CN1332915C - Method for recovering solvent from alkine in high-grade - Google Patents
Method for recovering solvent from alkine in high-grade Download PDFInfo
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- CN1332915C CN1332915C CNB2005100731031A CN200510073103A CN1332915C CN 1332915 C CN1332915 C CN 1332915C CN B2005100731031 A CNB2005100731031 A CN B2005100731031A CN 200510073103 A CN200510073103 A CN 200510073103A CN 1332915 C CN1332915 C CN 1332915C
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- solvent
- basic cpd
- aqueous solution
- higher alkyne
- water
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- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
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Abstract
The present invention relates to a method for recovering solvent from higher alkyne. The method comprises: N-methyl pyrrolidone is used as solvent, selective absorption is carried out to mixed gas generated in the partial oxidation of hydrocarbons, the mixed gas is divided into tail gas, concentrated acetylene and higher alkyne, the higher alkyne is washed with water for recovering solvent entrained in the higher alkyne, the higher alkyne enters a water washing tower from the bottom of the water washing tower, aqueous solution containing alkaline compounds and washing water together enter the water washing tower from the top of the water washing tower, and mixed condensate containing alkaline compounds, water and solvent is collected from the bottom of the water washing tower and is sent into a solvent circulation system. The method provided by the present invention destroys the hydrolysis condition of N-methyl pyrrolidone, reduces the corrosion of the water washing tower, and reduces the consumption of solvent.
Description
Technical field
The present invention relates to from the technology of hydro carbons partial oxidation acetylene, utilize solvent to reclaim the method for solvent to acetylene concentration and from higher alkyne, particularly reclaim the processing method of N-Methyl pyrrolidone (NMP).
Background technology
In the technology of the hydro carbons partial oxidation acetylene of Germany BASF AG exploitation, use N-Methyl pyrrolidone (NMP) as solvent, by NMP the selectivity of acetylene is absorbed, finally the mixed gas that reaction is generated is separated into tail gas (CO, H
2Deng), dense acetylene, senior alkynes mixed gas (C
4Above component).Wherein to reclaim the nmp solvent of wherein carrying secretly by washing to higher alkyne.
Character according to nmp solvent can know, system moisture～50%, temperature more than 50 ℃ the time, hydrolysis can take place in NMP, generates the very strong acid of a kind of corrodibility.And the design operation condition of the higher alkyne water wash column of BASF AG meets the said hydrolyzed condition just, therefore can cause the tower internal corrosion.In order to prevent the corrosion of nmp solvent, in the technology of BASF AG's exploitation, with Na to water wash column
2CO
3Solution joins among the water wash column mixing condensation liquid, enters solvent circulation together in company with mixing condensation liquid again.But, adopt the long-term practice of BASF technology to prove by us, this production technique exists not enough, mainly shows Na
2CO
3All the time be present in the middle of the liquid phase of solvent, can't enter among the gas phase of solvent, also just can't regulate the pH value of the solvent that obtains by vapor condensation, cause the internal corrosion of higher alkyne water wash column more serious, and the actual consumption amount of this tower NMP is higher.
GB 1124750A discloses by add an alkali metal salt in solvent and has prevented to reclaim the ruined method of equipment in the acetylene process, wherein points out, with Na
2CO
3Join in the aqueous solution of NMP as the solvent that reclaims acetylene.The purpose of this invention is that the polymkeric substance that produces when preventing solvent recuperation acetylene deposits on equipment, rather than prevents corrosion.
Summary of the invention
The present invention proposes the novel method that reclaims solvent from higher alkyne, this method can reduce the content of higher alkyne water wash column inner acidic material, thereby reduces equipment corrosion, reduces NMP and consumes, and guarantees the stable long-term operation of total system.
The method that reclaims solvent from higher alkyne provided by the invention comprises that as solvent, the mixed gas that the hydro carbons partial oxidation is produced carries out the selectivity absorption, and mixed gas is separated into tail gas (CO, H with N-Methyl pyrrolidone (NMP)
2Deng), dense acetylene and higher alkyne (C
4Above component), higher alkyne is washed the solvent of wherein carrying secretly to reclaim, higher alkyne enters water wash column at the bottom of tower, the aqueous solution that contains basic cpd enters water wash column with wash water from cat head, at the bottom of tower, collect the mixing condensation liquid that contains basic cpd, water and solvent, and it is sent into solvent circulation.
Said basic cpd is selected from the oxyhydroxide of basic metal and alkaline-earth metal or carbonate, phosphoric acid salt, acetate, as in sodium hydroxide, potassium hydroxide, magnesium hydroxide, calcium hydroxide, hydrated barta, yellow soda ash, salt of wormwood, sodium bicarbonate, saleratus, Calcium hydrogen carbonate, sodium phosphate, potassiumphosphate, sodium-acetate and the Potassium ethanoate one or more, preferred sodium hydroxide, potassium hydroxide, yellow soda ash, salt of wormwood, sodium bicarbonate, most preferably yellow soda ash.
The concentration of the said basic cpd aqueous solution is controlled at 0.02～1wt%, between preferred 0.2～0.6wt%.The aqueous solution preferably adopts continuous adding mode.The flow control of the basic cpd aqueous solution is at 0.04～0.125m
3/ h's, preferred 0.05～0.08m
3The scope of/h, the flow control of wash water is at 2.5～7.5m
3/ h, preferred 3.5～5.5m
3The scope of/h.The add-on of the basic cpd aqueous solution preferably can make at the bottom of the tower pH value in the liquid phase greater than 5.5, to reduce the acid corrosion of system.
The present invention adopts new operational path, has destroyed the hydrolysising condition of N-Methyl pyrrolidone, has reduced the tower internal corrosion, has reduced the consumption of solvent, makes at the bottom of the tower that solvent reaches more than the 65wt% in the liquid phase.
Description of drawings
Accompanying drawing is the concrete technical process of adopting of carrying dense acetylene of the present invention.
Embodiment
As shown in drawings, at Na
2CO
3Compound concentration is the aqueous sodium carbonate of 0.6wt% in the solution Preparation tank, by a volume pump, adopts operate continuously, quantitatively with Na
2CO
3Solution with join higher alkyne water wash column top, Na after wash water mixes
2CO
3Solution successively descends on tower tray with wash water, and contact with the air-flow that rises, by the nmp solvent steam in the washing upstream, in time with system in the acidic substance that produce react, eliminate of the corrosion of this acidic substance to tower, at last, Na
2CO
3Solution with tower at the bottom of mixing condensation liquid enter in the solvent cycle of system, balance the pH value of system's solvent.Na
2CO
3The flow of solution and wash water is controlled at 0.065m respectively
3/ h and 3.2m
3/ h, mixing condensation liquid pH value is controlled at 8.5 at the bottom of the tower.
Implement after this technology, the corrosion situation of higher alkyne water wash column inside obviously reduces, and obviously corrosion is not found in operation for many years continuously, because of etching problem this tower is not overhauled yet; The consumption of solvent also significantly reduces simultaneously, and the consumption of average every month NMP is reduced to 5～20wt% of former technology.
Claims (7)
1. the C that from hydro carbons partial oxidation acetylene technology, produces
4Reclaim the method for solvent in the above higher alkyne, comprise, as solvent, the mixed gas that the hydro carbons partial oxidation is produced carries out the selectivity absorption, and mixed gas is separated into tail gas, dense acetylene and C with N-Methyl pyrrolidone
4Above higher alkyne, higher alkyne is washed the solvent of wherein carrying secretly to reclaim, higher alkyne enters water wash column at the bottom of tower, the aqueous solution that contains basic cpd enters water wash column with wash water from cat head, at the bottom of tower, collect the mixing condensation liquid that contains basic cpd, water and solvent, and it is sent into solvent circulation, said basic cpd is selected from alkali-metal oxyhydroxide, carbonate, phosphoric acid salt or acetate.
2. in accordance with the method for claim 1, it is characterized in that said basic cpd is sodium hydroxide, potassium hydroxide, yellow soda ash, salt of wormwood or sodium bicarbonate.
3. in accordance with the method for claim 1, it is characterized in that the concentration of the said basic cpd aqueous solution is controlled between 0.02～1wt%.
4. in accordance with the method for claim 3, it is characterized in that the concentration of the said basic cpd aqueous solution is controlled between 0.2～0.6wt%.
5. in accordance with the method for claim 1, it is characterized in that the flow control of the basic cpd aqueous solution is at 0.04～0.125m
3The scope of/h, the flow control of wash water is at 2.5～7.5m
3The scope of/h.
6. in accordance with the method for claim 5, it is characterized in that the flow control of the basic cpd aqueous solution is at 0.05～0.08m
3The scope of/h, the flow control of wash water is at 3.5～5.5m
3The scope of/h.
7. in accordance with the method for claim 1, it is characterized in that the add-on of the basic cpd aqueous solution makes at the bottom of the tower pH value in the liquid phase greater than 5.5.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2005100731031A CN1332915C (en) | 2005-05-31 | 2005-05-31 | Method for recovering solvent from alkine in high-grade |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2005100731031A CN1332915C (en) | 2005-05-31 | 2005-05-31 | Method for recovering solvent from alkine in high-grade |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1872821A CN1872821A (en) | 2006-12-06 |
| CN1332915C true CN1332915C (en) | 2007-08-22 |
Family
ID=37483444
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB2005100731031A Active CN1332915C (en) | 2005-05-31 | 2005-05-31 | Method for recovering solvent from alkine in high-grade |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1332915C (en) |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102701896B (en) * | 2012-06-06 | 2014-06-25 | 西南石油大学 | Composite solvent for purifying acetylene and purification method thereof |
| CN107954820A (en) * | 2016-10-17 | 2018-04-24 | 中国石油化工股份有限公司 | A kind of method for removing the thick middle-and-high-ranking alkynes of acetylene gas |
| CN113680180A (en) * | 2021-10-25 | 2021-11-23 | 东营科宏化工有限公司 | Acetylene gas recovery device for producing alkylphenol acetylene tackifying resin |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE1124750B (en) * | 1957-12-23 | 1962-03-01 | Ibm Deutschland | Arrangement for identifying characters |
| DE1908619A1 (en) * | 1969-02-21 | 1970-09-03 | Basf Ag | Process for the production of acetylene |
-
2005
- 2005-05-31 CN CNB2005100731031A patent/CN1332915C/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE1124750B (en) * | 1957-12-23 | 1962-03-01 | Ibm Deutschland | Arrangement for identifying characters |
| DE1908619A1 (en) * | 1969-02-21 | 1970-09-03 | Basf Ag | Process for the production of acetylene |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1872821A (en) | 2006-12-06 |
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