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Process for producing cellulose ether by directly separating and recovering diluent

A cellulose ether and production process technology, applied in the field of cellulose ether production and preparation, can solve the problems of high energy consumption, slow speed, consumption of sodium hydroxide, etc., shorten the recovery time, improve production efficiency, and reduce the amount of acetic acid or hydrochloric acid Effect

Active Publication Date: 2011-01-26
山东赫达集团股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This process is now mature, but there are major shortcomings in this process. First, in the reaction process itself, part of the catalytic sodium hydroxide is consumed in large quantities; second, in the solvent recovery process, heat energy is used to evaporate first. , and then carry out condensation, which involves the liquid-gas phase conversion process, so there are always disadvantages such as high energy consumption and slow speed.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0013] Add mixed diluent 800kg (component mass ratio is toluene: isopropanol: water=1: 0.3: 0.15) in etherification tank, sodium hydroxide 60kg, after temperature is controlled at 28 ℃, add refined cotton 100kg, carry out The alkalization reaction is timed for 2 hours (1-3 hours are all acceptable), then 80 kg of methyl chloride and 40 kg of ethylene oxide are added, the temperature is raised to 45-85° C., the reaction pressure is controlled at 0.2-0.5 MPa, and the reaction time is 3 hours. After the reaction finishes, the mixed material (slurry) is separated, adopts a decanter centrifuge, and the rotating speed is 3000 rev / min, and the liquid enters the solvent intermediate tank (its composition is mainly toluene 71.1%, isopropanol 18.7%, hydrogen oxidized Sodium content 1.5%, water and others 8.7%), recovery and reuse, the solid enters the washing tank, neutralizes to PH6-7 with acetic acid, heats up to recover the remaining solvent, then adds water to wash, then separates, t...

Embodiment 2

[0015] Add 1000kg of mixed diluent (component mass ratio is toluene: isopropanol: water = 1: 0.2: 0.1) and 80kg of sodium hydroxide in the etherification kettle. After controlling the temperature at 28°C, add 100kg of refined cotton to carry out The alkalization reaction was timed for 2 hours, then 100 kg of methyl chloride and 30 kg of propylene oxide were added, the temperature was raised to 55-95° C., the reaction pressure was controlled at 0.3-0.6 MPa, and the reaction time was 3 hours. After the reaction finishes, the mixed material is separated, adopts a decanter centrifuge, and the rotating speed is 3000 rpm, and the liquid enters the solvent intermediate tank (after testing, its composition is mainly toluene 78.2%, isopropanol 12.7%, sodium hydroxide content 1.6%) , water and other 7.5%), recovery and reuse, the solid enters the washing tank, after being neutralized with acetic acid, the temperature is raised to recover the remaining solvent, then water is added to wash...

Embodiment 3

[0017] Add mixed diluent 900kg (component mass ratio is toluene: isopropanol: water=1: 0.2: 0.2) in etherification tank, sodium hydroxide 90kg, after temperature is controlled at 28 ℃, add refined cotton 100kg, carry out The alkalization reaction was timed for 1 hour, then 120 kg of methyl chloride was added, the temperature was raised to 70-95° C., the reaction pressure was controlled at 0.4-0.6 MPa, and the reaction time was 3 hours. After the reaction finishes, the mixed materials are separated, using a decanter centrifuge with a rotating speed of 3000 rpm, and the liquid enters the solvent intermediate tank (after testing, its composition is mainly toluene 78.5%, isopropanol 12.9%, sodium hydroxide content 1.2%) , water and other 8.4%), recovery and reuse, the solid was washed in the kettle, after being neutralized with acetic acid, the temperature was raised to recover the remaining solvent, then washed with water, dried and pulverized after separation to obtain 116.5kg of...

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PUM

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Abstract

The invention discloses a process for producing cellulose ether by directly separating and recovering diluent, which comprises the following steps: adding sodium hydroxide and refined cottons into a mixed diluent system to carry out alkalization reaction; then adding etherifying agent into the obtained mixture to carry out etherification reaction, after the etherification reaction is completed, obtaining a mixed slurry of cellulose ether and organic diluent; and then recycling the organic diluent, and washing and refining the separated cellulose ether so as to obtain a finished product. The process is characterized in that the mixed slurry obtained in the step of etherification reaction is pumped to a centrifugal machine to carry out solid-liquid separation directly; then the obtained liquid mainly comprising the diluent enters into a settling tank to carry out gravity settling, and the obtained liquid subjected to gravity settling is directly used as diluent for recycling; and the obtained solid enters into a recover kettle and then neutralized with acid, and a small amount of diluent contained in the solid is recycled by way of steam heating and distillation. The invention not only greatly reduces the energy consumption in the process of diluent evaporation and recycling, but also recycles the alkali which is not consumed in the reaction, thereby reducing the consumption of acid used in alkali neutralization, saving energy and reducing consumption, and improving the utilization rate of raw materials.

Description

technical field [0001] The invention belongs to the technical field of cellulose preparation, and relates to a method for producing cellulose ether. Background technique [0002] The current traditional cellulose ether preparation process is to add sodium hydroxide and refined cotton to the mixed diluent system in a certain ratio for alkalization, and then add etherification agent to it, depending on the type of cellulose ether , the etherification agent may be one or both of methyl chloride, ethyl chloride, propylene oxide, and ethylene oxide. After etherification, after neutralization, the steam is heated to recover the diluent, and then washed and dried And crushing and other processes to get finished products. In this process, the diluent system generally adopts a mixed system of toluene, isopropanol and water, and its composition mass ratio is: toluene: isopropanol: water=1: 0.1~0.5: 0.2~1. After the etherification reaction is completed, the organic diluent must be re...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08B11/00C08B11/22C08B11/193C08B11/06C08B11/02
Inventor 毕心德毕于东毕英德邱建军毕研恒王荣新
Owner 山东赫达集团股份有限公司
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