CN107162873B - Ethylene glycol purification process - Google Patents
Ethylene glycol purification process Download PDFInfo
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- CN107162873B CN107162873B CN201710233079.6A CN201710233079A CN107162873B CN 107162873 B CN107162873 B CN 107162873B CN 201710233079 A CN201710233079 A CN 201710233079A CN 107162873 B CN107162873 B CN 107162873B
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- ethylene glycol
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- reduced pressure
- polyphosphoric acid
- filling
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C29/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
- C07C29/74—Separation; Purification; Use of additives, e.g. for stabilisation
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- Organic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention belongs to the technical field of chemical preparations, and relates to an ethylene glycol purification process which comprises the steps of adding ethylene oxide and polyphosphoric acid into an ethylene glycol crude product, adding an antioxidant, carrying out reduced pressure distillation, and then filling under the protection of nitrogen. The process can obtain glycol with extremely high purity and difficult acidification, meets the use requirement of the precision electronic industry, and has better market competitiveness.
Description
Technical Field
The invention relates to the technical field of chemical preparations, in particular to a purification process capable of producing glycol suitable for the requirement of the precision electronic industry.
Background
Ethylene glycol (ethylene glycol) is also known as "glycol",1, 2-ethylene glycol, EG for short, of the chemical formula (CH)2OH)2Is the simplest diol. The glycol can be used as solvent, antifreezing agent and raw material for synthesizing terylene.
In the precision electronics industry, the requirements for ethylene glycol are more stringent. On one hand, the glycol usually contains impurities of other metal salts, if metal ions are reduced in the manufacturing process and remain on electronic products; on the other hand, ethylene glycol is easily oxidized by air in the using process and is converted into an acidic substance, so that the ethylene glycol has a corrosion effect on metal and brings about resistance change of a lead. These may seriously affect the conductivity of the product, and become the bottleneck of improving the quality of the product.
Therefore, a new purification method is needed to obtain high-purity ethylene glycol suitable for the requirement of the precision electronics industry.
Disclosure of Invention
The invention mainly aims to provide a purification process capable of producing glycol suitable for the requirement of the precision electronic industry.
The invention realizes the purpose through the following technical scheme:
a process for purifying ethylene glycol comprises the following steps:
dehydrating: adding 1-2 wt% of ethylene oxide and 2-3 wt% of polyphosphoric acid into the crude ethylene glycol product, and stirring at 50-70 ℃ for 1.5-2 hours to obtain an organic solution;
oxidation resistance: adding 1-2 wt% of antioxidant into the organic solution obtained in the step I, and uniformly stirring to obtain a suspension;
③ reduced pressure distillation: carrying out reduced pressure distillation on the suspension obtained in the step two, and collecting fractions at the temperature of 110-115 ℃;
and fourthly, filling: and (4) filling the distillate obtained in the step (III) under the protection of nitrogen.
Specifically, the antioxidant in the second step is zinc powder.
Furthermore, the using amount of the zinc powder is 1 wt% of the crude product.
Specifically, the decompression pressure in the third step is 0.09 MPa.
Specifically, the dosage of the ethylene oxide in the step (i) is 1 wt% of the crude product, and the dosage of the polyphosphoric acid is 2 wt% of the crude product.
By adopting the technical scheme, the technical scheme of the invention has the beneficial effects that:
the process can obtain glycol with extremely high purity and difficult acidification, meets the use requirement of the precision electronic industry, and has better market competitiveness.
Detailed Description
A process for purifying ethylene glycol comprises the following steps:
dehydrating: adding 1-2 wt% of ethylene oxide and 2-3 wt% of polyphosphoric acid into the crude ethylene glycol product, and stirring at 50-70 ℃ for 1.5-2 hours to obtain an organic solution;
oxidation resistance: adding 1-2 wt% of antioxidant into the organic solution obtained in the step I, and uniformly stirring to obtain a suspension;
③ reduced pressure distillation: carrying out reduced pressure distillation on the suspension obtained in the step two, and collecting fractions at the temperature of 110-115 ℃;
and fourthly, filling: and (4) filling the distillate obtained in the step (III) under the protection of nitrogen.
The present invention will be described in further detail with reference to specific examples.
Example 1:
adding 100g of crude ethylene oxide and 200g of crude polyphosphoric acid into 10kg of crude ethylene glycol, stirring for 2 hours at the temperature of 50 ℃, wherein the ethylene oxide can protect the ethylene glycol from being oxidized, the polyphosphoric acid can deprive the crude ethylene glycol of water to generate phosphoric acid crystals, and other non-oil-soluble components containing metal impurities can be precipitated together due to loss of solvent water, so that an organic solution with low metal impurities can be obtained;
adding 100g of antioxidant zinc powder into the organic solution obtained in the step I, and uniformly stirring to obtain suspension;
③ reduced pressure distillation: carrying out reduced pressure distillation on the suspension obtained in the step II under the low pressure of 0.09MPa, and collecting fractions at the temperature of 110-115 ℃;
and fourthly, filling: filling the purified ethylene glycol into the distillate obtained in the step three under the protection of nitrogen.
Example 2:
adding 200g of crude ethylene oxide and 300g of crude polyphosphoric acid into 10kg of crude ethylene glycol, and stirring at 70 ℃ for 1.5 hours, wherein the ethylene oxide can protect the ethylene glycol from being oxidized, the polyphosphoric acid can deprive the crude ethylene glycol of water to generate phosphoric acid crystals, and other non-oil-soluble components containing metal impurities can be precipitated together due to loss of solvent water, so that an organic solution with low metal impurities can be obtained;
adding 200g of antioxidant zinc powder into the organic solution obtained in the step I, and uniformly stirring to obtain suspension;
③ reduced pressure distillation: carrying out reduced pressure distillation on the suspension obtained in the step II under the low pressure of 0.09MPa, and collecting fractions at the temperature of 110-115 ℃;
and fourthly, filling: filling the purified ethylene glycol into the distillate obtained in the step three under the protection of nitrogen.
Example 3:
adding 150g of crude ethylene oxide and 250g of crude polyphosphoric acid into 10kg of crude ethylene glycol, and stirring at 60 ℃ for 1.8 hours, wherein the ethylene oxide can protect the ethylene glycol from being oxidized, the polyphosphoric acid can deprive the crude ethylene glycol of water to generate phosphoric acid crystals, and other non-oil-soluble components containing metal impurities can be precipitated together due to loss of solvent water, so that an organic solution with low metal impurities can be obtained;
adding 150g of antioxidant zinc powder into the organic solution obtained in the step I, and uniformly stirring to obtain suspension;
③ reduced pressure distillation: carrying out reduced pressure distillation on the suspension obtained in the step II under the low pressure of 0.09MPa, and collecting fractions at the temperature of 110-115 ℃;
and fourthly, filling: filling the purified ethylene glycol into the distillate obtained in the step three under the protection of nitrogen.
The purity and acidity of the ethylene glycol obtained in examples 1 to 3 were measured according to the experimental method of GB/T7714-2005 "Industrial glycol".
Comparative example:
adding anhydrous sodium sulfate into 10kgkg of crude ethylene glycol, drying, and rectifying under normal pressure.
The purity and acidity of the ethylene glycol obtained in the control example were measured according to the experimental method of GB/T7714-2005 "Industrial ethylene glycol".
The comparison of the ethylene glycol obtained in examples 1 to 3 with that obtained in the comparative example is shown in Table 1.
Table 1:
| example 1 | Example 2 | Example 3 | Comparative example | |
| Purity/%) | 99.9 | 99.8 | 99.8 | 99.5 |
| Acidity/%) | 0.0004 | 0.0004 | 0.0005 | 0.001 |
As can be seen from Table 1, the process can obtain high-purity ethylene glycol with the purity of over 99.8 percent, and the high-purity ethylene glycol reaches the GB/T7714-. The ethylene glycol can prevent metal ions from remaining on electronic products, can reduce glycol acidification to corrode metal materials, meets the use requirements of the precision electronic industry, and has better market competitiveness.
What has been described above are merely some embodiments of the present invention. It will be apparent to those skilled in the art that various changes and modifications can be made without departing from the inventive concept thereof, and these changes and modifications can be made without departing from the spirit and scope of the invention.
Claims (3)
1. The process for purifying the ethylene glycol is characterized by comprising the following steps:
dehydrating: adding 1-2 wt% of ethylene oxide and 2-3 wt% of polyphosphoric acid into the crude ethylene glycol product, and stirring at 50-70 ℃ for 1.5-2 hours to obtain an organic solution;
oxidation resistance: adding 1-2 wt% of crude antioxidant into the organic solution obtained in the step I, wherein the antioxidant is zinc powder, and uniformly stirring to obtain a suspension;
③ reduced pressure distillation: carrying out reduced pressure distillation on the suspension obtained in the step II, wherein the reduced pressure is 0.09MPa, and collecting fractions at the temperature of 110-115 ℃;
and fourthly, filling: filling the purified ethylene glycol into the distillate obtained in the step three under the protection of nitrogen.
2. The process for purifying ethylene glycol according to claim 1, characterized in that: the amount of the zinc powder is 1 wt% of the crude product.
3. The process for purifying ethylene glycol according to claim 1, characterized in that: the dosage of the ethylene oxide in the step I is 1 wt% of the crude product, and the dosage of the polyphosphoric acid is 2 wt% of the crude product.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710233079.6A CN107162873B (en) | 2017-04-11 | 2017-04-11 | Ethylene glycol purification process |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710233079.6A CN107162873B (en) | 2017-04-11 | 2017-04-11 | Ethylene glycol purification process |
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| Publication Number | Publication Date |
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| CN107162873A CN107162873A (en) | 2017-09-15 |
| CN107162873B true CN107162873B (en) | 2021-04-13 |
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| CN201710233079.6A Active CN107162873B (en) | 2017-04-11 | 2017-04-11 | Ethylene glycol purification process |
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| JP2008024616A (en) * | 2006-07-19 | 2008-02-07 | Tohoku Univ | Blue-green algae-derived surface-active substance and method for synthesizing the same |
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