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Method for refining crude glycerol

A crude glycerin and glycerol technology, applied in chemical instruments and methods, preparation of hydroxyl compounds, preparation of organic compounds, etc., can solve the problems of high manufacturing cost, complicated process and high production cost, and achieve reduced production cost, high reactivity, The effect of not easy to carbonize

Inactive Publication Date: 2019-08-02
深圳市前海博扬研究院有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

These methods will produce a certain amount of waste residue and waste water, and the investment is high, the manufacturing cost is high, and the separation process is mostly cumbersome and energy-consuming.
If glycerin is used as a food-grade or pharmaceutical-grade reagent, no matter which refining method is used, it must go through an ion exchange process to ensure that the glycerin meets the quality standards, and the production cost is high and the process is complicated.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment example 1

[0048] Add 250g of crude glycerin and 25g of A15 resin catalyst into a 1000mL round bottom flask, heat to 75°C, slowly feed 410g of isobutylene gas, and continue the reaction at 75°C for 8 hours. After the temperature drops to room temperature, unreacted isobutene is recovered, the catalyst is filtered off, and glycerin tert-butyl ether is obtained by distillation under reduced pressure.

[0049] Glycerin tert-butyl ether was transferred to the cracking reaction kettle, and 25g of cracking catalyst A15 resin catalyst was added, and the reaction temperature was 110°C, and the reaction was carried out for 2 hours, and then lowered to room temperature, and the isobutylene obtained by cracking was recovered, and the catalyst was filtered off. Dilute with methanol, obtain the effluent through the filter membrane, add acid clay with 2% glycerin mass to the effluent, stir at 90°C for 2 hours, then filter the acid clay, distill the filtrate under normal pressure and distill the methano...

Embodiment example 2

[0052] Add 500g of crude glycerin, 383g of methyl tert-butyl ether and 25g of A35 resin catalyst into a 1000mL round-bottomed flask for ether formation reaction, heat to 80°C, and continue the reaction at 80°C for 8 hours. After the temperature drops to room temperature, the unreacted isobutene cracked is recovered, the catalyst is filtered off, and glycerol tert-butyl ether is obtained by distillation under reduced pressure.

[0053] Glycerol tert-butyl ether is transferred to the cracking reactor, and 25g cracking catalyst SO is added 3 H-MCM-41, the reaction temperature is 90°C, react for 4 hours, cool down to room temperature, recover the isobutene obtained by cracking, filter off the catalyst, dilute the obtained glycerin with 0.5 times the mass of methanol, obtain the effluent through the filter membrane, and pour it into the effluent Add acid clay with 3% glycerin mass to the liquid, stir at 80°C for 2 hours, then filter the acid clay, and distill the filtrate to obtain...

Embodiment example 3

[0056] In a 1000mL round bottom flask, add 500g of crude glycerin, 643g of tert-butanol and 35g of SO 4 2- / SiO 2 The resin catalyst undergoes ether-forming reaction, is heated to 70°C, and continues to react at 70°C for 20 hours. After the temperature drops to room temperature, the unreacted isobutene cracked is recovered, the catalyst is filtered off, and glycerol tert-butyl ether is obtained by distillation under reduced pressure.

[0057] Glycerol tert-butyl ether is transferred to the cracking reactor, and 25g cracking catalyst SO is added 4 2- / ZrO 2 -MnO 3 , the reaction temperature is 90°C, react for 4 hours, lower to room temperature, recover the isobutene obtained by cracking, filter off the catalyst, dilute the obtained glycerin with 0.2 times the mass of methanol, obtain the effluent through the filter membrane, and add the mass of glycerin to the effluent 3% acid clay, stirred at 80°C for 2 hours, then filtered the acid clay, distilled the filtrate under nor...

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PUM

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Abstract

The invention discloses a method for refining crude glycerol and relates to the technical field of chemical synthesis. The method comprises the following steps: S1, performing etherification reactionon a tert-butyl donor and the crude glycerol under the action of a solid acid catalyst according to the mole ratio of (1 to 10):1 and carrying out reduced pressure distillation to obtain glycerol tert-butyl ether; S2, performing cracking reaction on the glycerol tert-butyl ether under the catalytic action of a solid acid catalyst to obtain glycerol; diluting the glycerol with methanol, and then separating the glycerol from a catalyst through a filtering film; S3, adding acid clay into effluent to obtain a mixture, wherein the acid clay is 2 to 3 percent of the mass of the mixture, fully stirring, neutralizing and filtering; distilling and concentrating filtrate to obtain high-purity glycerol, wherein the solid acid catalyst is an acid resin catalyst or a carrier-supported acid catalyst. According to the method, the refined glycerol is obtained through direct reaction, so that the steps of neutralization, centrifugation, multi-stage distillation / distillation and the like in a traditional separation process are avoided; the process is simple; the cost is low.

Description

technical field [0001] The invention relates to the technical field of chemical synthesis, in particular to a synthesis method for refining crude glycerin. Background technique [0002] Glycerin, namely glycerol, has the general chemical properties of trihydric alcohols and can participate in various chemical reactions. Due to its many important physical and chemical properties, glycerin plays an important role in the production of coatings, salt, medicine, toothpaste, cellophane, insulating materials and other industries. At present, my country's glycerin production has been in short supply, especially high-purity (99.5%) glycerin is almost entirely dependent on imports. [0003] Glycerol is generally produced by chemical or biological fermentation. In recent years, crude oil prices have continued to rise, prompting the rapid development of the biodiesel industry in the world. About 10% of the by-product glycerol will be produced during the preparation of biodiesel. It ...

Claims

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Application Information

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IPC IPC(8): C07C29/92C07C29/80C07C31/22
CPCC07C29/80C07C29/92C07C31/225
Inventor 莫志文王源源熊东路龙绪俭肖增钧鲁晓
Owner 深圳市前海博扬研究院有限公司
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