Glycerol black residue recycling process

A glycerin black foot and process technology, applied in the field of glycerin black foot recovery process, can solve the problems of no re-distillation, inability to discharge directly, troublesome treatment of glycerin black foot, etc., and achieve the effects of reducing energy consumption, protecting the environment, and achieving great social benefits.

Inactive Publication Date: 2019-04-05
NANTONG XINBANG CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At this time, the salt content in the black foot is relatively high, reaching more than 20%, but there are still about 75% glycerin and polyglycerol. The processing of glycerin black foot is troublesome, and it cannot be directly discharged, and it cannot be distilled again.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] The present embodiment glycerin black foot recovery process, this recovery process comprises the steps:

[0016] Step S1: Add 1.0 tons of glycerin black foot into the reaction kettle, and then add 1.8 tons of methanol into the reaction kettle to dissolve;

[0017] Step S2: After the glycerin blackfoot is fully dissolved in methanol, it is pumped into 4.25 tons of ethyl acetate, and fully stirred for 30 minutes, and then filtered through a filter to obtain a filter residue and a filtrate;

[0018] Step S3: After standing the filtrate in step S2 for 1 hour, separate the liquid, collect the upper layer solution, and put the lower layer waste liquid into barrels;

[0019] Step S4: The upper layer solution collected in step S3 was distilled under reduced pressure at 45-50°C and concentrated to obtain 880kg of glycerol and polyglycerol. The measured glycerin content was 94.9%, and the yield was 88.0%. Methanol was recovered.

Embodiment 2

[0021] The present embodiment glycerin black foot recovery process, this recovery process comprises the steps:

[0022] Step S1: Add 1.0 tons of glycerin black foot into the reaction kettle, and then add 1.8 tons of methanol into the reaction kettle to dissolve;

[0023] Step S2: After the glycerin blackfoot is fully dissolved in methanol, it is pumped into 4.75 tons of ethyl acetate, and fully stirred for 30 minutes, and then filtered through a filter to obtain a filter residue and a filtrate;

[0024] Step S3: After standing the filtrate in step S2 for 1 hour, separate the liquid, collect the upper layer solution, and put the lower layer waste liquid into barrels;

[0025] Step S4: The upper layer solution collected in step S3 was distilled under reduced pressure at 45-50°C and concentrated to obtain 750kg of glycerol and polyglycerol. The glycerol content was measured to be 96.5%, and the yield was 75.0%. Methanol was recovered.

Embodiment 3

[0027] The present embodiment glycerin black foot recovery process, this recovery process comprises the steps:

[0028] Step S1: Add 1.0 tons of glycerin black foot into the reaction kettle, and then add 1.8 tons of methanol into the reaction kettle to dissolve;

[0029] Step S2: After the glycerol blackfoot is fully dissolved in methanol, pump it into 4.5 tons of ethyl acetate, and fully stir for 30 minutes, then filter through a filter to obtain a filter residue and a filtrate;

[0030] Step S3: After standing the filtrate in step S2 for 1 hour, separate the liquid, collect the upper layer solution, and put the lower layer waste liquid into barrels;

[0031] Step S4: The upper layer solution collected in step S3 was distilled under reduced pressure at 45-50°C and concentrated to obtain 800kg of glycerol and polyglycerol. The measured glycerol content was 95.9%, and the yield was 80.0%. Methanol was recovered.

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PUM

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Abstract

The invention relates to a glycerol black residue recycling process. The glycerol black residue recycling process comprises the following steps: step S1, adding glycerol black residues in a reaction kettle, adding an alcohol solvent in the reaction kettle and dissolving the glycerol black residues; step S2, after fully dissolving the glycerol black residues with the alcohol solvent, pumping the glycerol black residues into ethyl acetate, fully stirring for 20-40 min, and filtering via a filter to obtain filter residues and filtrate; step S3, leaving the filtrate in step S2 standstill for 0.5-2h, then carrying out liquid separation, collecting an upper solution, and packing lower waste liquid in a barrel; and step S4, distilling the upper solution collected in step S3 under reduced pressure at the temperature of 45-50 DEG C, concentrating to obtain glycerol and polyglycerol, and recycling the alcohol solvent and the ethyl acetate. The glycerol black residue recycling process has the advantages that by the glycerol black residue recycling process, the glycerol and the polyglycerol can be recycled effectively, energy consumption is reduced, and the environment is protected.

Description

technical field [0001] The invention relates to a process for treating chemical waste, in particular to a process for recovering glycerin and black feet. Background technique [0002] The waste glycerin and black feet produced in chemical production will undoubtedly increase the production cost as waste. For this reason, manufacturers who currently produce glycerin generally distill the remaining glycerin and black feet for re-distillation. At this time, the salt content in the black foot is relatively high, reaching more than 20%, but there are still about 75% glycerin and polyglycerol. The processing of glycerol black foot is troublesome, and it cannot be directly discharged, and it cannot be distilled again. [0003] In this context, it is urgent to deal with glycerin black feet through a series of technologies, recover glycerin and polyglycerol, reduce energy consumption and protect the environment. Contents of the invention [0004] The technical problem to be solved...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C29/74C07C29/80C07C29/86C07C31/22C07C41/34C07C41/38C07C41/42C07C43/13C08J11/08C08L71/02
CPCC07C29/74C07C29/80C07C29/86C07C41/34C07C41/38C07C41/42C08J11/08C08J2371/02C07C31/225C07C43/13C07C43/135Y02W30/62
Inventor 周松涛王霄林石盈银
Owner NANTONG XINBANG CHEM
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