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Environmentally-friendly synthesis method of bisphenol fluorene

A technology of green synthesis and bisphenol fluorene, which is applied in the field of catalysis, can solve the problems of harsh reaction conditions, expensive catalysts, and low process requirements, and achieve the effects of mild reaction conditions, excellent catalytic effect, and good application prospects

Active Publication Date: 2018-07-06
MEIWA PLASTIC SHANGHAI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the disadvantages of this process are that the catalyst is seriously corrosive to metal equipment; the amount of acid is large and it is not easy to recycle; the product produces a large amount of wastewater containing phenol, sulfuric acid and methanol in the post-treatment process, which is difficult to treat
The advantage of the hydrogen chloride method is that the reaction conditions are mild, the operation is simple, the raw material is cheap, and it is suitable for large-scale production.
The mercaptosulfonic acid method can effectively avoid the problem of equipment corrosion caused by inorganic acid catalysts in the synthesis project, and can produce bisphenol fluorene with high efficiency in a short period of time; the advantage of this method is that the process requirements are low and the product quality is good , higher yield, less environmental pollution, the disadvantage is that mercaptosulfonic acid catalysts are expensive and not suitable for large-scale production
The quality of the product obtained by the heteropoly acid method is good and has little impact on the environment, but the reaction conditions are harsh, the catalyst is easily deactivated, the production energy consumption is large, the product yield is low, and the equipment maintenance is expensive.

Method used

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  • Environmentally-friendly synthesis method of bisphenol fluorene

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] 1) NiFe 2 o 4 preparation of

[0031] 3.0 mmol FeCl 3 ·6H 2 O and 1.5 mmol NiSO 4 ·6H 2 O was dissolved in 40.0 mL of ethylene glycol solution, and then 22.0 mmol of sodium acetate and 6.0 mmol of CTAB were added to it and ultrasonically treated for 30 min to obtain a mixture; then reacted in a water bath at 180°C for 24 h to obtain a suspension, and the suspension was naturally After cooling to room temperature, centrifuge, wash and dry at 105°C for 12 hours to obtain NiFe 2 o 4 magnetic nanocrystals;

[0032] 2) NiFe 2 o 4 Surface TiO 2 clad

[0033] Same as Example 1

[0034] 3) Loading of ionic liquids

[0035] 1g of NiFe 2 o 4 @TiO 2 The carrier was placed in 20mL aqueous solution, and then ionic liquid W was added to disperse for 2h under ultrasonic conditions of 150w, and then it was placed in a vacuum oven at 70°C for 12h to obtain an immobilized ionic liquid catalyst; wherein, ionic liquid W and NiFe 2 o 4 @TiO 2 The mass ratio of carrier is ...

Embodiment 2

[0039] 1) NiFe 2 o 4 preparation of

[0040] 3.0 mmol FeCl 3 ·6H 2 O and 1.5 mmol NiSO 4 ·6H 2 O was dissolved in 40.0 mL of ethylene glycol solution, and then 22.0 mmol of sodium acetate and 6.0 mmol of CTAB were added to it and ultrasonically treated for 30 minutes to obtain a mixture; then reacted in a water bath at 220°C for 12 hours to obtain a suspension, and the suspension was naturally After cooling to room temperature, centrifuge, wash and dry at 105°C for 12 hours to obtain NiFe 2 o 4 magnetic nanocrystals;

[0041] 2) NiFe 2 o 4 Surface TiO 2 clad

[0042] Same as Example 1

[0043] 3) Loading of ionic liquids

[0044] 1g of NiFe 2 o 4 @TiO 2 The carrier was placed in 20mL aqueous solution, and then ionic liquid W was added to disperse for 30min under 300w ultrasonic conditions, and then it was placed in a vacuum oven at 70°C for 12h to obtain an immobilized ionic liquid catalyst; wherein, ionic liquid W and NiFe 2 o 4 @TiO 2 The mass ratio of car...

Embodiment 3

[0048] 1) NiFe 2 o 4 preparation of

[0049] 3.0 mmol FeCl 3 ·6H 2 O and 1.5 mmol NiSO 4 ·6H 2 O was dissolved in 40.0 mL of ethylene glycol solution, and then 22.0 mmol of sodium acetate and 6.0 mmol of CTAB were added to it and ultrasonically treated for 30 min to obtain a mixture; then reacted in a water bath at 200°C for 18 h to obtain a suspension, and the suspension was naturally After cooling to room temperature, centrifuge, wash and dry at 105°C for 12 hours to obtain NiFe 2 o 4 magnetic nanocrystals;

[0050] 2) NiFe 2 o 4 Surface TiO 2 clad

[0051] Same as Example 1

[0052] 3) Loading of ionic liquids

[0053] 1g of NiFe 2 o 4 @TiO 2 The carrier was placed in 20mL aqueous solution, then ionic liquid W was added to disperse for 1h under ultrasonic conditions of 250w, and then it was placed in a vacuum oven at 70°C for 12h to obtain an immobilized ionic liquid catalyst; wherein, ionic liquid W and NiFe 2 o 4 @TiO 2 The mass ratio of carrier is 25wt...

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PUM

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Abstract

The invention discloses an environmentally-friendly synthesis method of bisphenol fluorine. The method comprises the following steps: adding phenol, 9-fluorenone, 3-thiohydracrylic acid and an immobilized ionic liquid catalyst into an ultrasonic reaction kettle at 150 to 400 w, and placing the reaction kettle into a water bath at 25 to 50 DEG C for reaction for 1 to 3 h; collecting the immobilizedionic liquid catalyst through a magnetic field, and washing and drying the collected immobilized ionic liquid catalyst for repeated use; washing the residual reaction liquid without the immobilized ionic liquid catalyst with boiled water to separate out crystals, performing suction filtration and vacuum drying on the crystals to obtain a bisphenol fluorine coarse product, and recrystalizing the bisphenol fluorine coarse product to obtain white bisphenol fluorine crystals. Compared with a conventional preparation catalyst of the bisphenol fluorine, the catalyst disclosed by the invention has the advantages of high reaction cavity and high selectivity; furthermore, reaction conditions are mild, and the reaction efficiency is high; and in addition, the quality of the bisphenol fluorine is obviously improved.

Description

technical field [0001] The technical field of catalysis of the present invention relates to a catalytic preparation method of bisphenol fluorene, in particular to a green synthesis method for preparing bisphenol fluorene by using ionic liquid. Background technique [0002] Bisphenol fluorene is an important class of fine chemical raw materials, widely used, mainly used in the synthesis of a variety of new polymer materials. Bisphenol fluorene is a bisphenol compound with a skeleton structure obtained by condensation reaction of fluorenone and phenol as raw materials in the presence of an acidic catalyst. According to the different catalysts used, the methods for preparing bisphenol fluorene in the prior art mainly include sulfuric acid method, hydrogen chloride method, mercaptosulfonic acid method and heteropolyacid method. [0003] The sulfuric acid method is the most conventional method for synthesizing bisphenol fluorene, which has the advantages of simple synthesis proc...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C39/17C07C37/20B01J31/02
CPCB01J31/0292C07C37/20C07C39/17Y02P20/52
Inventor 王强
Owner MEIWA PLASTIC SHANGHAI
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