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Recovery method for ionic liquid solvent generated from homogeneous acylation reaction of cellulose

An ionic liquid solvent, acylation reaction technology, applied in molecular distillation and other directions, can solve the problems of not involving the ionic liquid solvent waste liquid recovery, polluting the ionic liquid solvent, low ionic liquid concentration, etc., achieving low cost and simple process. , the effect of high recovery rate

Inactive Publication Date: 2012-03-14
INST OF PROCESS ENG CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although these two methods have good enrichment effect, the process is complex, and because the introduction of inorganic salts will pollute the ionic liquid solvent, it needs to be further studied; Chinese patent CN101219840A adopts pretreatment, ultrafiltration, nanofiltration or reverse osmosis, Combined method of vacuum distillation for the recovery of ionic liquid solvents from spinning wastewater
Due to the relatively expensive membrane materials, the recycling of the membrane is more difficult and costly, and the concentration of the recovered ionic liquid is not high
Chinese patent CN101003510A only uses molecular distillation to purify the synthetic crude ionic liquid, and does not involve the recovery of the ionic liquid solvent waste liquid after participating in the reaction

Method used

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  • Recovery method for ionic liquid solvent generated from homogeneous acylation reaction of cellulose
  • Recovery method for ionic liquid solvent generated from homogeneous acylation reaction of cellulose

Examples

Experimental program
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Effect test

Embodiment 1

[0035] Weigh 500 g of the ionic liquid solvent 1-butyl-3-methylimidazolium tetrafluoroborate waste liquid after preparing cellulose acetate, add 5 g of activated carbon, and stir at 30 ° C for 30 min; Ethylene membrane filtration; then add to the rotary evaporator, under the condition of 60°C and 2kpa, distill under reduced pressure for 3 hours, then add the resultant to the feeder of the wiped film molecular distillation apparatus, and turn on the feeder heating device , set the heating temperature to 50°C, turn on the evaporation temperature device of the wiped film molecular distillation apparatus, set the evaporation surface temperature to 80°C, turn on the circulating cooling pump, set the condensation temperature to -15°C, and keep it for 20 minutes, turn on the vacuum pump , make the pressure reach 1Pa, start the wiper, make the rotating speed of the wiper rotor be 275r / min, open the injection valve, control the feed rate at 10ml / min, start dripping molecular distillatio...

Embodiment 2

[0038] Weigh 500 g of the ionic liquid solvent 1-allyl-3-methylimidazolium chloride waste liquid after preparing cellulose acetate, add 10 g of activated carbon, stir at 50 ° C for 60 min, and then use a 0.45 μm polytetrafluoroethylene membrane Filter, then add to a rotary evaporator, distill under reduced pressure at 90°C and 10kpa for 6 hours, then add the resultant to the feeder of the wiped-film molecular distillation device, turn on the feeder heating device, set the temperature 70°C, turn on the evaporation temperature device of the wiped film molecular distillation apparatus, set the temperature to 100°C, turn on the circulating cooling pump, set the condensation temperature to -10°C, and keep it for 20 minutes, turn on the vacuum pump to make the pressure reach 50Pa, start the scraping Membrane device, make the rotating speed of the scraping membrane rotor be 385r / min, open the injection valve, feed speed control at 5ml / min, start dripping molecular distillation to obta...

Embodiment 3

[0041]Weigh 500 g of the ionic liquid solvent 1-butyl-3-methylimidazolium iodide salt waste liquid after preparing cellulose acetate, add 25 g of activated carbon, stir at 80 ° C for 120 min, and then filter with a 1 μm polytetrafluoroethylene membrane, Then add it to the rotary evaporator, distill under reduced pressure at 110°C and 30kpa for 15 hours, then add the resultant to the feeder of the molecular distillation device, turn on the heating device of the feeder, set the temperature at 80°C, and turn on the molecule Set the temperature of the evaporation temperature device of the distillation apparatus to 110°C, turn on the circulating cooling pump, set the condensation temperature to 15°C, and keep it for 20 minutes, turn on the vacuum pump to make the pressure reach 100Pa, start the wiper, and make the speed of the wiper rotor be 385r / min, open the injection valve, control the feed rate at 1ml / min, start dripping molecular distillation to obtain distillate, collect the o...

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Abstract

The present invention relates to a recovery method for an ionic liquid solvent generated from a homogeneous acylation reaction of cellulose. According to the method, the ionic liquid waste solution generated from the homogeneous acylation reaction of the cellulose is decolorized and filtered; the filtered ionic liquid waste solution is subjected to vacuum distillation; the resulting ionic liquid waste solution is added to a molecular distillation device; appropriate conditions of a feeding temperature, a feeding speed, an evaporation temperature, an evaporation pressure, a wiped film rotationspeed and a condensation temperature are selected to carry out molecular distillation, the collected heavy components are the recovered ionic liquid. With the method of the present invention, the vacuum distillation technology and the molecular distillation technology are combined, such that organic residues and water in the ionic liquid waste solution generated from the homogeneous acylation reaction of the cellulose can be efficiently removed, the purity of the resulting ionic liquid is more than 99%. The method has advantages of lower energy consumption, simple process and high efficiency.The recovered ionic liquid can be recycled.

Description

technical field [0001] The invention relates to a method for recovering an ionic liquid solvent, in particular to a method for recovering an ionic liquid solvent after a cellulose homogeneous acylation reaction. Background technique [0002] Cellulose is the most abundant renewable resource in nature and widely exists in plant fibers. With the continuous consumption and scarcity of non-renewable resources such as petroleum and coal, the development of environmentally friendly and high value-added green industrial products through the modification of cellulose has attracted more and more attention. Among them, the research on cellulose organic acid esters has become a hot research topic. As a modified product of cellulose, cellulose organic acid ester plays a very important role in coatings, coatings, paints, and medicine, and is widely used in national defense, chemical industry, biology, medicine, construction, aerospace and other fields. [0003] Ionic liquid solvents ar...

Claims

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Application Information

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IPC IPC(8): B01D3/12
Inventor 李会泉吴睿黄科林曹妍
Owner INST OF PROCESS ENG CHINESE ACAD OF SCI
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