CN103360221A - Method for deeply removing sulfides in MTBE - Google Patents
Method for deeply removing sulfides in MTBE Download PDFInfo
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- CN103360221A CN103360221A CN2013103001406A CN201310300140A CN103360221A CN 103360221 A CN103360221 A CN 103360221A CN 2013103001406 A CN2013103001406 A CN 2013103001406A CN 201310300140 A CN201310300140 A CN 201310300140A CN 103360221 A CN103360221 A CN 103360221A
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Abstract
A provided method for deeply removing sulfides in MTBE comprises the following steps: sulfur-containing MTBE enters into a tower kettle from the bottom of a first sulfide absorbing tower and the first sulfide absorbing tower is a rectifying tower; the absorption of most sulfides is completed via countercurrent contacting between the gasified MTBE mixture and a liquid-phase sulfide absorbent; then the gasified MTBE mixture containing a small amount of the sulfides enters into a second sulfide absorbing tower and is dispersed to the interior of the liquid-phase absorbent, and the deep absorption of the sulfides is completed via contacting of gas phase and liquid phase; and finally an absorbent absorbing the sulfides and a MTBE product subjected to deep removing of the sulfides are obtained. The high-purity low-sulfur-content MTBE product is obtained at the top of the second sulfides absorbing tower; the sulfur-containing absorbent can be regenerated for cycle use by a method of normal-pressure distillation or underpressure distillation, and the sulfides are recovered at the same time; and the method helps to reduce the sulfide content in MTBE from 600-1000 [mu]g/g to 10 [mu]g/g or less, and the product yield of MTBE is larger than 99.8%.
Description
Technical field
The invention belongs to the petrochemical technology field, be specifically related to the technology of deep removal MTBE medium sulphide content.
Background technology
Methyl tertiary butyl ether (being called for short MTBE) is iso-butylene and methyl alcohol addition reaction product in the liquefied petroleum gas (LPG) C-4-fraction, as gasoline dope, has good anti-knocking property.The compatibility of it and gasoline is good, and suction is few, environmentally safe.As the organic synthesis raw material, but the iso-butylene of preparing high-purity.
Sulphur in the MTBE product that the MTBE device is produced mostly is greatly organosulfur, mostly be mercaptan, thiophene, thioether class material, because of the raw liquefied petroleum gas difference, the MTBE medium sulphide content has the diversity of composition, the characteristics of sulphur content a wider range, especially under the situation that the lower boiling sulfide content is higher among the MTBE, with the method for general rectifying, sulfide is difficult to deep removal.
Summary of the invention
The object of the invention is to: in order to solve sulphur content a wider range in the prior art, the deficiency of the MTBE product rectifying desulfurization technology that particularly the lower boiling sulfide content is higher, develop a kind of split type absorption tower device and method with double absorption function, thereby realized the deep desulfuration of MTBE.
In order to achieve the above object, the present invention is by the following technical solutions:
A kind of method of deep removal MTBE medium sulphide content is provided, may further comprise the steps: sulfur-bearing MTBE enters tower reactor from bottom, the first sulfide absorption tower, the first sulfide absorption tower is rectifying tower, the absorption that the MTBE mixture of gasification and liquid phase sulfide absorption agent counter current contact are finished most of sulfide, then the gas phase MTBE mixture that contains a small amount of sulfide enters the second sulfide absorption tower, and be dispersed to liquid absorbent inside, the degree of depth of finishing sulfide by gas-liquid two-phase contact absorbs, the absorption agent of the sulfide that finally has been absorbed and through the MTBE of deep desulfuration product.
In a kind of preferred scheme of the present invention, the absorption agent of sulfide that comprised the absorption that to obtain in described the first sulfide absorption tower and the second sulfide absorption tower, discharge from described the first sulfide absorption tower and bottom, the second sulfide absorption tower respectively, enter the absorbent regeneration tower, after regenerator column is processed, the sulfide that the reclaiming cat head obtains returns the absorbent regeneration that obtains at the bottom of the recovery tower simultaneously the first and second sulfide absorption towers and recycles.
In the another kind of preferred scheme of the present invention, comprise with obtain in described the second sulfide absorption tower through the MTBE of deep desulfuration product through the cooling after, part MTBE refluxes and enters described the first sulfide absorption tower, another part MTBE is through MTBE product introduction products pot, and reflux ratio is: 0.2～10.
At the bottom of the first sulfide absorption tower tower reactor of the present invention and the second sulfide absorbing tower, can also further load dumped packing.
Described dumped packing comprises one or more the mixture in rectangular saddle ring, cascade ring, Pall ring, Raschig ring, conjugate ring, Taylor's garland, hollow many-sided ball, ball float or the θ type filler.
The absorption agent that uses in the inventive method is selected from acetonitrile, propionitrile, vinylformic acid, Monomethylamine solution, dimethylamine solution, trimethylamine solution, N, N-N,N-DIMETHYLACETAMIDE, N-Methyl pyrrolidone, morpholine, N-methylmorpholine, methane amide, ethanamide, dimethyl formamide, N-formyl morpholine N-or acetyl morphine, can be a kind of simple absorption agent, also can be composite absorber; Preferred methane amide, ethanamide, dimethyl formamide, N-formyl morpholine N-, acetyl morphine or two or more mixture wherein.
Absorption agent add-on and MTBE inlet amount mass ratio are 0.5～3:1 in the first sulfide absorption tower of the present invention.
The preferred method of the present invention, as shown in Figure 1, sulfur methyl tertiary butyl ether (MTBE) enters the first sulfide absorption tower 3-2 tower reactor from sulfur-bearing MTBE opening for feed 2, feed pressure is 0.1～1.5MPa, feeding temperature is 40～150 ℃, 65～90 ℃ of tower reactor control temperature, with the absorption agent counter current contact of the first sulfide absorption tower 3-2 middle part by 1 adding of the first sulfide absorptive tower absorbent opening for feed, in the first sulfide absorption tower, finish removing of most of sulfide, the MTBE that removes most of sulfide enters the second sulfide absorption tower 3-1 by the gaseous phase outlet pipe 3-3 of the first sulfide absorption tower 3-2 cat head again, in the second sulfide absorption tower, MTBE is dispersed to liquid absorbent inside, finish degree of depth Absorption Desulfurization by the gas-liquid two-phase contact, the qualified MTBE that obtains enters the second sulfide absorption tower cat head condenser 4, cat head control temperature is 50～60 ℃, pressure is normal pressure, after overhead condenser 4 coolings, temperature is that 40～50 ℃ MTBE enters return tank 5, enter reflux pump 7 through return tank outlet pipe 6,7 effect next section MTBE enter the first sulfide absorption tower 3-2 through return line 10 at reflux pump, another part MTBE enters products pot through MTBE products export pipe 11, and reflux ratio is: 0.2～10; Contain sulfur absorbing agent from the first sulfide absorption tower 3-2 tower reactor and the second sulfide absorption tower 3-1 bottom, treat that through the first sulfide absorption tower absorbent regeneration outlet pipe 8 and the second sulfide absorption tower treat that absorbent regeneration outlet pipe 12 enters absorbent regeneration tower 13, during regenerator column 13 normal pressure: the tower reactor temperature is 200～250 ℃, and tower top temperature is 90～160 ℃; During decompression: the tower reactor temperature is 60～90 ℃, and tower top temperature is 50～60 ℃, and the sulfide of removed overhead is delivered to sulfur recovery system through condenser 14 by sulfide outlet pipe 15; The rear absorption agent of regeneration enters absorption agent pipeline 1 and recycles behind condenser 17 at the bottom of the tower.
Separate absorbent and the degree of depth on the second sulfide absorption tower two-part secondary deep sulfur method that absorb of the present invention by adopting the first sulfide absorption tower, the MTBE desulfurization degree of acquisition is significantly improved, in addition, the inventive method also has the following advantages compared with the prior art:
(1) the MTBE Absorption Desulfurization belongs to physical process, and technical process is simple, invests low;
(2) absorption agent is renewable recycles, and reclaims sulfide.
(3) can use sulfide content 600～1000 μ g/g in the wider situation of MTBE medium sulphide content content.
(4) MTBE yield and desulfurization degree are high, and below the final sulphur content 10 μ g/g, MTBE purpose product yield is greater than 99.8%.
(5) the MTBE desulfurization process is simple, invests low.
Description of drawings
Fig. 1 is the process flow sheet of the described methyl tertiary butyl ether of embodiment 2-5 (MTBE) integrated secondary reboiled absorber deep desulfuration.
Among the figure: 1, the first sulfide absorptive tower absorbent opening for feed; 2, sulfur-bearing MTBE opening for feed; 3-1, the second sulfide absorption tower; 3-2, the first sulfide absorption tower; 3-3, the first sulfide absorption tower top gaseous phase outlet pipe; 4, the second sulfide absorption tower cat head condenser; 5, return tank; 6, return tank outlet pipe; 7, reflux pump; 8, the absorbent regeneration outlet pipe is treated on the first sulfide absorption tower; 9, the first sulfide absorption tower tower bottom reboiler; 10, return line; 11, MTBE products export pipe; 12, the absorbent regeneration outlet pipe is treated on the second sulfide absorption tower; 13, absorbent regeneration tower; 14, regenerator column overhead condenser; 15, sulfide outlet pipe; 16, well heater at the bottom of the regenerator column tower; 17, absorption agent water cooler.
Embodiment
Embodiment 1
The method of the contained MTBE sulfide of a kind of deep removal, that sulfur-bearing MTBE enters tower reactor from bottom, the first sulfide absorption tower, the first sulfide absorption tower is rectifying tower, the absorption that the MTBE mixture of gasification and liquid phase sulfide absorption agent counter current contact are finished most of sulfide, then the gas phase MTBE mixture that contains a small amount of sulfide enters the second sulfide absorption tower, and be dispersed to liquid absorbent inside, the degree of depth of finishing sulfide by gas-liquid two-phase contact absorbs, the absorption agent of the sulfide that finally has been absorbed and through the MTBE of deep desulfuration product; With the absorption that obtains in described the first sulfide absorption tower and the second sulfide absorption tower absorption agent of sulfide discharge from described the first sulfide absorption tower and bottom, the second sulfide absorption tower respectively, enter the absorbent regeneration tower, after regenerator column is processed, the sulfide that the reclaiming cat head obtains returns the absorbent regeneration that obtains at the bottom of the recovery tower simultaneously the first and second sulfide absorption towers and recycles; With obtain in described the second sulfide absorption tower through the MTBE of deep desulfuration product after cooling, a part of MTBE refluxes and enters described the first sulfide absorption tower, another part MTBE is through MTBE product introduction products pot, reflux ratio is: 5; The first sulfide absorption tower tower reactor and bottom, the second sulfide absorption tower, the filling dumped packing;
As shown in Figure 1, its step is as follows:
Measuring first pure methane amide absorption agent 200ml adds in the first sulfide absorption tower tower reactor, and then measure pure methane amide absorption agent 100ml and add in the second sulfide absorption tower tower body, sulphur content is that the MTBE of 620 μ g/g steeps charging through the first sulfide absorption tower tower reactor pucking, MTBE volume pump flow is 300ml/h, the first sulfide absorption tower is rectifying tower, the tower reactor temperature is controlled at 75～80 ℃, the absorption agent counter current contact that the METB mixture is added by the first sulfide absorptive tower absorbent opening for feed 1 with the first sulfide absorption tower 3-2 middle part under thermogenic action, in the first sulfide absorption tower, finish removing of most of sulfide, the MTBE that removes most of sulfide enters the second sulfide absorption tower 3-1 by the gaseous phase outlet pipe 3-3 of the first sulfide absorption tower 3-2 cat head again, in the second sulfide absorption tower, MTBE is dispersed to liquid absorbent inside, finish degree of depth Absorption Desulfurization by the gas-liquid two-phase contact, the qualified MTBE that obtains enters the second sulfide absorption tower cat head condenser 4, tower top temperature is 52～56 ℃, pressure is normal pressure, after overhead condenser 4 coolings, temperature is that 40～50 ℃ MTBE enters return tank 5, enter reflux pump 7 through return tank outlet pipe 6,7 effect next section MTBE enter the first sulfide absorption tower 3-2 through return line 10 at reflux pump, another part MTBE enters products pot through MTBE products export pipe 11, and reflux ratio is: 5; The methane amide absorption agent of sulphur content 53000 μ g/g is from the first sulfide absorption tower 3-2 tower reactor and the second sulfide absorption tower 3-1 bottom, treat that through the first sulfide absorption tower absorbent regeneration outlet pipe 8 and the second sulfide absorption tower treat that absorbent regeneration outlet pipe 12 enters absorbent regeneration tower 13, regenerator column 13, the tower reactor temperature is 230～240 ℃, tower top temperature is 120～150 ℃, and pressure is normal pressure; The sulfide of removed overhead is delivered to sulfur recovery system through condenser 14 by sulfide outlet pipe 15; The rear absorption agent of regeneration enters absorption agent pipeline 1 and recycles behind condenser 17 at the bottom of the tower.
The absorption agent sulphur content is 5000 μ g/g after the regeneration; MTBE sulphur content after the desulfurization reaches 7 μ g/g, and mass yield is 99.93%.
The method of the contained MTBE sulfide of a kind of deep removal, overall flow is identical with embodiment 1, but difference is: 1. add 100ml θ ring filler in the first and second sulfide absorption tower tower reactors, 2. the MTBE sulphur content is 850 μ g/g, 3. MTEB volume pump flow is 200ml/h, and 4. reflux ratio is 0.2.
The absorption agent sulphur content is 5000 μ g/g after the present embodiment regeneration; MTBE sulphur content after the desulfurization reaches 6 μ g/g, and mass yield is 99.91%.
The method of the contained MTBE sulfide of a kind of deep removal, overall flow is identical with embodiment 1, but difference is: the absorption agent that 1. uses is that the mixture of morpholine, methane amide is total to 300ml, and 2. the MTBE sulphur content is 750 μ g/g, 3. MTEB volume pump flow is 200ml/h, and 4. reflux ratio is 10.
The absorption agent sulphur content is 5000 μ g/g after the present embodiment regeneration; MTBE sulphur content after the desulfurization reaches 5 μ g/g, and mass yield is 99.92%.
Embodiment 4
The method of the contained MTBE sulfide of a kind of deep removal, overall flow is identical with embodiment 3, but difference is: 1. regenerator column tower reactor temperature is 60～90 ℃, and tower top temperature is 50～60 ℃, and pressure is 25KPa (absolute pressure), and 2. reflux ratio is 0.2.
The absorption agent sulphur content is 4800 μ g/g after the present embodiment regeneration; MTBE sulphur content after the desulfurization reaches 5 μ g/g, and mass yield is 99.90%.
Claims (9)
1. the method for a deep removal MTBE medium sulphide content, may further comprise the steps: sulfur-bearing MTBE enters tower reactor from bottom, the first sulfide absorption tower, the first sulfide absorption tower is rectifying tower, the absorption that the MTBE mixture of gasification and liquid phase sulfide absorption agent counter current contact are finished most of sulfide, then the gas phase MTBE mixture that contains a small amount of sulfide enters the second sulfide absorption tower, and be dispersed to liquid absorbent inside, the degree of depth of finishing sulfide by gas-liquid two-phase contact absorbs, the absorption agent of the sulfide that finally has been absorbed and through the MTBE of deep desulfuration product.
2. method claimed in claim 1, it is characterized in that: further comprise the absorption that will obtain in described the first sulfide absorption tower and the second sulfide absorption tower absorption agent of sulfide discharge from described the first sulfide absorption tower and bottom, the second sulfide absorption tower respectively, enter the absorbent regeneration tower, after regenerator column is processed, the sulfide that the reclaiming cat head obtains returns the absorbent regeneration that obtains at the bottom of the recovery tower simultaneously the first and second sulfide absorption towers and recycles.
3. claim 1 or 2 described any one methods, it is characterized in that: further comprise with obtain in described the second sulfide absorption tower through the MTBE of deep desulfuration product through the cooling after, part MTBE refluxes and enters described the first sulfide absorption tower, another part MTBE is through MTBE product introduction products pot, and reflux ratio is: 0.2～10.
4. method claimed in claim 1 is characterized in that: described the first sulfide absorption tower tower reactor and bottom, the second sulfide absorption tower, also further filling dumped packing.
5. method claimed in claim 4 is characterized in that: described dumped packing comprises one or more the mixture in rectangular saddle ring, cascade ring, Pall ring, Raschig ring, conjugate ring, Taylor's garland, hollow many-sided ball, ball float or the θ type filler.
6. method claimed in claim 1, it is characterized in that: described absorption agent is selected from one or more the mixture in acetonitrile, propionitrile, vinylformic acid, Monomethylamine solution, dimethylamine solution, trimethylamine solution, N,N-dimethylacetamide, N-Methyl pyrrolidone, morpholine, N-methylmorpholine, methane amide, ethanamide, dimethyl formamide, N-formyl morpholine N-or the acetyl morphine.
7. method claimed in claim 1 is characterized in that: described absorption agent is selected from methane amide, ethanamide, dimethyl formamide, N-formyl morpholine N-, acetyl morphine or two or more mixture wherein.
8. method claimed in claim 1, it is characterized in that: absorption agent add-on and MTBE inlet amount mass ratio are 0.5～3:1 in described the first sulfide absorption tower.
9. the method shown in the claim 1, it is characterized in that: sulfur-bearing MTBE enters the first sulfide absorption tower (3-2) tower reactor from sulfur-bearing MTBE opening for feed (2), feed pressure is 0.1～1.5MPa, feeding temperature is 40～150 ℃, 65～90 ℃ of tower reactor control temperature, with the absorption agent counter current contact of middle part, the first sulfide absorption tower (3-2) by absorption agent opening for feed (1) adding, in the first sulfide absorption tower (3-2), finish removing of most of sulfide, the MTBE that removes most of sulfide enters the second sulfide absorption tower (3-1) by the gaseous phase outlet pipe (3-3) of the first sulfide absorption tower (3-2) cat head again, in the second sulfide absorption tower, MTBE is dispersed to liquid absorbent inside, finish degree of depth Absorption Desulfurization by the gas-liquid two-phase contact, the qualified MTBE that obtains enters overhead condenser (4), cat head control temperature is 50～60 ℃, pressure is normal pressure, after overhead condenser (4) cooling, temperature is that 40～50 ℃ MTBE enters return tank (5), enter reflux pump (7) through return tank outlet pipe (6), MTBE enters the first sulfide absorption tower (3-2) through return line (10) in reflux pump (7) effect next section, another part MTBE enters products pot through MTBE products export pipe (11), and reflux ratio is: 0.2～10; Contain sulfur absorbing agent from the first sulfide absorption tower (3-2) tower reactor and bottom, the second sulfide absorption tower (3-1), enter absorbent regeneration tower (13) through pipeline (8) and (12), during regenerator column (13) normal pressure: the tower reactor temperature is 200～250 ℃, and tower top temperature is 90～160 ℃; During decompression: the tower reactor temperature is 60～90 ℃, and tower top temperature is 50～60 ℃, and the sulfide of removed overhead is delivered to sulfur recovery system through condenser (14) by pipeline (15); The rear absorption agent of regeneration enters absorption agent pipeline (1) and recycles behind condenser (17) at the bottom of the tower.
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| CN2013103001406A CN103360221A (en) | 2013-07-17 | 2013-07-17 | Method for deeply removing sulfides in MTBE |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103721544A (en) * | 2013-12-14 | 2014-04-16 | 蚌埠玻璃工业设计研究院 | Washing tower used for treating low-radiation coating exhaust |
| CN104262116A (en) * | 2014-06-23 | 2015-01-07 | 贺立明 | MTBE deep desulfurization device and method thereof |
| CN106748675A (en) * | 2016-11-16 | 2017-05-31 | 凯瑞环保科技股份有限公司 | A kind of method of sulfide in deep removal MTBE |
| CN108440255A (en) * | 2018-04-25 | 2018-08-24 | 陈久仓 | A kind of synthetic method of high-purity methyl tertbutyl ether |
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| CN103145534A (en) * | 2013-03-26 | 2013-06-12 | 南开大学 | Method for deeply removing sulfides in gasoline additive, namely methyl tert-butyl ether |
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| US4144138A (en) * | 1978-01-18 | 1979-03-13 | Texaco Inc. | Recovery of ethers |
| US4404409A (en) * | 1979-03-05 | 1983-09-13 | Nippon Oil Co., Ltd. | Process for preparing methyl tertiary-butyl ether |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103721544A (en) * | 2013-12-14 | 2014-04-16 | 蚌埠玻璃工业设计研究院 | Washing tower used for treating low-radiation coating exhaust |
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| CN108440255A (en) * | 2018-04-25 | 2018-08-24 | 陈久仓 | A kind of synthetic method of high-purity methyl tertbutyl ether |
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Application publication date: 20131023 |