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Continuous production method of furandicarboxylic acid with furan as raw material

A technology of furandicarboxylic acid and production method, applied in the chemical field, can solve the problems of long FDCA reaction route, poor atom economy and high raw material cost, and achieve the effects of high atom utilization rate, high total yield and lower production cost

Active Publication Date: 2020-05-22
QUZHOU RES INST OF ZHEJIANG UNIV +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

X.Li et al. reported the process of obtaining FDCA by acylation and hydrolysis of furan and oxalyl iodide (Preparation method of 2,5-furandicarboxylic acid.), but this route has poor atom economy and high raw material cost
J.G.Wang et al. reported the process of FDCA (From Furan to High Quality Bio-based Poly(ethylenefurandicarboxylate).) from furan and acetic anhydride through acetylation and demethylation steps. There are many steps and poor atom economy. low yield
[0008] To sum up, many reported FDCA production routes have problems such as long reaction routes and harsh conditions. To realize efficient and green production of FDCA involves route selection and the development of efficient catalytic systems

Method used

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  • Continuous production method of furandicarboxylic acid with furan as raw material
  • Continuous production method of furandicarboxylic acid with furan as raw material

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Experimental program
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Effect test

Embodiment 1

[0039] Embodiment 1, a kind of continuous production method of furandicarboxylic acid, take furan and carbon dioxide as raw material, carry out following steps successively:

[0040]1), preparation of Pd / 4A type molecular sieve catalyst by impregnation method: dissolve 3.732g palladium potassium chlorate (containing palladium 1.01g) in 100mL water, fully disperse and dissolve; at the same time fully disperse 100g 4A type molecular sieve in 1000mL water, mix the two Thoroughly stir (about 600r / min) and mix for 3 hours, let it stand for 2 hours, conventionally dry (dry at 40°C for 12 hours), and then calcinate at 400°C for 5 hours to obtain about 101g of Pd / 4A molecular sieve catalyst.

[0041] 2) Fix 100 g of the Pd / 4A molecular sieve catalyst obtained in step 1) in the fixed bed reactor 2, add 1.0 kg of furan into the furan gas generator 1, control the gaseous furan and carbon dioxide to mix according to the molar ratio of 1:3 (as fresh mixed raw material gas) enters the fixed...

Embodiment 2

[0042] Embodiment 2, a kind of continuous production method of furandicarboxylic acid, take furan and carbon dioxide as raw materials, carry out the following steps successively:

[0043] 1) Preparation of Ni / Y-type molecular sieve catalyst by impregnation method: Dissolve 2.665g of nickel chloride (containing 1.21g of nickel) in 100mL of water, fully disperse and dissolve; Mix well for 6 hours, let stand for 1 hour, dry and roast at 600°C for 3 hours to obtain about 101.2 g of Ni / Y molecular sieve catalyst;

[0044] 2), fix 75g of the Ni / Y type molecular sieve catalyst obtained in step 1) in the fixed bed reactor 2, add 1.0kg of furan into the furan gas generator 1, control the gaseous furan and carbon dioxide to mix according to the molar ratio of 1:5 Enter the fixed bed reactor 2, and the reaction temperature in the fixed bed reactor 2 is set to 120°C. The unreacted furan gas and carbon dioxide are discharged from the gas outlet 22 at the bottom of the fixed-bed reactor 2,...

Embodiment 3

[0045] Embodiment 3, a kind of continuous production method of furandicarboxylic acid, take furan and carbon dioxide as raw material, carry out the following steps successively:

[0046] 1), preparation of Rh / X type molecular sieve catalyst by impregnation method: 3.059g rhodium trichloride (containing rhodium 1.51g) is dissolved in the water of 100mL, fully disperses and dissolves; The X type molecular sieve of 100g is fully dispersed in 1000mL water at the same time, will The two are fully mixed for 4 hours, left to stand for 1.5 hours, dried and calcined at 500°C for 4.5 hours to obtain about 101.5g of Rh / X molecular sieve catalyst;

[0047] 2) Fix 50 g of the Rh / X molecular sieve catalyst obtained in step 1) in the fixed bed reactor 2, add 1.0 kg of furan into the furan gas generator 1, and control the gaseous furan and carbon dioxide to mix according to the molar ratio of 1:4 Enter the fixed-bed reactor 2, and the reaction temperature in the fixed-bed reactor 2 is set to ...

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Abstract

The invention discloses a continuous production method of furandicarboxylic acid with furan as a raw material. The continuous production method comprises the following steps: heating furan used as a raw material to form gaseous furan, mixing the gaseous furan with carbon dioxide to form mixed raw gas, and allowing the mixed raw gas to enter a fixed bed reactor for a reaction, wherein a transitionmetal supported catalyst is fixed in the fixed bed reactor; discharging unreacted gaseous furan and carbon dioxide from a gas outlet at the bottom of the fixed bed reactor, mixing with the unreacted gaseous furan and carbon dioxide with the mixed raw gas, and feeding the obtained mixture into the fixed bed reactor from the top end of the fixed bed reactor for a reaction; and discharging furandicarboxylic acid generated by the reaction from a discharge hole in the bottom of the reactor. The method for preparing furandicarboxylic acid has the characteristics of simple process, environmental friendliness, high yield and the like.

Description

technical field [0001] The invention belongs to the field of chemical industry, and in particular relates to a continuous production method of furandicarboxylic acid using furan as raw material. Background technique [0002] 2,5-Furandicarboxylic acid (FDCA), also known as anhydromucic acid, is a stable compound that was initially detected in human urine. There are two carboxyl groups in the FDCA molecule, which can be used as a monomer for polycondensation reaction with diol or diamine to replace the traditional petroleum-based monomer terephthalic acid to produce new polymer materials such as polyester and polyamide. At present, the FDCA material market contains businesses worth tens of billions of RMB, including plastics, plasticizers, thermosetting materials and coatings, etc.; FDCA is also listed as one of the high value-added bio-based chemical substances by the US Department of Energy. The research on new preparation technology has important economic and social signi...

Claims

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Application Information

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IPC IPC(8): C07D307/68
CPCC07D307/68Y02P20/584
Inventor 钱超靳浩周少东阮建成王帅陈新志
Owner QUZHOU RES INST OF ZHEJIANG UNIV