon is then added
Acid solution, obtained solution A；Then siliceous hexamethylene colloidal sol is made using sol-gal process；
Then solution A is added drop-wise to certain speed containing in silica solution, by adjusting the rate of addition of solution A, to control
The rate of addition of precipitating is made, catalyst activity obtained is high, and porosity is big, can effective catalytic hydrogenation reaction.It is of the invention public
The method opened is easy to operate, and preparation cost is low, and target product yield is high.
Specific embodiment：
In order to better understand the present invention, below by embodiment, the present invention is further described, and embodiment is served only for solving
The present invention is released, any restriction will not be constituted to the present invention.
Embodiment 1
The high-efficiency environment friendly preparation method of 2- methylfuran, includes the following steps：
(1) copper nitrate, aluminum nitrate are dissolved in stirring to solid in deionized water to dissolve, mixed liquor is made；Into mixed liquor
Citric acid solution is added, is stirred, obtained solution A；Wherein, in mixed liquor, aluminum ions concentration is 3mol/L, copper ion
Concentration is 2mol/L；The mass concentration of citric acid solution is 10%；The molar ratio of citric acid and copper nitrate is 1：3；
(2) ethyl alcohol and hexamethylene are mixed evenly, oleic acid, triethylamine is then added, after being stirred, is finally added dropwise
Ethyl orthosilicate is transferred in reaction kettle after being stirred and reacts 20h at 150 DEG C, after reaction, siliceous hexamethylene is made
Alkane colloidal sol；Wherein, the rate of addition of the ethyl orthosilicate is 1mL/min；
(3) solution A made from step (1) is added drop-wise to hexamethylene colloidal sol siliceous made from step (2), is stirred when being added dropwise
It mixes, ammonia precipitation process is then added dropwise after being added dropwise, is filtered after precipitating, and is successively washed and is sunk with deionized water, dehydrated alcohol
It forms sediment, it is dry, catalyst is made；Wherein, the rate of addition of solution A is 2ml/L；The catalyst, copper oxide and silica
Mass ratio is 2：1；
(4) catalyst obtained above is placed in autoclave, and furfural and isopropanol is added to reaction under high pressure
In kettle, it is passed through hydrogen 5min in advance into autoclave, then proceedes to be passed through hydrogen, 2h is reacted at 2MPa, 200 DEG C, instead
It is cooled to room temperature, filters after answering, remove catalyst, 2- methylfuran is made；Wherein, the catalyst：The quality of furfural
Than being 0.01：4.The yield of 2- methylfuran is 97.5%.
Embodiment 2
The high-efficiency environment friendly preparation method of 2- methylfuran, includes the following steps：
(1) copper nitrate, aluminum nitrate are dissolved in stirring to solid in deionized water to dissolve, mixed liquor is made；Into mixed liquor
Citric acid solution is added, is stirred, obtained solution A；Wherein, in mixed liquor, aluminum ions concentration is 4.6mol/L, copper ion
Concentration be 5.5mol/L；The mass concentration of citric acid solution is 20%；The molar ratio of citric acid and copper nitrate is 1：7；
(2) ethyl alcohol and hexamethylene are mixed evenly, oleic acid, triethylamine is then added, after being stirred, is finally added dropwise
Ethyl orthosilicate is transferred in reaction kettle after being stirred and reacts 20h at 150 DEG C, after reaction, siliceous hexamethylene is made
Alkane colloidal sol；Wherein, the rate of addition of the ethyl orthosilicate is 2.5mL/min；
(3) solution A made from step (1) is added drop-wise to hexamethylene colloidal sol siliceous made from step (2), is stirred when being added dropwise
It mixes, ammonia precipitation process is then added dropwise after being added dropwise, is filtered after precipitating, and is successively washed and is sunk with deionized water, dehydrated alcohol
It forms sediment, it is dry, catalyst is made；Wherein, the rate of addition of solution A is 4.5ml/L；The catalyst, copper oxide and silica
Mass ratio be 5.5：1；
(4) catalyst obtained above is placed in autoclave, and furfural and isopropanol is added to reaction under high pressure
In kettle, it is passed through hydrogen 5min in advance into autoclave, then proceedes to be passed through hydrogen, 5h is reacted at 3MPa, 270 DEG C, instead
It is cooled to room temperature, filters after answering, remove catalyst, 2- methylfuran is made；Wherein, the catalyst：The quality of furfural
Than being 0.03：4.The yield of 2- methylfuran is 96.9%.
Embodiment 3
The high-efficiency environment friendly preparation method of 2- methylfuran, includes the following steps：
(1) copper nitrate, aluminum nitrate are dissolved in stirring to solid in deionized water to dissolve, mixed liquor is made；Into mixed liquor
Citric acid solution is added, is stirred, obtained solution A；Wherein, in mixed liquor, aluminum ions concentration is 3.5mol/L, copper ion
Concentration be 3mol/L；The mass concentration of citric acid solution is 12%；The molar ratio of citric acid and copper nitrate is 1：4；
(2) ethyl alcohol and hexamethylene are mixed evenly, oleic acid, triethylamine is then added, after being stirred, is finally added dropwise
Ethyl orthosilicate is transferred in reaction kettle after being stirred and reacts 20h at 150 DEG C, after reaction, siliceous hexamethylene is made
Alkane colloidal sol；Wherein, the rate of addition of the ethyl orthosilicate is 1.5mL/min；
(3) solution A made from step (1) is added drop-wise to hexamethylene colloidal sol siliceous made from step (2), is stirred when being added dropwise
It mixes, ammonia precipitation process is then added dropwise after being added dropwise, is filtered after precipitating, and is successively washed and is sunk with deionized water, dehydrated alcohol
It forms sediment, it is dry, catalyst is made；Wherein, the rate of addition of solution A is 3ml/L；The catalyst, copper oxide and silica
Mass ratio is 3：1；
(4) catalyst obtained above is placed in autoclave, and furfural and isopropanol is added to reaction under high pressure
In kettle, it is passed through hydrogen 5min in advance into autoclave, then proceedes to be passed through hydrogen, reacts 4h at 2.2MPa, 220 DEG C,
It is cooled to room temperature, filters after reaction, remove catalyst, 2- methylfuran is made；Wherein, the catalyst：The matter of furfural
Amount is than being 0.015：4.The yield of 2- methylfuran is 97.5%.
Embodiment 4
The high-efficiency environment friendly preparation method of 2- methylfuran, includes the following steps：
(1) copper nitrate, aluminum nitrate are dissolved in stirring to solid in deionized water to dissolve, mixed liquor is made；Into mixed liquor
Citric acid solution is added, is stirred, obtained solution A；Wherein, in mixed liquor, aluminum ions concentration is 4mol/L, copper ion
Concentration is 4mol/L；The mass concentration of citric acid solution is 14%；The molar ratio of citric acid and copper nitrate is 1：5；
(2) ethyl alcohol and hexamethylene are mixed evenly, oleic acid, triethylamine is then added, after being stirred, is finally added dropwise
Ethyl orthosilicate is transferred in reaction kettle after being stirred and reacts 20h at 150 DEG C, after reaction, siliceous hexamethylene is made
Alkane colloidal sol；Wherein, the rate of addition of the ethyl orthosilicate is 2mL/min；
(3) solution A made from step (1) is added drop-wise to hexamethylene colloidal sol siliceous made from step (2), is stirred when being added dropwise
It mixes, ammonia precipitation process is then added dropwise after being added dropwise, is filtered after precipitating, and is successively washed and is sunk with deionized water, dehydrated alcohol
It forms sediment, it is dry, catalyst is made；Wherein, the rate of addition of solution A is 3.5ml/L；The catalyst, copper oxide and silica
Mass ratio be 4：1；
(4) catalyst obtained above is placed in autoclave, and furfural and isopropanol is added to reaction under high pressure
In kettle, it is passed through hydrogen 5min in advance into autoclave, then proceedes to be passed through hydrogen, reacts 6h at 2.4MPa, 240 DEG C,
It is cooled to room temperature, filters after reaction, remove catalyst, 2- methylfuran is made；Wherein, the catalyst：The matter of furfural
Amount is than being 0.02：4.The yield of 2- methylfuran is 98.5%.
Embodiment 5
The high-efficiency environment friendly preparation method of 2- methylfuran, includes the following steps：
(1) copper nitrate, aluminum nitrate are dissolved in stirring to solid in deionized water to dissolve, mixed liquor is made；Into mixed liquor
Citric acid solution is added, is stirred, obtained solution A；Wherein, in mixed liquor, aluminum ions concentration is 4.5mol/L, copper ion
Concentration be 5mol/L；The mass concentration of citric acid solution is 16%；The molar ratio of citric acid and copper nitrate is 1：6；
(2) ethyl alcohol and hexamethylene are mixed evenly, oleic acid, triethylamine is then added, after being stirred, is finally added dropwise
Ethyl orthosilicate is transferred in reaction kettle after being stirred and reacts 20h at 150 DEG C, after reaction, siliceous hexamethylene is made
Alkane colloidal sol；Wherein, the rate of addition of the ethyl orthosilicate is 2mL/min；
(3) solution A made from step (1) is added drop-wise to hexamethylene colloidal sol siliceous made from step (2), is stirred when being added dropwise
It mixes, ammonia precipitation process is then added dropwise after being added dropwise, is filtered after precipitating, and is successively washed and is sunk with deionized water, dehydrated alcohol
It forms sediment, it is dry, catalyst is made；Wherein, the rate of addition of solution A is 4ml/L；The catalyst, copper oxide and silica
Mass ratio is 5：1；
(4) catalyst obtained above is placed in autoclave, and furfural and isopropanol is added to reaction under high pressure
In kettle, it is passed through hydrogen 5min in advance into autoclave, then proceedes to be passed through hydrogen, reacts 7h at 2.6MPa, 260 DEG C,
It is cooled to room temperature, filters after reaction, remove catalyst, 2- methylfuran is made；Wherein, the catalyst：The matter of furfural
Amount is than being 0.02：4.The yield of 2- methylfuran is 99.0%.
Embodiment 6
The high-efficiency environment friendly preparation method of 2- methylfuran, includes the following steps：
(1) copper nitrate, aluminum nitrate are dissolved in stirring to solid in deionized water to dissolve, mixed liquor is made；Into mixed liquor
Citric acid solution is added, is stirred, obtained solution A；Wherein, in mixed liquor, aluminum ions concentration is 5mol/L, copper ion
Concentration is 6mol/L；The mass concentration of citric acid solution is 20%；The molar ratio of citric acid and copper nitrate is 1：7；
(2) ethyl alcohol and hexamethylene are mixed evenly, oleic acid, triethylamine is then added, after being stirred, is finally added dropwise
Ethyl orthosilicate is transferred in reaction kettle after being stirred and reacts 20h at 150 DEG C, after reaction, siliceous hexamethylene is made
Alkane colloidal sol；Wherein, the rate of addition of the ethyl orthosilicate is 3mL/min；
(3) solution A made from step (1) is added drop-wise to hexamethylene colloidal sol siliceous made from step (2), is stirred when being added dropwise
It mixes, ammonia precipitation process is then added dropwise after being added dropwise, is filtered after precipitating, and is successively washed and is sunk with deionized water, dehydrated alcohol
It forms sediment, it is dry, catalyst is made；Wherein, the rate of addition of solution A is 5ml/L；The catalyst, copper oxide and silica
Mass ratio is 6：1；
(4) catalyst obtained above is placed in autoclave, and furfural and isopropanol is added to reaction under high pressure
In kettle, it is passed through hydrogen 5min in advance into autoclave, then proceedes to be passed through hydrogen, 10h is reacted at 3MPa, 280 DEG C, instead
It is cooled to room temperature, filters after answering, remove catalyst, 2- methylfuran is made；Wherein, the catalyst：The quality of furfural
Than being 0.03：4.The yield of 2- methylfuran is 98%.
Comparative example
The high-efficiency environment friendly preparation method of 2- methylfuran, includes the following steps：
(1) copper nitrate, aluminum nitrate are dissolved in stirring to solid in deionized water to dissolve, mixed liquor is made；Into mixed liquor
Citric acid solution is added, is stirred, obtained solution A；Wherein, in mixed liquor, aluminum ions concentration is 5mol/L, copper ion
Concentration is 6mol/L；The mass concentration of citric acid solution is 20%；The molar ratio of citric acid and copper nitrate is 1：7；
(2) ethyl alcohol and hexamethylene are mixed evenly, oleic acid, triethylamine is then added, after being stirred, is finally added dropwise
Ethyl orthosilicate is transferred in reaction kettle after being stirred and reacts 20h at 150 DEG C, after reaction, siliceous hexamethylene is made
Alkane colloidal sol；Wherein, the rate of addition of the ethyl orthosilicate is 3mL/min；
(3) solution A made from step (1) is added drop-wise to hexamethylene colloidal sol siliceous made from step (2), is stirred when being added dropwise
It mixes, ammonia precipitation process is then added dropwise after being added dropwise, is filtered after precipitating, and is successively washed and is sunk with deionized water, dehydrated alcohol
It forms sediment, it is dry, catalyst is made；Wherein, the rate of addition of solution A is 10ml/L；The catalyst, copper oxide and silica
Mass ratio is 6：1；
(4) catalyst obtained above is placed in autoclave, and furfural and isopropanol is added to reaction under high pressure
In kettle, it is passed through hydrogen 5min in advance into autoclave, then proceedes to be passed through hydrogen, 10h is reacted at 3MPa, 280 DEG C, instead
It is cooled to room temperature, filters after answering, remove catalyst, 2- methylfuran is made；Wherein, the catalyst：The quality of furfural
Than being 0.03：4.The yield of 2- methylfuran is 69%.
The foregoing is only a preferred embodiment of the present invention, but scope of protection of the present invention is not limited thereto,
Anyone skilled in the art in the technical scope disclosed by the present invention, according to the technique and scheme of the present invention and its
Inventive concept is subject to equivalent substitution or change, should be covered by the protection scope of the present invention.
Claims (10)
- The high-efficiency environment friendly preparation method of 1.2- methylfuran, which is characterized in that include the following steps：(1) copper nitrate, aluminum nitrate are dissolved in stirring to solid in deionized water to dissolve, mixed liquor is made；It is added into mixed liquor Citric acid solution is stirred, obtained solution A；(2) ethyl alcohol and hexamethylene are mixed evenly, oleic acid, triethylamine is then added, after being stirred, positive silicon is finally added dropwise Acetoacetic ester is transferred in reaction kettle after being stirred and reacts 20h at 150 DEG C, and after reaction, the hexamethylene for being made siliceous is molten Glue；(3) solution A made from step (1) is added drop-wise to hexamethylene colloidal sol siliceous made from step (2), is stirred when being added dropwise, Then ammonia precipitation process is added dropwise after being added dropwise, is filtered after precipitating, and successively wash precipitating with deionized water, dehydrated alcohol, It is dry, catalyst is made；(4) catalyst obtained above is placed in autoclave, and furfural and isopropanol is added in autoclave, It is passed through hydrogen 5min in advance into autoclave, then proceedes to be passed through hydrogen, reacted at 2-3MPa, 200-280 DEG C, reacted After be cooled to room temperature, filter, remove catalyst, be made 2- methylfuran.
- 2. the high-efficiency environment friendly preparation method of 2- methylfuran as described in claim 1, it is characterised in that：In step (1), mixing In liquid, aluminum ions concentration is 3-5mol/L, and the concentration of copper ion is 2-6mol/L.
- 3. the high-efficiency environment friendly preparation method of 2- methylfuran as described in claim 1, it is characterised in that：It is described in step (1) The mass concentration of citric acid solution is 10-20%.
- 4. the high-efficiency environment friendly preparation method of 2- methylfuran as described in claim 1, it is characterised in that：It is described in step (1) The molar ratio of citric acid and copper nitrate is 1：(3-7).
- 5. the high-efficiency environment friendly preparation method of 2- methylfuran as described in claim 1, it is characterised in that：It is described in step (2) Ethyl alcohol, hexamethylene, oleic acid, triethylamine, ethyl orthosilicate volume ratio be 1:50:0.5:1:1.
- 6. the high-efficiency environment friendly preparation method of 2- methylfuran as described in claim 1, it is characterised in that：It is described in step (2) The rate of addition of ethyl orthosilicate is 1-3mL/min.
- 7. the high-efficiency environment friendly preparation method of 2- methylfuran as described in claim 1, it is characterised in that：In step (3), solution The rate of addition of A is 2-5ml/L.
- 8. the high-efficiency environment friendly preparation method of 2- methylfuran as described in claim 1, it is characterised in that：It is described in step (3) The mass ratio of catalyst, copper oxide and silica is (2-6)：1.
- 9. the high-efficiency environment friendly preparation method of 2- methylfuran as described in claim 1, it is characterised in that：It is described in step (4) Catalyst：The mass ratio of furfural is (0.01-0.03)：4.
- 10. the high-efficiency environment friendly preparation method of 2- methylfuran as described in claim 1, it is characterised in that：In step (4), institute The time for stating reaction is 2-10h.
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|---|---|---|---|---|
| CN115043745A (en) * | 2022-07-26 | 2022-09-13 | 盐城工学院 | Preparation method of amino acid surfactant |
| CN115043745B (en) * | 2022-07-26 | 2023-08-22 | 盐城工学院 | Preparation method of amino acid surfactant |
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Application publication date: 20181123 |