CN103435446A - Method and device for increasing chroma of finished ethylene glycol product - Google Patents
Method and device for increasing chroma of finished ethylene glycol product Download PDFInfo
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- CN103435446A CN103435446A CN2013103892364A CN201310389236A CN103435446A CN 103435446 A CN103435446 A CN 103435446A CN 2013103892364 A CN2013103892364 A CN 2013103892364A CN 201310389236 A CN201310389236 A CN 201310389236A CN 103435446 A CN103435446 A CN 103435446A
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- ethylene glycol
- alkali lye
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- methyl alcohol
- alkali
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Abstract
The invention relates to a method for increasing the chroma of a finished ethylene glycol product, which is implemented through adding prepared alkaline liquor from a spare flange port at the top of a crude ethylene glycol tank in an industrial device for producing ethylene glycol by using synthesis gas, wherein the alkaline liquor is prepared from 90% of methanol and 10% of alkali; and after the alkaline liquor is added into the crude ethylene glycol tank, stirring the obtained product. After the method and device disclosed by the invention are applied to a process of producing ethylene glycol by using synthesis gas, a situation that the chroma of an ethylene glycol product reaches a required quality index can be ensured.
Description
Technical field
The present invention relates to improve the method for ethylene glycol finished product colourity, specifically improve the method and apparatus of ethylene glycol finished product colourity in synthetic gas preparing ethylene glycol full scale plant.
Background technology
Synthetic gas preparing ethylene glycol operational path comprises esterification, carbonylation, hydrogenation and refining four operations.Current Technology present situation is as shown in Figure 1:
The methyl nitrite CH come from esterification step
3oNO(is called for short MN) with the CO that out-of-bounds comes, enter in the oxonation device, at certain temperature, certain pressure and Pt/Al
2o
3following oxonation: 2CH occurs under the effect of catalyzer
3oNO+2CO → (COOCH
3)
2+ 2NO, the dimethyl oxalate (COOCH of generation
3)
2(being called for short DMO) enters gas-liquid separator separates after condensation, and the DMO be not condensed on a small quantity in gas phase enters scrubber tower again.Because methyl alcohol can dissolve DMO, do further washing absorption with methanol solution, the still liquid after absorption is after method separation tower is isolated methyl alcohol, and the pure DMO liquid obtained at the bottom of tower and the liquid-phase product DMO of gas-liquid separator come along hydrogenation process.
The DMO that carbonylation comes enters in hydrogenator with the hydrogen out-of-bounds come after DMO gasifier heating and gasifying, at certain temperature, certain pressure and Cu/SiO
2hydrogenation reaction occurs under the effect of catalyzer: (COOCH
3)
2+ 4H
2→ (CH
2oH)
2+ 2CH
3oH, the ethylene glycol (CH of generation
2oH)
2after condensation, gas-liquid separation, the thick ethylene glycol of the liquid phase obtained entered thick ethylene glycol groove, more different rectifying tower is separated, purifies through refining step, finally obtains the ethylene glycol product of required quality (being called for short EG).
The problem existed is as follows:
In the art production process of whole ethylene glycol, the thick ethylene glycol obtained be not that clear, colorless, but slightly yellow with one all the time, this has had a strong impact on the requirement to colourity of quality product.To thick ethylene glycol product analysis, show that causing thick ethylene glycol is because have acidic substance in thick ethylene glycol product in the reason of colourity jaundice, is specially oxalic acid through repeatedly.The reason of oxalic is because the methyl alcohol in scrubber tower contains moisture content, to the oxalic acid diformazan hydrolysis oxalic made in scrubber tower.
In the scrubber tower of carbonylation operation, methyl alcohol as absorption liquid, water content is pressed the methyl alcohol national standard, in the top grade product, H2O is also 0.1%, DMO meets water electrode and hydrolysis easily occurs and oxalic, and in scrubber tower, the methyl alcohol absorption liquid just with DMO, the hydrolysis oxalic occurs containing micro-water like this, makes still liquid be slightly acidic, and method separation tower can't remove oxalic acid, the final so thick ethylene glycol of hydrogenation products that causes is slightly acidic.Inventing problem to be solved is exactly how to make the colourity of thick ethylene glycol become transparent clarification.
Summary of the invention
Technical problem solved by the invention is to provide a kind of method that can improve ethylene glycol finished product colourity in synthetic gas preparing ethylene glycol full scale plant, makes the colourity of thick ethylene glycol become transparent clarification.This invention can guarantee that the colourity of ethylene glycol product reaches required quality index.
For achieving the above object, the present invention is by the following technical solutions:
A kind of method that improves ethylene glycol finished product colourity, be in synthetic gas preparing ethylene glycol full scale plant, and the backup flange mouth place at thick ethylene glycol groove top therein adds the alkali lye prepared, and the methyl alcohol that described alkali lye is 90% and 10% alkali are formulated; After it is added to thick ethylene glycol groove, stirred.
Aforesaid method, described alkali lye, for the oxalic acid of neutralized crude ethylene glycol, can be selected according to technician's experience, and operable alkali includes but not limited to sodium hydroxide, potassium hydroxide, sodium bicarbonate etc.
A kind of synthetic gas preparing ethylene glycol full scale plant, be in synthetic gas preparing ethylene glycol full scale plant, and an alkali lye conservation tank is added at thick ethylene glycol groove top therein, for the alkali lye by having prepared, adds described thick ethylene glycol groove; The methyl alcohol that described alkali lye is 90% and 10% alkali are formulated.
Technical scheme of the present invention is can not meet the characteristics of water in conjunction with this technique mesoxalic acid dimethyl ester, in the preparation of alkali lye, just can not carry out by water, can only be prepared with methanol solution, and prepared by 90% methyl alcohol and 10% alkali, go neutralization acid wherein, add at the backup flange mouth place at thick ethylene glycol groove top the alkali lye prepared, and stirred, through such processing, will find that the color of thick ethylene glycol becomes as clear as crystal color by original micro-yellow.The methyl alcohol added in thick ethylene glycol enters in the first treating tower of refining step and is separated, methyl alcohol is from the top extraction of dealcoholize column, and still liquid further separates, purifies through second, third treating tower again and finally obtains meeting the polyester grade ethylene glycol product of quality index.
The beneficial effect that the present invention obtains has:
The present invention can guarantee that the colourity of ethylene glycol product reaches required quality index after applying on synthetic gas preparing ethylene glycol production technique.
The accompanying drawing explanation
Fig. 1 is the artwork before improving, wherein: 1, NO circulation gas de-esterifying operation; 2, esterification carrys out methyl nitrite; 3, out-of-bounds carry out CO; 4, oxonation device; 5 and 12, nitrogen compressor; 6 and 14, gas-liquid separator; 7, scrubber tower; 8, out-of-bounds carry out methyl alcohol; 9, DMO recovery tower; 10, out-of-bounds supplement H
2; 11, DMO gasifier; 13, hydrogenator; 15, thick ethylene glycol groove; 16, the first treating tower; 17, the second treating tower; 18, remove the 3rd treating tower;
Fig. 2 is the artwork after improving, wherein: 1, NO circulation gas de-esterifying operation; 2, esterification carrys out methyl nitrite; 3, out-of-bounds carry out CO; 4, oxonation device; 5 and 12, nitrogen compressor; 6 and 14, gas-liquid separator; 7, scrubber tower; 8, out-of-bounds carry out methyl alcohol; 9, DMO recovery tower; 10, out-of-bounds supplement H
2; 11, DMO gasifier; 13, hydrogenator; 15, alkali lye conservation tank; 16, thick ethylene glycol groove; 17, the first treating tower; 18, the second treating tower; 19, remove the 3rd treating tower.
Embodiment
For further illustrating the present invention, illustrate with the following Examples:
As shown in Figure 2, a kind of synthetic gas preparing ethylene glycol full scale plant, be in synthetic gas preparing ethylene glycol full scale plant, and an alkali lye conservation tank 15 is added at thick ethylene glycol groove top therein, for the alkali lye by having prepared, adds described thick ethylene glycol groove; The methyl alcohol that described alkali lye is 90% and 10% alkali are formulated.
Alkali lye, for the oxalic acid of neutralized crude ethylene glycol, can be selected according to technician's experience, and operable alkali includes but not limited to sodium hydroxide, potassium hydroxide, sodium bicarbonate etc.After it is added to thick ethylene glycol groove, stirred.Through such processing, will find that the color of thick ethylene glycol becomes as clear as crystal color by original micro-yellow.The methyl alcohol added in thick ethylene glycol enters in the first treating tower of refining step and is separated, methyl alcohol is from the top extraction of dealcoholize column, and still liquid further separates, purifies through second, third treating tower again and finally obtains meeting the polyester grade ethylene glycol product of quality index.
Above-described embodiment is described the preferred embodiment of the present invention; not scope of the present invention is limited; design under the prerequisite of spirit not breaking away from the present invention; various distortion and improvement that the common engineering technical personnel in this area make technical scheme of the present invention, all should fall in the definite protection domain of claims of the present invention.
Claims (3)
1. a method that improves ethylene glycol finished product colourity, it is characterized in that: in synthetic gas preparing ethylene glycol full scale plant, the backup flange mouth place at thick ethylene glycol groove top therein adds the alkali lye prepared, and the methyl alcohol that described alkali lye is 90% and 10% alkali are formulated; After it is added to thick ethylene glycol groove, stirred.
2. method according to claim 1 is characterized in that: described alkali lye is for the oxalic acid of neutralized crude ethylene glycol.
3. a synthetic gas preparing ethylene glycol full scale plant is characterized in that: in synthetic gas preparing ethylene glycol full scale plant, an alkali lye conservation tank is added at thick ethylene glycol groove top therein, for the alkali lye by having prepared, adds described thick ethylene glycol groove; The methyl alcohol that described alkali lye is 90% and 10% alkali are formulated.
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| Application Number | Priority Date | Filing Date | Title |
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| CN2013103892364A CN103435446A (en) | 2013-08-31 | 2013-08-31 | Method and device for increasing chroma of finished ethylene glycol product |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2013103892364A CN103435446A (en) | 2013-08-31 | 2013-08-31 | Method and device for increasing chroma of finished ethylene glycol product |
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| CN2013103892364A Pending CN103435446A (en) | 2013-08-31 | 2013-08-31 | Method and device for increasing chroma of finished ethylene glycol product |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116514637A (en) * | 2023-03-10 | 2023-08-01 | 南京化学试剂股份有限公司 | High-purity high-stability ethylene glycol refining process and application |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4349417A (en) * | 1980-01-18 | 1982-09-14 | Hoechst Aktiengesellschaft | Process for the manufacture of extremely pure monoethylene glycol |
| CN101462961A (en) * | 2008-01-28 | 2009-06-24 | 上海戊正工程技术有限公司 | Process flow for producing ethylene glycol with coproduction product dimethyl carbonate |
| CN102649704A (en) * | 2011-02-25 | 2012-08-29 | 中国石油化工股份有限公司 | Method for purifying ethylene glycol product |
-
2013
- 2013-08-31 CN CN2013103892364A patent/CN103435446A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4349417A (en) * | 1980-01-18 | 1982-09-14 | Hoechst Aktiengesellschaft | Process for the manufacture of extremely pure monoethylene glycol |
| CN101462961A (en) * | 2008-01-28 | 2009-06-24 | 上海戊正工程技术有限公司 | Process flow for producing ethylene glycol with coproduction product dimethyl carbonate |
| CN102649704A (en) * | 2011-02-25 | 2012-08-29 | 中国石油化工股份有限公司 | Method for purifying ethylene glycol product |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116514637A (en) * | 2023-03-10 | 2023-08-01 | 南京化学试剂股份有限公司 | High-purity high-stability ethylene glycol refining process and application |
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Application publication date: 20131211 |