CN107987041A - A kind of method of synthesis 2,5- furandicarboxylic acids - Google Patents

A kind of method of synthesis 2,5- furandicarboxylic acids Download PDF

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CN107987041A
CN107987041A CN201711014827.8A CN201711014827A CN107987041A CN 107987041 A CN107987041 A CN 107987041A CN 201711014827 A CN201711014827 A CN 201711014827A CN 107987041 A CN107987041 A CN 107987041A
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furandicarboxylic acid
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李晓明
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Guide (suzhou) Fine Chemical Co Ltd
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J23/00Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
    • B01J23/002Mixed oxides other than spinels, e.g. perovskite
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J23/00Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
    • B01J23/02Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the alkali- or alkaline earth metals or beryllium
    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07DHETEROCYCLIC COMPOUNDS
    • C07D307/00Heterocyclic compounds containing five-membered rings having one oxygen atom as the only ring hetero atom
    • C07D307/02Heterocyclic compounds containing five-membered rings having one oxygen atom as the only ring hetero atom not condensed with other rings
    • C07D307/34Heterocyclic 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
    • C07D307/56Heterocyclic 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 hetero atoms or with carbon atoms having three bonds to hetero atoms with at the most one bond to halogen, e.g. ester or nitrile radicals, directly attached to ring carbon atoms
    • C07D307/68Carbon atoms having three bonds to hetero atoms with at the most one bond to halogen
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2523/00Constitutive chemical elements of heterogeneous catalysts

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Abstract

The invention discloses one kind synthesis 2, the method of 5 furandicarboxylic acids, nanocatalyst is made using method of co-precipitation first in it, and pass sequentially through in preparation process and to add Sodium Polyacrylate, sodium sulfanilate effectively controls the speed of precipitation, so as to control the particle size of catalyst;Then 5 hydroxymethylfurfurals are placed in N, are uniformly mixed, are transferred in three-necked flask in N dimethylformamides, nanocatalyst obtained above is added, oxygen is continually fed into three-necked flask, 2 3h of stirring reaction at 30 DEG C, then heat to 90 DEG C, continue to be passed through oxygen, stirring 2 4h of reaction, are cooled to room temperature after reaction, filtering, it is dry after obtained washing of precipitate, obtain 2,5 furandicarboxylic acids.Method synthesis step disclosed by the invention is simple, and reaction condition is gentle, and the catalyst of use is environmentally protective, cheap, and target product yield is high, and purity is high.

Description

A kind of method of synthesis 2,5- furandicarboxylic acids
Technical field:
The present invention relates to medicine intermediate preparation field, is specifically related to a kind of method for synthesizing 2,5-furandicarboxylic acid.
Background technology:
2,5-furandicarboxylic acid as a kind of of great value industrial chemicals and intermediate, be frequently used in medicine, pesticide, Insecticide, antiseptic, perfume etc..The conventional method that foreign countries prepare 2,5- furandicarboxylic acids is that the environment of oxygen your gold be passed through Belong to catalysis oxidation.But this method catalyst is of high cost, the reaction time generally wants several hours.Therefore, low cost, few energy are explored Consumption, efficient preparation method is inevitable trend.
Patent 201410834523.6 discloses a kind of preparation method of 2,5-furandicarboxylic acid, it is characterised in that by as follows Step carries out:A, 5 hydroxymethyl furfural is added in organic solvent, then add catalyst tetramethyl piperidine nitrogen oxides, Catalyst activator ferric nitrate and additive basic metal halide, 4~12h is reacted in stirring at room temperature in atmosphere, obtains containing 2,5- The reaction mixture of furans dicarbaldehyde;It is water-soluble that tert-Butanol peroxide is added in the reaction mixture of the dicarbaldehyde of furans containing 2,5- Liquid, stirs 4~8h, then cooled to room temperature, obtains reaction product at 100~120 DEG C;To reaction product centrifugation point From that must precipitate, wash the precipitation and dry, up to target product 2,5-furandicarboxylic acid.The method reaction condition temperature of the present invention With, cheap and product yield high.But its catalyst used has certain toxicity.
The content of the invention:
The object of the present invention is to provide a kind of 2,5-furandicarboxylic acid, its synthesis step is simple, and reaction condition is gentle, uses Catalyst it is environmentally protective, cheap, target product yield is high, and purity is high.
To achieve the above object, the present invention uses following technical scheme:
A kind of method for synthesizing 2,5-furandicarboxylic acid, comprises the following steps:
(1) using deionized water as solvent, aluminum nitrate solution, the magnesium nitrate solution of 1moL/L that concentration is 1moL/L are prepared; The calcium nitrate solution of 1moL/L;
(2) sodium hydroxide solution is added dropwise into calcium nitrate solution, stirs 30min, then adds Sodium Polyacrylate, be placed in three 1-2h is ground in roller mill, obtains mixed material;
(3) mixed material is transferred in three-necked flask, then adds aluminum nitrate solution obtained above, magnesium nitrate at the same time Solution, stirs while adding, and 70-90 DEG C is warming up to after addition, and stirring reaction 1-3h, is cooled to room temperature after reaction, Then into reaction system, sodium sulfanilate is added, 40 DEG C is warming up to, is stirred 10min, be continuously heating to 80 DEG C, Stirring reaction 1-1.5h, is cooled to room temperature after reaction, by reacting liquid filtering, obtains filtration washing drying, obtains solid;
(4) solid is placed in Muffle furnace, 1-3h is handled under 200-300 DEG C, inert gas shielding, after treatment is cold But nanocatalyst is obtained to room temperature, grinding;
(5) 5 hydroxymethyl furfural is placed in n,N-Dimethylformamide and is uniformly mixed, is transferred in three-necked flask, Nanocatalyst obtained above is added, oxygen is continually fed into three-necked flask, the stirring reaction 2-3h, Ran Housheng at 30 DEG C Temperature continues to be passed through oxygen, stirring reaction 2-4h, is cooled to room temperature, filters, after obtained washing of precipitate after reaction to 90 DEG C It is dry, obtain 2,5-furandicarboxylic acid.
As the preferred of above-mentioned technical proposal, in step (2), calcium nitrate, the mass ratio of Sodium Polyacrylate are (5-11):1.
As the preferred of above-mentioned technical proposal, in step (3), the calcium nitrate, aluminum nitrate, the molar ratio of magnesium nitrate are 3: 1:1。
As the preferred of above-mentioned technical proposal, in step (3), the calcium nitrate, the mass ratio of sodium sulfanilate are 1:(0.01-0.03).
As the preferred of above-mentioned technical proposal, in step (5), the 5 hydroxymethyl furfural, n,N-Dimethylformamide Amount ratio is (20-300) g:1L.
As the preferred of above-mentioned technical proposal, in step (5), the 5 hydroxymethyl furfural, the mass ratio of nanocatalyst For 1:(0.003-0.006).
As the preferred of above-mentioned technical proposal, in step (2), the mass concentration of the sodium hydroxide solution is 20%.
As the preferred of above-mentioned technical proposal, in step (2), the molar ratio of calcium nitrate and sodium hydroxide is 1:(2.2-3).
The invention has the advantages that:
The present invention prepares metal oxide composite catalyst using calcium nitrate, aluminum nitrate, magnesium nitrate, during preparation Mixed first using calcium nitrate solution and sodium hydroxide solution, and the sodium hydroxide solution of excessive addition, mixed serum is made;And Sodium Polyacrylate is added during nitric acid calcium precipitate, magnesium nitrate, aluminum nitrate mixing is then added, mixes at a certain temperature Close, effectively control the settling velocity of magnesium nitrate, aluminum nitrate, effectively control metal hydroxides presoma crystal property and Particle size;Then add sodium sulfanilate to be modified, and handle at a certain temperature, it is obtained nano level to ammonia The catalyst of base benzene sulfonic acid sodium salt modification, its catalytic activity is high, can fully be contacted with reactant;
Method synthesis step disclosed by the invention is simple, and reaction condition is gentle, and the catalyst of use is environmentally protective, and price is low Honest and clean, target product yield is high, and purity is high.
Embodiment:
In order to be better understood from 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 formed to the present invention.
Embodiment 1
A kind of method for synthesizing 2,5-furandicarboxylic acid, comprises the following steps:
(1) using deionized water as solvent, aluminum nitrate solution, the magnesium nitrate solution of 1moL/L that concentration is 1moL/L are prepared; The calcium nitrate solution of 1moL/L;
(2) sodium hydroxide solution is added dropwise into calcium nitrate solution, stirs 30min, then adds Sodium Polyacrylate, be placed in three 1-2h is ground in roller mill, obtains mixed material;Wherein, calcium nitrate, the mass ratio of Sodium Polyacrylate are 5:1;Calcium nitrate with The molar ratio of sodium hydroxide is 1:2.2;
(3) mixed material is transferred in three-necked flask, then adds aluminum nitrate solution obtained above, magnesium nitrate at the same time Solution, stirs while adding, and 70-90 DEG C is warming up to after addition, stirring reaction 1h, is cooled to room temperature, so after reaction In backward reaction system, sodium sulfanilate is added, 40 DEG C is warming up to, is stirred 10min, be continuously heating to 80 DEG C, stir Reaction 1h is mixed, is cooled to room temperature after reaction, by reacting liquid filtering, filtration washing drying is obtained, obtains solid;Wherein, nitre Sour calcium, the mass ratio of sodium sulfanilate are 1:0.01;
(4) solid is placed in Muffle furnace, 1h, after treatment cooling is handled under 200-300 DEG C, inert gas shielding To room temperature, grinding obtains nanocatalyst;
(5) 5 hydroxymethyl furfural is placed in n,N-Dimethylformamide and is uniformly mixed, is transferred in three-necked flask, Nanocatalyst obtained above is added, oxygen is continually fed into three-necked flask, stirring reaction 2h, then heats up at 30 DEG C To 90 DEG C, continue to be passed through oxygen, stirring reaction 2h, is cooled to room temperature, filters, do after obtained washing of precipitate after reaction It is dry, obtain 2,5-furandicarboxylic acid;Wherein, 5 hydroxymethyl furfural, the amount ratio of n,N-Dimethylformamide are 20g:1L;5- hydroxyls Methyl furfural, the mass ratio of nanocatalyst are 1:0.003.
Embodiment 2
A kind of method for synthesizing 2,5-furandicarboxylic acid, comprises the following steps:
(1) using deionized water as solvent, aluminum nitrate solution, the magnesium nitrate solution of 1moL/L that concentration is 1moL/L are prepared; The calcium nitrate solution of 1moL/L;
(2) sodium hydroxide solution is added dropwise into calcium nitrate solution, stirs 30min, then adds Sodium Polyacrylate, be placed in three 2h is ground in roller mill, obtains mixed material;Wherein, calcium nitrate, the mass ratio of Sodium Polyacrylate are 11:1;Calcium nitrate and hydrogen The molar ratio of sodium oxide molybdena is 1:3;
(3) mixed material is transferred in three-necked flask, then adds aluminum nitrate solution obtained above, magnesium nitrate at the same time Solution, stirs while adding, and 70-90 DEG C is warming up to after addition, stirring reaction 3h, is cooled to room temperature, so after reaction In backward reaction system, sodium sulfanilate is added, 40 DEG C is warming up to, is stirred 10min, be continuously heating to 80 DEG C, stir Reaction 1.5h is mixed, is cooled to room temperature after reaction, by reacting liquid filtering, filtration washing drying is obtained, obtains solid;Wherein, Calcium nitrate, the mass ratio of sodium sulfanilate are 1:0.03;
(4) solid is placed in Muffle furnace, 3h, after treatment cooling is handled under 200-300 DEG C, inert gas shielding To room temperature, grinding obtains nanocatalyst;
(5) 5 hydroxymethyl furfural is placed in n,N-Dimethylformamide and is uniformly mixed, is transferred in three-necked flask, Nanocatalyst obtained above is added, oxygen is continually fed into three-necked flask, stirring reaction 3h, then heats up at 30 DEG C To 90 DEG C, continue to be passed through oxygen, stirring reaction 4h, is cooled to room temperature, filters, do after obtained washing of precipitate after reaction It is dry, obtain 2,5-furandicarboxylic acid;Wherein, 5 hydroxymethyl furfural, the amount ratio of n,N-Dimethylformamide are 300g:1L;5- Hydroxymethylfurfural, the mass ratio of nanocatalyst are 1:0.006.
Embodiment 3
A kind of method for synthesizing 2,5-furandicarboxylic acid, comprises the following steps:
(1) using deionized water as solvent, aluminum nitrate solution, the magnesium nitrate solution of 1moL/L that concentration is 1moL/L are prepared; The calcium nitrate solution of 1moL/L;
(2) sodium hydroxide solution is added dropwise into calcium nitrate solution, stirs 30min, then adds Sodium Polyacrylate, be placed in three 1.2h is ground in roller mill, obtains mixed material;Wherein, calcium nitrate, the mass ratio of Sodium Polyacrylate are 6:1;Calcium nitrate with The molar ratio of sodium hydroxide is 1:2.5;
(3) mixed material is transferred in three-necked flask, then adds aluminum nitrate solution obtained above, magnesium nitrate at the same time Solution, stirs while adding, and 70-90 DEG C is warming up to after addition, and stirring reaction 1.5h, is cooled to room temperature after reaction, Then into reaction system, sodium sulfanilate is added, 40 DEG C is warming up to, is stirred 10min, be continuously heating to 80 DEG C, Stirring reaction 1.1h, is cooled to room temperature after reaction, by reacting liquid filtering, obtains filtration washing drying, obtains solid;Its In, calcium nitrate, the mass ratio of sodium sulfanilate are 1:0.015;
(4) solid is placed in Muffle furnace, 1.5h is handled under 200-300 DEG C, inert gas shielding, after treatment is cold But nanocatalyst is obtained to room temperature, grinding;
(5) 5 hydroxymethyl furfural is placed in n,N-Dimethylformamide and is uniformly mixed, is transferred in three-necked flask, Nanocatalyst obtained above is added, oxygen is continually fed into three-necked flask, the stirring reaction 2.2h, Ran Housheng at 30 DEG C Temperature continues to be passed through oxygen, stirring reaction 2.5h, is cooled to room temperature, filters, after obtained washing of precipitate after reaction to 90 DEG C It is dry, obtain 2,5-furandicarboxylic acid;Wherein, 5 hydroxymethyl furfural, the amount ratio of n,N-Dimethylformamide are 50g:1L;5- Hydroxymethylfurfural, the mass ratio of nanocatalyst are 1:0.035.
Embodiment 4
A kind of method for synthesizing 2,5-furandicarboxylic acid, comprises the following steps:
(1) using deionized water as solvent, aluminum nitrate solution, the magnesium nitrate solution of 1moL/L that concentration is 1moL/L are prepared; The calcium nitrate solution of 1moL/L;
(2) sodium hydroxide solution is added dropwise into calcium nitrate solution, stirs 30min, then adds Sodium Polyacrylate, be placed in three 1.4h is ground in roller mill, obtains mixed material;Wherein, calcium nitrate, the mass ratio of Sodium Polyacrylate are 7:1;Calcium nitrate with The molar ratio of sodium hydroxide is 1:2.6;
(3) mixed material is transferred in three-necked flask, then adds aluminum nitrate solution obtained above, magnesium nitrate at the same time Solution, stirs while adding, and 70-90 DEG C is warming up to after addition, stirring reaction 2h, is cooled to room temperature, so after reaction In backward reaction system, sodium sulfanilate is added, 40 DEG C is warming up to, is stirred 10min, be continuously heating to 80 DEG C, stir Reaction 1.2h is mixed, is cooled to room temperature after reaction, by reacting liquid filtering, filtration washing drying is obtained, obtains solid;Wherein, Calcium nitrate, the mass ratio of sodium sulfanilate are 1:0.02;
(4) solid is placed in Muffle furnace, 2h, after treatment cooling is handled under 200-300 DEG C, inert gas shielding To room temperature, grinding obtains nanocatalyst;
(5) 5 hydroxymethyl furfural is placed in n,N-Dimethylformamide and is uniformly mixed, is transferred in three-necked flask, Nanocatalyst obtained above is added, oxygen is continually fed into three-necked flask, the stirring reaction 2.4h, Ran Housheng at 30 DEG C Temperature continues to be passed through oxygen, stirring reaction 3h, is cooled to room temperature, filters, do after obtained washing of precipitate after reaction to 90 DEG C It is dry, obtain 2,5-furandicarboxylic acid;Wherein, 5 hydroxymethyl furfural, the amount ratio of n,N-Dimethylformamide are 100g:1L;5- Hydroxymethylfurfural, the mass ratio of nanocatalyst are 1:0.003.
Embodiment 5
A kind of method for synthesizing 2,5-furandicarboxylic acid, comprises the following steps:
(1) using deionized water as solvent, aluminum nitrate solution, the magnesium nitrate solution of 1moL/L that concentration is 1moL/L are prepared; The calcium nitrate solution of 1moL/L;
(2) sodium hydroxide solution is added dropwise into calcium nitrate solution, stirs 30min, then adds Sodium Polyacrylate, be placed in three 1.6h is ground in roller mill, obtains mixed material;Wherein, calcium nitrate, the mass ratio of Sodium Polyacrylate are 8:1;Calcium nitrate with The molar ratio of sodium hydroxide is 1:2.7;
(3) mixed material is transferred in three-necked flask, then adds aluminum nitrate solution obtained above, magnesium nitrate at the same time Solution, stirs while adding, and 70-90 DEG C is warming up to after addition, and stirring reaction 2.5h, is cooled to room temperature after reaction, Then into reaction system, sodium sulfanilate is added, 40 DEG C is warming up to, is stirred 10min, be continuously heating to 80 DEG C, Stirring reaction 1.4h, is cooled to room temperature after reaction, by reacting liquid filtering, obtains filtration washing drying, obtains solid;Its In, calcium nitrate, the mass ratio of sodium sulfanilate are 1:0.02;
(4) solid is placed in Muffle furnace, 2h, after treatment cooling is handled under 200-300 DEG C, inert gas shielding To room temperature, grinding obtains nanocatalyst;
(5) 5 hydroxymethyl furfural is placed in n,N-Dimethylformamide and is uniformly mixed, is transferred in three-necked flask, Nanocatalyst obtained above is added, oxygen is continually fed into three-necked flask, the stirring reaction 2.6h, Ran Housheng at 30 DEG C Temperature continues to be passed through oxygen, stirring reaction 3.5h, is cooled to room temperature, filters, after obtained washing of precipitate after reaction to 90 DEG C It is dry, obtain 2,5-furandicarboxylic acid;Wherein, 5 hydroxymethyl furfural, the amount ratio of n,N-Dimethylformamide are 150g:1L; 5 hydroxymethyl furfural, the mass ratio of nanocatalyst are 1:0.04.
Embodiment 6
A kind of method for synthesizing 2,5-furandicarboxylic acid, comprises the following steps:
(1) using deionized water as solvent, aluminum nitrate solution, the magnesium nitrate solution of 1moL/L that concentration is 1moL/L are prepared; The calcium nitrate solution of 1moL/L;
(2) sodium hydroxide solution is added dropwise into calcium nitrate solution, stirs 30min, then adds Sodium Polyacrylate, be placed in three 1.8h is ground in roller mill, obtains mixed material;Wherein, calcium nitrate, the mass ratio of Sodium Polyacrylate are 10:1;Calcium nitrate with The molar ratio of sodium hydroxide is 1:2.8;
(3) mixed material is transferred in three-necked flask, then adds aluminum nitrate solution obtained above, magnesium nitrate at the same time Solution, stirs while adding, and 70-90 DEG C is warming up to after addition, and stirring reaction 2.5h, is cooled to room temperature after reaction, Then into reaction system, sodium sulfanilate is added, 40 DEG C is warming up to, is stirred 10min, be continuously heating to 80 DEG C, Stirring reaction 1.5h, is cooled to room temperature after reaction, by reacting liquid filtering, obtains filtration washing drying, obtains solid;Its In, calcium nitrate, the mass ratio of sodium sulfanilate are 1:0.03;
(4) solid is placed in Muffle furnace, 3h, after treatment cooling is handled under 200-300 DEG C, inert gas shielding To room temperature, grinding obtains nanocatalyst;
(5) 5 hydroxymethyl furfural is placed in n,N-Dimethylformamide and is uniformly mixed, is transferred in three-necked flask, Nanocatalyst obtained above is added, oxygen is continually fed into three-necked flask, the stirring reaction 2.8h, Ran Housheng at 30 DEG C Temperature continues to be passed through oxygen, stirring reaction 3.5h, is cooled to room temperature, filters, after obtained washing of precipitate after reaction to 90 DEG C It is dry, obtain 2,5-furandicarboxylic acid;Wherein, 5 hydroxymethyl furfural, the amount ratio of n,N-Dimethylformamide are 25g:1L;5- Hydroxymethylfurfural, the mass ratio of nanocatalyst are 1:0.005.
After testing, when the concentration of reactant 5 hydroxymethyl furfural solution is 300g/L, the yield of target product is 96.33%, the concentration of 5 hydroxymethyl furfural solution is 25g/L, and the yield of target product is 99.05%, and 5 hydroxymethyl furfural is molten The concentration of liquid is 100g/L, and the yield of target product is 97.3%.

Claims (8)

  1. A kind of 1. method for synthesizing 2,5-furandicarboxylic acid, it is characterised in that comprise the following steps:
    (1) using deionized water as solvent, aluminum nitrate solution, the magnesium nitrate solution of 1moL/L that concentration is 1moL/L are prepared;1moL/ The calcium nitrate solution of L;
    (2) sodium hydroxide solution is added dropwise into calcium nitrate solution, stirs 30min, then adds Sodium Polyacrylate, be placed in three rollers and grind 1-2h is ground in grinding machine, obtains mixed material;
    (3) mixed material is transferred in three-necked flask, it is molten then adds aluminum nitrate solution obtained above, magnesium nitrate at the same time Liquid, stirs while adding, and 70-90 DEG C is warming up to after addition, stirring reaction 1-3h, is cooled to room temperature, so after reaction In backward reaction system, sodium sulfanilate is added, 40 DEG C is warming up to, is stirred 10min, be continuously heating to 80 DEG C, stir Reaction 1-1.5h is mixed, is cooled to room temperature after reaction, by reacting liquid filtering, filtration washing drying is obtained, obtains solid;
    (4) solid is placed in Muffle furnace, 1-3h is handled under 200-300 DEG C, inert gas shielding, after treatment is cooled to Room temperature, grinding obtain nanocatalyst;
    (5) 5 hydroxymethyl furfural is placed in n,N-Dimethylformamide and be uniformly mixed, is transferred in three-necked flask, added Nanocatalyst obtained above, oxygen is continually fed into three-necked flask, and stirring reaction 2-3h, then heats at 30 DEG C 90 DEG C, continue to be passed through oxygen, stirring reaction 2-4h, is cooled to room temperature, filters, do after obtained washing of precipitate after reaction It is dry, obtain 2,5-furandicarboxylic acid.
  2. A kind of 2. method for synthesizing 2,5-furandicarboxylic acid as claimed in claim 1, it is characterised in that:In step (2), nitric acid Calcium, the mass ratio of Sodium Polyacrylate are (5-11):1.
  3. A kind of 3. method for synthesizing 2,5-furandicarboxylic acid as claimed in claim 1, it is characterised in that:It is described in step (3) Calcium nitrate, aluminum nitrate, the molar ratio of magnesium nitrate are 3:1:1.
  4. A kind of 4. method for synthesizing 2,5-furandicarboxylic acid as claimed in claim 1, it is characterised in that:It is described in step (3) Calcium nitrate, the mass ratio of sodium sulfanilate are 1:(0.01-0.03).
  5. A kind of 5. method for synthesizing 2,5-furandicarboxylic acid as claimed in claim 1, it is characterised in that:It is described in step (5) 5 hydroxymethyl furfural, the amount ratio of N,N-dimethylformamide are (20-300) g:1L.
  6. A kind of 6. method for synthesizing 2,5-furandicarboxylic acid as claimed in claim 1, it is characterised in that:It is described in step (5) 5 hydroxymethyl furfural, the mass ratio of nanocatalyst are 1:(0.003-0.006).
  7. A kind of 7. method for synthesizing 2,5-furandicarboxylic acid as claimed in claim 1, it is characterised in that:It is described in step (2) The mass concentration of sodium hydroxide solution is 20%.
  8. A kind of 8. method for synthesizing 2,5-furandicarboxylic acid as claimed in claim 1, it is characterised in that:In step (2), nitric acid The molar ratio of calcium and sodium hydroxide is 1:(2.2-3).
CN201711014827.8A 2017-10-26 2017-10-26 A kind of method of synthesis 2,5- furandicarboxylic acids Withdrawn CN107987041A (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111377890A (en) * 2018-12-28 2020-07-07 中国石油化工股份有限公司 Method for producing 2,5-furandicarboxylic acid from 5-hydroxymethylfurfural
CN112138679A (en) * 2020-09-10 2020-12-29 厦门大学 Bimetallic oxide catalyst and preparation and use methods thereof
JP2022530602A (en) * 2019-03-20 2022-06-30 サムヤン コーポレイション Method for producing 2,5-furandicarboxylic acid

Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111377890A (en) * 2018-12-28 2020-07-07 中国石油化工股份有限公司 Method for producing 2,5-furandicarboxylic acid from 5-hydroxymethylfurfural
CN111377890B (en) * 2018-12-28 2022-10-11 中国石油化工股份有限公司 Method for producing 2,5-furandicarboxylic acid from 5-hydroxymethylfurfural
JP2022530602A (en) * 2019-03-20 2022-06-30 サムヤン コーポレイション Method for producing 2,5-furandicarboxylic acid
US11795154B2 (en) 2019-03-20 2023-10-24 Samyang Corporation Method for the synthesis of 2,5-furandicarboxylic acid
CN112138679A (en) * 2020-09-10 2020-12-29 厦门大学 Bimetallic oxide catalyst and preparation and use methods thereof
CN112138679B (en) * 2020-09-10 2021-10-26 厦门大学 Bimetallic oxide catalyst and preparation and use methods thereof
US11702395B2 (en) 2020-09-10 2023-07-18 Xiamen University Bimetal oxide catalyst and methods

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